Anna Surribas - Aplicaciones industriales de la biocatálisis

Nombre conferencia
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


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


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


R+D+i market oriented services

1 2 3 4

4


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


INDEX

1. LEITAT presentation

2. Enzymatic fibre recovery and valorization
3. Industrial cotton processing
4. Fats and oils modification

5. Concluding remarks

PROCESS 1: Enzymatic fibre recovery and
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


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


Project substrates

Mechanically separated Mechanically separated and
fibers. chemically treated fibers.

Skin separated from the 9
wood.


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

Diapositiva 10

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


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


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

PROCESS 2: Enzymatic cotton processing

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


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


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


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


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


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


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


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


Investigation in healthy ingredients and
food products

23


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

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

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


5. RESULTS:

70:30 Fat:Oil E1 gives promising SFC results + good fatty acid composition

27


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

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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


Acknowledgments

31


Thank you for your attention

asurribas@leitat.org

CENTRO TECNOLÓGICO DE LAS TECNOLOGÍAS DE LA PRODUCCIÓN

Anna Surribas - Aplicaciones industriales de la biocatálisis

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