Aplicaciones industriales de la biocatálisis Por Anna Surribas, Elena Genescà, Aleix Conesa, Roshan Paul, Marolda Brouta-Agnésa i Meritxell de la Varga.

1. Nombre conferencia
Aplicaciones industriales de la biocatálisis
Aplicaciones industriales de la biocatálisis
Anna Surribas
Elena Genescà, Aleix Conesa, Roshan Paul, Marolda Brouta-Agnésa i Meritxell de la Varga.
Barcelona, 16th November 2011
EL PARTNER TECNOLÓGICO

2. Aplicaciones industriales de la biocatálisis
INDEX
1. LEITAT presentation
2. Enzymatic fibre recovery and valorization (Textile sector)
3. Industrial cotton processing (Textile sector)
4. Fats and oils modification (Food sector)
5. Concluding remarks

3. Aplicaciones industriales de la biocatálisis
LEITAT’s Corporate presentation
OBJECTIVE
R+D+2I collaboration, adding technological value and a clear adaptation
and evolution to the constant market changes.
1 2 3 4
(*) Images: applications of Leitat Technological Center to the FotCiencia’06, FotCiencia’07, FotCiencia’08 contests:
1.- Tineoella bisselliella larva adhered to a wool fiber
2.- Surface tension modified by plasma treatment in a textile surface
3- Poliamides (transversal section)
4- Scratch test of ABS (Acrilonitrilo, Butadieno, Estireno)
3

4. Aplicaciones industriales de la biocatálisis
R+D+i market oriented services
1 2 3 4
4

5. Aplicaciones industriales de la biocatálisis
Industrial Biotech:
Biocatalysis
R & D in biotechnological solutions with
application in industrial processes; applied Industrial Bioprocesses
microbiology and microencapsulation. Bioproduct production
Environmental Biotechnology
Applied microbiology (process validation,
biofilm models, strain isolation and
characterization…)
Microbiology testing
Microencapsulation of antimicrobial
products
5

6. Aplicaciones industriales de la biocatálisis
INDEX
1. LEITAT presentation
2. Enzymatic fibre recovery and valorization
3. Industrial cotton processing
4. Fats and oils modification
5. Concluding remarks

7. PROCESS 1: Enzymatic fibre recovery and
Aplicaciones industriales de la biocatálisis
valorization from hemp
FIBNATEX is a SUDOE (Sudoeste Europeo) project
whose partners are: CITEVE (PT), IPN (PT), LEITAT
(ES), ASINTEC (ES), ICAM (FR), GIH (FR)
OBJECTIVES:
– To create innovative textiles based on hemp
natural fibers.
– To develop a future market of hemp fibers.
– Cover the whole process: from plant to
product
7

8. Aplicaciones industriales de la biocatálisis
Fibres separation process
Traditional separation process:
1. Cultivation
2. Retting Cultivation
3. Drying
4. Separation and carding
Water retting
Conventional separation process:
Chemical and mechanical process: Air drying
1. Breaking links between pectin/fibers
and fibers/wood.
2. Use of chemicals (sodium Oven drying
hydroxide).
3. High temperature process. Grinding (siglo XVIII)
8

9. Aplicaciones industriales de la biocatálisis
Project substrates
Mechanically separated Mechanically separated and
fibers. chemically treated fibers.
Skin separated from the 9
wood.

10. Aplicaciones industriales de la biocatálisis
Enzymatic retting set up
1. Enzymes: 3. Equipment:
Commercial enzymes Proveedor
Texazym BFE (pectinase) Inotex
Polygalacturonase Biocon
Xylanase Biocon
Scourzyme (pectinase) Color Center
2. Process variables:
Process variables LU1 Ugolini equipment
Enzyme cocktail
Process time
Temperature
pH
Buffer / Chelant agent
Agitation type
Fiber polishing
Agitated Incubator
Bath/Fiber ratio
10

11. Diapositiva 10
LU1 es una pectinase? o cel·lulasa???
Lenovo User; 11/09/2011

12. Aplicaciones industriales de la biocatálisis
Results of the project
Fibers separation with enzymes (P6):
– Ecological separation process.
– Low temperature process.
– Short time process (catalyzing action of the enzyme).
Fibers obtained with the enzymatic process (P6).
11

13. Aplicaciones industriales de la biocatálisis
Results of the project
Fibers characterization:
• Fibers fineness and yarn count (microscope ZEISS Axioplan and the program Delta Pix
300).
• Length of the fibers, individual measurements (UNE 40152).
• Microscopic inspection (microscope ZEISS Axioplan and program Delta Pix 300).
• Tensile strength (UNE EN ISO 5079).
• SEM (Scanning Electron Microscope).
Mechanically Mechanically Hemp skin fibers polished with
treated fibers. treated and enzymes.
enzymatic
polishing of fibers.
12

14. Aplicaciones industriales de la biocatálisis
INDEX
1. LEITAT presentation
2. Enzymatic fibre recovery and valorization
3. Industrial cotton processing
4. Fats and oils modification
5. Concluding remarks

15. PROCESS 2: Enzymatic cotton processing
Aplicaciones industriales de la biocatálisis
OBJETIVES:
Substitution of conventional cotton wet processing :
(1) less harmful
(2) less aggressive towards the environment and fibre
(3) applied at mild conditions
(4) cost-effective
14

16. Aplicaciones industriales de la biocatálisis
Process 2: chemical processing
STARTING FABRICS
The fabric used was a plain weave 100% cotton raw fabric.
CONVENTIONAL CHEMICAL PROCESS
Chemical desizing, scouring and bleaching was carried out in a single bath with a final fabric rinsing.
Cotton was thereafter dried and tested to assess the final quality.
15

17. Aplicaciones industriales de la biocatálisis
Process 2: Two step enzymatic process
- Enzymatic desizing and scouring in shorter
time.
- An alternative amylase and pululanase
(Dextrozyme) for the desizing/scouring. A
pectinase, humectant, chelating agent and buffer
KH2PO4 are used.
- Process conditions : 62ºC and 60 min at pH 4.1
- Transfer to a second bath for chemical
bleaching.
16

18. Aplicaciones industriales de la biocatálisis
Process 2: One step preindustrial process
Single step continuous enzymatic process using thermoresistent enzymes
One step continuous process
- Enzymatic desizing /scouring with a
commercial thermostable amylase (Texazyme
TA10)
- Simultaneous chemical bleaching with H2O2
- Process conditions : 105ºC during 60 min.
17

19. Aplicaciones industriales de la biocatálisis
SEM Images
A B C
Scanning Electron Microscopy pictures of treated cotton fibres.
(A)Chemical desizing, scouring and bleaching
(B)Two step enzymatic process
(C) One step continuous enzymatic processing
18

20. Aplicaciones industriales de la biocatálisis
Textile Quality
QUALITY ASSESSMENT:
- Desizing and scouring : iodine test and the water penetration test (UNE EN 20811).
- Bleaching: CIE whiteness using DATACOLOR spectrophotometer.
- Weight loss and tensile properties of the fabrics (EN ISO 13934/1:1999)
Whiteness
Weight loss (CIE) Iodine test Drop test
15% 63,1 OK OK
Conventional Treatment
Enzymatic
semicontinuous 11,75% 65 OK OK
treatment
Alternative enzymatic
semicontinuous 13,37% 61 OK OK
treatment
Single step enzymatic 12,57% 71 OK OK
process
19

21. Aplicaciones industriales de la biocatálisis
Reutilizations and Savings
ALTERNATIVE SEMI-CONTINUOUS ENZYMATIC PROCESS
Bath relation1:20.
10% amylase loss and 50% pectinase loss
Bath loss around 20%.
3 bath reutilizations are possible due glucose formation causing textile yellowing.
SINGLE STEP ENZYMATIC PROCESS
Bath relation1:10.
90% amylase loss. Pectinase use is optional
Bath loss around 20%.
4 bath reutilizations are possible.
20

22. Aplicaciones industriales de la biocatálisis
Industrialization and Tech Transfer
SATI, S.A. is devoted to:
Design, weaving, dyeing, printing and finishing of
home textiles, technical textiles for filtration and
medical textiles.
SATI, S.A. has :
1. Scaled up the one step proces to a pilot plant autoclave level
2. Adjusted process parameters and compared other commercial enzymes
Product Laboratory trials (CIE whiteness) Autoclave (CIE whiteness)
Texazyme TA10L 72,9 58,2
Bialfa T 72,8 61,4
Aquazym SDL 69,3 57,1
SATI, S.A. will ( 2011) :
1. Transfer the process to the continuous cotton processing industrial line.
21

23. Aplicaciones industriales de la biocatálisis
INDEX
1. LEITAT presentation
2. Enzymatic fibre recovery and valorization
3. Industrial cotton processing
4. Fats and oils modification
5. Concluding remarks

24. Aplicaciones industriales de la biocatálisis
Investigation in healthy ingredients and
food products
23

25. Aplicaciones industriales de la biocatálisis
Specific objective
A fat product with this solid fat content (SFC) profile and better nutritional properties using
enzymatic interesterification.
Processing temperature (20ºC)
Mouth temperature (37ºC)
24

26. PROCESS 3: Fats biocatálisis modification
Aplicaciones industriales de la and oils
ENZYMATIC
INTERESTERIFICATION
2. FAT AND OIL SELECTION based on:
1. Composition (% of MUFA and PUFA)
2. Origin
3. Commercial availability
4. SFC
5. Economical aspects.
Selected products:
Vegetal fat with high melting temperature and good structural properties.
Vegetal oil with a high percentage of PUFA and good SFC profiles in EIE reactions.
25

27. PROCESS 3: Fatslaand oils modification
Aplicaciones industriales de biocatálisis
3. Process optimization: Variables
Enzyme type and quantity
Enzyme Characteristics Process time
E1 Commercial Immobilized non-specific enzyme Temperature
E2 Commercial immobilized specific enzyme Fat /oil ratio
Agitation
4. Process conditions :
Commercial immobilized lipase (E1,E2)
Fat:oil ratio from 80:20 to 20:80
Initial N2 blanketing to avoid product oxidation.
Process time 24h
Temperature around 60ºC
Agitation around 200rpm
26

28. PROCESS 3: Fatslaand oils modification
Aplicaciones industriales de biocatálisis
5. RESULTS:
70:30 Fat:Oil E1 gives promising SFC results + good fatty acid composition
27

29. PROCESS 3: Fatslaand oils modification
Aplicaciones industriales de biocatálisis
5. Characterization: Sample 70:30 Fat:Oil E1
Differential scanning Calorimetry (DSC):
- Crystallization starts around 22ºC
- Two fusion ranges: higher and lower melting
triglycerides.
Slip melting point:
SMP (ºC)
30,7
28

30. Aplicaciones industriales de la biocatálisis
INDEX
1. LEITAT presentation
2. Enzymatic fibre recovery and valorization
3. Industrial cotton processing
4. Fats and oils modification
5. Concluding remarks

31. Aplicaciones industriales de la biocatálisis
Conclusions
1. Bioprocess industrialization in different sectors is a reality although not common in Spain
2. After basic research, process optimization for industrialization must consider certain aspects:
a. Costs
b. Existing or required equipment
c. Savings (energy, chemicals, water)
3. Raw materials, and specially enzyme sources, must be stable and reliable.
30

32. Aplicaciones industriales de la biocatálisis
Acknowledgments
31

33. Aplicaciones industriales de la biocatálisis
Thank you for your attention
asurribas@leitat.org
CENTRO TECNOLÓGICO DE LAS TECNOLOGÍAS DE LA PRODUCCIÓN