4576 4580.output

* GB784983 (A)
Description: GB784983 (A) ? 1957-10-23
Improvements in or relating to pumps, more particularly for lubrication
systems
Description of GB784983 (A)
PATENT SPECIFICATION
784983 & @ Date of Application and filing Complete Specification: July
4, 1956.
No 20745/56.
Complete Specification Published: Oct 23, 1957.
Index at acceptance:-Class 102 ( 1), Al(A 1 B: A 2: B 7: B 8 A:Cl: C
3), A 2 A 2 A, A 3 A( 1 A: 3 B), A 4 (E 1: J: P: Q: Y).
International Classification:-F 06 b.
COMPLETE SPECIFICATION
Improvements in or relating to Pumps, more particularly for
Lubrication Systems We, TECALEMIT LIMITED, a British Company, of Great
West Road, Brentford, 'Middlesex, do hereby declare the invention,
(Communicated by Deutsche Tecalemnit G m b EI, a German Body Corporate
of WindelsbleicheBielefeld, Germany), for which we pray that a patent
may be granted to us, and the method by which it is to be performed,
to be particularly described in and by the following statement:This
invention relates to pumps and has amongst its objects tile provision
of an improved pump for delivering a liquid, and more particularly a
lubricant, from a reservoir or container to a place or places of use
The invention is more especially applicable to pumps for delivering
oil under pressure into a central lubrication system in which the oil
is conveyed to a number of bearings or other places of use The
invention is, however, applicable to pumps for other purposes.
With the usual types of pumps which draw liquid from a reservoir and
deliver it to a place or places of use there is a risk that, if the
pump is operated after the reservoir has been emptied, air will be
drawn in, by the pump and delivered to the place of use This is often
undesirable, particularly in the case of lubricant pumps which are
used to supply oil to bearings or other points which have to be kept

lubricated It is, accordingly, one of the objects of this invention to
provide a pump which includes means which will prevent it from being
operated when there is an insufficient supply of the liquid in the
reservoir.
A further object of the invention is the provision of such a pump
which is of compact and reliable construction.
According to the invention a pump is provided for delivering a
lubricant or other liquid to a place of use comprising a pump cylinder
having a piston operating therein, means including an operating member
for operating the piston and a reservoir supplylPoice 3 s 6 d l ing
the liquid to the cylinder wherein locking means are provided
responsive to the quantity of liquid in the reservoir for preventing
operation of the pump when this quantity is less than a minimum value
50 Preferably the pump cylinder is arranged within the lower part lof
the casing forming the reservoir and according to a preferred form of
construction the pump cylinder and the body of the casing are cast
integrally with 55 each other.
In a preferred arrangement the locking means comprises a float which
is movably mounted in the reservoir and a locking element which, when
the float descends below 6) a predetermined level moves into a
position in which it engages the piston to arrest the movement of the
latter.
For the better understanding of the invention, the same will now be
more fully de 65 scribed, by way of example, with reference to the
accompanying drawings.
In the drawing: Figure 1 is an elevational view, partly broken-away
and in section, showing a single 70 piston lubricating pump
exemplifying the invention; Figure 2 is a vertical sectional view, to
a larger scale, showing the lower part of the pump of Figure 1; 75
Figure 3 is a detail view in the form of a horizontal section showing
a small part of the pump of Figures 1 and 2.
Referring to the drawing, the pump comprises a casing 1 which is
preferably formed 80 of cast iron and which includes a pair of lugs 2
by means of which the pump may be bolted or otherwise secured to a
wall, bulkhead or other support.
The casing 1 provides a reservoir chamber 85 3 for the oil and a
cylinder 4 for the delivery pump The bottom of the reservoir 3 is
arranged to slope downwardly towards a port (Figure 2) which opens
into the cylinder 4 towards one end of the latter Below the 90 port 5
the cylinder 4 is formed with a drainage port 6 which is closed by
means of a plug 7.
Slidably mounted in the cylinder 4 is a piston 8 which is formed with
an axial bore 9 At its inner end the bore 9 is formed with a shoulder
10 to provide an inner bore 11 of reduced diameter This bore 11 is

connected by means of an axial passage 12 with a vertical passage 13
drilled in the piston, which provides a fluid connection between the
port 5 and the bore 11, as well as between the port and the drainage
port 6.
The end of the piston 8, which is cut away on each side as shown in
Figure 3, forms a head 14 by which the piston is operated Arcuate
grooves 15 of saw-tooth section are formed in the outer surface of the
head 14 for a purpose to, be described.
A packing ring 16 is fitted in a groove in the piston 8, within the
cylinder 4, to prevent escape of oil between the piston and cylinder.
Fitted in the bore 9 of the piston 8 is a guide member 17 having a
bore 18 in which a valve element 19 is slidably mounted This element
19 is formed near its inner end with a groove 20 in which is fitted a
washer 21 made of synthetic rubber or other suitable resilient
material The edge of this washer 21 normally projects at an angle to
the axis of the piston beyond the end of the valve element 19 so as to
bear, by virtue of its natural resiliency, against the inner end of
the bore 11 which forms a seat for the valve.
The guide 17 is of square section having a diagonal corresponding to
the diameter of the bore 9 It thus provides edge passages through
which oil passing the valve element 19 can enter the cylinder The
piston 8 is biassed to the left by means of a return spring 22 which
is under compression between the guide member 17 and the body 23 of a
non-return delivery valve, which is indicated generally by the
reference 24 This body 23 is screwed into the end of the cylinder 4
and is provided with a sealing ring 25 to prevent the escape of oil.
The body 23 is formed internally with a bore 26 the outer end portion
27 of which is of increased diameter and is screw-threaded to receiver
a union, 28 This union serves for the attachment of a delivery pipe
(not shown).
A valve element 29 is slidably mounted in the bore 26 and is pressed
by means of a spring 30 against a valve seat provided by a shoulder 31
formed in the body 23 near the inner end of the bore 26 The outer end
of the spring 30 extends into a bore 32 in the union 28 and abuts
against a shoulder at the end of this bore, The cylinder 4 is formed
in its upper portion with a socket 35 the lower end of which opens by
means of a port 36 into the end, of the cylinder 4 A spring
controlled' pressure relief valve 37 is screwed into the socket 35,
this valve being arranged to open when the delivery pressure exceeds a
predetermined value.
Oil escaping through the valve 37 is returned to the reservoir 3
through a pipe 38 the upper 70 open end of which is located beneath a
transparent inspection dome or window 39 The sight of oil discharged
from the pipe 38 shows that the pump is working.

The pump is operated by means of an oper 75 ating shaft 40 which is
rotatably mounted in the end of the cylinder 4 and which carries a
pump handle 41 The lower end of this handle is screwed and pinned into
a split boss 42 which is clamped to the projecting end of the 80 shaft
40.
The shaft 40 is formed with an eccentric cut-away groove 43 (Figure 3)
leaving a reduced neck 44 of circular section which forms an operating
cam or eccentric for the 85 piston 8, the head 14 of which piston
engages in the groove 43 and' is pressed against the cam neck 44 by
the spring 22 The engagement of the piston head 14 in the groove 43
between the main part of the shaft 40 and the 90 end part 45 thereof
prevents turning of the piston in the cylinder.
The reservoir 3 is closed by means of a cover 46 which is screwed or
otherwise secured to the upper end of the casing 1, with the 95
interposition of a packing ring if necessary.
The cover 46 is provided with a removable filler cap 47.
Secured to the under side of the cover 46 by screws or other means, if
desired with the 100 interposition of a suitable packing, is a filter
48, which may be of a wire mesh or other suitable type All oil
introduced into the reservoir 3 must pass through this filter before
it enters the port 5 of the pump 105 A transparent window 49 is
provided in the side of the casing 1 to enable the level of the oil in
the reservoir 3 to be seen when this level falls to a low value.
The pump is provided with locking means 110 which are arranged to
prevent the pump piston from being operated when the oil level falls
below a minimum value This locking means comprises anil arm 51 which
is pivotally mounted in the lower part of the reservoir 115 3 In the
construction shown the arm 51 includes a pair of side flanges 52
'which extend on opposite sides of the upper part of the cylinder 4,
to which they are pivoted at 53 The arm 51 carries a ball float 54
which is 120 secured in a recess 55 in the arm 51 by means of a
resilient strip 56.
The arm 51 also carries a downwardly-projecting locking tooth 57 the
pointed end of which is adapted to engage in the groove 15 125 in the
piston head 14 in order to lock the piston 8 in its right-hand
position.
The operation of the pump is as follows:
Before use the reservoir 3 is filled with oil by removing the filler
cap 47, which cap is 130 784,983 ders and pistons which could be
arranged parallel to each other below the reservoir, from which they
would deliver oil separately to individual bearings or other places of
use.
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* GB784984 (A)
Description: GB784984 (A) ? 1957-10-23
Improvements relating to testing of compressors
Date of Application and filing Complete Specification: July 13, 1956.
784,984 No 21751/56.
71 t 1 ka 4} | Application made in United States of America on July
13, 1955.
Index at acceptance:-Class 8 ( 1), CX.
International Classification:-G 011 COMPLETE SPECIFICATION
Improvements relating to Testing of Compressors We, GENERAL ELECTRIC
COMPANY, a Corporation of the State of New York, United States of
America, having its office at Schenectady 5, State of New York, United
States of America, do hereby declare the invention, for which we pray
that a patent may be granted to us, and the method by which it is to
be performed, to be particularly described in and by the following
statement:-
This invention relates to the testing of compressors, particularly
refrigerant compressors such as those which are employed in the
refrigeration system for household refrigerators.
Heretofore the factory testing in the final stages of the manufacture
of household refrigerator compressors consisted in reading on a
pressure gauge the maximum pressure developed by the compressor
against a fixed restrictor The pressure reading was ordinarily taken
when the pressure had become stabilized and as a net result the test
for each compressor usually required from two to three minutes of

running time for each compressor This test was not only time consuming
but also involved an accuracy problem in separating the acceptable
compressors from the unacceptable since the usual pressure gauge
capable of reading pressures from zero to 120 or more psi are normally
calibrated in one pound increments and the spread of compressors in
this range is normally small As a difference of as little as one psi
in the maximum pressure developed by a given compressor may represent
the difference between an acceptable compressor and one which is not
acceptable, it is obvious that such test procedures and apparatus are
not completely satisfactory.
It is an object of the present invention to provide a method and
apparatus for quickly and accurately testing a compressor The present
invention is based in part on the discovery that the time required for
a cornlPrice 3/6 l pressor to build up a given or predetermined
discharge pressure against a fixed restrictor, which pressure is less
than the maximum pressure developed by the compressor, is both a
faster and more accurate measure 50 ment of the quality of the
compressor than is the measure -of maximum pressure developed by the
compressor.
According to the invention there is provided compressor testing
apparatus compris 55 ing means for initiating operation of a
compressor with unrestricted flow of discharge gas, means for
restricting discharge flow, timing means and means for starting the
timing means concurrently with the opera 60 tion of the flow
restricting means and for stopping the timing means when the
compressor discharge pressure increases to a predetermined value.
In a particular embodiment of the inven 65 tion, there is provided
test equipment or apparatus comprising a fixed restrictor such as a
capillary and means for connecting the restrictor to the compressor
discharge conduit The connecting means or line has 70 ' connected
thereto a normally closed pressure switch and a normally open solenoid
operated relief valve which normally permits the compressor to operate
against zero or a relatively low discharge back pressure When 75 the
relief valve is closed, the compressor operates against the fixed
restrictor or capillary and to provide means for measuring the time
required for the compressor to build up a discharge pressure of a
predeter 80 ( mined value after the valve is closed there is provided
electrically-operated timing means, such as an electric clock, and an
electric circuit for controlling the operation of the valve and for
connecting the pressure 85 switch in series with the clock The closing
of the switch in the electric circuit when the compressor is running
serves to close the valve and start the clock Opening of the pressure
switch when the compressure dis 90 784,984 charge increases toi a
predetermined value deenergizes the timing means The running time of

the clock is a measure of the performance of the compressor.
For a better understanding of the invention, reference may be had to
the accompanying drawings in which Fig 1 is a somewhat schematic
illustration of the apparatus employed in carrying out the present
invention; and Fig 2 is a plot of representative pressure-time curves
of different compressors operated on the test system of the present
invention.
The drawing shows a fixed restrictor or capillary 1 connected by a
line 2 to the discharge conduit 3 of a hermetic compressor 4.
During test of the compressor 4 the suction conduit 5 thereof is
opened to the atmosphere Also connected to the line 2 between the
connection thereof to the compressor 4 and the capillary 1, is a side
line including a solenoid operated valve 6 which also opens to the
atmosphere A pressure switch 7 is connected by a conduit 8 to the line
2 so that the operation of this switch is responsive to the pressures
within the line 2.
The pressure switch 7 is electrically connected in series with an
electric timer or clock 9 and this circuit includes a manually
operated switch 10 which also controls the circuit energizing the coil
11 effecting operation of the valve 6.
In the use of this test apparatus, a compressor 4 is first connected
to the line 2 and to a power source 12 by the closing of a switch 13
During this initial operation of the compressor the switch 10 is open
so that the circuits including the solenoid 11 and the clock 9 are
de-energized The air compressed by the compressor 4 and discharged
through the discharge conduit 3 into the line 2 passes through the
normally open valve 6 and is again discharged to the atmosphere so
that the compressor is operating under a no-load condition, that is,
with no restriction in the discharge line The pressure gauge switch 7
is set at zero pressure and the electric timer 9 is similarly set at
zero The pressure gauge switch 7 includes electrical contacts (not
shown) which are normally closed and which are opened when the
pressure within the line 2 reaches a predetermined value.
With the compressor 4 operating against zero back pressure in the
discharge line 2, the switch 10 is closed thereby energizing the
solenoid 11 and the timer 9 Upon closing of the solenoid valve 6,
pressure is built up in the system against the flow restriction of the
capillary 1, the flow through the capillary 1 being, of course, a
function of the pressure within the line 2 When the pressure in the
system reaches a predetermined value at which the pressure gauge
switch 7 is set, this switch opens stopping the timer 9.
The measure of the capacity of the compressor 4 is the time required
for the compressor to build up the predetermined pressure against the
restriction of the capillary 1.

The starting time of the compressor is not 70 involved as the
compressor runs continuously Whenever it is found necessary, the test
may be repeated immediately merely by opening the switch 10 thereby
releasing the pressure within the line 2 and re-setting the 75
pressure gauge switch 7 and the timer 9 to zero settings.
As has been previously indicated, the tests are conducted with the
pressure gauge switch 7 set to de-energize the clock circuit 80 when
the pressure within the line 2 reaches a value which is somewhat below
the maximum pressure which can be developed by the compressor 4 For
maximum accuracy, all of the lines or conduits such a 2 and 8 85
should be as short as possible so that the entire test system will
have a relatively small volume as compared with the pumping rate of
the compressor 4.
For a further understanding of the advan 90 tages of the present
invention reference should be had to Fig 2 of the drawing in which are
plotted the pressuretime curves of three compressors A, B and C All
three of these compressors were of the same type 95 and tested on the
same test equipment and were designed to produce a maximum discharge
pressure somewhat in excess of 120 psi.
From a consideration of these curves it 100 will be noted that the
pressure build up for all three compressors during the initial few
seconds of the test was substantially constant or linear and at the
rate of approximately pounds per second However after the 105
pressures reached about 60 psi the rate of build up of pressure
against the fixed restrictor begins to decrease so that the slopes of
the curves gradually decrease Also at this point, the curves tend to
spread apart 110 and this spread is greater with regard to the time
axis than the pressure axis For this reason and for the additional
reason that a timer calibrated in seconds can be more easily and
accurately read than a pressure 115 gauge calibrated in five pounds
major increments and one pound minor increments, it will be seen that
time is not only a more accurate but also a more significant factor
than pressure in sorting compressor samples 120 In setting up the
test, correlation tests are required to establish the reject level on
a given test set up for a specific type of compressor, that is, the
engineering specifications for capacity of a given type compressor 125
are established as a part of the machine design and compressors with
these known values are used in determining the comparative time-cycle
values as attained on a given test set up and arn used to establish
the 130 754,984 proper reject levels.
Preferably, the pressure gauge switch 7 is set to open the clock
circuit at a pressure of from about 70 % to 90 % of the maximum
pressure which can be developed in the test system by an average
acceptable compressor.

For example in the diagram shown in Fig.
1, if the curve for compressor B be taken as the reject level curve
for a type of compressor engineered to develop a maximum of about 125
psi against a given restrictor, the pressure gauge switch 7 may be set
to open within a range of pressure of from about 85 to 112 psi For
example if the switch is set to.
open at 110 psi it will be noted that the reject level is
approximately 15 seconds.
Therefore any compressor which does not raise the pressure within the
line 2 to this valve within 15 seconds is properly rejected.
For example compressor A reaches pressure of 110 pounds within 12
seconds while compressor C which required 20 seconds does not meet the
standard and is therefore rejected.
These time differences of approximately three seconds between
compressors Aand B and five seconds between B and C can be accurately
read from the usual electric timer However, it will be noted from Fig.
2 that the pressure differences between the three compressors at the
15 second mark, are relatively small particularly for the usual
pressure gauge which measures pressure anywhere from zero to for
example 150 psi.
The present test method employing time as the significant test factor
is particularly useful in testing and sorting compressors of the type
mass produced for household refrigerators wherein economic
considerations dictate the design of the refrigerating machine to
closer specifications as affect the cost thereof One of the principal
advantages of the present test method is in the separation of
borderline compressors, that is compressors very close to the reject
level and on either side thereof all of which will have approximately
the same total pull down or maximum pull down if allowed to run long
enough but which nevertheless would not give a satisfactory
performance in a refrigerating system for a household refrigerator In
many household refrigerators now on the market a compressor which
requires too much time for proper pull down is not acceptable even
though its maximum pull down is high For example in those systems.
where defrosting of the evaporator is accomplished between each
operating cycle of the refrigerating system, it is more desirable to
employ a compressor which cycles frequently for short periods of time
and which quickly establishes the desired pressure differentials
within the system rather than one which requires a relatively long
running time to 66 establish such pressures.
While the test procedure has been described as including initial
operation of the compressor against a zero or atmospheric back
discharge pressure, significant and useable results can also be
obtained in a 70 shorter time by initially connecting line 2 to a

pressure tank as a source of a constant pressure within the range of
pressure where the time-pressure curves are substantially linear,
closing the connection when the clock 75 is started and noting the
time required for the compressor to build up the pressure in line 2
from the starting pressure to the predetermined test pressure.
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* GB784985 (A)
Description: GB784985 (A) ? 1957-10-23
Manufacture of organic phosphorus compounds
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The EPO does not accept any responsibility for the accuracy of data
and information originating from other authorities than the EPO; in
particular, the EPO does not guarantee that they are complete,
up-to-date or fit for specific purposes.
Date of Application and filing Complete Specification: Oct 28, 1953.
No 6973/57.
Application made in United States of America on Oct 29, 1952.
Application made in United States of America on April 15, 1953.
(Divided out of No 783,697) ' /T Complete Specification Published: Oct
23, 1957.
Index at acceptance:-Class 2 ( 3), C( 1 B 7: 3 B).

International Classification:-CO 7 f.
Manufacture of Organic Phosphorus Compounds We, FOOD MACHINERY AND
CHEMICAL CORPORATION, a Corporation organised according to the laws of
the State of New York, of 161, East 42nd Street, New York 17, State of
New York, United States of America, do hereby declare the invention,
for which we pray that a patent may be granted to us, and the method
by which it is to be performed, to be particularly described in and by
the following statement: -
This invention provides a process for the manufacture of monovinyl or
E-substituted monovinyl esters of phosphoric acid or of a phosphonic
acid, which esters correspond to the general formula:
P-o-C C-R in which R 1 is a substituted or unsubstituted alkyl, aryl,
alkoxy or aryloxy group, R 2 is a substituted or unsubstituted alloxy
or aryloxy group, R, and R 4 are hydrogen or a substituted or
unsubstituted alkyl, aryl, alkoxy or aryloxy group, wherein a tertiary
phosphite or secondary phosphonite of the general formula:
R,x /p-o-R R 2 in which R 1 and R 2 have the meanings given above, and
R is a substituted or unsubstituted alkyl group, is reacted with an
appropriate a monohalogenated aldehyde In this manner, for example,
diethyl vinyl phosphate can be obtained by reacting triethyl phosphite
with monochloracetaldehyde.
Prior art attempts to prepare such compounds have involved reactions
which are lPr/ce 3 s 6 d l relatively more complicated or more
difficult to carry out than the process of the present invention For
example, Schrader has described (PB 87,923 R, p 33, 1947) a process
for the preparation of substituted vinyl phosphates involving the
reaction of a chlorophosphate with a sodium enolate Such a process is
handicapped by the fact that relatively few sodium enolates can be
readily prepared.
In United States Specification No.
2,557; 805, is described the preparation of diethyl vinyl phosphate by
the dehydrohalogenation of a 2-halogen-ethyl phosphate.
This reaction also presents certain difficulties.
In the first place, the dehydrohalogenation cannot be carried out in
alcohols, or even in inert solvents, with ordinary bases such as
metallic hydroxides and alkoxides, due to solvolysis of the
halogen-ethyl phosphate In the second place, attempts to carry out the
dehydrohalogenation in inert solvents, such as ether, by special
agents such as sodium hydride, give a very low yield of vinyl
phosphate.
The process of the present invention overcomes the foregoing and other
disadvantages of the prior processes, involves the use of readily
obtainable reactants, does not necessitate the use of a solvent

medium, and gives very satisfactory yields The products are useful and
of interest as monomers and as chemical intermediates.
-The tertiary phosphite or secondary phosphonite must contain at least
one alkyl group which may be unsubstituted or substituted Alklyl
groups of low molecular weight are preferred, such as ethyl or
chlorethyl.
The o -halogen atom of the aldehyde is removed during the reaction and
the resulting vinyl ester does not contain halogen attached directly
to the vinyl group Halogen may be present elsewhere in the molecule.
Although the reaction is not understood with certainty, the probable
reaction is as follows; 784,985 ' t, 11 _ 7 A, I I I #; P-O + o=c-C-R
-o 4 + A ha I A'2 HI R 2 Sal A'2 The reaction may be carried out by
the gradual addition of one of the reactants to the other at any
suitable temperature, but the preferred range is approximately 25 C to
C The temperature selected depends in part upon the activity of the
halogen atom involved, and also to a lesser extent upon the activity
of the phosphite or phosphonite used.
In general, bromine compounds may be reacted at lower temperatures
than in the case of chlorine compounds.
Any suitable proportions of the two reactants may be used, but it is
preferred to use equimolar proportions Although a solvent medium may
be used, it is usually unnecessary and undesirable, and it is
preferable to avoid the additional time and effort which is involved
in removing a solvent medium from the product Either the monomeric or
polymeric form of the carbonyl compound may be used.
The following Examples and the Table illustrate the invention:
EXAMPLE 1.
Four moles ( 665 grams) of commercial triethyl phosphite were
gradually added, while stirring, to 4 moles ( 314 grams) of
monochloracetaldehyde over a period of 40 minutes with sufficient
cooling to keep the temperature of the reaction mixture at 50-60 C The
reactor was vented through a trap cooled by dry ice and
trichlorethylene, in order to condense the by-product ethyl chloride
When all the phosphite had been added the temperature of the reaction
mixture was gradually raised to 110 C to expel the ethyl chloride, the
yield of the latter (boiling at 130 C) being % of theory Fractionation
of the main product by means of a 2-foot column packed with glass
helices gave a yield of 67 %' of diethyl vinyl phosphate boiling at
790 C.
( 5-7 mm) and having n DD= 1 4100 and sp.gr 35/4 = 1 0724 The compound
reacted vigorously with bromine and had an intense infra-red
absorption band at 6 1 microns (absorption characteristic of the vinyl
group).
EXAMPLE 2 -

Under conditions similar to those of Example 1 trischlorethyl
phosphite was reacted in equimolar proportions with
monochloracetaldehyde, yielding the product bis-chlorethyl vinyl
phosphate, boiling at 133-148 C.
under 1 mm pressure EXAMPLE 3.
To 35 4 grams ( 0 45 mole) of chloracetaldehyde were added 156 7 grams
( 0 45 mole) of bis-2-( 21 methoxyethoxy)-ethyl benzene-phosphonire at
55-75 C The reaction was only mildly exothermic and it was necessary
to apply heat in order to maintain the desired temperature When the
mixing operation was complete the temperature was raised to 125 C, to
complete the reaction, and the pressure was then reduced to 1 mm.
while still heating at 125 C to remove the byproduct 2-(
21-methoxyethoxy)-ethyl chloride.
The yield of by-product was 80 % of theory, and the yield of crude 2-(
21-methoxyethoxy)ethyl vinyl benzene-phosphonate was 107 % of theory
Calculated for CQH,,0 P: P= 10 8 %.
Found: P= 10 9 %.
Further examples of products of the general formula:
piO Ii C / P -C = C A ' I?, which can be made by the process of this
invention are those having the substituents given in the following
Table.
R 2 Et O Et O CHI -CCH 3 Et O Et O H -CH 2 C 1 Et O Et O H -CHCICHII,
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* GB784986 (A)
Description: GB784986 (A) ? 1957-10-23
Manufacture of organic phosphorus compounds

784,986 Date of Application and filing Complete Specification: Oct 28,
1953.
No 6974/57.
Application made in United States of America on Oct 29, 1952.
(Divided out of No 783,697).
Index at acceptance:-Classes 2 ( 3), C 1 A( 12: 19: 22), C 1 B( 7:
13); and 81 ( 1), E 1 A 4 A( 2: 3: 4), E 1 C 4 A( 2: 3: 4).
International Classification:-A 611 C 07 f.
Manufacture of Organic Phosphorus Compounds We, FOOD MACHINERY AND
CHEMICAL CORPORATION, a Corporation organised according to the laws of
the State of New York, of 161, East 42nd Street, New York 17, State of
New York, United States of America, do hereby declare the invention,
for which we pray that a paternt may be granted to us, and the method
by which it is to be performed, to be particularly described in and by
the following statement: -
This invention provides esters of acids of pentavalent phosphorus,
which esters have the general formula /_P O-c C -II in which X 1 and X
2 are halogen atoms, R, and R, are substituted or unsubstituted alkyl,
aryl, alkoxy, aryloxy or alkylamido or arylamido groups or R, and R 2
together form an unsubstituted or substituted divalent alkylenedioxy
or arylenedioxy group, R 3 is hydrogen or an unsubstituted or
substituted alkyl or aryl group, R 4 and R, are hydrogen or halogen
atoms or unsubstituted or substituted alkyl or aryl groups, or R, and
R 4 together or R, and R, together form an unsubstituted or
substituted divalent alkylene or cycloalkylene group.
The invention also provides a process for the manufacture of the
esters of the above general formula, wherein an alkenyl ester of an
acid of pentavalent phosphorus of the general formula p O-C=C -R 5 R 2
in which R 1, R 2, R 3, R 4 and R, have the meanings given above, is
reacted with an appropriate elemental halogen, halogen-halide or other
halogenating agent.

The halogen may be introduced by carrying out the reaction in the
presence or absence of a suitable inert solvent, such as chlorinated
solvent, for example, carbon tetrachloride, in the presence or absence
of actinic radiation, and at temperatures ranging from O C or lower,
up to about 100 C or even as high as the boiling point of the alkenyl
ester used as starting material The halogenation temperature used,
either in the liquid or gas phase, is a function at least in part of
the thermal stability of the reactants and products The halogen may be
used in the elemental state, which may be solid, liquid or gaseous
Mixed halogens may also be used, for example, a mixture of chlorine
and bromine, which yields a compound containing both chlorine and
bromine Also, halogen may be introduced by means of an interhalogen
compound (halogen-halide) or halogenating agent or carrier, such as
iodine chloride, antimony pentachloride or dioxane bromine addition
product.
The preferred method for introduction of a halogen is to add elemental
halogen to a solution of the vinyl compound in a chlorinated solvent,
such as carbon tetrachloride, at a temperature of about 40-60 C
Actinic light may be advantageously used to accelerate the reaction
when the vinyl radical carries electronegative atoms or groups, such
as halogen atoms, but in their absence such activation is unnecessary
The halogen and the vinyl compound are preferably reacted in equimolar
proportions, but other proportions may be effectively used.
The following Examples and Table 1 illustrate this form of the
invention:
EXAMPLE 1.
In a 250 minl capacity 3-neck flask equipped with a stirrer, graduated
dropping funnel, and an adaptor bearing a Dry Ice condenser and
thermometer dipping into the contents of the flask, were placed 10 ml
of carbon tetrachloride and 50 5 grams ( 0 28 mole) of diethyl vinyl
phosphate A Dry Ice condenser was then connected to the top of the
dropping funnel, and gaseous chlorine was introduced into the
condenser until 13 ml.
( 0.28 mole) of liquid chlorine had collected in the dropping funnel
The liquid chlorine was introduced dropwise into the stirred solution
of diethyl vinyl phosphate, which was cooled to maintain it at a
temperature of 0-10 C The reaction was instantaneous and much heat was
evolved When addition of the chlorine was complete stirring was
continued until the reaction mixture had warmed to room temperature
The solvent was removed by heating at C under a pressure of 15 mm of
mercury, leaving a crude product weighing 67 6 grams, which is 96 % of
theory Distillation of the crude product under 1 mm pressure gave 56 6
grams of diethyl 1: 2-dichlorethyl phosphate distilling at 75-92 C and
having sp gr.

35/4 1 2549 and N 3 "D = 1 4346 The weight of distilled product
represents an 81 %' yield.
Calcd for CAH 13 Cl OP: Cl, 28 3 %'; P, 12.4 % Found: C 1, 26 O %; P
12 1,.
EXAMPLE 2.
In the apparatus described in Example 1, except that the Dry Ice
condensers were eliminated, 20 grams ( 0 125 mole) of bromine were
added dropwise to 31 grams ( 0 15 mole) of diethyl 2:2-dimethylvinyl
phosphate dissolved in 52 ml of carbon tetrachloride, the solution
being cooled to maintain a temperature of approximately O C Removal of
the solvent in vacua left a 99 6 % yield of diethyl
1:2dibromo-2-methylpropyl phosphate Calculated for CH,7 Br 2 OP: Br=
434 %; P= 8 4 %.
Found: Br= 43 5 %; P= 8 6 %.
EXAMPLE 3.
Using the apparatus and method of Example 2, 4 1 grams ( 0 026 mole)
of bromine were reacted with 6 grams ( 0 026 mole) of diethyl
1cyclohexenyl phosphate dissolved in 25 ml of carbon tetrachloride The
resulting diethyl 1: 2dibromocyclohexyl phosphate was not distilled.
Calculated for CQH 1,Br 2 Oz P: Br= 40 6 %; P= 7 9 %; Found: Br = 40 9
%'; P = 7 9 o EXAMPLE 4.
In apparatus similar to that described in Example 1, 8 6 ml ( O 19
mole) of liquid chlorine were added gradually to 63 6 grams ( 0.2
mole) of bis-2-chloroethyl 2:2-dichlorovinyl phosphate dissolved in 59
ml of carbon tetrachloride Since the latter compound does not react
readily with chlorine in the dark, the reaction mixture was
illuminated with a mercury vapour lamp placed about 2 inches from the
reactor The reaction mixture was not cooled and the temperature
eventually rose to 74 C, when mild refluxing took place.
The reaction was essentially complete as soon as all the chlorine had
been added, as shown by the absence of colour in the reaction mixture
65 The solvent was removed in vacua, and the crude product,
bis-2-chlorethyl 1: 2: 2: 2-tetrachlorethyl phosphate, obtained in 100
% yield, was analyzed Calculated for C 6 HC 10 O P:
C 1 = 54 7 %i; P= 8 0 % Found: Cl= 53 1 %; 70 P= 8 3 %.
EXAMPLE 5.
Using the apparatus of Example 2 and the light from a mercury vapour
lamp, 3 6 ml.
( 0.07 mole) of bromine were gradually added 75 to 30 3 grams ( 0 1
mole) of 2:2-dichlorovinyl bis-diethylamido-phosphate (Et 2 N)2 P(O)
OCH=C C 12, dissolved in 55 ml of carbon tetrachloride, the mixture
being cooled to maintain a temperature 80 of 57-58 C When the addition
of bromine was complete, the solvent was removed in vacua, leaving a
100 % yield of crude, 1:2dibromo-2: 2-dichlorethyl

bis-diethylamidophcsphate Calculatedfor C 1 II,2 Br 2 C 12 NO P: 85
halogen= 8 6 milli-equivalents per gram; P = 6.7 % Found: halogen= 8 0
milli-equivalents per gram; P = 7 79 %.
EXAMPLE 6.
Using the apparatus of Example 2 and the 90 light from a mercury
vapour lamp, 3 6 ml.
( 0.07 mole) of bromine were added gradually to 23 3 grams ( 0 1 mole)
of 2:2-dichlorovinyl trimethylene phosphate, (CH 2),02 P(O)OCH= CC
12, dissolved in 57 ml of carbon tetra 95 chloride, the temperature
rising from about C to 65 C When the colour due to bromine had
disappeared, the solvent was removed in vacuo, leaving a 100 % yield
of crude 1: 2-dibromo-2: 2-dichlorethyl tri 100 methylene phosphate
Calculated for C 1 H 7 Br 2 C 120 P: halogen = 10 2 milliequivalents
per gram; P = 7 9 %o Found:
halogen= 10 1 milli-equivalents per gram; P= 8 60/o 105 EXAMPLE 7.
Equimolar quantities of bromine and chlorine were reacted with diethyl
vinyl phosphate to form 2-bromo-1-chlorethyl diethyl phosphate.
The reaction was carried out in the apparatus 110 of Example 1 by
dissolving 0 1 mole each of bromine and chlorine in 75 ml of carbon
tetrachloride and gradually adding 0 2 mole ( 36 grams) of diethyl
vinyl phosphate at 10-25 C No activation by light was required but 115
considerable cooling was necessary to maintain the said temperature
range Removal of the carbon tetrachloride in vacua left 53 5 grams (a
91 % yield) of crude product Distillation of the product under 1 mm
pressure gave 28 2 120 grams (a 48 % yield) of the product distilling
at 106-112 C The distilled product had a specific gravity 35/4 = 1
4579 and n'D = 1.4518 Calculated for CGH 1,Br Cl O,P:
halogen= 6 8 milli-equivalents per gram; P= 125 10.4 % Found: halogen=
6 7 miilli-equivalents per gram; P= 10 0 %.
784,986 784,986 3 Ex AMPLE 8.
Using the apparatus of Example 1, 7 1 mal.
( 0.15 mole) of liquid chlorine were added gradually to 42 9 grams ( 0
15 mole) of mnethioxycthioxyethyl vinyl b;nzene phosphonale Ph P(O) (
O OH CH,)OCIH 2-C Hd OCH2 CH,,OCH,, dissolved in 62 ml of carbon
tetrachioride.
Activation of the chlorine by light was not necessary, but cooling of
the reaction mixture was necessary to maintain the desired temperature
range of 40- 45 O C Removal of the solvent in vacuo left a 100 % yield
of 1: 2dichlorethyl methoxyethoxyethyl benzenephosphonate ( 54 grams)
Calculated for C 1 H,1 C,02 P:cl=-198 %; P = 8 7 %.
Found: Cl= 21 1 %; P= 18 8 %.
Ri R Et OEt OAdditional examples of the new compounds of this
invention are given in Table 1, in which the compounds are identified
by reference to, the groups 'R 1, R, R,, R,, R, and the 20 halogens X,

and X 2, in the general formula:
,0 34 1,' j R, R, R,, X 2 H cl cl Br Br Et OEt On-Pr OEt OEt OMce OC 2
H 4 11 00 z 4 Et OEt OEt On-Pr O Et OEt OMe OCJ 4,O 1 z II 40Et Oi-Bu
OH H Me H HI Br Br H Br Br H cl cl Br Br H H cl Br Br Me H H 01 cl HI
cl cl Br Br C 1 CH 2 H H cl H cl Br Er Br Br 1 > 5 C Ha CH(CO 2 Eff)O
n-Bu OC 2,H 4 OCCI3 CH 2 OBu CH Et CH 20Et OCe Vi C# CM, 0 O CW,-ei
CH,1 CH(C 02 Et)On-Bu OCJ,H 01 CGC 11 C 2 OBu CH Et CH 20Et OH cl cl
Br Br H cl cl Br Br H cl cl Br Br H cl cl Br Br H cl cl Br Br HI H cl
cl cl Me CO 2 Et Cl Br Br H 'Cl cl Br Br Cli 0 CICH 2 CH 2 OCICH 2 CH
20C 1 C H 2 C H 2 O C l C HI C I H 20 H cl cl Br Br H cl Cl cl cl Et
OEt O784,986 CIGHCH,0784,986 TABLE 1-continued.
R 2 H Cl C 1 Br Br Et OEt OCl CH, CH 20Cl CH 2 CH 20CICH 2 CH 20Me OCH
10 C 2 H t OCl CH 2 CH 20CICCHC 20CICH 2 CH 20H Br Br Br Br H H H Br
Br H H H Br Br H H Cl Br Br H H Cl Cl Cl The compounds of this
invention are useful in a wide range of valuable and interesting
applications, for example, as biocides and medicaments Some of the
compounds exhibit extremely interesting properties as rodenticides
Others are potent contact insecticides and acaricides Still others are
particularly effective as systemic insecticides or acar-icids.
Some of the compounds show promise as powerful cholinesterase
inhibitors Examples of these biocidal properties are set forth in
Tables 2 and 3.
Conc 2-Spotted Pea Compound ppm Mite Aphid A B 150 TABLE 2
Contact Insecticidal and Acaricidal Activity The contact insecticidal
and acaricidal activity of these products is illustrated in the
following table The materials were formulated as 15 % wettable
powders, diluted with water to the desired concentration, and sprayed
on suitable plant foliage The treated plants were then infested with
the desired insect, and mortality counts, shown as percentages, were
taken 72 hours later.
German Milkwood Mex Bean Roach Bug Beetle C 156 7 30 6 ' + e =
necab/,; t/ 784,986 Compound C Conc.
ppm D 150 TABLE-continued 2-Spotted Pea Mite Aphid German Millwood Mex
Bean Roach Bug Beetle E 156 F 156 2.5 G 1250 156 A = (Et O)2 P(O)OCH
Br-CH 2 Br B = (Et O)2 P(O)OCHBr CH Br Cl C = (Et O)2 P(O)OCHC 1 HC
12 D = (Et O)2 P(O)OCHCICC 13 TABLE 3
Systemic Insecticidal and Acaricidal Activities.
The systemic insecticidal and acaricidal activities of these products
are illustrated in E = (Et O)2 P(O)OCHBr C Br 3 F = (Et O)2 P(O)OCHC
1 CH 2 Br G = (CICH 2 CH 2 O)2 P(O)OCHCl CHCI 2 the following table
Stems of excised bean plants were placed in test tubes containing 25
ml of a solution or emulsion of the active material in water, and the
plants were held in 10 place by non-absorbent cotton plugs which also
prevented evaporation The plants were days later Data obtained with

Systox (the then infested with two-spotted mites or pea word "Systox"
being a registered Trade Mark) aphids, and mortality counts were taken
4 are shown for comparison.
Mites Aphids Compound Conc ppm % Kill Conc ppm % Kill A 78 100 20 100
100 10 100 100 5 85 95 2.5 45 B 156 100 156 100 78 100 39 100 100 10
100 100 5 100 96 2 5 80 1.25 63 1 25 70 0.625 26 0 625 15 C 78 100 20
100 100 10 100 98 5 100 84 2 5 50 2.5 50 1.25 25 D 10 100 10 100 100 5
100 2.5 27 2 5 100 1.25 23 1 25 85 0.625 20 0 625 80 A -= (Et O)2
P(O)OC(CH3)CI-CH 2 Cl B= (Et O)2 P(O)OCHCICH C 12 C = (Et O)2 P(O)OCH
Br CH Br CI D Systox (Et O)2 P(S)OCH2 CH 25 C 2 H 5 784,986 valent
phosphorus given in Table 1 herein, with the exception of the
compounds claimed in claims 10 to 15.
17 A process for the manufacture of an 45 ester claimed in any one of
claims 1 to 16, wherein an alkenyl ester of an acid of pentavalent
phosphorus of the general formula R/.P o-e=e-, 5 R 2 R
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* GB784987 (A)
Description: GB784987 (A) ? 1957-10-23
Improvements in or relating to the bonding of metal to moulded compositions

e ri A f C 7 RI
Inventors: GORDON ARTHUR CAPEWELL and GEORGE WILLIAM RIPPINGTON Date
of filing Complete Specification Feb 25, 1954.
Application Date May 7, 1953.
784987 No 12806/53.
I/ r 'Complete Specification Published Oct 23, 1957.
Index at Acceptance:-Classes 87 ( 2), Al R 14 (A: C 2: D), A 1 R 39 X;
and 140, A 2 (F: A: H: M 5); A 5 G( 1 A: 1 B: 4: 8: 9), A 16 A.
International Classification: -B 29 d, g.
Improvements in or relating to the Bonding of Metal to Moulded
Compositions ERRATA SPECIFICATION No 784,987
Page 1, line 53, for "polyivnyl-butyral" read "polyvinyl-butyrai" Page
5, line 23, for " 1,700 lbs -sq in " read " 1,700 lbs /sq in " THE
PATENT OFFICE, 13th Yanuary, 1958.
O i 5 organic or inorganic and natural or synthetic and may be in any
state of sub-division, and bonding agents comprising thermosetting or
thermoplastic resins The fillers may be fibrous or non-fibrous and in
the former case may take the form of filaments or yarns which may be
woven or felted Examples of fibrous fillers in their various forms are
glass filaments randomly disposed in the form of a mat or web, nylon
yarns woven into a fabric, cotton yarns in the form of a woven fabric
and cut into pieces, treated wood fibres in the form of paper sheets,
wood fibres in the form of a flour and asbestos fibres in the form of
a flock.
The process of bonding a metal component to the surface of a moulded
composition may be carried out either by bonding the component, e g,
with adhesive, to a premoulded composition or by bonding the component
to the moulded composition during the process of lP) carrying out the
processes of bonding and moulding simultaneously.
Where the moulded composition and the metal component are bonded
together during the moulding process it is possible to establish a
bond between the two without the use of a special adhesive, but it has
been found that an improved bond is obtained in many cases by
interposing an adhesive, such as a
phenol-formaldehyde/polyvinyl-butyral resin mixture, between the metal
component and the moulded composition.
According to the present invention there is provided a method for
forming a moulded product embodying as a surface layer a metal
component which method comprises the provision of a layer comprising
an amino-formaldehyde resin between the said surface metal component

and a mouldable composition comprising a filler and a bonding agent,
the provision of a layer of adhesive between the layer tt,' PY X
Inventors: GORDON ARTHUR CAPEWELL and GEORGE WILLIAM RIPPINGTON Date
of filing Complete Specification Feb 25, 1954.
Application Date May 7, 1953.
784987 No 12806/53.
> Complete Specification Published Oct23, 1957.
Index at Acceptance:-Classes 87 ( 2), AIR 14 (A: C 2: D), A 1 R 39 X;
and 140, A 2 (F: 'G: H: M 5); A 5 G( 1 A: 1 B: 4: 8: 9), A 16 A.
International Classification: -B 29 d, g.
Improvements in or relating to the Bonding of Metal to Moulded
Compositions We, BAKELITE LIMITED, a British Company, of 12, Hobart
Place, London, S W 1, do hereby declare the invention, for which we
pray that a patent may be granted to us, and the method by which it is
to be performed, to be particularly described in and by the following
statement:-
This invention is for improvements in the bonding of metal components
to moulded compositions comprising a filler and a bonding agent.
The combination of metals and moulded compositions comprising a filler
and a bonding agent is widely practised Typical examples of metal
surfaced products are mouldings produced from moulding powders bearing
a decorative metal foil and laminated materials bearing e g a copper
foil, which are used for the production of printed electrical
circuits.
The invention may be applied to the union of metals of all kldnds with
moulded compositions comprising fillers, which may be organic or
inorganic and natural or synthetic and may be in any state of
sub-division, and bonding agents comprising thermosetting or
thermoplastic resins The fillers may be fibrous or non-fibrous and in
the former case may take the form of filaments or yarns which may be
woven or felted Examples of fibrous fillers in their various forms are
glass filaments randomly disposed in the form of a mat or web, nylon
yarns woven into a fabric, cotton yarns in the form of a woven fabric
and cut into pieces, treated wood fibres in the form of paper sheets,
wood fibres in the form of a flour and asbestos fibres in the form of
a flock.
The process of bonding a metal component to the surface of a moulded
composition may be carried out either by bonding the component, e g,
with adhesive, to a premoulded composition or by bonding the component
to the moulded composition during the process of lPl _ moulding the
latter It has hitherto been 45 found that the former (two-stage)
method has given a bond superior to that produced by the latter

(one-stage) method.
Although the two-stage process in which the metal component is bonded
to the surface 50 of the premoulded composition by means of an
adhesive, consisting e g of a phenol-formaldehyde/polyivnyl-butyral
resin mixture, gives a superior bond, the process suffers from two
main defects, viz ( 1) it is longer and 55 is, therefore, more
expensive than the onestage process, and ( 2) where a metal component,
particularly in the form of a foil, is applied to a premoulded
composition it is difficult to ensure complete elimination of the air
trapped 60 between the component and the composition and the bond is
thus weakened at those points where this occurs.
It is an aim of the present invention try obtain an improved bond
between a surface 65 metal component and a moulded composition
comprising a filler and a bonding agent while carrying out the
processes of bonding and moulding simultaneously.
Where the moulded composition and the 70 metal component are bonded
together during the moulding process it is possible to establish a
bond between the two without the use of a special adhesive, but it has
been found that an improved bond is obtained in many 75 cases by
interposing an adhesive, such as a
phenol-formaldehyde/polyvinyl-butyral resin mixture, between the metal
component and the moulded composition.
According to the present invention there is 80 provided a method for
forming a moulded product embodying as a surface layer a metal
component which method comprises the provision of a layer comprising
an amino-formaldehyde resin between the said surface metal 85
component and a mouldable composition comprising a filler and a
bonding agent, the provision of a layer of adhesive between the layer
b 2 784,9 7 comprising the amino-formaldehyde resin and the metal
component and subjecting the assembly to moulding conditions.
The term "metal component" includes metal sheets foils and blocks.
In the one-step process of bonding, e g.
copper foil to the surface of a laminated product based on paper
impregnated with a phenol-formaldehyde thermosetting resin, hitherto
it has been found that the best bond has been obtained by applying a
suitable adhesive, e g a mixture comprising phenol-formaldehyde resin
and polyivnyl-butyral resin, to the surfaces of the copper foil and/or
the resin impregnated sheets of paper where they are in contact and
then subjecting the stacked assembly to heat and pressure The bond,
however, has not been entirely satisfactory, particularly where the
copper-faced laminated product has been used in the production of
printed circuits; thus where electrical components have been fixed
thereto there has been a tendency for the bond btween the copper foil
and the insulating base to be broken.

We have now found that it is possible to unite more effectively a
surface metal component and a moulded composition comprising a filler
and a bonding agent when using the onestep process of manufacture by
interposing a layer comprising an amino-formaldehyde resin between the
mouldable composition and the adhesive for the metal component The
amino-formaldehyde resin may be in the form of a supported or an
unsupported film Thus it may be applied to a sheet of fibrous material
e.g, a sheet of paper, before being interposed between the adhesive
layer and the mouldable composition or it may be applied as a solution
to, e g, the adhesive-treated metal component and allowed to dry
before the mould?ing operation takes place.
The amino-formaldehyde resin has further advantages when used in the
production of electrical products and particularly where the bonding
agent of the moulded composition is a relatively poor anti-tracking
material Thus, a melamine-formaldehyde resin is obviously advantageous
in the production of printed electrical circuits where the bonding
agent of the moulded composition is a relatively poor anti-tracking
material, e g a phenol-formaldehyde resin In a combination utilising a
layer comprising a melamine-formaldehyde resin, it has been observed
that the union between the metal component and the moulded composition
is stronger than in the case where a urea-formaldehyde layer is used.
The adhesive for the metal may be applied in a number of ways For
example, it may be applied to the metal component, or to the sheet of
paper treated with the amino-formaldehyde resin or to both, or it may
be inter, posed between the metal and the amino-formaldehyde layer as
a supported or unsupported film.
In some cases it is preferable to etch the metal component before
bonding it to the moulded composition and this may be done chemically
or mechanically In some instances, e.g in the case of
electro-deposited copper foil, a suitably etched surface is produced
during manufacture.
Following is a description by way of example of methods of carrying
the invention into effect.
EXAMPLE I
Electro-deposited copper foil O 002 " thick was coated on its etched
surface with a layer consisting of a blend in organic solvent of equal
proportions by weight of a heat-hardenable phenol-formaldehyde resin
and a polyvinyl butyral resin The coated metal was dried at 90 to 160
C for 20 to 230 minutes.
A stack was then built up as follows:1 sheet of copper foil treated as
described above (adhesive-treared surface uppermost).
A layer consisting of a sheet of x-cellulose paper (O j 015 " thick)
impregnated with melamine-formaldehyde resin to a resin content of 55
G'.

sheets of cotton based paper ( 0 005 ' thick) impregnated with
cresol-formaldehyde resin to give a final resin content of 55 %o.
A layer consisting of a sheet of >-cellulose paper impregnated with
melanmir ne-formaldehyde resin as above.
1 sheet of copper foil as abeve (adhesive treated surface downwards).
The stack was pressed between polished steel plates for 30 minutes at
170 C under a pressure of 1,700 lb /sq in The resulting sheet which
consisted of a paper filled laminated product faced on both sides with
copper foil was cooled under pressure before removing it from the
press.
EXAMPLE II
A stack was built up as follows:1 sheet of aluminium 7/,' thick etched
on 110 one surface only and with the etched surface uppermost.
A layer consisting of a sheet of 7 -cellulose paper ( O 0015 " thick)
treated with a melamine-formaldehyde resin to give a final 115 resin
content of 55 % and subsequently coated on the surface to contact the
metal sheet with a blend of equal proportions of heat-hardenable
phenol-forfmaldehlydj resin and polyvinyl butyral to give an 120
adhesive content of 5 %.
x '/,th" gaboon veneers with a liquid phenol-formaldehyde glue
interposed.
A melamine-formaldehyde layer consisting of a sheet as above, with the
adhesive 125 coated surface uppermost.
1 sheet of aluminium /5th" thick etched on one surface only and with
the etched surface facing downwards.
784,987
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