CN107699596B - One kind cleaning plant cellulose extractant and its preparation method and application - Google Patents
One kind cleaning plant cellulose extractant and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to one kind to clean plant cellulose extractant and its preparation method and application, belongs to biotechnology and processing of farm products production field.One kind cleaning plant cellulose extractant, the extractant is mixed gained by A liquid with B liquid, the volume ratio of the A liquid and B liquid is 3:1~5:1, the A liquid is lye, the B liquid is made of crude enzyme liquid and enzyme stabilizers, wherein, the crude enzyme liquid is the clear crude enzyme liquid obtained after separating thallus after Bacillus subtillis CGMCC1.836 is fermented.Extractant of the present invention mainly varies widely the colloid in fibrinogen on molecular structure using alkaline pectate lyase, alkaline polygalacturonase, sig water, the stability of colloidal complex is seriously destroyed, swelling-modification-is formed except the alternating and circulation of colloid, reaches under normal temperature condition quickly the purpose of to jute fiber degumming, reed slurrying and cotton stalk pulping.
Description
Technical field
The present invention relates to one kind to clean plant cellulose extractant and its preparation method and application, belong to biotechnology with
Processing of farm products production field.
Background technique
Plant fiber is the fiber that storage is maximum, application field is most wide, applicating history is long on the earth.Textile industry,
Paper industry is even more the application history for having more than one thousand years, at present country's textile industry, nearly hundred million tons of paper industry plant fiber dosage.Plant
Fiber is the supramolecular system being made of cellulose, hemicellulose, lignin, pectin etc., and structure is complicated.It realizes to cellulose
Utilization, must just carry out the pretreatment procedures such as degumming, removal partial lignin, hemicellulose, pectin etc..Existing processing technique
A large amount of acid, alkali, water, steam etc. will be consumed, resource-conserving, environmentally friendly modern business development direction are not met.
The goal in research of this project is exactly that research and development are inexpensive, pollution-free, added value is high, the plant fiber of fining cleans pre-treatment skill
Art promotes the efficient utilization of plant fiber especially waste straw and ramie bast fiber；Promote traditional agriculture to modern agriculture
Conversion；Promote textile industry, paper industry, the transition and upgrade of relevant crops processing industry and technological progress.
Currently, cellulose extracting method has chemical degumming law and biological degumming method both at home and abroad, chemical degumming law is due to using
Strong acid and strong base, high temperature and pressure boiling-off, complex process is at high cost, safety difference and a large amount of waste water of generation, containing a large amount of in waste water
Cellulose, lignin and various chemicals, oxygen demand is big, and the waste water of exclusion is extremely serious to the pollution of environment, discharge of wastewater
Amount is big, is to cause one of entire water pollution, the important pollution sources of ecological environment destruction.Another kind, its strain of biological degumming produce
Enzyme ability is low, not only degumming low efficiency, but also Spawn incubation technical requirements are high, and from industrial production, there are also with a distance from very big.But its
Solve chemical Degumming water consumption it is more, seriously polluted the problems such as.
Summary of the invention
The purpose of the present invention is to provide the preparation method that one kind cleans plant cellulose extractant (degumming agent), the party
Method is simple and easy, is conducive to commercial introduction application.
One kind cleaning plant cellulose extractant, and the extractant is mixed gained by A liquid with B liquid, wherein the A liquid
Volume ratio with B liquid is 3:1~5:1,
The A liquid is grouped as by following groups by mass percentage: sodium hydroxide 10~15%；Sodium carbonate 1.0~
3.0%；Sodium chloride 1.5~3.0%；Calcium chloride 1.0~2.0%；Sodium phosphate 0.2~0.8%；Sodium formate 0.1~0.5%；Silicon
Sour sodium 2.0~4.0%；Sodium sulfite 2.0~2.5%；Water 69.2~82.2%；
The B liquid is made of crude enzyme liquid and enzyme stabilizers, wherein the crude enzyme liquid is Bacillus subtillis (Bacillus
Subtilis after) CGMCC1.836 is fermented, the clear crude enzyme liquid that is obtained after separating thallus.
Bacillus subtillis described in the method for the invention (Bacillus subtilis) CGMCC1.836 can be general by China
Logical Microbiological Culture Collection administrative center (China General Microbiological Culture Collection
Center, CGMCC) it obtains.
Further, concentration of the enzyme stabilizers in B liquid is 4~6mM；Further, the preferably described enzyme is stablized
Concentration of the agent in B liquid is 5mM.
It is of the present invention to clean plant cellulose extractant, the preferably described A liquid, by mass percentage, by following components
Composition: sodium hydroxide 13%；Sodium carbonate 2.3%；Sodium chloride 2.1%；Calcium chloride 1.3%；Sodium phosphate 0.6%；Sodium formate
0.2%；Sodium metasilicate 3.0%；Sodium sulfite 2.2%；Water 75.3%.
Enzyme stabilizers of the present invention are polyol, preferably ethylene glycol or glycerol.
Further, the crude enzyme liquid is made as follows:
A. Bacillus subtillis (Bacillus subtilis) CGMCC1.836 is inoculated into seed culture medium, 36 DEG C
Shake culture 18h, is prepared into seed liquor；35L fermentation medium is prepared, is poured into 50L fermentor, it is cold after 121 DEG C of sterilizing 20min
But；According to 5% (v/v) inoculum concentration, seed liquor is connected in fermentation medium, 36 DEG C of culture 60h, ventilation quantity 15L/min are obtained
Fermentation liquid, wherein
The constituent of the seed culture medium is as follows: sucrose 20g/L, peptone 10g/L, corn pulp 30g/L, sulfuric acid
Ammonium 4g/L, dipotassium hydrogen phosphate 18.4g/L, potassium dihydrogen phosphate 6g/L, pH7.0；
The constituent of the fermentation medium is as follows: glucose 30g/L, corn pulp 15g/L, ammonium sulfate 4g/L, phosphoric acid
Hydrogen dipotassium 9.2g/L, potassium dihydrogen phosphate 3g/L, pH7.0；
B. the fermentation liquid obtained by step a is continuously accessed in tube centrifuge, revolution 14000rpm takes supernatant, i.e.,
For crude enzyme liquid.
Further, the B liquid is made as follows: being 4~6mM to thick by concentration of the enzyme stabilizers in B liquid
Enzyme stabilizers are added in enzyme solution
Further, the plant cellulose extractant that cleans is made as follows: B liquid is mixed with A liquid,
The volume ratio of middle A liquid and B liquid is 3:1~5:1.
It is a further object of the present invention to provide the above-mentioned applications for cleaning plant cellulose extractant.
Extractant is diluted to original by the step of method that a kind of pair of plant fiber extracts, the method includes boilings
As cooking liquor (referred to as brand-new cooking liquor), the raffinate of Liang containing Gu≤10%, except after residue and lignin after 8~20 times of volume
At least one of waste water, wherein
The extractant is mixed gained by A liquid with B liquid, wherein and the volume ratio of the A liquid and B liquid is 3:1~5:1,
The A liquid is grouped as by following groups by mass percentage: sodium hydroxide 10~15%；Sodium carbonate 1.0~
3.0%；Sodium chloride 1.5~3.0%；Calcium chloride 1.0~2.0%；Sodium phosphate 0.2~0.8%；Sodium formate 0.1~0.5%；Silicon
Sour sodium 2.0~4.0%；Sodium sulfite 2.0~2.5%；Water 69.2~82.2%；
The B liquid is made of crude enzyme liquid and enzyme stabilizers, wherein crude enzyme liquid is Bacillus subtillis (Bacillus
Subtilis after) CGMCC1.836 is fermented, the clear crude enzyme liquid that is obtained after separating thallus.
" raffinate of Liang containing Gu≤10% " of the present invention refers to the resulting boiling raffinate after once boiling process.In boiling
In the process, once boiling is carried out to wood fibre using cooking liquor, carries out solid filtering after boiling, Liang containing Gu after filtering≤
10% cooking liquor is named as " raffinate of Liang containing Gu≤10% "
It is of the present invention to refer to resulting removing residue and wood after secondary boiled process " except the waste water after residue and lignin "
The waste water of element.During the cooking process, boiling twice is carried out to wood fibre using cooking liquor, after the second boiling in cooking liquor
Containing a large amount of residue and lignin solid, the cooking liquor after residue and lignin are removed is named as " except useless after residue and lignin
Water ".
In boiling step of the present invention cooking liquor used be the dilution of cellulose extractant, Liang containing Gu≤10% it is residual
Liquid, except one of waste water after residue and lignin or in which any two kinds or any three kinds of mixing.
Further, when the raffinate of dilution, Liang containing Gu≤10% that cooking liquor is cellulose extractant, except residue and wood
When being used in mixed way for two or three in the waste water after element, each component can be used in mixed way with arbitrary proportion, meet boiling needed for boiling
Bath raio.
Further, conditions of cooking in the step of boiling are as follows: 50~80 DEG C of boiling temperature；Cooking pressure is normal
Pressure；Bath raio 1:8~1:10 of 40~120min of digestion time, material and cooking liquor.
It cleans plant cellulose extractant the invention has the benefit that the present invention provides one kind and utilizes the extractant
The method that plant fiber is extracted.Extractant of the present invention mainly utilizes alkaline pectate lyase, the poly- galactolipin of alkalinity
Aldehydic acid enzyme, sig water handle flaxen fiber in a bath, handle reed, cotton stalk, salt willow, bamboo willow etc. in two baths.So that fibrinogen
In colloid varied widely on molecular structure, the stability of colloidal complex is seriously destroyed, formation be swollen-change
Property-except the alternating and circulation of colloid, reach under normal temperature condition quickly to mesh such as jute fiber degumming, reed slurrying and cotton stalk pulpings
's.
Detailed description of the invention
The fermentation process of Fig. 1 alkaline pectate lyase；
The fermentation process of Fig. 2 alkaline polygalacturonase；
Influence of Fig. 3 stabilizer to alkaline pectate lyase stability.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as
Without specified otherwise, commercially obtain.
The preparation process of the present invention for cleaning plant cellulose extractant (degumming agent), includes the following steps:
One, the preparation of cellulose extractant (degumming agent) is cleaned, steps are as follows:
A. Bacillus subtillis (Bacillus subtilis) CGMCC1.836 is inoculated into seed culture medium, 36 DEG C
Shake culture 18h, is prepared into seed liquor.35L fermentation medium is prepared, is poured into 50L fermentor, it is cold after 121 DEG C of sterilizing 20min
But.According to 5% inoculum concentration, seed liquor is connected in fermentation medium.36 DEG C of cultures 72h, ventilation quantity 15L/min.
The seed culture medium (g/L): sucrose 20, peptone 10, corn pulp 30, ammonium sulfate 4, dipotassium hydrogen phosphate 18.4,
Potassium dihydrogen phosphate 6, pH7.0.
The fermentation medium (g/L): glucose 30, corn pulp 15, ammonium sulfate 4, dipotassium hydrogen phosphate 9.2, biphosphate
Potassium 3, pH7.0.
B. the fermentation liquid obtained in step a is continuously accessed in tube centrifuge, revolution 14000rpm takes supernatant
Liquid can be made into crude enzyme liquid.
C. concentration is added in crude enzyme liquid to stablize for the ethylene glycol (Dalian Pharmaceutical Group Hua Bo factory) or glycerol of 4~6mM
Agent, after mixing B liquid, B liquid is mixed with A liquid, the volume ratio of A liquid and B liquid is respectively 3:1,4:1,5:1,
The A liquid is grouped as by following groups by mass percentage: sodium hydroxide 10~15%；Sodium carbonate 1.0~
3.0%；Sodium chloride 1.5~3.0%；Calcium chloride 1.0~2.0%；Sodium phosphate 0.2~0.8%；Sodium formate 0.1~0.5%；Silicon
Sour sodium 2.0~4.0%；Sodium sulfite 2.0~2.5%；Water 69.2~82.2%；
Two, it is as follows in the detection of the various indexs of plant cellulose of the invention and its detection method:
A. the enzyme activity determination of alkaline pectate lyase
Crude enzyme liquid obtained in step b is taken, the measurement of enzyme activity is carried out.Detection method is as follows:
(1) measuring method: taking five 25mL color-comparison tubes, and 1, No. 2 pipe is blank control, and it is thick that 0.2mL is added in No. 1 pipe
Enzyme solution and 2mL buffer, buffer are the Glycine-NaOH solution (pH=for the calcium chloride that concentration is 0.44mol/L
9.0).2mL 0.2% (w/v) polygalacturonic acid solution is added in No. 2 pipes.3,4 and No. 5 pipes are sample cell, are added thereto
0.2mL crude enzyme liquid and 2mL 0.2% (w/v) polygalacturonic acid solution, handle 15min under 55 DEG C of waters bath with thermostatic control, add rapidly
Enter 10mL hydrochloric acid (0.05mol/L) inactivation.After cooling plus water is settled to 25mL.Using deionized water as blank, with ultraviolet spectrometry light
Degree meter measures A value (light absorption value) at 235nm.
(2) calculation method of enzyme activity
Enzyme-activity unit definition: 1mL enzyme solution under the conditions of pH is 9.0, per minute generates polygalacturonic acid cleavage at 55 DEG C
The enzyme amount of 1 μm of ol unsaturation polygalacturonic acid.Unit is U/mL.
25-reaction system volumes (mL)；
D-enzyme solution extension rate；
Molar absorption coefficient of the 4600-unsaturated polygalacturonic acids at 235nm, (Lmol-1·cm-1)；
15 --- the reaction time (min)；
1 --- cuvette width (cm)
(3) residual enzyme motility rate
B. the measurement of alkaline polygalacturonase
(1) 5 color-comparison tubes or test tube, No. 1 addition crude enzyme liquid 0.2mL and 2ml buffer are taken, 2mL is added in No. 2 pipes
0.2% (w/v) polygalacturonic acid solution is as blank control.3,4 and No. 5 are sample cells.0.2mL crude enzyme liquid and 2mL is added
Polygalacturonic acid solution, 50 DEG C of waters bath with thermostatic control react 30min, add the DNS (3,5- dinitrosalicylic acid) of 1.5mL, boiling water boiling
5min is cooled down immediately, is added the distilled water of 5mL, is shaken up, its A value is measured at 540nm.
(2) enzyme activity defines
At the conditions of the experiments described above, enzyme amount needed for generating 1 μm of ol galacturonic acid with every min bottom exploded object is 1 enzyme
Unit of activity, unit U/mL.
K --- standard song money slope
V --- reaction volume (mL)
D --- enzyme solution extension rate
30 --- the reaction time (min)
0.2 --- take enzyme solution volume (mL)
212.2 --- D- galacturonic acid molecules amount
C. reducing sugar test
It restores sugar detection and uses 3,5- dinitrosalicylic acid (DNS) development process, specific method reference literature < Guo Jinge, Zheng
Set court, the Hebei research [J] the chemical industry of the Determination of Reducing Sugars such as virtue, 2008,11 (31): 1~2 > recorded in method.
Various reagents used in the present invention are analytical reagents.
D. influence of the enzyme stabilizers to B liquid neutral and alkali pectin lyase heat resistance and alkali resistance
(1) 0.2mL crude enzyme liquid is taken, the enzyme stabilizers of 2mL buffer and various concentration (4~6mM), 70 DEG C of heat treatments are added
15min, it is cooling.2mL polygalacturonic acid solution is added, detection alkaline pectate lyase activity calculates residual enzymic activities.
(2) 0.2mL crude enzyme liquid is taken, the enzyme stabilizers of 2mL buffer and various concentration (4~6mM) are added, add 5mLA
After liquid (pH value=13) is handled 15 minutes, 2mL polygalacturonic acid solution is added, detection alkaline pectate lyase activity calculates
Residual enzymic activities.
Three, implementing process:
According to the preparation method of B liquid described above by Bacillus subtillis (Bacillus subtilis) CGMCC 1.836
Seed liquor is inoculated into fermentor, 36 DEG C of fermentation 72h, every 12h detection alkaline pectate lyase and alkaline polygalacturonic acid
The enzyme activity and reduction sugar amount, the result is shown in Figure 1 and Fig. 2 of enzyme.
From Fig. 1 and 2 as it can be seen that Bacillus subtillis (Bacillus subtilis) CGMCC 1.836 can produce alkaline pectin
Lyases and alkaline polygalacturonase.Ferment 12h, and two kinds of enzymes have generation.With the extension of fermentation period, both enzymes
Secretion gradually increases.Ferment 48h, and alkaline polygalacturonase enzyme activity first reaches maximum, is 12.6U/mL.Ferment 60h, alkalinity
Pectin lyase enzyme activity also reaches highest, is 1.4U/mL.Continue fermentation to 72h, two enzymatic activitys have different degrees of decline.Cause
This takes the fermentation liquid of 60h, and bactofugation body obtains crude enzyme liquid.
Influence of 1 stabilizer of embodiment to the alkaline pectate lyase stability in B liquid
Carry out the experiment of heat-resisting and alkali resistance respectively according to method described above.After measurement addition various concentration enzyme stabilizers
Residual enzyme motility rate, as a result see Fig. 3.
It can be seen from figure 3 that the optimum concentration of addition enzyme stabilizers is 5mmol/L, heat resistance tests remnant enzyme activity under the concentration
Rate improves 27.6%, and alkali resistance experiment residual enzyme motility rate improves 34.6%.
Four, cleaning cellulose extracts (degumming) technique and detection method, and steps are as follows:
A. bast-fibre degumming: flaxen fiber shredding, removal of impurities are sent into digester, and addition thinner ratio is 1:10~1:15
Cooking liquor, then 40~80min of boiling under normal pressure at 50~80 DEG C washed, bleached, health, fining carding step.
B. prepared by reed pulp: reed being removed the peel, dust removal of pneumatic separation, after cutting, is sent into digester and thinner ratio is added is
1:8~1:20 cooking liquor, 40~60min of atmospheric cooking at 60~80 DEG C, after squeeze and grinding sub-wire, carry out secondary boiled 30~
60min is removed the gred, after sizing screening, prepares paper pulp.
C. cotton stem pulp prepare: cotton stalk is removed the peel, is cut off, after dedusting, be sent into digester in be added thinner ratio be 1:8~
1:16 cooking liquor, 50~80min of atmospheric cooking at 60~80 DEG C carry out secondary boiled 40~70min after squeeze and grinding sub-wire,
It is removed the gred, after sizing screening, prepares paper pulp.
In plant cellulose extractant preparation method of the invention, the fiber before and after degumming is according to " FZ T 30001-1992
Ramie main chemical compositions systematic quantification analysis method " is detected:
(1) sample for weighing numb 4 parts of 1.2g of sample, dry to constant weight in 105 ± 3 DEG C and (generally need 4h) drying weighing W0, will
Sample moves into 100mL triangular flask, and 0.5%EDTA 60mL is added and is placed in autoclave, final vacuum of boiling
5min controls 105 ± 1 DEG C with adjustable transformer, extracts 45min.It takes out, is filtered with sand core funnel, retain filter residue, in 105 ± 3
It DEG C dries to constant weight and (generally needs 4h), cooling weighing W1, it is accurate to 0.0001g, pectin weight is W1-W0-WSand core。
(2) above-mentioned gained filter residue is moved into triangular flask in sand core funnel with glass bar and small brushes, is added
2moL/L hydrochloric acid 60mL, which is placed in autoclave, extracts hemicellulose, extracts 60min, and cold water is cooling, uses sand core immediately
Funnel filtering, hot distilled water wash filter residue 4~5 times, retain filter residue, dry to constant weight in 105 ± 3 DEG C and (generally need 4h), cooling to claim
Weight is accurate to 0.0001g, drying weighing W2, hemicellulose is W containing weight2-W1。
(3) above-mentioned gained filter residue is moved into 150mL beaker in tall form in sand core funnel, is added and is cooled to 10~15 DEG C in advance
72% sulfuric acid 15mL be placed in refrigerator after 10~15 DEG C of reaction 4h, with glass bar extruding make homogenate, every 30min mono-
It is secondary, totally 3 times, distilled water 100mL is added to place 12h, filtered with the sand core funnel of known weight, thermal distillation is washed 5~6 times, is retained
Filter residue dries to constant weight in 105 ± 3 DEG C and (generally needs 4h), cooling weighing, is accurate to 0.0001g, drying weighing W3, cellulose weight
Amount is W3-W2。
(4) lignin weight is W3-WSand core。
CX--- pectin content；Hemicellulose level；Content of cellulose；Content of lignin.
WX--- pectin weight；Hemicellulose weight；Cellulose；Lignin weight (g).
W0--- sample dry weight (g).
E. the experimental method of pulping process alpha-cellulose Testing index
(1) paper pulp alpha-cellulose detection method GB/T-1989 is pressed, 2g pulp drying weighing W is weighed0, it is added
30mL17.5%NaOH solution dipping sample is simultaneously vigorously stirred into paste, and mercerization finish is carried out in 20 DEG C of water bath with thermostatic control
45min.The distilled water of 30mL is added and is filtered with vacuum pump, and repeats to filter 2~3 times.It is washed with the 9.5%NaOH solution of 25mL
It washs 3 times.After using the distillation water washing of 400mL, addition acetic acid solution to impregnate 5min in filter again, with regard to water washing to neutrality.
It moves to baking oven and is dried to constant temperature, weigh W1。
C1--- alpha-cellulose content.
W1--- alpha-cellulose weight (g).
W0--- sample dry weight (g).
F. the experimental method of pulping process screened stock rate Testing index
(1) by ZT3-001 type pulp screen, screen slot width is 0.2mm, carries out the inspection of screened stock rate to prepared reed pulp
It surveys, takes 100 grams of wet pulp (moisture content 68%), water 2L stirring is added to discongest 15min；
(2) 15L tap water is added into pulp screen slurry bucket, the slurries after above-mentioned discongest are poured into, power of agitator is set as
11, starting blender stirs 5min；
(3) starting vibration screening the pulp motor, opens screened stock drain valve, vibrates screening the pulp 15min, wherein screening the pulp to 10min when mend
Fill tap water 10L.
(4) blender is closed in order, vibration screening the pulp motor is closed, closes screened stock drain valve, is opened thick slurry drain valve, is twisted
Lower thick slurry discharge outlet metal bar plug, starts to discharge thick slurry；
(5) connection water pipe opens tap water to screened stock drain valve, and starting vibration screening the pulp motor starts to backwash 5min；
(6) screening the pulp motor is closed, tap water is closed, closes screened stock drain valve, puts back to metal bar plug, closes thick slurry discharge
Valve；
(7) will slightly starch, screened stock distinguish 105 DEG C when drying weighing W1、W2。
C1--- screened stock rate.
W1--- screened stock dry measure (g).
W2--- slightly starch dry weight (g).
Cellulose extractant used is made as follows in following embodiments 2~10:
A. Bacillus subtillis (Bacillus subtilis) CGMCC1.836 is inoculated into seed culture medium, 36 DEG C
Shake culture 18h, is prepared into seed liquor.35L fermentation medium is prepared, is poured into 50L fermentor, it is cold after 121 DEG C of sterilizing 20min
But.According to 5% inoculum concentration, seed liquor is connected in fermentation medium.36 DEG C of cultures 60h, ventilation quantity 15L/min.
The seed culture medium (g/L): sucrose 20, peptone 10, corn pulp 30, ammonium sulfate 4, dipotassium hydrogen phosphate 18.4,
Potassium dihydrogen phosphate 6, pH7.0.
The fermentation medium (g/L): glucose 30, corn pulp 15, ammonium sulfate 4, dipotassium hydrogen phosphate 9.2, biphosphate
Potassium 3, pH7.0.
B. the fermentation liquid obtained in step a is continuously accessed in tube centrifuge, revolution 14000rpm takes supernatant
Liquid can be made into crude enzyme liquid.
C. ethylene glycol (Dalian Pharmaceutical Group Hua Bo factory) stabilizer that concentration is 5mM is added in crude enzyme liquid, after mixing
B liquid, B liquid is mixed with A liquid, the volume ratio of A liquid and B liquid is respectively 3:1,4:1,5:1,
The A liquid is grouped as by following groups by mass percentage: sodium hydroxide 13%；Sodium carbonate 2.3%；Sodium chloride
2.1%；Calcium chloride 1.3%；Sodium phosphate 0.6%；Sodium formate 0.2%；Sodium metasilicate 3.0%；Sodium sulfite 2.2%；Water 75.3%.
2 cellulose extractant of embodiment is applied in hemp degumming engineering
1. cooking liquor is prepared: being prepared in cellulose extractant and be --- the volume ratio of A liquid and B liquid is 5:1；Again by 1:10's
Ratio is diluted with water, is configured to cooking liquor.
2. technique: shredding, removal of impurities hemp raw material 5kg；Bath raio is 1:10；Atmospheric cooking 50min after addition cooking liquor；
Reaction temperature is 80 DEG C；The testing results such as hemp ingredient are shown in Table 1 after washing, bleaching, drying, health, fining combing.
Embodiment 3
1. cooking liquor is prepared: a part of boiling raffinate (whole) as cooking liquor in embodiment 2 is required according to bath raio,
Brand-new cooking liquor that cooking liquor insufficient section embodiment 2 is prepared (volume ratio of A liquid and B liquid is 5 i.e. in cellulose extractant:
1；Cellulose extractant is diluted with water in the ratio of 1:10, the cooking liquor being formulated) supplemented that (cooking liquor newly prepared accounts for
The 30% of whole cooking liquors), wherein boiling raffinate is as filtered " raffinate of Liang containing Gu≤10% "
2. technique the results are shown in Table 1 with embodiment 2, hemp composition detection.
Embodiment 4
1. cooking liquor is prepared: a part of the raffinate (whole) of boiling in embodiment 3 as cooking liquor is wanted according to bath raio
It asks, cooking liquor insufficient section is supplemented with the new preparation cooking liquor that embodiment 2 is prepared, and (cooking liquor newly prepared accounts for whole boilings
The 30% of liquid).
2. technique the results are shown in Table 1 with embodiment 2, hemp composition detection.
As seen from Table 1, plant cellulose extractant all plays good degumming effect in flaxen fiber three times scouring processes
Fruit, cellulose extraction effect is preferable, and lignin is effectively reduced with pectin.The cooking liquor developed in this patent can answer extensively
In hemp fiber degumming engineering.
1 hemp degumming of table combing front and back testing result
5 plant cellulose extractant of embodiment is applied in reed pulp preparation engineering
1. cooking liquor is prepared: the volume ratio of A liquid and B liquid is 4:1 in cellulose extractant；Again in the ratio water of 1:10 into
Row dilution, is configured to cooking liquor.
2. technique: cutting selection by winnowing reed raw material 5kg；Bath raio is 1:8；Boiling temperature is 80 DEG C, is steamed to one sub-atmospheric pressure of reed
Boil 40min；Secondary atmospheric cooking 60min is carried out after squeezing and grinding sub-wire, secondary boiled bath raio is 1:8；Boiling temperature is 80 DEG C.Two
Cooking liquor used in secondary boiling is step 1 gained cooking liquor.Reed pulp after secondary boiled, which is squeezed, to be ground, washes, carrying out after screening the pulp
Detection, slurrying testing result are shown in Table 2.
Embodiment 6
1. cooking liquor is prepared: a part of the raffinate (whole) of boiling in embodiment 5 as cooking liquor is wanted according to bath raio
It asks, (i.e. A liquid and the volume ratio of B liquid are the brand-new cooking liquor that cooking liquor insufficient section is prepared with embodiment 5 in cellulose extractant
4:1；Cellulose extractant is diluted with water in the ratio of 1:10, the cooking liquor being formulated) supplemented (cooking liquor newly prepared
Account for the 30% of whole cooking liquors).
2. technique is shown in Table 2 with embodiment 5, slurrying testing result.
Embodiment 7
1. cooking liquor is prepared: a part of the raffinate (whole) of boiling in embodiment 6 as cooking liquor is wanted according to bath raio
It asks, cooking liquor insufficient section is supplemented with the brand-new cooking liquor that embodiment 5 is prepared, and (cooking liquor newly prepared accounts for whole cooking liquors
30%).
2. technique is shown in Table 2 with embodiment 5, slurrying testing result.
As seen from Table 2, the cellulose extraction effect of the reed pulp of boiling is preferably three times, screened stock rate is high, beating degree is good, this is specially
The plant cellulose extractant (degumming agent) developed in benefit can be applied in reed Pulp and Paper Engineering.
The detection of 2 reed pulp indices of table
8 plant cellulose extractant of embodiment is applied in cotton stalk pulping engineering
1. cooking liquor is prepared: the volume ratio of A liquid and B liquid is 3:1 in cellulose extractant；Again in the ratio water of 1:10 into
Row dilution, is configured to cooking liquor.
2. technique: cutting selection by winnowing cotton stalk raw material 5kg；Bath raio is 1:8；Boiling temperature is 80 DEG C；One sub-atmospheric pressure of cotton stalk is steamed
60min is boiled, secondary atmospheric cooking 80min is carried out after squeezing and grinding sub-wire, secondary boiled bath raio is 1:8；Boiling temperature is 80 DEG C.Two
Cooking liquor used in secondary boiling is step 1 gained cooking liquor.Cotton stem pulp after secondary boiled, which is squeezed, to be ground, washes, carrying out after screening the pulp
Detection, slurrying testing result are shown in Table 3.
Embodiment 9
1. cooking liquor is prepared: a part of the raffinate (whole) of boiling in embodiment 8 as cooking liquor is wanted according to bath raio
It asks, (i.e. A liquid and the volume ratio of B liquid are the brand-new cooking liquor that cooking liquor insufficient section is prepared with embodiment 8 in cellulose extractant
3:1；Cellulose extractant is diluted with water in the ratio of 1:10, the cooking liquor being formulated) supplemented (cooking liquor newly prepared
Account for the 30% of whole cooking liquors)).
2. technique is shown in Table 3 with embodiment 8, slurrying testing result.
Embodiment 10
1. cooking liquor is prepared: a part of the raffinate (whole) of boiling in embodiment 9 as cooking liquor is wanted according to bath raio
It asks, cooking liquor insufficient section is supplemented with the brand-new cooking liquor that embodiment 8 is prepared, and (cooking liquor newly prepared accounts for whole cooking liquors
30%)).
2. technique is shown in Table 3 with embodiment 8, slurrying testing result.
As seen from Table 2, the cellulose extraction effect of the cotton stem pulp of boiling is preferable three times, screened stock rate is high, grinds in this patent
The cooking liquor of system can be widely used in cotton stalk pulping papermaking engineering.
The detection of 3 cotton stem pulp dregs of rice indices of table
Embodiment 11
The preparation of cellulose extractant used and boiling preparation process are same as Example 2, and difference is that cellulose extracts
A liquid described in agent is grouped as by following groups by mass percentage: sodium hydroxide 11%；Sodium carbonate 2%；Sodium chloride 2.3%；Chlorine
Change calcium 1.5%；Sodium phosphate 0.4%；Sodium formate 0.3%；Sodium metasilicate 3.0%；Sodium sulfite 2.3%；Water 77.2%.The present embodiment
Good degumming effect is all played in the plant cellulose extractant scouring processes, cellulose extraction effect is preferable, wood
Quality is effectively reduced with pectin.
Embodiment 12
The preparation of cellulose extractant used and boiling preparation process are same as Example 2, and difference is that cellulose extracts
A liquid described in agent is grouped as by following groups by mass percentage: sodium hydroxide 14%；Sodium carbonate 2.5%；Sodium chloride 2.8%；
Calcium chloride 1.5%；Sodium phosphate 0.8%；Sodium formate 0.3%；Sodium metasilicate 3.3%；Sodium sulfite 2.4%；Water 72.4%.This implementation
Good degumming effect is all played in the example plant cellulose extractant scouring processes, cellulose extraction effect is preferable,
Lignin is effectively reduced with pectin.
Claims (8)
1. one kind cleans plant cellulose extractant, it is characterised in that: the extractant is mixed gained by A liquid with B liquid,
In, the volume ratio of the A liquid and B liquid is 3:1~5:1,
The A liquid is grouped as by following groups by mass percentage: sodium hydroxide 10~15%；Sodium carbonate 1.0~3.0%；Chlorine
Change sodium 1.5~3.0%；Calcium chloride 1.0~2.0%；Sodium phosphate 0.2~0.8%；Sodium formate 0.1~0.5%；Sodium metasilicate 2.0~
4.0%；Sodium sulfite 2.0~2.5%；Water 69.2~82.2%；
The B liquid is made of crude enzyme liquid and enzyme stabilizers, wherein the crude enzyme liquid is Bacillus subtillis (Bacillus
Subtilis after) CGMCC1.836 is fermented, the clear crude enzyme liquid that is obtained after separating thallus.
2. extractant according to claim 1, it is characterised in that: concentration of the enzyme stabilizers in B liquid is 4~6mM.
3. extractant according to claim 2, it is characterised in that: concentration of the enzyme stabilizers in B liquid is 5mM.
4. extractant according to claim 1 or 2, it is characterised in that: the enzyme stabilizers are ethylene glycol or glycerol.
5. extractant according to claim 1, it is characterised in that: the A liquid is grouped by following groups by mass percentage
At: sodium hydroxide 13%；Sodium carbonate 2.3%；Sodium chloride 2.1%；Calcium chloride 1.3%；Sodium phosphate 0.6%；Sodium formate 0.2%；
Sodium metasilicate 3.0%；Sodium sulfite 2.2%；Water 75.3%.
6. extractant according to claim 2, it is characterised in that: the B liquid is made as follows:
A. Bacillus subtillis (Bacillus subtilis) CGMCC1.836 is inoculated into seed culture medium, 36 DEG C of concussions
18h is cultivated, seed liquor is prepared into；35L fermentation medium is prepared, is poured into 50L fermentor, it is cooling after 121 DEG C of sterilizing 20min；
According to 5% inoculum concentration, seed liquor is connected in fermentation medium, 36 DEG C of cultures 60h, ventilation quantity 15L/min obtain fermentation liquid,
Wherein,
The constituent of the seed culture medium is as follows: sucrose 20g/L, peptone 10g/L, corn pulp 30g/L, ammonium sulfate
4g/L, dipotassium hydrogen phosphate 18.4g/L, potassium dihydrogen phosphate 6g/L, pH7.0；
The constituent of the fermentation medium is as follows: glucose 30g/L, corn pulp 15g/L, ammonium sulfate 4g/L, phosphoric acid hydrogen two
Potassium 9.2g/L, potassium dihydrogen phosphate 3g/L, pH7.0；
B. the fermentation liquid obtained by step a is continuously accessed in tube centrifuge, revolution 14000rpm takes supernatant, as slightly
Enzyme solution is that enzyme stabilizers are added into crude enzyme liquid by 4~6mM by concentration of the enzyme stabilizers in B liquid.
7. the method that a kind of pair of plant fiber extracts, it is characterised in that: the step of the method includes boilings, the boiling
Cooking liquor used are as follows: extractant described in claim 1 be diluted with water to original volume 8~20 times of resulting solution and Liang containing Gu≤
10% raffinate, except the combination of at least one of waste water after residue and lignin.
8. according to the method described in claim 7, it is characterized by: conditions of cooking in the step of boiling are as follows: boiling temperature 50~
80℃；Cooking pressure is normal pressure；Bath raio 1:8~1:10 of 40~120min of digestion time, material and cooking liquor.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1754020A (en) * | 2002-12-20 | 2006-03-29 | 诺维信北美公司 | Treatment of fabrics, fibers, or yarns |
| CN103540581A (en) * | 2013-10-19 | 2014-01-29 | 沅江浣溪沙酶技术有限公司 | Production method and applications of compound enzyme liquid used in papermaking and pulping process of wheat straws and rice straws |
| CN103642774A (en) * | 2013-11-13 | 2014-03-19 | 宁夏夏盛实业集团有限公司 | Mixed neutral cellulase, preparation method thereof and application thereof to papermaking beating |
| CN106085607A (en) * | 2016-06-28 | 2016-11-09 | 郭迎庆 | A kind of preparation method of high-performance enzyme detergent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1754020A (en) * | 2002-12-20 | 2006-03-29 | 诺维信北美公司 | Treatment of fabrics, fibers, or yarns |
| CN103540581A (en) * | 2013-10-19 | 2014-01-29 | 沅江浣溪沙酶技术有限公司 | Production method and applications of compound enzyme liquid used in papermaking and pulping process of wheat straws and rice straws |
| CN103642774A (en) * | 2013-11-13 | 2014-03-19 | 宁夏夏盛实业集团有限公司 | Mixed neutral cellulase, preparation method thereof and application thereof to papermaking beating |
| CN106085607A (en) * | 2016-06-28 | 2016-11-09 | 郭迎庆 | A kind of preparation method of high-performance enzyme detergent |
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