CN107699596A - One kind cleans plant cellulose extractant and its preparation method and application - Google Patents
One kind cleans 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 cleans plant cellulose extractant, and the extractant is mixed gained by A liquid with B liquid, and the volume ratio of the A liquid and B liquid is 3:1~5:1, the A liquid is alkali lye, and the B liquid is made up of crude enzyme liquid and enzyme stabilizers, wherein, the crude enzyme liquid is the crude enzyme liquid of the clarification obtained after separating thallus after Bacillus subtillis CGMCC1.836 fermented.Extractant of the present invention mainly causes the colloid in fibrillation to be varied widely on molecular structure using alkaline pectate lyase, alkaline polygalacturonase, sig water, the stability of colloidal complex is by heavy damage, the modified alternating and circulation except colloid of swelling is formed, 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 technology
String 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, current domestic textile industry, nearly hundred million tons of paper industry string dosage.Plant
Fiber is the supramolecular system being made up of cellulose, hemicellulose, lignin, pectin etc., complicated.Realize to cellulose
Utilization, must just carry out the pretreatment procedures such as degumming, remove partial lignin, hemicellulose, pectin etc..Existing treatment technology
Substantial amounts of acid, alkali, water, steam etc. will be consumed, does not meet resource-conserving, environmentally friendly modern business development direction.
This item purpose goal in research is exactly to research and develop the string that inexpensive, pollution-free, added value is high, becomes more meticulous to clean pre-treatment skill
Art, promote the efficient utilization of string particularly waste straw and ramie bast fiber；Traditional agriculture is promoted to modern agriculture
Conversion；Promote textile industry, paper industry, correlation crops processing industry transition and upgrade and technological progress.
At present, domestic and international cellulose extracting method has chemical degumming law and biological degumming method, and chemical degumming law is due to using
Strong acid and strong base, HTHP boiling-off, its complex process, cost is high, security 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 pollution of the waste water of exclusion to environment is extremely serious, discharge of wastewater
Amount is big, is to cause whole water pollution, one of the important pollution sources of environmental destruction.Another kind, biological degumming its strain production
Enzyme ability is low, and not only degumming efficiency is low, and Spawn incubation technical requirements are high, also has from industrial production with a distance from very big.But its
Solve chemical Degumming water consumption it is more, seriously polluted the problems such as.
The content of the invention
It is an object of the invention to provide the preparation method that one kind cleans plant cellulose extractant (degumming agent), the party
Method is simple and easy, beneficial to commercial introduction application.
One kind cleans 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, by mass percentage, it is made up of following components：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 up of crude enzyme liquid and enzyme stabilizers, wherein, the crude enzyme liquid is Bacillus subtillis (Bacillus
Subtilis after) CGMCC1.836 is fermented, the crude enzyme liquid of the clarification 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) obtain.
Further, concentration of the enzyme stabilizers in B liquid is 4~6mM；Further, preferably described enzyme is stable
Concentration of the agent in B liquid is 5mM.
It is of the present invention to clean plant cellulose extractant, 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 glycerine.
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
Concussion and cultivate 18h, is prepared into seed liquor；35L fermentation mediums are prepared, are poured into 50L fermentation tanks, 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 15L/min, obtained
Zymotic fluid, wherein,
The constituent of described seed culture medium is as follows：Sucrose 20g/L, peptone 10g/L, corn steep liquor 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 steep liquor 15g/L, ammonium sulfate 4g/L, phosphoric acid
Hydrogen dipotassium 9.2g/L, potassium dihydrogen phosphate 3g/L, pH7.0；
B. it will continuously be accessed in zymotic fluid obtained by step a in tube centrifuge, and revolution 14000rpm, take supernatant, i.e.,
For crude enzyme liquid.
Further, the B liquid is made as follows：It is 4~6mM to thick by concentration of the enzyme stabilizers in B liquid
Enzyme stabilizers are added in enzyme liquid
Further, the plant cellulose extractant that cleans is made as follows：B liquid is mixed with A liquid, its
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 application for cleaning plant cellulose extractant.
A kind of method extracted to string, the step of methods described includes boiling, extractant is diluted to original
After 8~20 times of volume as cooking liquor (referred to as brand-new cooking liquor), the raffinate of Liang containing Gu≤10%, except residue and lignin after
At least one of waste water, wherein,
The extractant is mixed gained by A liquid with B liquid, wherein, the volume ratio of the A liquid and B liquid is 3:1~5:1,
The A liquid, by mass percentage, it is made up of following components：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 up of crude enzyme liquid and enzyme stabilizers, wherein, crude enzyme liquid is Bacillus subtillis (Bacillus
Subtilis after) CGMCC1.836 is fermented, the crude enzyme liquid of the clarification obtained after separating thallus.
" raffinate of Liang containing Gu≤10% " of the present invention refers to the boiling raffinate of the gained after once boiling process.In boiling
During, once boiling is carried out to wood fibre using cooking liquor, boiling carries out solid filtering after terminating, after filtering containing solid amount≤
10% cooking liquor is named as " raffinate of Liang containing Gu≤10% "
It is of the present invention to refer to the removing residue of gained and wood after secondary boiled process " except residue and the waste water after lignin "
The waste water of element.In digestion process, boiling twice is carried out to wood fibre using cooking liquor, the second boiling terminates in rear cooking liquor
Containing substantial amounts of residue and lignin solid, the cooking liquor after residue and lignin are removed is named as " except residue and giving up after 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 kind in the waste water after residue and lignin, or wherein any two kinds or any three kinds of mixing.
Further, when cooking liquor is the dilution of cellulose extractant, the raffinate of Liang containing Gu≤10%, 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 is in the step of boiling：50~80 DEG C of boiling temperature；Cooking pressure is normal
Pressure；The bath raio 1 of 40~120min of digestion time, material and cooking liquor:8~1:10.
Beneficial effects of the present invention are：The present invention provides one kind and cleans plant cellulose extractant and utilize the extractant
The method extracted to string.Extractant of the present invention mainly utilizes alkaline pectate lyase, the poly- galactolipin of alkalescence
Aldehydic acid enzyme, sig water handle flaxen fiber in a bath, and reed, cotton stalk, salt willow, bamboo willow etc. are handled in two baths.So that fibrillation
In colloid varied widely on molecular structure, the stability of colloidal complex is swelled-changed by heavy damage, formation
Property-except colloid alternating and circulation, reach under normal temperature condition quickly to mesh such as jute fiber degumming, reed slurrying and cotton stalk pulpings
's.
Brief description of the drawings
The fermentation process of Fig. 1 alkaline pectate lyases；
The fermentation process of Fig. 2 alkaline polygalacturonases；
Influence of Fig. 3 stabilizers to alkaline pectate lyase stability.
Embodiment
Following non-limiting examples can make one of ordinary skill in the art be more fully understood the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments, it is conventional method unless otherwise specified；The reagent and material, such as
Without specified otherwise, commercially obtain.
The preparation technology of the present invention for cleaning plant cellulose extractant (degumming agent), comprises the following steps:
First, the preparation of cellulose extractant (degumming agent) is cleaned, step is as follows:
A. Bacillus subtillis (Bacillus subtilis) CGMCC1.836 is inoculated into seed culture medium, 36 DEG C
Concussion and cultivate 18h, is prepared into seed liquor.35L fermentation mediums are prepared, are poured into 50L fermentation tanks, 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 15L/min.
The seed culture medium (g/L):Sucrose 20, peptone 10, corn steep liquor 30, ammonium sulfate 4, dipotassium hydrogen phosphate 18.4,
Potassium dihydrogen phosphate 6, pH7.0.
The fermentation medium (g/L):Glucose 30, corn steep liquor 15, ammonium sulfate 4, dipotassium hydrogen phosphate 9.2, biphosphate
Potassium 3, pH7.0.
B. the zymotic fluid obtained in step a is continuously accessed in tube centrifuge, revolution 14000rpm, takes supernatant
Liquid, you can crude enzyme liquid is made.
C. the ethylene glycol (Dalian Pharmaceutical Group Hua Bo factories) or glycerine stabilization that concentration is 4~6mM are added in crude enzyme liquid
Agent, B liquid is obtained after mixing, 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, by mass percentage, it is made up of following components：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%；
2nd, 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
The crude enzyme liquid obtained in step b is taken, carries out the measure of enzyme activity.Detection method is as follows：
(1) assay method:Five 25mL color-comparison tubes are taken, 1, No. 2 pipe is blank control, and it is thick to add 0.2mL in No. 1 pipe
Enzyme liquid and 2mL buffer solutions, buffer solution are the Glycine-NaOH solution (pH=for the calcium chloride that concentration is 0.44mol/L
9.0).No. 2 pipes add 2mL 0.2% (w/v) polygalacturonic acid solution.3rd, 4 and No. 5 pipes are sample cell, are added thereto
0.2mL crude enzyme liquids and 2mL 0.2% (w/v) polygalacturonic acid solution, 15min is handled under 55 DEG C of waters bath with thermostatic control, rapid to add
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 determines A values (light absorption value) under 235nm.
(2) computational methods of enzyme activity
Enzyme-activity unit defines:1mL enzyme liquids are per minute to produce polygalacturonic acid cleavage under the conditions of pH is 9.0 at 55 DEG C
The enzyme amount of 1 μm of ol unsaturation polygalacturonic acid.Unit is U/mL.
25-reaction system volume (mL)；
D-enzyme liquid extension rate；
Molar absorption coefficient of the 4600-unsaturated polygalacturonic acid at 235nm, (Lmol-1·cm-1)；
15 --- the reaction time (min)；
1 --- cuvette width (cm)
(3) residual enzyme motility rate
B. the measure of alkaline polygalacturonase
(1) 5 color-comparison tubes or test tube, No. 1 addition crude enzyme liquid 0.2mL and 2ml buffer solution are taken, No. 2 pipes add 2mL
0.2% (w/v) polygalacturonic acid solution is as blank control.3rd, 4 and No. 5 are sample cells.Add 0.2mL crude enzyme liquids and 2mL
Polygalacturonic acid solution, 50 DEG C of waters bath with thermostatic control react 30min, add 1.5mL DNS (3,5- dinitrosalicylic acid), boiling water boiling
5min, cool down immediately, add 5mL distilled water, shake up, its A value is determined at 540nm.
(2) enzyme activity defines
At the conditions of the experiments described above, using the enzyme amount needed for every min bottom explodeds thing 1 μm of ol galacturonic acid of generation as 1 enzyme
Unit of activity, unit U/mL.
K --- standard song money slope
V --- reaction volume (mL)
D --- enzyme liquid extension rate
30 --- the reaction time (min)
0.2 --- take enzyme liquid volume (mL)
212.2 --- D- galacturonic acid molecules amounts
C. reducing sugar test
Reduction sugar detection uses 3,5- dinitrosalicylic acids (DNS) development process, specific method reference literature<Guo Jinge, Zheng
Court is set, research [J] the Hebei chemical industry of the Determination of Reducing Sugars such as virtue, 2008,11 (31):1~2>Described method.
Various reagents used in the present invention are AR.
D. influence of the enzyme stabilizers to B liquid neutral and alkali pectin lyase heat resistance and alkali resistance
(1) 0.2mL crude enzyme liquids are taken, add the enzyme stabilizers of 2mL buffer solutions and various concentrations (4~6mM), 70 DEG C of heat treatments
15min, cooling.2mL polygalacturonic acid solutions are added, detection alkaline pectate lyase activity, calculate residual enzymic activities.
(2) 0.2mL crude enzyme liquids are taken, the enzyme stabilizers of 2mL buffer solutions and various concentrations (4~6mM) is added, adds 5mLA
After liquid (pH value=13) is handled 15 minutes, 2mL polygalacturonic acid solutions are added, detection alkaline pectate lyase activity, are calculated
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 fermentation tank, 36 DEG C of fermentation 72h, alkaline pectate lyase and alkaline polygalacturonic acid is detected every 12h
The enzyme activity and reduction sugar amount of enzyme, are as a result shown in Fig. 1 and Fig. 2.
Alkaline pectin can be produced from Fig. 1 and 2, Bacillus subtillis (Bacillus subtilis) CGMCC 1.836
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, alkalescence
Pectin lyase enzyme activity also reaches highest, is 1.4U/mL.Continuing fermentation to 72h, two enzymatic activitys has different degrees of decline.Cause
This takes 60h zymotic fluid, bactofugation body, obtains crude enzyme liquid.
Influence of the stabilizer of embodiment 1 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 measure addition various concentrations 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 experiment remnant enzyme activity under the concentration
Rate improves 27.6%, and alkali resistance experiment residual enzyme motility rate improves 34.6%.
4th, clean cellulose extraction (degumming) technique and detection method, step are as follows:
A. bast-fibre degumming:Flaxen fiber shredding, removal of impurities are sent into digester, it is 1 to add thinner ratio:10~1:15
Cooking liquor, 40~80min of boiling under normal pressure at 50~80 DEG C, then washed, bleached, health, become more meticulous carding step.
B. prepared by reed pulp:Reed is removed the peel, dust removal of pneumatic separation, after cut-out, is sent into digester and adds thinner ratio and be
1:8~1:20 cooking liquors, 40~60min of atmospheric cooking at 60~80 DEG C, after squeeze and grinding sub-wire, carry out secondary boiled 30~
60min, removed the gred, after sizing screening, prepare paper pulp.
C. prepared by cotton stem pulp:Cotton stalk is removed the peel, cut off, after dedusting, it is 1 to be sent into digester and add thinner ratio:8~
1:16 cooking liquors, 50~80min of atmospheric cooking at 60~80 DEG C, after squeeze and grinding sub-wire, secondary boiled 40~70min is carried out,
Removed the gred, after sizing screening, prepare paper pulp.
In the plant cellulose extractant preparation method of the present 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) numb 4 parts of 1.2g of sample sample is weighed, dries to constant weight in 105 ± 3 DEG C and (typically needs 4h) and dry the W that weighs0, will
Sample is moved into 100mL conical flask with stopper, is added 0.5%EDTA 60mL and is placed in autoclave, final vacuum of seething with excitement
5min, 105 ± 1 DEG C are controlled with adjustable transformer, extracts 45min.Take out, filtered with sand core funnel, retain filter residue, in 105 ± 3
DEG C dry to constant weight and (typically need 4h), cooling is weighed W1, 0.0001g is accurate to, pectin weight is W1-W0-WCore。
(2) above-mentioned gained filter residue is moved into conical flask with stopper in sand core funnel with glass bar and small brushes, added
2moL/L hydrochloric acid 60mL, which is placed in autoclave, extracts hemicellulose, extracts 60min, cold water cooling, uses core immediately
Funnel filters, and hot distilled water washing filter residue 4~5 times, retains filter residue, dries to constant weight in 105 ± 3 DEG C and (typically need 4h), cooling claims
Weight, 0.0001g is accurate to, dries the W that weighs2, hemicellulose is W containing weight2-W1。
(3) above-mentioned gained filter residue is moved into 150mL beakers in tall form in sand core funnel, addition is cooled to 10~15 DEG C in advance
72% sulfuric acid 15mL be placed in refrigerator 10~15 DEG C of reaction 4h after, make homogenate with glass bar extruding, often 30min mono-
It is secondary, totally 3 times, add distilled water 100mL to place 12h, filtered with the sand core funnel of known weight, thermal distillation is washed 5~6 times, is retained
Filter residue, dry to constant weight in 105 ± 3 DEG C and (typically need 4h), cooling is weighed, and is accurate to 0.0001g, dries the W that weighs3, cellulose weight
Measure as W3-W2。
(4) lignin weight is W3-WCore。
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 pulps is weighed and dries the W that weighs0, add
30mL17.5%NaOH solution impregnates sample and is stirred vigorously into pastel, and mercerization finish is carried out in 20 DEG C of water bath with thermostatic control
45min.Add 30mL distilled water and filtered with vavuum pump, and repeat to filter 2~3 times.Washed with 25mL 9.5%NaOH solution
Wash 3 times.After using 400mL distillation water washing, addition acetic acid solution to soak 5min in filter again, with regard to water washing to neutrality.
Move to baking oven and be 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 screens, screen slot width is 0.2mm, and screened stock rate inspection is carried out to prepared reed pulp
Survey, take wet pulp 100 grams (moisture content 68%), add water 2L stirrings to discongest 15min；
(2) 15L running water is added into pulp screen slurry bucket, the slurries after above-mentioned discongest are poured into, power of agitator is arranged to
11, start agitator stirring 5min；
(3) Vibration on Start-up screening the pulp motor, screened stock drain valve is opened, is mended when vibration screening the pulp 15min, wherein screening the pulp are to 10min
Fill running water 10L.
(4) agitator 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 floss hole metal bar plug, starts to discharge thick slurry；
(5) connecting water pipe opens running water, Vibration on Start-up screening the pulp motor, starts to backwash 5min to screened stock drain valve；
(6) screening the pulp motor is closed, closes running water, closes screened stock drain valve, puts back to metal bar plug, closes thick slurry discharge
Valve；
(7) will thick slurry, screened stock respectively 105 DEG C when drying weigh 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
Concussion and cultivate 18h, is prepared into seed liquor.35L fermentation mediums are prepared, are poured into 50L fermentation tanks, 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 15L/min.
The seed culture medium (g/L):Sucrose 20, peptone 10, corn steep liquor 30, ammonium sulfate 4, dipotassium hydrogen phosphate 18.4,
Potassium dihydrogen phosphate 6, pH7.0.
The fermentation medium (g/L):Glucose 30, corn steep liquor 15, ammonium sulfate 4, dipotassium hydrogen phosphate 9.2, biphosphate
Potassium 3, pH7.0.
B. the zymotic fluid obtained in step a is continuously accessed in tube centrifuge, revolution 14000rpm, takes supernatant
Liquid, you can crude enzyme liquid is made.
C. ethylene glycol (Dalian Pharmaceutical Group Hua Bo factories) stabilizer that concentration is 5mM is added in crude enzyme liquid, after mixing
B liquid is obtained, 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, by mass percentage, it is made up of following components：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%.
The cellulose extractant of embodiment 2 is applied in hemp degumming engineering
1. cooking liquor is prepared:Prepared in cellulose extractant and be --- the volume ratio of A liquid and B liquid is 5:1；1 is pressed again:10
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；Through washing, bleach, dry, health, the testing result such as hemp composition is shown in Table 1 after the combing that becomes more meticulous.
Embodiment 3
1. cooking liquor is prepared:A part of the boiling raffinate (whole) as cooking liquor, is required according to bath raio in embodiment 2,
(volume ratio of A liquid and B liquid is 5 to the brand-new cooking liquor that cooking liquor insufficient section embodiment 2 is prepared i.e. in cellulose extractant:
1；By 1:Cellulose extractant is diluted with water in 10 ratio, the cooking liquor being formulated) supplemented that (cooking liquor newly prepared accounts for
Whole cooking liquors 30%), 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, will according to bath raio
Ask, the new preparation cooking liquor that cooking liquor insufficient section is prepared with embodiment 2 is supplemented, and (cooking liquor newly prepared accounts for whole boilings
Liquid 30%).
2. technique the results are shown in Table 1 with embodiment 2, hemp composition detection.
As seen from Table 1, plant cellulose extractant all serves good degumming effect in flaxen fiber three times scouring processes
Fruit, its cellulose extraction effect is preferable, and lignin effectively reduces with pectin.The cooking liquor developed in this patent can answer extensively
In hemp fiber degumming engineering.
Testing result before and after the hemp degumming of table 1 combs
The plant cellulose extractant of embodiment 5 is applied in reed pulp preparation engineering
1. cooking liquor is prepared:The volume ratio of A liquid and B liquid is 4 in cellulose extractant:1；1 is pressed again:10 ratio is entered with water
Row dilution, is configured to cooking liquor.
2. technique:Cut off selection by winnowing reed raw material 5kg；Bath raio is 1:8；Boiling temperature is 80 DEG C, and the sub-atmospheric pressure of reed one is steamed
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 is carried out after squeezing stone roller, washing, 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, will according to bath raio
Ask, (i.e. the volume ratio of A liquid and B liquid is the brand-new cooking liquor that cooking liquor insufficient section is prepared with embodiment 5 in cellulose extractant
4:1；By 1:Cellulose extractant is diluted with water in 10 ratio, the cooking liquor being formulated) supplemented (cooking liquor newly prepared
Account for whole cooking liquors 30%).
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, will according to bath raio
Ask, the brand-new cooking liquor that cooking liquor insufficient section is prepared with embodiment 5 is supplemented, 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, and this is specially
The plant cellulose extractant (degumming agent) developed in profit can be applied in reed Pulp and Paper Engineering.
The reed pulp indices of table 2 detect
The plant cellulose extractant of embodiment 8 is applied in cotton stalk pulping engineering
1. cooking liquor is prepared:The volume ratio of A liquid and B liquid is 3 in cellulose extractant:1；1 is pressed again:10 ratio is entered with water
Row dilution, is configured to cooking liquor.
2. technique:Cut off selection by winnowing cotton stalk raw material 5kg；Bath raio is 1:8；Boiling temperature is 80 DEG C；The sub-atmospheric pressure of cotton stalk one 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 is carried out after squeezing stone roller, washing, 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, will according to bath raio
Ask, (i.e. the volume ratio of A liquid and B liquid is the brand-new cooking liquor that cooking liquor insufficient section is prepared with embodiment 8 in cellulose extractant
3:1；By 1:Cellulose extractant is diluted with water in 10 ratio, the cooking liquor being formulated) supplemented (cooking liquor newly prepared
Account for whole cooking liquors 30%)).
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, will according to bath raio
Ask, the brand-new cooking liquor that cooking liquor insufficient section is prepared with embodiment 8 is supplemented, 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, its three times the cotton stem pulp of boiling cellulose extraction effect preferably, screened stock rate it is high, ground in this patent
The cooking liquor of system can be widely used in cotton stalk pulping papermaking engineering.
The cotton stem pulp dregs of rice indices of table 3 detect
Embodiment 11
The preparation of cellulose extractant used and boiling preparation technology are same as Example 2, and difference is that cellulose extracts
A liquid described in agent, by mass percentage, it is made up of following components：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 served in the plant cellulose extractant scouring processes, its cellulose extraction effect is preferable, wood
Quality effectively reduces with pectin.
Embodiment 12
The preparation of cellulose extractant used and boiling preparation technology are same as Example 2, and difference is that cellulose extracts
A liquid described in agent, by mass percentage, it is made up of following components：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 served in the example plant cellulose extractant scouring processes, its cellulose extraction effect is preferable,
Lignin effectively reduces 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, its
In, the volume ratio of the A liquid and B liquid is 3:1~5:1,
The A liquid, by mass percentage, it is made up of following components：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 up of crude enzyme liquid and enzyme stabilizers, wherein, the crude enzyme liquid is Bacillus subtillis
(Bacillussubtilis) after CGMCC1.836 is fermented, the crude enzyme liquid of the clarification 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 glycerine.
5. extractant according to claim 1, it is characterised in that：The A liquid, by mass percentage, by following component groups
Into：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, is prepared into seed liquor；35L fermentation mediums are prepared, are poured into 50L fermentation tanks, are cooled down after 121 DEG C of sterilizing 20min；
According to 5% inoculum concentration, seed liquor is connected in fermentation medium, 36 DEG C of culture 60h, ventilation 15L/min, obtains zymotic fluid,
Wherein,
The constituent of described seed culture medium is as follows：Sucrose 20g/L, peptone 10g/L, corn steep liquor 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 steep liquor 15g/L, ammonium sulfate 4g/L, phosphoric acid hydrogen two
Potassium 9.2g/L, potassium dihydrogen phosphate 3g/L, pH7.0；
B. it will continuously be accessed in zymotic fluid obtained by step a in tube centrifuge, and revolution 14000rpm, take supernatant, and be thick
Enzyme liquid, it is that 4~6mM adds enzyme stabilizers into crude enzyme liquid by concentration of the enzyme stabilizers in B liquid.
A kind of 7. method extracted to string, it is characterised in that：Methods described includes the step of boiling, the boiling
Cooking liquor used is：Extractant described in claim 1 be diluted with water to the solution of 8~20 times of original volume gained, Liang containing Gu≤
10% raffinate, except at least one of waste water after residue and lignin.
8. according to the method for claim 7, it is characterised in that：Conditions of cooking is in the step of boiling：Boiling temperature 50~
80℃；Cooking pressure is normal pressure；The bath raio 1 of 40~120min of digestion time, material and cooking liquor:8~1:10.
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| CN110983845A (en) * | 2019-12-11 | 2020-04-10 | 江西吉润花炮新材料科技有限公司 | Biological bamboo cellulose extracting agent, preparation method and application thereof |
| CN113718541A (en) * | 2021-07-13 | 2021-11-30 | 大连工业大学 | Preparation method of intrinsic hydrophobic oleophylic nanocellulose |
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| 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 |
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| CN113718541A (en) * | 2021-07-13 | 2021-11-30 | 大连工业大学 | Preparation method of intrinsic hydrophobic oleophylic nanocellulose |
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