CN107287972A - A kind of preparation method for cleaning reed pulp - Google Patents

A kind of preparation method for cleaning reed pulp Download PDF

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Publication number
CN107287972A
CN107287972A CN201710533845.0A CN201710533845A CN107287972A CN 107287972 A CN107287972 A CN 107287972A CN 201710533845 A CN201710533845 A CN 201710533845A CN 107287972 A CN107287972 A CN 107287972A
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China
Prior art keywords
liquid
boiling
reed
sodium
pulp
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CN201710533845.0A
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CN107287972B (en
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季英超
高晨
张欣
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Sheng Yi Tianxiang Natural Fiber Technology Co Ltd
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Sheng Yi Tianxiang Natural Fiber Technology Co Ltd
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    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/12Pulp from non-woody plants or crops, e.g. cotton, flax, straw, bagasse
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12NMICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
    • C12N9/00Enzymes; Proenzymes; Compositions thereof; Processes for preparing, activating, inhibiting, separating or purifying enzymes
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12NMICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
    • C12N9/00Enzymes; Proenzymes; Compositions thereof; Processes for preparing, activating, inhibiting, separating or purifying enzymes
    • C12N9/96Stabilising an enzyme by forming an adduct or a composition; Forming enzyme conjugates
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00Pulping cellulose-containing materials
    • D21C3/22Other features of pulping processes
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C5/00Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
    • D21C5/005Treatment of cellulose-containing material with microorganisms or enzymes
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C7/00Digesters

Abstract

The present invention relates to a kind of preparation method for cleaning reed pulp, belong to paper industry and field of environment protection.A kind of preparation method for cleaning reed pulp, the step of methods described includes boiling at least one times, in the boiling step cooking liquor used be the dilution of cellulose extractant, the raffinate of Liang containing Gu≤10%, except at least one of waste water after residue and lignin, the extractant mixes gained with B liquid by A liquid, the A liquid is that B liquid described in alkali lye is made up of crude enzyme liquid and enzyme stabilizers, wherein, the crude enzyme liquid be Bacillus subtillis it is fermented after, the crude enzyme liquid of the clarification obtained after separating thallus.Boiling, slurrying are carried out to reed using the method for the invention, feature is that short used time, normal temperature and pressure, energy-conservation, cooking liquor repeat the waste water of boiling 3~4 times, boiling raffinate through slagging-off and lignin and can be continuing with, so as to reach reed pulping process wastewater zero discharge, the problems such as pulping process environmental pollution is serious, production cost is high is solved.

Description

A kind of preparation method for cleaning reed pulp
Technical field
The present invention relates to a kind of preparation method for cleaning reed pulp, belong to paper industry and field of environment protection.
Background technology
After 1990s mid-term, domestic paper industry relation between market supply and demand there occurs great changes, domestic paper life The growth of yield is significantly less than the growth of consumption figure.
China's paper industry is in a fast growth phase.Statistics over the years shows, China's paper and cardboard it is total Yield is significantly less than aggregate consumption always.It is universal superfluous at this stage in processing manufacturing industry production capacity, paper-making industry be for number not One of industry that many demands constantly increase and supply falls short of demand, belongs to typical demand pull type industry.China's paper and cardboard Output and consumption figure rank first in the world, and import demand of the China to wood pulp is up to the total of whole world wood pulp import and export With.With world economy situation the transition of Important Adjustment and China economic society it is significantly accelerated, China's papermaking industrial technology exists While progress, there is also more many problems:
1. lumber fibre growth cycle is long, there is lack of raw materials
First, although its primary raw material lumber fibre belongs to the plant that can be regenerated, by cultivating the pipe with cutting and regeneration The re-using of resource can be achieved in reason, but its growth cycle is too very long.So, those are using wood pulp as the expensive goods of raw material Critical shortage, has to lean on from external a large amount of imports every year to solve.The situation of Chinese wood pulp dependence on import is increasingly severe.
Reed as a kind of widely distributed perennial grass family reed platymiscium, the cycle of growing is annual 4~ In November, be one of main plant for growing in Wetland Environment.Reed stem is thick, bar is long, and fiber content is high, and impurity is few, thus is excellent Good papermaking material.
2. slurrying water consumption is huge, waste water environmental pollution is serious
In the whole production process of pulp and paper industry, including from getting the raw materials ready to the process into paper, it is required for substantial amounts of fresh Water is as medium, for transporting, washing, disperse and the purposes such as cooling device.
On the other hand, the contaminated wastewater of pulping and paper-making is also extremely serious, in waste water containing substantial amounts of cellulose, lignin and Various chemicals, oxygen demand is big, and the pollution of the waste water of exclusion to environment is extremely serious, and wastewater discharge is big, is to cause whole water One of body pollution, important pollution sources of environmental destruction, to the health and the great prestige of protection structure of ecological environment of people The side of body, is to influence one of subject matter of paper industry sustainable development.
3) construction investment is big, transform difficult
The mashing off of traditional slurrying is backward in technique and repetition cooking is poor, and the alkali lye and chemicals content in waste liquid are high, right Environmental pollution is serious, does not reach discharging standards.
The content of the invention
Wastewater zero discharge reed pulping technique is cleaned it is an object of the invention to provide one kind, be this method solve existing Pulping technique environmental pollution is big, water consumption power consumption height, mixing time length, the low technical problem of energy utilization rate.Slurrying is conducive to make The fast development and technological progress of paper industry.
A kind of preparation method for cleaning reed pulp, the step of methods described includes boiling at least one times, the boiling step In rapid cooking liquor used be the dilution of cellulose extractant, the raffinate of Liang containing Gu≤10%, except the waste water after residue and lignin At least one of,
The extractant mixes gained with B liquid by A liquid, wherein, the volume ratio of the A liquid and B liquid is 3:1~5:1,
The A liquid, by mass percentage, is made up of following components:Sodium hydroxide 10~16%;Sodium carbonate 1.5~ 3.0%;Sodium chloride 2.5~3.5%;Calcium chloride 1.5~2.5%;Sodium phosphate 0.2~0.8%;Sodium formate 0.1~0.5%;Silicon Sour sodium 2.2~4.2%;Sodium sulfite 2.0~2.5%;Water 67.0~80.0%;
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.
" 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, and gained contains after filtering Gu the cooking liquor of Liang≤10% is named as " raffinate of Liang containing Gu≤10% "
" except residue and the waste water after lignin " of the present invention refers to the removing residue of gained and wood after secondary boiled process 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 the dilution that cooking liquor is 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.
The dilution of cellulose extractant of the present invention is preferably 8~20 times of institutes that extractant is diluted with water to original volume The solution obtained.
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.
Cellulose extractant of the present invention, preferably described A liquid, by mass percentage, is made up of following components:Hydroxide Sodium 13%;Sodium carbonate 2.2%;Sodium chloride 2.8%;Calcium chloride 2.1%;Sodium phosphate 0.5%;Sodium formate 0.3%;Sodium metasilicate 3.1%;Sodium sulfite 2.1%;Water 73.9%.
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 is 15L/min, is 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, revolution is 14000rpm, takes 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.
Conditions of cooking is in the step of preparation method of the present invention for cleaning reed pulp preferred boiling:Boiling temperature 60 ~80 DEG C;Cooking pressure is normal pressure;70~120min of digestion time;Boiling bath raio (herein refers to the matter of fibrous raw material and cooking liquor Amount ratio) it is 1:8~1:10.
A preferred technical scheme of the invention is:
A kind of preparation method for cleaning reed pulp, methods described includes following processing steps:
Step 1:Cutoff process is carried out to reed, to 3~5cm;And the reed piece cut is subjected to selection by winnowing removal of impurities, washing;
Step 2:By the reed piece feeding stirring digester after washing, cooking liquor is added, once boiling, boiling bath raio is carried out For 1:8~1:10, normal pressure, reaction temperature be 60 DEG C~80 DEG C under the conditions of, digestion time be 30~60min, be stirred simultaneously, Speed of agitator is 30~80r/min;
Step 3:The reed pulp that once boiling is crossed, which is sent to squeeze, to be ground in devillicate machine, and sub-wire is discongested in progress;
Step 4:By in the reed feeding stirring digester of sub-wire, cooking liquor is added, progress is secondary boiled, and boiling bath raio is 1:8~1:10, normal pressure, reaction temperature be 60 DEG C~80 DEG C under the conditions of, digestion time be 40~60min, speed of agitator be 30~ 80r/min;
Step 5:Reed pulp after will be secondary boiled is washed;
Step 6:Screening the pulp, tabletting are carried out to the reed pulp after washing.
Beneficial effects of the present invention are:The present invention is done in reed pulping process from cooking liquor, pulping process flow Numerous studies innovations.Boiling, slurrying are carried out to reed using the method for the invention, feature is short used time, normal temperature and pressure, section Energy, cooking liquor repeat the waste water of boiling 3~4 times, boiling raffinate through slagging-off and lignin and can be continuing with, so that the reed system of reaching Slurry process wastewater zero discharge, solves the problems such as pulping process environmental pollution is serious, production cost is high.
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, is conventional method unless otherwise specified;The reagent and material, such as Without specified otherwise, commercially obtain.
1. cleaning the preparation of plant cellulose extractant, 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 culture 60h, ventilation is 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 is 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, is made up of following components:Sodium hydroxide 13%;Sodium carbonate 2.2%;Sodium chloride 2.8%;Calcium chloride 2.1%;Sodium phosphate 0.5%;Sodium formate 0.3%;Sodium metasilicate 3.1%;Sodium sulfite 2.1%;Water 73.9%.
2. cleaning the preparation of cooking liquor, step is as follows:Cellulose extractant is diluted with water to 8~20 times, boiling is obtained Liquid (cooking liquor referred to hereinafter as newly prepared).
3. cleaning reed pulp preparation technology, step is as follows:
Step 1:Cutoff process is carried out to reed, to 3~5cm;And the reed piece cut is subjected to selection by winnowing removal of impurities, washing;
Step 2:By the reed piece feeding stirring digester after washing, the cooking liquor newly prepared is added, once boiling is carried out, Boiling bath raio is 1:8~1:10, normal pressure, reaction temperature is under the conditions of 60 DEG C~80 DEG C, digestion time is 30~60min, simultaneously It is stirred, speed of agitator is 30~80r/min.
Step 3:The reed pulp that once boiling is crossed, which is sent to squeeze, to be ground in devillicate machine, and sub-wire is discongested in progress.
Step 4:By in the reed feeding stirring digester of sub-wire, the cooking liquor newly prepared is added, secondary boiled, steaming is carried out It is 1 to boil bath raio:8~1:10, normal pressure, reaction temperature is under the conditions of 60 DEG C~80 DEG C, digestion time is 40~60min, and stirring turns Speed is 30~80r/min.
Step 5:Reed pulp after will be secondary boiled is washed.
Step 6:Screening the pulp, tabletting are carried out to the reed pulp after washing.
4. in the present invention cleans reed pulp, the detection of various indexs and its detection method are as follows:
A. the experimental method of reed slurrying 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 100 grams of wet pulp (moisture content 68%), 15min is discongested in the 2L that adds water stirrings;
(2) 15L running water is added into pulp screen slurry bucket, the slurries after above-mentioned discongest are poured into, power of agitator is set to 11, start agitator stirring 5min;
(3) Vibration on Start-up screening the pulp motor, opens screened stock drain valve, 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 to screened stock drain valve, and Vibration on Start-up screening the pulp motor starts to backwash 5min;
(6) screening the pulp motor is closed, running water is closed, screened stock drain valve is closed, metal bar plug is put back to, thick slurry discharge is closed 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).
B. the experimental method of reed slurrying alpha-cellulose Testing index
(1) 2 grams of pulps (claiming standard to 0.0001 gram) are accurately weighed by paper pulp alpha-cellulose detection method GB/T-1989 to determine The moisture ω % of pulp, and tear 10*10 millimeters of fragment and be placed in 100~150 milliliters of beaker, add 30 milliliter of 17.5% hydrogen Sodium hydroxide solution impregnates pulp.
(2) 15 milliliters are first added;Stirred 2~3 minutes with tack glass handle with care, make into uniform pastel, then will be surplus Under a part of alkali lye add, while uniform and careful stirring 1 minute, and violent stirring and then cap upper surface should be avoided Ware, is placed on progress mercerization effect in 20 ± 0.5C water bath with thermostatic control.
After (3) 45 minutes, 30 milliliters of 20 ± 0.5C distilled water is added immediately, is carefully stirred 1~2 minute.Then will Slurry in beaker is moved into the glass filter of constant weight, with vavuum pump slowly suction strainer.In order to avoid slurry loses, it should repeat Filter 2~3 times, until fiber by untill trapping completely, then with 20 ± 0.5C 9.5% hydroxide under faint vacuum suction filter Sodium solution washs 3 times (every time 25 milliliters).Washing every time, when preceding primary wash liquor is by filtering to the greatest extent, that is, adds new washing lotion, during washing Between be 2~3 minutes, when the filter of whole washing lotions to the greatest extent when, then with 400 milliliters of 18~20C distilled water washing by several times.
(4) in the case of without using vacuum suction filter, add 18~20C 2M acetums in filter to cellulose quilt Submergence.Immersion 5 minutes, then acetum is filtered off with suction filtration, continue to be washed with water untill filtrate is not in acidity.Wash Finish, suck dry moisture.
(5) until still pressed with tack glass bar and filter lower end still without water droplet untill.Filter is taken out, is rinsed with distilled water Outside filter, move into baking oven, dried in 105 ± 3C to constant weight, the weight W of the increased weight of filter, as alpha-cellulose0
W1=2 × ω %
C0--- alpha-cellulose content
W1--- pulp weight (g)
W2--- alpha-cellulose weight (g)
C. beating degree method of testing:DJD-100 type beating degree analyzers
(1) beating degree is measured to sample using DJD-100 type beating degree analyzers, weighs the slurry sample after quantitative screening the pulp (equivalent to 2 grams oven dry stock samples), is put into dilution in measuring cup and is evenly stirred until 1000ml;
(2) separation chamber is stably placed in the infracentral framework of sealing, rotating rope sheave makes seal cones enter separation chamber Locking is compressed afterwards;
(3) slurry diluted at the uniform velocity pours into separation chamber, registration graduated cylinder is placed under separation chamber's inclined tube delivery port, straight tube It is lower to place another graduated cylinder water receiving, gently promote handle seal cones is increased automatically after standing 3 seconds;
(4) sealing centrum stands 1 minute after rising automatically, waits after the no longer water outlet of separation chamber's inclined tube delivery port, then from registration Freeness value (° SR) is read on graduated cylinder;
(5) separation chamber is taken out after the completion of determining, slurry is removed from copper mesh;
(6) fall the water of access in two graduated cylinders, rinse seal cones and separation chamber.
The cellulose extractant of embodiment 1 is applied in reed slurrying engineering
1. cooking liquor is prepared:Cellulose extractant is prepared --- and A liquid is 5 with B liquid volume ratio:1;1 is pressed again:12 ratio It is diluted with water, 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;To reed once boiling 40min, secondary boiled 60min is carried out after squeezing and grinding sub-wire.Reed pulp after secondary boiled is carried out after squeezing stone roller, washing, screening the pulp Detection, testing result is shown in Table 1, is specially:
Step 1:Cutoff process is carried out to reed, to 3~5cm;And the reed piece cut is subjected to selection by winnowing removal of impurities, washing;
Step 2:By the reed piece 5kg feeding stirring digesters after washing, the cooking liquor newly prepared is added, is once steamed Boil, boiling bath raio is 1:8, normal pressure, reaction temperature is under the conditions of 80 DEG C, digestion time is 40min, is stirred simultaneously, stirring Rotating speed is 50r/min.
Step 3:The reed pulp that once boiling is crossed, which is sent to squeeze, to be ground in devillicate machine, and sub-wire is discongested in progress.
Step 4:By in the reed feeding stirring digester of sub-wire, the cooking liquor newly prepared is added, secondary boiled, steaming is carried out It is 1 to boil bath raio:8, normal pressure, reaction temperature is under the conditions of 80 DEG C, digestion time is 60min, and speed of agitator is 50r/min.
Step 5:Reed pulp after will be secondary boiled is washed.
Step 6:Screening the pulp, tabletting are carried out to the reed pulp after washing.
Embodiment 2
1. cooking liquor is prepared:In embodiment 1 step 2 and obtained by step 4 whole boiling raffinates (Liang containing Gu≤10% it is residual Liquid) as a part for cooking liquor, required according to bath raio, cooking liquor (the i.e. A that cooking liquor insufficient section is newly prepared with embodiment 1 Liquid is 5 with B liquid volume ratio:1;1 is pressed again:12 ratio is diluted with water, the cooking liquor being formulated) supplemented and (newly matched somebody with somebody The cooking liquor of system account for whole cooking liquors 30%).
2. technique be the same as Example 1.
Embodiment 3
1. cooking liquor is prepared:In embodiment 2 step 2 and obtained by step 4 whole boiling raffinates (Liang containing Gu≤10% it is residual Liquid) as a part for cooking liquor, required according to bath raio, the cooking liquor that cooking liquor insufficient section is newly prepared with embodiment 1 is carried out Supplement (cooking liquor newly prepared accounts for the 30% of whole cooking liquors).
2. technique be the same as Example 1.
The reed pulp indices of table 1 are detected
The cellulose extractant of embodiment 4 is applied in reed slurrying engineering
1. cooking liquor is prepared:Cellulose extractant is prepared --- and A liquid is 4 with B liquid volume ratio:1;1 is pressed again:16 ratio With in embodiment 1 step 5 washing reed pulp obtained by waste water be diluted (waste water be through the way of distillation handled gained) preparation steaming Boil liquid.
2. technique:Cut off selection by winnowing reed raw material 5kg;Bath raio is 1:8;Boiling temperature is 80 DEG C;To reed once boiling 40min, secondary boiled 60min is carried out after squeezing and grinding sub-wire.Reed pulp after secondary boiled is carried out after squeezing stone roller, washing, screening the pulp Detection, testing result is shown in Table 2, is specially:
Step 1:Cutoff process is carried out to reed, to 3~5cm;And the reed piece cut is subjected to selection by winnowing removal of impurities, washing;
Step 2:By the reed piece 5kg feeding stirring digesters after washing, the cooking liquor newly prepared is added, is once steamed Boil, boiling bath raio is 1:8, normal pressure, reaction temperature is under the conditions of 80 DEG C, digestion time is 40min, is stirred simultaneously, stirring Rotating speed is 50r/min.
Step 3:The reed pulp that once boiling is crossed, which is sent to squeeze, to be ground in devillicate machine, and sub-wire is discongested in progress.
Step 4:By in the reed feeding stirring digester of sub-wire, the cooking liquor newly prepared is added, secondary boiled, steaming is carried out It is 1 to boil bath raio:8, normal pressure, reaction temperature is under the conditions of 80 DEG C, digestion time is 60min, and speed of agitator is 50r/min.
Step 5:Reed pulp after will be secondary boiled is washed.
Step 6:Screening the pulp, tabletting are carried out to the reed pulp after washing.
Embodiment 5
1. cooking liquor is prepared:In embodiment 4 step 2 and obtained by step 4 whole boiling raffinates (Liang containing Gu≤10% it is residual Liquid) as a part for cooking liquor, required according to bath raio, the cooking liquor that cooking liquor insufficient section is prepared with embodiment 4 is mended Fill (cooking liquor newly prepared accounts for the 30% of whole cooking liquors).
2. technique be the same as Example 4.
Embodiment 6
1. cooking liquor is prepared:In embodiment 5 step 2 and obtained by step 4 whole boiling raffinates (Liang containing Gu≤10% it is residual Liquid) as a part for cooking liquor, required according to bath raio, the cooking liquor that cooking liquor insufficient section is prepared with embodiment 4 is mended Fill (cooking liquor newly prepared accounts for the 30% of whole cooking liquors).
2. technique be the same as Example 4.
The reed pulp indices of table 2 are detected
Embodiment 7
To the reed pulp 1%H in embodiment 32O2Carry out two sections of bleachings to be bleached, bleaching temperature is 60 DEG C;Drift The white time each 1h.Reed pulp handsheet after bleaching, send national papermaking research institute to be detected.Partial detection see the table below 3 Hes 4:
Table 3
Table 4

Claims (10)

1. a kind of preparation method for cleaning reed pulp, it is characterised in that:The step of methods described includes boiling at least one times, institute Cooking liquor used is stated in boiling step for the dilution of cellulose extractant, the raffinate of Liang containing Gu≤10%, except residue and lignin At least one of waste water afterwards,
The extractant mixes gained with B liquid by A liquid, wherein, the volume ratio of the A liquid and B liquid is 3:1~5:1,
The A liquid, by mass percentage, is made up of following components:Sodium hydroxide 10~16%;Sodium carbonate 1.5~3.0%;Chlorine Change sodium 2.5~3.5%;Calcium chloride 1.5~2.5%;Sodium phosphate 0.2~0.8%;Sodium formate 0.1~0.5%;Sodium metasilicate 2.2~ 4.2%;Sodium sulfite 2.0~2.5%;Water 67.0~80.0%;
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.
2. according to the method described in claim 1, it is characterised in that:Concentration of the enzyme stabilizers in B liquid is 4~6mM.
3. method according to claim 2, it is characterised in that:Concentration of the enzyme stabilizers in B liquid is 5mM.
4. method according to claim 1 or 2, it is characterised in that:The enzyme stabilizers are ethylene glycol or glycerine.
5. according to the method described in claim 1, it is characterised in that:The A liquid, by mass percentage, is made up of following components: Sodium hydroxide 13%;Sodium carbonate 2.2%;Sodium chloride 2.8%;Calcium chloride 2.1%;Sodium phosphate 0.5%;Sodium formate 0.3%;Silicic acid Sodium 3.1%;Sodium sulfite 2.1%;Water 73.9%.
6. method 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 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 is 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, revolution is 14000rpm, takes supernatant, and be thick Enzyme liquid, is that 4~6mM adds enzyme stabilizers into crude enzyme liquid by concentration of the enzyme stabilizers in B liquid.
7. according to the method described in claim 1, it is characterised in that:The dilution of the cellulose extractant is extractant water It is diluted to the solution of 8~20 times of gained of original volume.
8. method according to claim 7, it is characterised in that:Conditions of cooking is in the step of boiling:Boiling temperature 60~ 80℃;Cooking pressure is normal pressure;70~120min of digestion time;Boiling bath raio is 1:8~1:10.
9. according to the method described in claim 1, it is characterised in that:When cooking liquor is for the dilution of cellulose extractant, containing solid The raffinate of Liang≤10%, except residue mixed with two or more in the waste water after lignin when, its each component is mixed with arbitrary proportion.
10. according to the method described in claim 1, it is characterised in that:Methods described includes following processing steps:
Step 1:Cutoff process is carried out to reed, to 3~5cm;And the reed piece cut is subjected to selection by winnowing removal of impurities, washing;
Step 2:By the reed piece feeding stirring digester after washing, cooking liquor is added, once boiling is carried out, boiling bath raio is 1: 8~1:10, normal pressure, reaction temperature stirs under the conditions of 60 DEG C~80 DEG C, digestion time is 30~60min, is stirred simultaneously Rotating speed is 30~80r/min;
Step 3:The reed pulp that once boiling is crossed, which is sent to squeeze, to be ground in devillicate machine, and sub-wire is discongested in progress;
Step 4:By in the reed feeding stirring digester of sub-wire, cooking liquor is added, progress is secondary boiled, boiling bath raio is 1:8 ~1:10, normal pressure, reaction temperature is under the conditions of 60 DEG C~80 DEG C, digestion time is 40~60min, and speed of agitator is 30~80r/ min;
Step 5:Reed pulp after will be secondary boiled is washed;
Step 6:Screening the pulp, tabletting are carried out to the reed pulp after washing.
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CN108978304A (en) * 2018-09-02 2018-12-11 大连圣多教育咨询有限公司 A kind of paper-making pulping process
CN109024034A (en) * 2018-09-02 2018-12-18 大连圣多教育咨询有限公司 A kind of paper-making pulping digestant
CN109183484A (en) * 2018-09-02 2019-01-11 大连圣多教育咨询有限公司 A kind of technique that slurrying is carried out as raw material using gramineae plant
WO2024016698A1 (en) * 2022-07-22 2024-01-25 新乡化纤股份有限公司 Juncao spinning pulp, and preparation method therefor and use thereof

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CN103523945A (en) * 2012-07-04 2014-01-22 上海橡本永拓环保科技发展有限公司 Clean production method of plant fiber product
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CN102535215A (en) * 2011-11-14 2012-07-04 东莞市绿微康生物科技有限公司 Papermaking plant fiber pretreatment method
CN103243597A (en) * 2012-02-03 2013-08-14 王新军 Non-wood raw material clean pulping method
CN103523945A (en) * 2012-07-04 2014-01-22 上海橡本永拓环保科技发展有限公司 Clean production method of plant fiber product
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CN108978304A (en) * 2018-09-02 2018-12-11 大连圣多教育咨询有限公司 A kind of paper-making pulping process
CN109024034A (en) * 2018-09-02 2018-12-18 大连圣多教育咨询有限公司 A kind of paper-making pulping digestant
CN109183484A (en) * 2018-09-02 2019-01-11 大连圣多教育咨询有限公司 A kind of technique that slurrying is carried out as raw material using gramineae plant
CN109183484B (en) * 2018-09-02 2021-05-28 广西宏瑞泰纸浆有限责任公司 Pulping process using gramineous plants as raw materials
WO2024016698A1 (en) * 2022-07-22 2024-01-25 新乡化纤股份有限公司 Juncao spinning pulp, and preparation method therefor and use thereof

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