CN104404105A - Membrane condensation technology for preparing feed-grade xylo-oligosaccharide from viscose fiber squeezed liquid - Google Patents
Membrane condensation technology for preparing feed-grade xylo-oligosaccharide from viscose fiber squeezed liquid Download PDFInfo
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- CN104404105A CN104404105A CN201410622100.8A CN201410622100A CN104404105A CN 104404105 A CN104404105 A CN 104404105A CN 201410622100 A CN201410622100 A CN 201410622100A CN 104404105 A CN104404105 A CN 104404105A
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- 239000002994 raw material Substances 0.000 claims description 28
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- JCSJTDYCNQHPRJ-UHFFFAOYSA-N 20-hydroxyecdysone 2,3-acetonide Natural products OC1C(O)C(O)COC1OC1C(O)C(O)C(OC2C(C(O)C(O)OC2)O)OC1 JCSJTDYCNQHPRJ-UHFFFAOYSA-N 0.000 description 2
- 241000186000 Bifidobacterium Species 0.000 description 2
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- SRBFZHDQGSBBOR-LECHCGJUSA-N alpha-D-xylose Chemical compound O[C@@H]1CO[C@H](O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-LECHCGJUSA-N 0.000 description 2
- JCSJTDYCNQHPRJ-FDVJSPBESA-N beta-D-Xylp-(1->4)-beta-D-Xylp-(1->4)-D-Xylp Chemical compound O[C@@H]1[C@@H](O)[C@H](O)CO[C@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O)C(O)OC2)O)OC1 JCSJTDYCNQHPRJ-FDVJSPBESA-N 0.000 description 2
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Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention provides a membrane condensation technology for preparing feed-grade xylo-oligosaccharide from viscose fiber squeezed liquid. The technology comprises the following steps: step A, membrane condensation: pre-filtering the squeezed liquid, which is generated in the viscose fiber production process, to remove the large particle impurities, then processing the squeezed liquid by a micro-filter membrane, cyclically condensing the filtrate by a nano-filter membrane for 2 to 4 times, diluting the final condensate by water, then filtering with a ceramic membrane so as to obtain condensate of squeezed alkali solution, wherein in the cyclic condensation process through a nano-filter membrane, before filtration, the fluid should be diluted by water in advance; step B, semi-fiber extraction: adding acid into the obtained condensate of squeezed alkali solution to neutralize the condensate so as to obtain a semi-fiber solution; step C, enzymatic hydrolysis: adding composite enzymes into the obtained semi-fiber solution to carry out enzymatic hydrolysis reactions so as to obtain enzymatic hydrolysate; step D, purification: filtering the enzymatic hydrolysate by a ceramic membrane, filtering the filtrate by a nano-filter membrane to remove the salts so as to obtain the condensate namely the purified solution of xylo-oligosaccharide, and finally evaporating and drying the condensate so as to obtain the feed-grade xylo-oligosaccharide.
Description
Technical field
The present invention relates to xylo-oligosaccharide preparation field, be specifically related to the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide.
Background technology
Xylo-oligosaccharide, also known as wood oligose, is the general name of the IMO be combined into β-Isosorbide-5-Nitrae-glycosidic link by 2-7 wood sugar.Effective constituent is xylo-bioses, xylotriose, Xylotetrose, wooden pentasaccharides etc., wherein based on xylo-bioses and xylotriose.Have unique advantage compared with soybean oligosaccharide, oligofructose, oligomeric isomaltose etc. that xylo-oligosaccharide is used with usual people, it optionally can promote the proliferation activity of intestinal bifidobacteria, and its bifidobacterium factor functional is 10-20 times of other polymerization carbohydrate.Xylo-oligosaccharide is considered to desirable protective foods sweeting agent because of advantages such as its significant bifidus bacillus multiplication capacity, decomposition difficult to digest, low carious tooth, effectively intake are few, and its acidproof heat-proof also makes it be applied to the industries such as medicine, beverage, fodder additives simultaneously.
Xylo-oligosaccharide, to be rich in the plant of xylan for raw material, is produced by biochemical method.The production of current xylo-oligosaccharide is raw material mainly with corn cob, and complex manufacturing, cost is higher.And at chemical pulp plant celluloses such as () wood pulp, cotton pulp, straw pulp, reed pulps in the production process of viscose fiber of raw material, adopting alkali lye to process (dipping, squeezing) to Mierocrystalline cellulose is the first step manufacturing viscose fiber.Hemicellulose concentration is high, extremely adverse influence is produced to cellulose viscose manufacturing technique and final product quality, therefore must in impregnation technology with alkali lye by hemicellulose stripping, the Mierocrystalline cellulose of high strength could be obtained, so a large amount of high concentration alkali pressed liquors being rich in hemicellulose can be produced in above process.
Main component in alkali pressed liquor is sodium hydroxide and hemicellulose.Hemicellulose is therefrom separated by treatment process many employings nanofiltration of existing press lye, obtains comparatively pure alkali lye.Through purification alkali lye can direct reuse in technique, but part alkali only can be realized reuse by nanofiltration membrane, still containing a large amount of alkali in the concentrated solution that the hemicellulose in its trapped fluid obtains after concentrated.During at present this part feed liquid is used for as salkali waste and technique, hemicellulose enters wastewater treatment, or adopts calcination to reclaim sodium hydroxide, and hemicellulose is burned.From above existing technique, hemicellulose is not fully used.
Document " the membrane separation concentration technical study of xylo-oligosaccharide " (" foodstuffs industry ", 09 phase in 2012), pilot plant test device is adopted to carry out pilot plant test to the separation of lower concentration xylo-oligosaccharide solution is concentrated, the effect of the polyamide-based nanofiltration of comparative studies and reverse osmosis two kinds of membrane techniquies, determines the optimised process operational condition that nanofiltration membrane separation concentrates xylo-oligosaccharide solution.This technique nanofiltration membrane thickening temperature is low, and membrane filtration efficiency is lower, is unsuitable for industrialization scale operation.
Summary of the invention
For above-mentioned technical problem, the invention provides with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide.The xylo-oligosaccharide salinity obtained is low, and purity is high, and process operation efficiency is high, is adapted to scale operation.
For achieving the above object, the present invention adopts following technical scheme:
With the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, it is characterized in that: concrete technology step is as follows:
A, membrane concentration
The press lye produced by viscose fiber is first through pre-filtering removing large granular impurity, enter microfiltration membrane process, permeate is through concentrated 2-4 time of nanofiltration membrane circulation, and send after last concentrated solution thin up into ceramic membrane filter, gained concentrated solution is the concentrated solution of press lye; Concentrated 2-4 time of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up.
B, extraction half fibre
By the concentrated solution acid neutralization of press lye, obtain half fine liquid.
C, enzymolysis
In half fine liquid, add prozyme, enzyme digestion reaction occurs and obtains enzymolysis solution;
D, purification
Enzymolysis solution is through ceramic membrane filter, and permeate enters nanofiltration membrane desalination, and gained concentrated solution is the refined solution of xylo-oligosaccharide, then obtains feed grade xylo-oligosaccharide through evaporation, oven dry.
The xylo-oligosaccharide that preparation method of the present invention obtains meets the national standard GB/T 23747-2009 of feed grade xylo-oligosaccharide.
Step A of the present invention, described microfiltration membrane aperture is 5 microns, and the molecular weight cut-off of described nanofiltration membrane is 200-400, and the molecular weight cut-off of ceramic membrane is 800-1500.
Micro-filtrate membrane filtration amount is large, is conducive to improving filtration efficiency; The molecular weight cut-off of 200-400, makes alkali separate from permeate, progressively lowers alkali dense, promotes half fine concentration, retain a part of monose simultaneously; The molecular weight cut-off of ceramic membrane is 800-1500, can retain half fibre, improve the purity of product.
Step A of the present invention, before each nanofiltration membrane, the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume.While ensureing filtration efficiency, little to the damage of nanofiltration membrane.
Preferably, described permeate, containing alkali 200-300g/l, containing half fine 40-80 g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 12-75g/l, containing half fine 40-80g/l.Under lowering the dense prerequisite of alkali, ensure the filtration efficiency of film.
Step A of the present invention, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.While ensureing filtration efficiency, little to the damage of ceramic membrane.
Preferably, containing alkali 2-4g/l in the concentrated solution of described ceramic membrane filter, containing half fine 40-80 g/l.Be down to minimum by dense for alkali, ensure that the purity of half fibre.
Pre-filtering of the present invention refers to, press lye filters and Plate Filtration removing large granular impurity through rotary drum successively.Pre-filtering makes press lye not containing the solid impurity of more than 5 microns, and protection film is not below damaged by solid impurity.
Step A of the present invention, the temperature of micro-filtration is 40-50 DEG C, and the temperature of nanofiltration membrane is 40-60 DEG C, and the temperature of ceramic membrane filter is 60-80 DEG C, and filtration temperature is high, and liquid viscosity is lower, is conducive to filtration efficiency and improves.
Step A of the present invention, the mistake mould difference of micro-filtration is 1-2bar, and the mistake mould difference of nanofiltration membrane is 3-4bar, and the mistake mould difference of ceramic membrane is 5-6bar.For the feature that viscose glue press lye viscosity is higher, adopt higher pressure reduction to filter, can ensure that half fine concentration in alkali lye reaches processing requirement.
Step A of the present invention, feed liquid is 20-40 m at the flow of microfiltration membrane
3/ h, the flow in nanofiltration membrane is 25-40m
3/ h, the flow in ceramic membrane is 200-250m
3/ h.The surface velocity that bonding props up film is higher, film is not easy contaminated.
Step A of the present invention, it is 1m that the list of microfiltration membrane props up filtration area
2, it is 26.8m that the list of nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2, single film has larger filtration area under the prerequisite taking less space.
Step B of the present invention, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4-5.The advantage adding hydrochloric acid is that the molecules of salt amount formed is lower, and be conducive to the desalination in later stage, pH value is 4-5, adapts to the pH value requirement of enzymolysis.
Step C of the present invention, prozyme is zytase, cellulase and polygalacturonase, can improve sugared associative key susceptibility to enzymic hydrolysis after adding appropriate cellulase and pectin in zytase.
Preferably, the ratio of described zytase, cellulase and polygalacturonase is 3:2:1, and adopt the prozyme of this ratio to carry out degrading and can make the maximum production of xylo-oligosaccharide, the percent hydrolysis of hemicellulose is up to more than 95%.
Preferably, the enzymolysis time of described enzyme digestion reaction is 0.5-2h, and temperature is 50-60 DEG C, and the pH value of enzyme digestion reaction is 4-5, and under this condition, the activity of enzyme is the highest.
Preferably, the enzyme concentration of described enzyme digestion reaction is 0.5-1.5%, and now the catalytic effect of enzyme is best.
D step of the present invention, the molecular weight cut-off of ceramic membrane is 800-1500, and separating oligomeric wood sugar and undegradable half fibre, ensure product purity.
D step of the present invention, the molecular weight cut-off of described nanofiltration membrane is 100-200.Owing to adopting hydrochloric acid neutralization, the salt of generation is sodium-chlor, and the molecular weight of sodium-chlor is smaller, and far below 100, and xylo-oligosaccharide molecular weight is much larger than 100, effectively can realize being separated of salt and xylo-oligosaccharide.
Preferably, described nanofiltration membrane desalination, crossing mould difference is 3-4bar, and temperature is 30-40 DEG C, and single filtration area is 26.8 m
2, adapt to the change of low catching molecular, guarantee salt is separated with xylo-oligosaccharide.
Preferably, the material liquid volume before described nanofiltration membrane concentrates is 10-15 times of concentrated solution volume, is conducive to reducing the salt content in xylo-oligosaccharide.
Beneficial effect of the present invention is:
1, the present invention adopts microfiltration membrane, nanofiltration membrane and ceramic membrane to combine filtering and concentrating half fibre, because the filtration efficiency of micro-filtration and nanofiltration is higher than ceramic membrane, first with the macro-molecular protein in micro-filtrate membrane filtration removal alkali lye and bacterium, adopt repeatedly nanofiltration membrane that alkali concn is progressively dropped to certain degree again, concentrated half fibre simultaneously, reduce the damage to film, then adopt ceramic membrane filter; The feed liquid that ceramic membrane is applicable to filter the dense height of later stage low alkali half fine is run, and is the powerful guarantee that low alkali is dense.Nanofiltration membrane and ceramic membrane cooperatively interact, and have complementary advantages, and make containing alkali 2-4g/l in final concentrated solution, containing half fine 40-80 g/l, achieve low alkali dense, height half is fine; And process operation efficiency is high, little to the damage of film, cost is low.
2, the amount of nanofiltration membrane thin up of the present invention is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn; Ceramic membrane filter, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.This technique can realize nanofiltration membrane water 10m excessively per hour
3left and right, ceramic membrane is per hour crosses water 45m
3left and right, ensure that filtration efficiency; Meanwhile, little to the damage of film, the 2-3 that can reach its quality guarantee period work-ing life doubly, reduces cost to a great extent, is adapted to industrialization scale operation.
3, the present invention adds hydrochloric acid neutralization to the concentrated solution obtained, then adopts molecular weight cut-off to be the nanofiltration membrane desalination of 100-200.In hydrochloric acid and the salt generated be sodium-chlor, the molecular weight of sodium-chlor, far below 100, and xylo-oligosaccharide molecular weight is much larger than 100, effectively can realize being separated of salt and xylo-oligosaccharide.Be conducive to the desalination in later stage, further increase the purity of xylo-oligosaccharide.
4, enzymolysis solution is first used ceramic membrane separation xylo-oligosaccharide and undegradable half fibre by the present invention, ensure product purity, permeate enters nanofiltration membrane desalination again, thus have effectively achieved being separated of salt and xylo-oligosaccharide, the specific conductivity finally obtaining xylo-oligosaccharide is 8000-10000 μ s/cm, and ignition residue is 3-6%.Ignition residue is the direct indicator weighing inorganic salt, and the massfraction described in xylo-oligosaccharide shared by inorganic salt is only 3-6%; Specific conductivity is the electrolytical degree existed in reaction liquid, and the main electrolyte of xylo-oligosaccharide is exactly inorganic salts, so this index also can reflect the number of salinity in product.It is low that low conductivity and ignition residue describe the xylo-oligosaccharide salinity adopting the inventive method to obtain, high purity more than 80%.
Embodiment
Below in conjunction with embodiment, essentiality content of the present invention is described in further detail.
Embodiment 1
With the membrane concentration technique that viscose fiber pressed liquor is raw material production food-grade xylooligosaccharide, concrete technology step is as follows:
A, membrane concentration
The press lye produced by viscose fiber is first through pre-filtering removing large granular impurity, enter microfiltration membrane process, permeate is through concentrated 2 times of nanofiltration membrane circulation, and send after last concentrated solution thin up into ceramic membrane filter, gained concentrated solution is the concentrated solution of press lye; Concentrated 2 times of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up.
B, extraction half fibre
By the concentrated solution acid neutralization of press lye, obtain half fine liquid.
C, enzymolysis
In half fine liquid, add prozyme, enzyme digestion reaction occurs and obtains enzymolysis solution;
D, purification
Enzymolysis solution is through ceramic membrane filter, and permeate enters nanofiltration membrane desalination, and gained concentrated solution is the refined solution of xylo-oligosaccharide, then obtains feed grade xylo-oligosaccharide through evaporation, oven dry.
Embodiment 2
With the membrane concentration technique that viscose fiber pressed liquor is raw material production food-grade xylooligosaccharide, concrete technology step is as follows:
A, membrane concentration
The press lye produced by viscose fiber is first through pre-filtering removing large granular impurity, enter microfiltration membrane process, permeate is through concentrated 3 times of nanofiltration membrane circulation, and send after last concentrated solution thin up into ceramic membrane filter, gained concentrated solution is the concentrated solution of press lye; Concentrated 3 times of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up.
B, extraction half fibre
By the concentrated solution acid neutralization of press lye, obtain half fine liquid.
C, enzymolysis
In half fine liquid, add prozyme, enzyme digestion reaction occurs and obtains enzymolysis solution;
D, purification
Enzymolysis solution is through ceramic membrane filter, and permeate enters nanofiltration membrane desalination, and gained concentrated solution is the refined solution of xylo-oligosaccharide, then obtains feed grade xylo-oligosaccharide through evaporation, oven dry.
Embodiment 3
With the membrane concentration technique that viscose fiber pressed liquor is raw material production food-grade xylooligosaccharide, concrete technology step is as follows:
A, membrane concentration
The press lye produced by viscose fiber is first through pre-filtering removing large granular impurity, enter microfiltration membrane process, permeate is through concentrated 4 times of nanofiltration membrane circulation, and send after last concentrated solution thin up into ceramic membrane filter, gained concentrated solution is the concentrated solution of press lye; Concentrated 4 times of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up.
B, extraction half fibre
By the concentrated solution acid neutralization of press lye, obtain half fine liquid.
C, enzymolysis
In half fine liquid, add prozyme, enzyme digestion reaction occurs and obtains enzymolysis solution;
D, purification
Enzymolysis solution is through ceramic membrane filter, and permeate enters nanofiltration membrane desalination, and gained concentrated solution is the refined solution of xylo-oligosaccharide, then obtains feed grade xylo-oligosaccharide through evaporation, oven dry.
Embodiment 4
The present embodiment is substantially the same manner as Example 1, on this basis:
Described step A, microfiltration membrane aperture is 5 microns, and the molecular weight cut-off of nanofiltration membrane is 200, and the molecular weight cut-off of ceramic membrane is 800.
The nanofiltration membrane circulation of described step A is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
Embodiment 5
The present embodiment is substantially the same manner as Example 2, on this basis:
Described step A, microfiltration membrane aperture is 5 microns, and the molecular weight cut-off of nanofiltration membrane is 400, and the molecular weight cut-off of ceramic membrane is 1500.
The nanofiltration membrane circulation of described step A is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
Embodiment 6
The present embodiment is substantially the same manner as Example 3, on this basis:
Described step A, microfiltration membrane aperture is 5 microns, and the molecular weight cut-off of nanofiltration membrane is 300, and the molecular weight cut-off of ceramic membrane is 1000.
The nanofiltration membrane circulation of described step A is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
Embodiment 7
The present embodiment is substantially the same manner as Example 1, on this basis:
Described step A, microfiltration membrane aperture is 5 microns, and the molecular weight cut-off of nanofiltration membrane is 250, and the molecular weight cut-off of ceramic membrane is 900.
The nanofiltration membrane circulation of described step A is concentrated, and the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume at every turn.
Embodiment 8
The present embodiment is substantially the same manner as Example 4, on this basis:
Described step A, permeate, containing alkali 300g/l, containing half fine 80g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 75g/l, containing half fine 80g/l.
Embodiment 9
The present embodiment is substantially the same manner as Example 5, on this basis:
Described step A, permeate, containing alkali 260g/l, containing half fine 70g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 32.5g/l, containing half fine 80g/l.
Embodiment 10
The present embodiment is substantially the same manner as Example 6, on this basis:
Described step A, permeate, containing alkali 200g/l, containing half fine 40g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 12.5g/l, containing half fine 40g/l.
Embodiment 11
The present embodiment is substantially the same manner as Example 7, on this basis:
Described step A, permeate, containing alkali 220g/l, containing half fine 60g/l, after nanofiltration membrane circulation is concentrated, obtains concentrated solution containing alkali 55g/l, containing half fine 60g/l.
Embodiment 12
The present embodiment is substantially the same manner as Example 8, on this basis:
The ceramic membrane filter of described step A, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.
Described step A, containing alkali 2g/l in the concentrated solution of ceramic membrane filter, containing half fine 40g/l.
Embodiment 13
The present embodiment is substantially the same manner as Example 9, on this basis:
The ceramic membrane filter of described step A, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.
Described step A, containing alkali 4g/l in the concentrated solution of ceramic membrane filter, containing half fine 80 g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
Described step A, the temperature of micro-filtration is 40 DEG C, and the temperature of nanofiltration membrane is 40 DEG C, and the temperature of ceramic membrane filter is 60 DEG C.
Embodiment 14
The present embodiment is substantially the same manner as Example 10, on this basis:
The ceramic membrane filter of described step A, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.
Described step A, containing alkali 3g/l in the concentrated solution of ceramic membrane filter, containing half fine 50g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
Described step A, the temperature of micro-filtration is 50 DEG C, and the temperature of nanofiltration membrane is 60 DEG C, and the temperature of ceramic membrane filter is 80 DEG C.
Described step A, the mistake mould difference of micro-filtration is 1bar, and the mistake mould difference of nanofiltration membrane is 4bar, and the mistake mould difference of ceramic membrane is 6bar.
Embodiment 15
The present embodiment is substantially the same manner as Example 11, on this basis:
The ceramic membrane filter of described step A, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.
Described step A, containing alkali 2.5g/l in the concentrated solution of ceramic membrane filter, containing half fine 60g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
Described step A, the temperature of micro-filtration is 45 DEG C, and the temperature of nanofiltration membrane is 45 DEG C, and the temperature of ceramic membrane filter is 65 DEG C.
Described step A, the mistake mould difference of micro-filtration is 2bar, and the mistake mould difference of nanofiltration membrane is 3bar, and the mistake mould difference of ceramic membrane is 5bar.
Described step A, feed liquid is 20m at the flow of microfiltration membrane
3/ h, the flow in nanofiltration membrane is 25m
3/ h, the flow in ceramic membrane is 200m
3/ h.
Embodiment 16
The present embodiment is substantially the same manner as Example 11, on this basis:
The ceramic membrane filter of described step A, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.
Described step A, containing alkali 3.5g/l in the concentrated solution of ceramic membrane filter, containing half fine 70g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
Described step A, the temperature of micro-filtration is 46 DEG C, and the temperature of nanofiltration membrane is 55 DEG C, and the temperature of ceramic membrane filter is 75 DEG C.
The mistake mould difference of described micro-filtration is 1.5bar, and the mistake mould difference of nanofiltration membrane is 3.6bar, and the mistake mould difference of ceramic membrane is 5.6bar.
Described step A, feed liquid is 40m at the flow of microfiltration membrane
3/ h, the flow in nanofiltration membrane is 40m
3/ h, the flow in ceramic membrane is 250m
3/ h.
Described step A, it is 1m that the list of microfiltration membrane props up filtration area
2, it is 26.8m that the list of nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
Embodiment 17
The present embodiment is substantially the same manner as Example 11, on this basis:
The ceramic membrane filter of described step A, feed liquid first enters ceramic membrane device through thin up, and add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.
Described step A, containing alkali 3.8g/l in the concentrated solution of ceramic membrane filter, containing half fine 65g/l.
Described pre-filtering refers to, pressed liquor filters and Plate Filtration removing large granular impurity through rotary drum successively.
Described step A, the temperature of micro-filtration is 42 DEG C, and the temperature of nanofiltration membrane is 55 DEG C, and the temperature of ceramic membrane filter is 72 DEG C.
Described step A, the mistake mould difference of micro-filtration is 1.2bar, and the mistake mould difference of nanofiltration membrane is 3.6bar, and the mistake mould difference of ceramic membrane is 5.2bar.
Described step A, feed liquid is 30m at the flow of microfiltration membrane
3/ h, the flow in nanofiltration membrane is 30m
3/ h, the flow in ceramic membrane is 220m
3/ h.
Described step A, it is 1m that the list of microfiltration membrane props up filtration area
2, it is 26.8m that the list of nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
Embodiment 18
The present embodiment is substantially the same manner as Example 8, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.
Embodiment 19
The present embodiment is substantially the same manner as Example 9, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 5.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
Embodiment 20
The present embodiment is substantially the same manner as Example 10, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.5.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 0.5h, and temperature is 60 DEG C, and the pH value of enzyme digestion reaction is 4.5.
Embodiment 21
The present embodiment is substantially the same manner as Example 11, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.6.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 2h, and temperature is 50 DEG C, and the pH value of enzyme digestion reaction is 4.6.
The enzyme concentration of described enzyme digestion reaction is 0.5%.
Embodiment 22
The present embodiment is substantially the same manner as Example 16, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value 4.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 1h, and temperature is 52 DEG C, and the pH value of enzyme digestion reaction is 4.
The enzyme concentration of described enzyme digestion reaction is 1.5%.
Described D step, the molecular weight cut-off of ceramic membrane is 800.
Embodiment 23
The present embodiment is substantially the same manner as Example 17, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 5.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 1.5h, and temperature is 55 DEG C, and the pH value of enzyme digestion reaction is 5.
The enzyme concentration of described enzyme digestion reaction is 1%.
Described D step, the molecular weight cut-off of ceramic membrane is 1500.
Described D step, the molecular weight cut-off of nanofiltration membrane is 200.
Embodiment 24
The present embodiment is substantially the same manner as Example 17, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.2.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 0.6h, and temperature is 52 DEG C, and the pH value of enzyme digestion reaction is 4.2.
The enzyme concentration of described enzyme digestion reaction is 0.6%.
Described D step, the molecular weight cut-off of ceramic membrane is 1000.
Described D step, the molecular weight cut-off of nanofiltration membrane is 100.
The mistake mould difference of described nanofiltration membrane is 3bar, and temperature is 30 DEG C, and single filtration area is 26.8 m
2.
Embodiment 25
The present embodiment is substantially the same manner as Example 17, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.5.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 1.5h, and temperature is 58 DEG C, and the pH value of enzyme digestion reaction is 4.5.
The enzyme concentration of described enzyme digestion reaction is 0.8%.
Described D step, the molecular weight cut-off of ceramic membrane is 900.
Described D step, the molecular weight cut-off of nanofiltration membrane is 120.
The mistake mould difference of described nanofiltration membrane is 4bar, and temperature is 40 DEG C, and single filtration area is 26.8 m
2.
Described D step, the material liquid volume before nanofiltration membrane concentrates is 10 times of concentrated solution volume.
The specific conductivity obtaining xylo-oligosaccharide is 9500 μ s/cm, and ignition residue is 5.5%.
Embodiment 26
The present embodiment is substantially the same manner as Example 17, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 0.7h, and temperature is 52 DEG C, and the pH value of enzyme digestion reaction is 4.
The enzyme concentration of described enzyme digestion reaction is 0.8%.
Described D step, the molecular weight cut-off of ceramic membrane is 950.
Described D step, the molecular weight cut-off of nanofiltration membrane is 150.
The mistake mould difference of described nanofiltration membrane is 3.5bar, and temperature is 32 DEG C, and single filtration area is 26.8 m
2.
Described D step, the material liquid volume before nanofiltration membrane concentrates is 15 times of concentrated solution volume.
The specific conductivity obtaining xylo-oligosaccharide is 8500 μ s/cm, and ignition residue is 4%.
Embodiment 27
The present embodiment is substantially the same manner as Example 17, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 5.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 2h, and temperature is 56 DEG C, and the pH value of enzyme digestion reaction is 5.
The enzyme concentration of described enzyme digestion reaction is 1.2%.
Described D step, the molecular weight cut-off of ceramic membrane is 1200.
Described D step, the molecular weight cut-off of nanofiltration membrane is 180.
The mistake mould difference of described nanofiltration membrane is 3.6bar, and temperature is 35 DEG C, and single filtration area is 26.8 m
2.
Described D step, the material liquid volume before nanofiltration membrane concentrates is 12 times of concentrated solution volume.
The specific conductivity obtaining xylo-oligosaccharide is 9000 μ s/cm, and ignition residue is 5%.
Embodiment 28
The present embodiment is substantially the same manner as Example 8, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.3.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 0.9h, and temperature is 53 DEG C, and the pH value of enzyme digestion reaction is 4.3.
The enzyme concentration of described enzyme digestion reaction is 1.1%.
Described D step, the molecular weight cut-off of ceramic membrane is 800.
Described D step, the molecular weight cut-off of nanofiltration membrane is 105.
The mistake mould difference of described nanofiltration membrane is 3.6bar, and temperature is 36 DEG C, and single filtration area is 26.8 m
2.
Described D step, the material liquid volume before nanofiltration membrane concentrates is 13 times of concentrated solution volume.
The specific conductivity obtaining xylo-oligosaccharide is 10000 μ s/cm, and ignition residue is 6%.
Embodiment 29
The present embodiment is substantially the same manner as Example 9, on this basis:
Described step B, concentrated solution acid neutralization, refers to and adds hydrochloric acid neutralization, make pH value be 4.5.
Described step C, prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
The enzymolysis time of described enzyme digestion reaction is 1.5h, and temperature is 56 DEG C, and the pH value of enzyme digestion reaction is 4.5.
The enzyme concentration of described enzyme digestion reaction is 0.8%.
Described D step, the molecular weight cut-off of ceramic membrane is 1000.
Described D step, the molecular weight cut-off of nanofiltration membrane is 120.
The mistake mould difference of described nanofiltration membrane is 3bar, and temperature is 32 DEG C, and single filtration area is 26.8 m
2.
Described D step, the material liquid volume before nanofiltration membrane concentrates is 12 times of concentrated solution volume.
The specific conductivity obtaining xylo-oligosaccharide is 8000 μ s/cm, and ignition residue is 3%.
Claims (18)
1., with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, it is characterized in that: concrete technology step is as follows:
A, membrane concentration
The press lye produced by viscose fiber is first through pre-filtering removing large granular impurity, enter microfiltration membrane process, permeate is through concentrated 2-4 time of nanofiltration membrane circulation, and send after last concentrated solution thin up into ceramic membrane filter, gained concentrated solution is the concentrated solution of press lye; Concentrated 2-4 time of described nanofiltration membrane circulation, before each filtration, feed liquid all enters nanofiltration membrane after thin up;
B, extraction half fibre
By the concentrated solution acid neutralization of press lye, obtain half fine liquid;
C, enzymolysis
In half fine liquid, add prozyme, enzyme digestion reaction occurs and obtains enzymolysis solution;
D, purification
Enzymolysis solution is through ceramic membrane filter, and permeate enters nanofiltration membrane desalination, and gained concentrated solution is the refined solution of xylo-oligosaccharide, then obtains feed grade xylo-oligosaccharide through evaporation, oven dry.
2. according to claim 1 with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, it is characterized in that: described step A, the aperture of microfiltration membrane is 5 microns, and the molecular weight cut-off of nanofiltration membrane is 200-400, and the molecular weight cut-off of ceramic membrane is 800-1500.
3. according to claim 1 with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, it is characterized in that: described step A, before each nanofiltration membrane, the amount of thin up is 1 times of stock liquid volume, filters the concentrated solution volume obtained identical with stock liquid volume.
4. according to claim 3 with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, it is characterized in that: described permeate is containing alkali 200-300g/l, containing half fine 40-80 g/l, after nanofiltration membrane circulation is concentrated, obtain concentrated solution containing alkali 12-75g/l, containing half fine 40-80g/l.
5. according to claim 1 with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, it is characterized in that: described step A, feed liquid first enters ceramic membrane device through thin up, add water to feed liquid gradation in working cycle, total amount of water is 5 times of material liquid volume, and gained concentrated solution volume is identical with stock liquid volume.
6. according to claim 5 with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, it is characterized in that: containing alkali 2-4g/l in the concentrated solution of described ceramic membrane filter, containing half fine 40-80 g/l.
7. according to claim 1 with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, it is characterized in that: described step A, the temperature of micro-filtration is 40-50 DEG C, and the temperature of nanofiltration membrane is 40-60 DEG C, and the temperature of ceramic membrane filter is 60-80 DEG C.
8. according to claim 1 with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, it is characterized in that: described step A, the mistake mould difference of micro-filtration is 1-2bar, and the mistake mould difference of nanofiltration membrane is 3-4bar, and the mistake mould difference of ceramic membrane is 5-6bar.
9. according to claim 1ly it is characterized in that: described step A with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, feed liquid is 20-40m at the flow of microfiltration membrane
3/ h, the flow in nanofiltration membrane is 25-40m
3/ h, the flow in ceramic membrane is 200-250m
3/ h.
10. according to claim 1ly it is characterized in that: described step A with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, it is 1m that the list of microfiltration membrane props up filtration area
2, it is 26.8m that the list of nanofiltration membrane props up filtration area
2, it is 0.6m that the list of ceramic membrane props up filtration area
2.
11. according to claim 1ly is characterized in that: described step B, concentrated solution acid neutralization with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, refer to and add hydrochloric acid neutralization, make pH value be 4-5.
12. according to claim 1ly is characterized in that: described step C with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, and prozyme is zytase, cellulase and polygalacturonase, and ratio is 3:2:1.
13. is according to claim 12 with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, and it is characterized in that: the enzymolysis time of described enzyme digestion reaction is 0.5-2h, and temperature is 50-60 DEG C, the pH value of enzyme digestion reaction is 4-5.
14. is according to claim 12 with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, it is characterized in that: the enzyme concentration of described enzyme digestion reaction is 0.5-1.5%.
15. is according to claim 1 with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, and it is characterized in that: described D step, the molecular weight cut-off of ceramic membrane is 800-1500.
16. is according to claim 1 with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, and it is characterized in that: described D step, the molecular weight cut-off of nanofiltration membrane is 100-200.
17. is according to claim 16 with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, it is characterized in that: the mistake mould difference of described nanofiltration membrane is 3-4bar, and temperature is 30-40 DEG C, and single filtration area is 26.8 m
2.
18. is according to claim 1 with the membrane concentration technique of viscose fiber pressed liquor for raw material production feed grade xylo-oligosaccharide, it is characterized in that: described D step, and the material liquid volume before nanofiltration membrane concentrates is 10-15 times of concentrated solution volume.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6057438A (en) * | 1996-10-11 | 2000-05-02 | Eastman Chemical Company | Process for the co-production of dissolving-grade pulp and xylan |
| CN104099431A (en) * | 2014-08-01 | 2014-10-15 | 沈阳新华环境工程有限公司 | Method for extracting xylose from viscoce chemical fiber squeezed alkali liquor |
-
2014
- 2014-11-07 CN CN201410622100.8A patent/CN104404105A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6057438A (en) * | 1996-10-11 | 2000-05-02 | Eastman Chemical Company | Process for the co-production of dissolving-grade pulp and xylan |
| CN104099431A (en) * | 2014-08-01 | 2014-10-15 | 沈阳新华环境工程有限公司 | Method for extracting xylose from viscoce chemical fiber squeezed alkali liquor |
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| Title |
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| ROBERT SCHLESINGER ET AL.: "Evaluation of alkali resistant nanofiltration membranes for the separation of hemicellulose from concentrated alkaline process liquors", 《DESALINATION》 * |
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| 何亮亮: "复合酶解蔗渣木聚糖制备低聚木糖的研究", 《中国优秀硕士学位论文全文数据库》 * |
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