CN110528102A - A kind of cellulose viscose manufacturing technique based on hemp dissolving pulp - Google Patents
A kind of cellulose viscose manufacturing technique based on hemp dissolving pulp Download PDFInfo
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- CN110528102A CN110528102A CN201910734641.2A CN201910734641A CN110528102A CN 110528102 A CN110528102 A CN 110528102A CN 201910734641 A CN201910734641 A CN 201910734641A CN 110528102 A CN110528102 A CN 110528102A
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- raw material
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- dissolving pulp
- hemp dissolving
- crudefiber crop
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
- D21C5/005—Treatment of cellulose-containing material with microorganisms or enzymes
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/10—Bleaching ; Apparatus therefor
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Abstract
The present invention relates to textile production process technical field, in particular to a kind of cellulose viscose manufacturing technique based on hemp dissolving pulp.It includes the following steps: that (1) prepares raw material: crudefiber crop raw material is collected, it is spare；(2) it prepares hemp dissolving pulp: the crudefiber crop raw material prepared in step (1) being subjected to enzyme cold dome, oxygen bleaching, washing, drying and processing, prepares hemp dissolving pulp；(3) it prepares viscose rayon: the hemp dissolving pulp prepared in step (2) being crushed, sulfonation, dissolution, maturation, spinning, drawing-off, refining desulfuration, drying and processing, obtain viscose rayon.Simple production process of the present invention, and mild condition, environment protecting and power-saving, and the large specific surface area of the viscose rayon of production, the dye-uptake and elongation at break of fiber can be improved, the antibiotic property of viscose rayon is good, and antibiotic property can retain the 70-80% of raw ramie, so that textile fabric pendency degree is more preferable, the more soft cunning of feel moistens exquisiteness.
Description
Technical field
The present invention relates to textile production process technical field, in particular to a kind of viscose rayon based on hemp dissolving pulp produces work
Skill.
Background technique
Regenerated celulose fibre, that is, viscose rayon, be with native cellulose (cotton, fiber crops, bamboo, tree, shrub) for raw material, no
Change its chemical structure, only changes the physical structure of native cellulose, to manufacture the better regenerated fiber of performance
Cellulose fiber.Its structure composition is similar to cotton, the difference is that its hygroscopicity and gas permeability are better than cotton fiber, it may be said that it is all
Hygroscopicity and the best one kind of gas permeability, are known as " fabric that can be breathed " in chemical fibre.It also possesses cotton fiber not simultaneously
The certain advantages for the silk having.Therefore dress is more comfortable；It dyes beautiful property and is better than cotton fiber；It is soft, plentiful, sliding
It is refreshing, with the gloss as excellent drapability and silk；Thermal stability and photostability are high, do not play electrostatic；Intensity and elongation energy
Meet the needs of most of textiles, it is deep to be liked by broad masses.
Crudefiber crop is not only best in quality, and cultivation history is long, and its is many kinds of, mainly there is ramie, flax, the Chinese
Fiber crops, sisal hemp, jute and bluish dogbane etc., suitable for developing all kinds of novel products of different purposes.China is that crudefiber crop important in the world is raw
State is produced, while being also important bast fibre spinning processing state, hemp product is always that national conventional outlet is earned foreign exchange substance.Ramie, ramie
Stem hide fiber is elongated, tough, pure white, glossy, and pulling force is strong, resistance to water-wet, rich elastic force and insulating properties, can be made into grass cloth, aircraft
Wing cloth, the lining cloth of rubber industry, electric wire coating, incandescent lamp yarn, fishing net, artificial silk processed, synthetic cotton etc. are blended with wool, cotton
Advanced dress material can be made；Staple fiber can be the raw material of fine paper, gunpowder, artificial silk etc., and can weavening carpet, gunnysack etc..Flax, it is sub-
The value of exploiting and utilizing of fiber crops is high, and the fiber that flax stem is produced is the important source material of textile industry, pure can be spun, also can be with other fibers
It is blended.Since flax fiber is compared with animal origin, other plant fibers, synthetic fibers, have many unique irreplaceable
The advantages of, determine that it accounts for critical role in national economy.And Chinese fiber crops are as environmentally protective ecological fiber, fabric is except having
Natural antibacterial, shield ultraviolet radiation, moisture absorbing and sweat releasing, soft comfortable, skin care keep a public place clean, adsorb peculiar smell and the performances such as wear-resisting outside, also
With the honorable styles such as graceful, simple and unadorned, naturally practical, therefore, Chinese flax fabric is increasingly liked by people.
After numb ripe and harvested, two kinds of fibers can be produced, one is long fiber crops, are mostly used in high-count yarn spun, another kind is to fall
Fiber crops, noil be hemp spinning yarn leftover bits and pieces, i.e., fiber crops comb or automatically falls off in process on long bast-fiber spinning apparatus with 4 ㎝
Staple fiber based on following length, hemp skin, hards, hemp stalk etc., since fiber crops are high culm plants, noil fiber is in disorder, so individually
Spinning is difficult, is difficult to recycle, in general, enterprise is all that it is produced ramie cotton blending yarn on short spinning equipment to utilize well,
The blending product number is lower (usually following in 16 English branch), product wiriness, and blending product added value is not high；Or portion
Divide noil for the primary raw materials as papermaking, or even cook for making a fire, the utility value of fiber crops is caused to reduce.Due to ring
The happiness of the reduction for increasingly sharpening, ploughing of border protection and the increasingly depleted and people of petroleum resources to flaxen fiber clothes, home textile
Love, the supply and demand market of numb natural fiber is increasingly hot, then extracting flaxen fiber sufficiently to meet home textile, textile garment and functionality
The use of composite material is at the task of top priority.And the quality of pulp and the production technology of fiber and product quality have substantial connection,
Therefore, the quality of pulp is particularly important for good fiber quality cellulose fiber for preparing.
Such as 109295519 A of patent CN, a kind of preparation method of Chinese jute viscose is disclosed, comprising the following steps: 1)
Prepare raw material: by the root bast fiber of Chinese fiber crops and taper bast fiber uniform cut, raw material is made；2) Chinese hemp dissolving pulp is prepared:
Raw material described in step 1) is subjected to boiling, mashing, pulp washing, papermaking, Chinese hemp dissolving pulp is made；3) Chinese jute viscose is prepared: will
Step 2) the Chinese hemp dissolving pulp is impregnated, is experienced, sulfonation, dissolution, maturation, spinning, drawing-off, refining, drying, and Chinese fiber crops are obtained
Viscose rayon.The preparation method of Chinese jute viscose provided by the invention, it is fine in traditional viscose glue the characteristics of for Chinese fiber crops ingredient
On the basis of the production technology of dimension, corresponding improvement is done to auxiliary agent and concrete technology, so as to be suitable for Chinese jute viscose
Production guarantees the production effect and stable product quality of Chinese jute viscose.But there are following drawbacks, first is that first by Chinese fiber crops
Root bast fiber and taper bast fiber uniform cut, preparation raw material stage is complex, and production efficiency is low；Second is that it is being starched
In the preparation of the dregs of rice, it is necessary first to thermophilic digestion, it is larger to the damage of cellulose and hemicellulose；Third is that before boiling not to Chinese fiber crops into
Row pre-treatment, base amount is more, and the strand of cellulose crystals can be made to receive slight damage, and ordered fiber element structure is caused to subtract
Few, cellulose crystallity also decreases, while the COD value that will lead to discharge waste liquid is high, is unfavorable for environmental protection, meanwhile, because
It is more than common natural fiber for the crystal region of flaxen fiber, so some auxiliary agents are difficult to penetrate into fibrous inside, lead to the ratio of fiber
Surface area is smaller, and fiber is subsequent poor to auxiliary agent adsorption effect, thus will lead to spin come viscose rayon specific surface area it is small, upper dye
Rate is low, and the elongation at break of fiber is low, poor toughness.
Summary of the invention
In view of the deficienciess of the prior art, the technical problem to be solved by the invention is to provide a kind of production technology letters
Single, mild condition is friendly to environment, and the viscose rayon the produced degree of polymerization with higher, strength and wet modulus, specific surface
Product is big, and dye-uptake is high, and elongation at break is high, the good cellulose viscose manufacturing technique based on hemp dissolving pulp of good toughness, antibiotic property.
The present invention to achieve the above object the technical solution adopted is that: a kind of viscose rayon based on hemp dissolving pulp produces work
Skill includes the following steps:
(1) prepare raw material: collecting crudefiber crop raw material, it is spare, wherein crudefiber crop raw material includes Chinese fiber crops, flax, ramie；
(2) it prepares hemp dissolving pulp: enzyme cold dome, oxygen bleaching, washing, drying and processing, system is carried out to crudefiber crop raw material described in step (1)
Standby hemp dissolving pulp；
(3) prepare viscose rayon: the hemp dissolving pulp prepared in step (2) is crushed, sulfonation, dissolution, maturation, spinning,
After drawing-off, refining desulfuration, drying and processing, viscose rayon is obtained, the section of viscose rayon is the porous structure of similar round, more
Pore structure may make the anti-microbial property of viscose rayon, its antibiotic property is enable to retain the 70-80% of raw ramie, the quality of viscose rayon
Indication range are as follows: residual sulphur rate≤0.03%, alpha cellulose >=95.5-96.5%, ash content (725 degree)≤0.07-0.12%, iron
Content≤14-23mg/kg, whiteness >=80-82%, inhale base number are as follows: 500-750.
The above-mentioned cellulose viscose manufacturing technique based on hemp dissolving pulp, it is described to prepare hemp dissolving pulp specific steps in step (2)
It is as follows:
(1) crudefiber crop raw material pre-treatment
(1) enzyme cold dome
The sulfuric acid for being 25% by mass fraction, oxalic acid, metal chelating agent, wetting and penetrating agent, degumming composite enzyme, hydrogen peroxide exist
In auxiliary cylinder after mixing, it is put into crudefiber crop raw material, is impregnated, control bath raio is 1:15-20, and control is 80-90%, room temperature to liquid rate
Lower cold dome 12-24h, drain；
(2) oxygen bleaching is handled
By oxygenic bleaching aids, caustic soda, degumming catalyst, multi-functional processing auxiliary agent squeezes into saucepan in auxiliary cylinder after mixing
In, start to warm up operating, 90-95 DEG C of when, the hydrogen peroxide that mass fraction is 27% was added into saucepan, and control bath raio is 1:8-1:
15, after operating 55-65min, drain；
(3) washing neutralizes: first neutralizing acid is added to boiling in drift pot, control pH value is 6-7.5,40-50 DEG C of washing 20min,
Control bath raio is 1:8-1:15, and drain is washed 2-3 times；
(4) sofening treatment: being added lubricant to boiling in drift pot, boils drift pot and is warming up to 40 DEG C, after operating 20min, drain；
(5) it dries: half drying and processing finally being carried out to the crudefiber crop raw material after the completion of sofening treatment, is dehydrated using screw press
Machine drying and processing；
(6) wet shredding: the crudefiber crop raw material after drying is subjected to wet shredding processing, for use；
(2), prepared by pulp
(1) first piece alkali suitable quantity of water is mixed and is melted, be warming up to 55-60 DEG C；
(2) enhancing wetting agent, toughener is then added, dispersion defrother stirs evenly, and keeps the temperature 55-60 DEG C；
(3) it is eventually adding premenstrual treated crudefiber crop raw material, 55-60 DEG C is kept the temperature, stirs 60min；
(4) it dries again, after spiral pressing dehydrator is dried, cake of press finally obtains hemp dissolving pulp.
The above-mentioned cellulose viscose manufacturing technique based on hemp dissolving pulp, in step (3), the sulfonation is using at wet sulphidization
CS is added in wet sulphidization processing in reason2, controlled at 18-22 DEG C, time 90-110min, the CS2Additional amount
For the 36-40% of the mass fraction of the hemp dissolving pulp.
The above-mentioned cellulose viscose manufacturing technique based on hemp dissolving pulp, in step (3), when the dissolution, controlled at
It 29-33 DEG C, time 120-150min, when the drawing-off, after multistage drafting, forms thread and enters in coagulating bath, solidify
At strand, refining desulfuration then is carried out to strand, just obtains viscose rayon after dry.
The above-mentioned cellulose viscose manufacturing technique based on hemp dissolving pulp, it is described in the step (1) enzyme cold dome treatment process
The additional amount of sulfuric acid is the 1-3% of crudefiber crop raw material weight, and the additional amount of the oxalic acid is the 1-3% of crudefiber crop raw material weight, described
The additional amount of metal chelating agent is the 0.5-1.5% of crudefiber crop raw material weight, and the additional amount of the wetting and penetrating agent is crudefiber crop raw material
The 1-2% of weight, the additional amount of the degumming composite enzyme are the 0.5-2% of crudefiber crop raw material weight, the additional amount of the hydrogen peroxide
For the 3-5% of crudefiber crop raw material weight.
The above-mentioned cellulose viscose manufacturing technique based on hemp dissolving pulp, in the step (1) oxygen bleaching treatment process, the oxygen
The additional amount for floating auxiliary agent is 5-8g/L, and the additional amount of the caustic soda is 1-3g/L, and the additional amount of the degumming catalyst is 1-3g/
The additional amount of L, the multi-functional processing auxiliary agent are 1-3g/L, and the additional amount of the hydrogen peroxide is 8-12g/L, the step (1)
In sofening treatment technique, the additional amount of the lubricant is 5-10g/L, in the step (1) enzyme cold dome treatment process, in fiber crops
After class raw material carries out half drying and processing, control water content is 20%.
The above-mentioned cellulose viscose manufacturing technique based on hemp dissolving pulp, the additional amount of piece alkali described in step (2) are to be prepared
The 7-12% of pulp weight, the additional amount of the enhancing wetting agent are the 0.5-1.5% of pulp weight to be prepared, the toughener
Additional amount be pulp weight to be prepared 0.2-0.5%, the additional amount of the dispersion defrother is pulp weight to be prepared
0.2-0.5%, the additional amount of the crudefiber crop raw material are the 3.5-5.5% of pulp weight to be prepared, and the water is surplus, the step
Suddenly in (one) enzyme cold dome treatment process, the time of immersion is 12-24h.
The above-mentioned cellulose viscose manufacturing technique based on hemp dissolving pulp, the metal chelating agent include EDTA-2Na, citric acid
One or both of；The wetting and penetrating agent includes nonionic surfactant, the multi-functional processing auxiliary agent include it is non-from
Sub- surfactant, one or both of anionic surfactant, the enhancing wetting agent are nonionic surfactant,
The toughener is improved plant starch binder, and the dispersion defrother is special silicone grease dispersing agent, and the lubricant is by such as
The component of lower weight percent is prepared: four ester based quaternary ammonium salt 3%-6%；8809 2%-3% of polyoxyethylene ether；Silicon wax
6%-9%；Silane coupling agent KN-550 3%-5%；Catalyst T-50 2-3%；D4 octamethylcy-clotetrasiloxane 15%-
20%；Glacial acetic acid 0.5%-1.5%；Deionized water surplus.
The above-mentioned cellulose viscose manufacturing technique based on hemp dissolving pulp, the degumming composite enzyme is by following weight percent
Component is prepared:
Zytase: 6%-9%；
Cellulase: 2%-5%；
Pectase: 20%-25%；
Chelated dispersants: 35%-44%；
Inhibitor: 16%-34%；
Nonionic polymer surfactant: 1%-3%.
The above-mentioned cellulose viscose manufacturing technique based on hemp dissolving pulp, the oxygenic bleaching aids by following weight percent group
Divide and be prepared:
Anionic surfactant: 15%-20%；
Nonionic surfactant: 4%-5%；
Solid oxygen: 25%-30%；
Chelated dispersants: 5%-10%；
Defoaming agent: 1%-2%；
Metasilicate pentahydrate sodium: 40%-45%.
Beneficial effect the present invention is based on the cellulose viscose manufacturing technique of hemp dissolving pulp is:
First, the present invention first prepares hemp dissolving pulp, and the hemp dissolving pulp of preparation is recycled to prepare jute viscose.Preparing hemp dissolving pulp
In, it uses and the degumming of cold dome method first is carried out to crudefiber crop raw material, then prepare the new process theory of pulp again.Firstly, to crudefiber crop original
Material carries out the degumming of cold dome method, enables to cellulose after crudefiber crop raw material soaking to expand, helps degumming composite enzyme, oxygen bleaching
Agent, degumming catalyst, multi-functional processing auxiliary agent etc. can largely penetrate into inside crudefiber crop raw material, can sufficiently remove crudefiber crop raw material
On pectin, lignin, water soluble compound, hemp stalk, hards and hemp skin, removal rate is high, and degumming effect is good, significantly reduces
The degree of polymerization of crudefiber crop raw material and the rigidity of fiber, crystallinity have broken the hydrogen bond of fibrous inside, improve pulp dissolubility and
Stability, the regenerated fiber spinning solution to make stable create conditions.Then slurry is prepared using the crudefiber crop raw material after cold dome degumming
The dregs of rice, since the synergistic effect of enhancing wetting agent and toughener in pulp so that uniformly exist in solution, charge balance in solution,
Ionic equilibrium further creates conditions so that pulp will not be layered in the solution to be prepared into the uniform viscose rayon of silk,
To guarantee the quality of viscose rayon, while the damage to crudefiber crop raw material can be reduced.Secondly, the present invention uses low-temperature blanching, to fibre
The damage of dimension element and hemicellulose is small, and the degumming composite enzyme, oxygenic bleaching aids, the degumming catalyst that use can be accurately and efficiently
The impurity on fiber is removed, while very few to fibre damage.Third is that alkali charge is 1/3 of common process or so in the present invention, it is real
Showing under low alkali number cellulose to alkalize, pollutant is few in sewage effluent, environmentally protective, be conducive to environmental protection, while pulp
Stability increases, and viscosity stabilization, fiber basic hydrolysis is lacked.
Second, during preparing viscose rayon, does not have to aging drop and gather, to increase the high wet modulus of viscose rayon.
Using the spun viscose rayon large specific surface area of production technology of the present invention, dye-uptake is high, and the elongation at break of fiber is high, toughness
It is good, other than having the characteristics that high humidity strength, low elongation and low puffed degree and good alkali resistance, more important is have compared with
High wet modulus is the medium-to-high grade new material for making clothes.
Third, the present invention use multistage drafting, so that viscose rayon internal structure is steady during preparing viscose rayon
Fixed, internal stress is smaller, and the viscose rayon stability prepared is good.
4th, the viscose rayon prepared using production technology of the present invention, section is the porous structure of similar round, more
Pore structure may make the anti-microbial property of viscose rayon, its antibiotic property is enable to retain the 70-80% of raw ramie, so that textile fabric is outstanding
Sag is more preferable, the more soft cunning of feel moistens exquisiteness.
Simple production process of the present invention, mild condition, and produce the viscose rayon degree of polymerization with higher, strength and
Wet modulus, large specific surface area, dye-uptake is high, and elongation at break is high, good toughness；Pollutant is few in sewage effluent, environmentally protective, has
Conducive to environmental protection.
Detailed description of the invention
Fig. 1 is process flow chart of the invention；
Fig. 2 is the preparation technology flow chart of hemp dissolving pulp in the present invention.
Specific embodiment
With reference to the accompanying drawing and specific embodiment is described in further details the present invention；
Embodiment 1:
As shown in Figure 1, 2, a kind of cellulose viscose manufacturing technique based on hemp dissolving pulp, includes the following steps:
(1) prepare raw material: collecting Chinese fiber crops raw material, it is spare；
(2) it prepares Chinese hemp dissolving pulp: enzyme cold dome, oxygen bleaching, washing, drying and processing is carried out to Chinese fiber crops raw material described in step (1),
Prepare Chinese hemp dissolving pulp；
(3) it prepares viscose rayon: the Chinese hemp dissolving pulp prepared in step (2) being crushed, sulfonation, dissolution, maturation, spinning
After silk, drawing-off, refining desulfuration, drying and processing, viscose rayon is obtained, the section of obtained viscose rayon is the more of similar round
Pore structure, antibiotic property can retain the 70-80% of raw ramie.
Wherein, in step (3), sulfonation is handled using wet sulphidization, and in wet sulphidization processing, CS is added2, CS2Plus
Enter the 36% of the mass fraction that amount is Chinese hemp dissolving pulp, controlled at 18 DEG C, time 90min.When dissolution process, temperature is controlled
It is 29 DEG C, time 120min.When drawing-off, by level-one spinning nozzle, second level spinning nozzle, three-level spinning nozzle drawing-off after, formed
Thread, and enter in coagulating bath, it is frozen into strand, refining desulfuration then is carried out to strand, after the strand after refining desulfuration is dry,
Just viscose rayon is prepared.
In step (2), preparing Chinese hemp dissolving pulp, specific step is as follows:
(1), Chinese fiber crops raw material pre-treatment
(1) enzyme cold dome
The sulfuric acid for being 25% by mass fraction, oxalic acid, EDTA-2Na, nonionic surfactant, degumming composite enzyme, dioxygen
Water after mixing, is put into Chinese fiber crops raw material in auxiliary cylinder, impregnates, and time of immersion is 12h, and control bath raio is 1:15, control to
Liquid rate is 80%, cold dome 12h under room temperature, drain；Wherein, the additional amount of sulfuric acid is the 1% of Chinese fiber crops raw material weight, the addition of oxalic acid
Amount is that the additional amount of 1%, EDTA-2Na of Chinese fiber crops raw material weight is the 0.5% of Chinese fiber crops raw material weight, nonionic surfactant
Additional amount be the 1% of Chinese fiber crops raw material weight, the additional amount of degumming composite enzyme is the 0.5% of Chinese fiber crops raw material weight, hydrogen peroxide
Additional amount is the 3% of Chinese fiber crops raw material weight.
(2) oxygen bleaching is handled
The oxygenic bleaching aids for being 5g/L by additional amount, additional amount are the caustic soda of 1g/L, and additional amount is the degumming catalyst of 1g/L,
Additional amount is that the nonionic surfactant of 1g/L is squeezed into saucepan after mixing in auxiliary cylinder, starts to warm up operating, 90 DEG C
When into saucepan be added mass fraction be 27% additional amount be 8g/L hydrogen peroxide, control bath raio be 1:8, operating 55min after,
Drain；
(3) washing neutralizes: being first added neutralizing acid to boiling in drift pot, control pH value is 6.5,40 DEG C of washing 20min, controls and bathes
Than for 1:8, drain is washed 2 times；
(4) sofening treatment: being added the lubricant that additional amount is 5g/L to boiling in drift pot, will boil drift pot and is warming up to 40 DEG C,
After operating 20min, drain；
(5) it dries: half drying and processing finally being carried out to the Chinese fiber crops raw material after the completion of sofening treatment, control water content is
20%；
(6) wet shredding: the Chinese fiber crops raw material after drying is subjected to wet shredding processing, for use；
(2), prepared by pulp
(1) first piece alkali suitable quantity of water is mixed and is melted, be warming up to 55 DEG C, wherein the additional amount of piece alkali is pulp to be prepared
The 7% of weight, water are surplus；
(2) nonionic surfactant is then added, improved plant starch binder, special silicone grease water dispersant stirring is
It is even, 55 DEG C are kept the temperature, wherein the additional amount of nonionic surfactant is the 0.5% of pulp weight to be prepared, improved plant starch
The additional amount of binder is the 0.2% of pulp weight to be prepared, and the additional amount of special silicone grease water dispersant is pulp weight to be prepared
The 0.2% of amount；
(3) it is eventually adding premenstrual treated Chinese fiber crops raw material, 55 DEG C is kept the temperature, stirs 60min, the wherein addition of Chinese fiber crops raw material
Amount is the 3.5% of pulp weight to be prepared；
(4) it dries again, after drying, cake of press finally obtains Chinese hemp dissolving pulp.
Wherein, degumming composite enzyme by being prepared following weight percentage components: zytase: 6%；Cellulase:
2%；Pectase: 20%；Chelated dispersants；44%；Inhibitor: 27%；Nonionic polymer surfactant: 1%.
Oxygenic bleaching aids by being prepared following weight percentage components: anionic surfactant: 20%；Nonionic table
Face activating agent: 4%；Solid oxygen: 25%；Chelated dispersants: 5%；Defoaming agent: 1%；Metasilicate pentahydrate sodium: 45%.
Degumming catalyst by being prepared following weight percentage components: chelated dispersants: 25%；Stabilizer:
69.5%；Nonionic polymer surfactant: 2.5%；Potassium hydroxide solution (mass percentage concentration 50%): 3%.
Lubricant by being prepared following weight percentage components: four ester based quaternary ammonium salts 5%；Polyoxyethylene ether 8809
2.5%；Silicon wax 8%；Silane coupling agent KN-550 4%；Catalyst T-50 2.6%；D4 octamethylcy-clotetrasiloxane 18%；Ice
Acetic acid 1%；Deionized water surplus.
Using the quality index range for the viscose rayon that the production technology in the present invention is produced are as follows: residual sulphur rate≤
0.03%, alpha cellulose >=95.9%, ash content (725 degree)≤0.1%, content≤15mg/kg of iron, whiteness >=81%, suction
Base number are as follows: 560.
Degumming composite enzyme in the present invention, oxygenic bleaching aids, degumming catalyst using can it is more acurrate, to efficiently remove Chinese fiber crops former
Pectin, lignin, water soluble compound on material, and it is very few to the damage of Chinese fiber crops raw material, while sewage treatment load is alleviated, have
Conducive to improvement environment.
Embodiment 2:
As shown in Figure 1, 2, a kind of cellulose viscose manufacturing technique based on hemp dissolving pulp, includes the following steps:
(1) prepare raw material: collecting Chinese fiber crops raw material, it is spare；
(2) it prepares Chinese hemp dissolving pulp: enzyme cold dome, oxygen bleaching, washing, drying and processing is carried out to Chinese fiber crops raw material described in step (1),
Prepare Chinese hemp dissolving pulp；
(3) it prepares viscose rayon: the Chinese hemp dissolving pulp prepared in step (2) being crushed, sulfonation, dissolution, maturation, spinning
After silk, drawing-off, refining desulfuration, drying and processing, viscose rayon is obtained, the section of obtained viscose rayon is the more of similar round
Pore structure, antibiotic property can retain the 70-80% of raw ramie.
Wherein, in step (3), sulfonation is handled using wet sulphidization, and in wet sulphidization processing, CS is added2, CS2Plus
Enter the 38% of the mass fraction that amount is Chinese hemp dissolving pulp, controlled at 20 DEG C, time 100min.When dissolution process, control temperature
Degree is 31 DEG C, time 135min.When drawing-off, by level-one spinning nozzle, second level spinning nozzle, three-level spinning nozzle drawing-off after, shape
At thread, and enter in coagulating bath, be frozen into strand, refining desulfuration then is carried out to strand, the strand after refining desulfuration is dry
Afterwards, viscose rayon is just prepared.
In step (2), preparing Chinese hemp dissolving pulp, specific step is as follows:
(1), Chinese fiber crops raw material pre-treatment
(1) enzyme cold dome
The sulfuric acid for being 25% by mass fraction, oxalic acid, citric acid, nonionic surfactant, degumming composite enzyme, hydrogen peroxide
In auxiliary cylinder after mixing, it is put into Chinese fiber crops raw material, is impregnated, the time of immersion is 18h, and control bath raio is 1:17, is controlled to liquid
Rate is 85%, cold dome 18h, drain under room temperature；Wherein, the additional amount of sulfuric acid is the 2% of Chinese fiber crops raw material weight, the additional amount of oxalic acid
It is the 2% of Chinese fiber crops raw material weight, the additional amount of citric acid is the 1% of Chinese fiber crops raw material weight, the addition of nonionic surfactant
Amount is the 1.5% of Chinese fiber crops raw material weight, and the additional amount of degumming composite enzyme is the 1.2% of Chinese fiber crops raw material weight, the addition of hydrogen peroxide
Amount is the 4% of Chinese fiber crops raw material weight.
(2) oxygen bleaching is handled
The oxygenic bleaching aids for being 6.5g/L by additional amount, additional amount are the caustic soda of 2g/L, and the degumming that additional amount is 2g/L is catalyzed
Agent, additional amount are that the anionic surfactant of 2g/L is squeezed into saucepan after mixing in auxiliary cylinder, start to warm up operating, 92
DEG C when into saucepan be added mass fraction be 27% additional amount be 8-12g/L hydrogen peroxide, control bath raio be 1:11, operate
After 60min, drain；
(3) washing neutralizes: being first added neutralizing acid to boiling in drift pot, control pH value is 7,45 DEG C of washing 20min, control bath raio
For 1:11, drain is washed 2 times；
(4) sofening treatment: being added the lubricant that additional amount is 7.5g/L to boiling in drift pot, will boil drift pot and is warming up to 40
DEG C, after operating 20min, drain；
(5) it dries: half drying and processing finally being carried out to the Chinese fiber crops raw material after the completion of sofening treatment, control water content is
20%；
(6) wet shredding: the Chinese fiber crops raw material after drying is subjected to wet shredding processing, for use；
(2), prepared by pulp
(1) first piece alkali suitable quantity of water is mixed and is melted, be warming up to 57 DEG C, wherein the additional amount of piece alkali is pulp to be prepared
The 9% of weight, water are surplus；
(2) nonionic surfactant is then added, improved plant starch binder, special silicone grease water dispersant stirring is
It is even, 57 DEG C are kept the temperature, wherein the additional amount of nonionic surfactant is the 1.2% of pulp weight to be prepared, improved plant starch
The additional amount of binder is the 0.35% of pulp weight to be prepared, and the additional amount of special silicone grease water dispersant is pulp weight to be prepared
The 0.35% of amount；
(3) it is eventually adding premenstrual treated Chinese fiber crops raw material, 57 DEG C is kept the temperature, stirs 60min, the wherein addition of Chinese fiber crops raw material
Amount is the 4% of pulp weight to be prepared；
(4) it dries again, after drying, cake of press finally obtains Chinese hemp dissolving pulp.
Wherein, degumming composite enzyme by being prepared following weight percentage components: zytase: 7%；Cellulase:
4%；Pectase: 22%；Chelated dispersants: 39%；Inhibitor: 26%；Nonionic polymer surfactant: 2%.
Oxygenic bleaching aids by being prepared following weight percentage components: anionic surfactant: 15%；Nonionic table
Face activating agent: 5%；Solid oxygen: 28%；Chelated dispersants: 10%；Defoaming agent: 2%；Metasilicate pentahydrate sodium: 40%.
Degumming catalyst by being prepared following weight percentage components: chelated dispersants: 35%；Stabilizer:
57.5%；Nonionic polymer surfactant: 3.5%；Potassium hydroxide solution (mass percentage concentration 50%): 4%.
Lubricant by being prepared following weight percentage components: four ester based quaternary ammonium salts 5%；Polyoxyethylene ether 8809
2.5%；Silicon wax 8%；Silane coupling agent KN-550 4%；Catalyst T-50 2.6%；D4 octamethylcy-clotetrasiloxane 18%；Ice
Acetic acid 1%；Deionized water surplus.
Using the quality index range for the viscose rayon that the production technology in the present invention is produced are as follows: residual sulphur rate≤
0.03%, alpha cellulose >=96.2%, ash content (725 degree)≤0.08%, content≤14mg/kg of iron, whiteness >=82%, suction
Base number are as follows: 720.
Degumming composite enzyme in the present invention, oxygenic bleaching aids, degumming catalyst using can it is more acurrate, to efficiently remove Chinese fiber crops former
Pectin, lignin, water soluble compound on material, and it is very few to the damage of Chinese fiber crops raw material, while sewage treatment load is alleviated, have
Conducive to improvement environment.
Embodiment 3:
As shown in Figure 1, 2, a kind of cellulose viscose manufacturing technique based on hemp dissolving pulp, includes the following steps:
(1) prepare raw material: collecting Chinese fiber crops raw material, it is spare；
(2) it prepares Chinese hemp dissolving pulp: enzyme cold dome, oxygen bleaching, washing, drying and processing is carried out to Chinese fiber crops raw material described in step (1),
Prepare Chinese hemp dissolving pulp；
(3) it prepares viscose rayon: the Chinese hemp dissolving pulp prepared in step (2) being crushed, sulfonation, dissolution, maturation, spinning
After silk, drawing-off, refining desulfuration, drying and processing, viscose rayon is obtained, the section of obtained viscose rayon is the more of similar round
Pore structure, antibiotic property can retain the 70-80% of raw ramie.
Wherein, in step (3), sulfonation is handled using wet sulphidization, and in wet sulphidization processing, CS is added2, CS2Plus
Enter the 40% of the mass fraction that amount is Chinese hemp dissolving pulp, controlled at 22 DEG C, time 110min.When dissolution process, control temperature
Degree is 33 DEG C, time 150min.When drawing-off, by level-one spinning nozzle, second level spinning nozzle, three-level spinning nozzle drawing-off after, shape
At thread, and enter in coagulating bath, be frozen into strand, refining desulfuration then is carried out to strand, the strand after refining desulfuration is dry
Afterwards, viscose rayon is just prepared.
In step (2), preparing Chinese hemp dissolving pulp, specific step is as follows:
(1), Chinese fiber crops raw material pre-treatment
(1) enzyme cold dome
The sulfuric acid for being 25% by mass fraction, oxalic acid, EDTA-2Na, nonionic surfactant, degumming composite enzyme, dioxygen
Water after mixing, is put into Chinese fiber crops raw material in auxiliary cylinder, impregnates, and time of immersion is that for 24 hours, control bath raio is 1:20, control to
Liquid rate is 90%, under room temperature cold dome for 24 hours, drain；Wherein, the additional amount of sulfuric acid is the 3% of Chinese fiber crops raw material weight, the addition of oxalic acid
Amount is that the additional amount of 3%, EDTA-2Na of Chinese fiber crops raw material weight is the 1.5% of Chinese fiber crops raw material weight, nonionic surfactant
Additional amount be the 2% of Chinese fiber crops raw material weight, the additional amount of degumming composite enzyme is the 2% of Chinese fiber crops raw material weight, hydrogen peroxide plus
Enter 5% that amount is Chinese fiber crops raw material weight.
(2) oxygen bleaching is handled
The oxygenic bleaching aids for being 8g/L by additional amount, additional amount are the caustic soda of 3g/L, and additional amount is the degumming catalyst of 3g/L,
Additional amount is that the nonionic surfactant of 3g/L is squeezed into saucepan after mixing in auxiliary cylinder, starts to warm up operating, 95 DEG C
When into saucepan be added mass fraction be 27% additional amount be 12g/L hydrogen peroxide, control bath raio be 1:15, operating 65min
Afterwards, drain；
(3) washing neutralizes: being first added neutralizing acid to boiling in drift pot, control pH value is 7,50 DEG C of washing 20min, control bath raio
For 1:15, drain is washed 3 times；
(4) sofening treatment: being added the lubricant that additional amount is 10g/L to boiling in drift pot, will boil drift pot and is warming up to 40 DEG C,
After operating 20min, drain；
(5) it dries: half drying and processing finally being carried out to the Chinese fiber crops raw material after the completion of sofening treatment, control water content is
20%；
(6) wet shredding: the Chinese fiber crops raw material after drying is subjected to wet shredding processing, for use；
(2), prepared by pulp
(1) first piece alkali suitable quantity of water is mixed and is melted, be warming up to 60 DEG C, wherein the additional amount of piece alkali is pulp to be prepared
The 12% of weight, water are surplus；
(2) nonionic surfactant is then added, improved plant starch binder, special silicone grease water dispersant stirring is
It is even, 60 DEG C are kept the temperature, wherein the additional amount of nonionic surfactant is the 1.5% of pulp weight to be prepared, improved plant starch
The additional amount of binder is the 0.5% of pulp weight to be prepared, and the additional amount of special silicone grease water dispersant is pulp weight to be prepared
The 0.5% of amount；
(3) it is eventually adding premenstrual treated Chinese fiber crops raw material, 60 DEG C is kept the temperature, stirs 60min, the wherein addition of Chinese fiber crops raw material
Amount is the 5.5% of pulp weight to be prepared；
(4) it dries again, after drying, cake of press finally obtains Chinese hemp dissolving pulp.
Wherein, degumming composite enzyme by being prepared following weight percentage components: zytase: 9%；Cellulase:
5%；Pectase: 25%；Chelated dispersants: 35%；Inhibitor: 23%；Nonionic polymer surfactant: 3%.
Oxygenic bleaching aids by being prepared following weight percentage components: anionic surfactant: 18.9%；Nonionic
Surfactant: 3.9%；Solid oxygen: 27.2%；Chelated dispersants: 7.2%；Defoaming agent: 1.5%；Metasilicate pentahydrate sodium:
41.3%.
Degumming catalyst by being prepared following weight percentage components: chelated dispersants: 33%；Stabilizer:
60.5%；Nonionic polymer surfactant: 3%；Potassium hydroxide solution (mass percentage concentration 50%): 3.5%.
Lubricant by being prepared following weight percentage components: four ester based quaternary ammonium salts 5%；Polyoxyethylene ether 8809
2.5%；Silicon wax 8%；Silane coupling agent KN-550 4%；Catalyst T-50 2.6%；D4 octamethylcy-clotetrasiloxane 18%；Ice
Acetic acid 1%；Deionized water surplus.
Using the quality index range for the viscose rayon that the production technology in the present invention is produced are as follows: residual sulphur rate≤
0.03%, alpha cellulose >=96%, ash content (725 degree)≤0.1%, content≤20mg/kg of iron, whiteness >=81%, suction alkali
Value are as follows: 620.
Degumming composite enzyme in the present invention, oxygenic bleaching aids, degumming catalyst using can it is more acurrate, to efficiently remove Chinese fiber crops former
Pectin, lignin, water soluble compound on material, and it is very few to the damage of Chinese fiber crops raw material, while sewage treatment load is alleviated, have
Conducive to improvement environment.
Simply to illustrate that technical concepts and features of the invention, its purpose is allows in the art above-described embodiment
Those of ordinary skill cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all
It is the equivalent variation made of essence of content according to the present invention or repairs, should be covered by the scope of protection of the present invention.
Claims (10)
1. a kind of cellulose viscose manufacturing technique based on hemp dissolving pulp, which comprises the steps of:
(1) prepare raw material: collecting crudefiber crop raw material, it is spare；
(2) it prepares hemp dissolving pulp: enzyme cold dome, oxygen bleaching, washing, drying and processing, preparation fiber crops is carried out to crudefiber crop raw material described in step (1)
Pulp；
(3) prepare viscose rayon: the hemp dissolving pulp prepared in step (2) is crushed, sulfonation, dissolution, maturation, spinning, drawing-off,
After refining desulfuration, drying and processing, viscose rayon is obtained.
2. based on the cellulose viscose manufacturing technique of hemp dissolving pulp according to requiring 1, characterized in that in step (2), the system
Specific step is as follows for standby hemp dissolving pulp:
(1) crudefiber crop raw material pre-treatment
(1) enzyme cold dome
The sulfuric acid for being 25% by mass fraction, oxalic acid, metal chelating agent, wetting and penetrating agent, degumming composite enzyme, hydrogen peroxide is in auxiliary cylinder
In after mixing, be put into crudefiber crop raw material, impregnate, control bath raio is 1:15-20, and control is 80-90% to liquid rate, cold under room temperature
Heap 12-24h, drain；
(2) oxygen bleaching is handled
By oxygenic bleaching aids, caustic soda, degumming catalyst, multi-functional processing auxiliary agent squeezes into saucepan after mixing in auxiliary cylinder, opens
Begin heating operating, the hydrogen peroxide that mass fraction is 27% is added at 90-95 DEG C into saucepan, control bath raio is 1:8-1:15, is transported
After turning 55-65min, drain；
(3) washing neutralizes: being first added neutralizing acid to boiling in drift pot, control pH value is 6-7.5,40-50 DEG C of washing 20min, is controlled
Bath raio is 1:8-1:15, and drain is washed 2-3 times；
(4) sofening treatment: being added lubricant to boiling in drift pot, boils drift pot and is warming up to 40 DEG C, after operating 20min, drain；
(5) it dries: half drying and processing finally being carried out to the crudefiber crop raw material after the completion of sofening treatment；
(6) wet shredding: the crudefiber crop raw material after drying is subjected to wet shredding processing, for use；
(2), prepared by pulp
(1) first piece alkali suitable quantity of water is mixed and is melted, be warming up to 55-60 DEG C；
(2) enhancing wetting agent, toughener is then added, dispersion defrother stirs evenly, and keeps the temperature 55-60 DEG C；
(3) it is eventually adding premenstrual treated crudefiber crop raw material, 55-60 DEG C is kept the temperature, stirs 60min；
(4) it dries again, after drying, cake of press finally obtains hemp dissolving pulp.
3. based on the cellulose viscose manufacturing technique of hemp dissolving pulp according to requiring 1, it is characterized in that: in step (3), the sulphur
Change and handled using wet sulphidization, in wet sulphidization processing, CS is added2, controlled at 18-22 DEG C, time 90-
110min, the CS2Additional amount be the hemp dissolving pulp mass fraction 36-40%.
4. based on the cellulose viscose manufacturing technique of hemp dissolving pulp according to requiring 1, it is characterized in that: in step (3), it is described molten
Xie Shi, controlled at 29-33 DEG C, time 120-150min, when the drawing-off, after multistage drafting, formed thread into
Enter in coagulating bath, be frozen into strand, refining desulfuration then is carried out to strand, just obtains viscose rayon after dry.
5. based on the cellulose viscose manufacturing technique of hemp dissolving pulp according to requiring 2, it is characterized in that: the step (1) enzyme cold dome
In treatment process, the additional amount of the sulfuric acid is the 1-3% of crudefiber crop raw material weight, and the additional amount of the oxalic acid is crudefiber crop raw material weight
The 1-3% of amount, the additional amount of the metal chelating agent are the 0.5-1.5% of crudefiber crop raw material weight, and the wetting and penetrating agent adds
Enter the 1-2% that amount is crudefiber crop raw material weight, the additional amount of the degumming composite enzyme is the 0.5-2% of crudefiber crop raw material weight, described
The additional amount of hydrogen peroxide is the 3-5% of crudefiber crop raw material weight.
6. based on the cellulose viscose manufacturing technique of hemp dissolving pulp according to requiring 2, it is characterized in that: at the step (1) oxygen bleaching
In science and engineering skill, the additional amount of the oxygenic bleaching aids is 5-8g/L, and the additional amount of the caustic soda is 1-3g/L, the degumming catalyst
Additional amount be 1-3g/L, the additional amount of the multi-functional processing auxiliary agent is 1-3g/L, and the additional amount of the hydrogen peroxide is 8-
12g/L, in the step (1) sofening treatment technique, the additional amount of the lubricant is 5-10g/L, and the step (1) enzyme is cold
In heap treatment process, after crudefiber crop raw material carries out half drying and processing, control water content is 20%.
7. based on the cellulose viscose manufacturing technique of hemp dissolving pulp according to requiring 2, it is characterized in that: piece alkali described in step (2)
Additional amount be pulp weight to be prepared 7-12%, it is described enhancing wetting agent additional amount be pulp weight to be prepared 0.5-
1.5%, the additional amount of the toughener is the 0.2-0.5% of pulp weight to be prepared, and the additional amount of the dispersion defrother is
The 0.2-0.5% of pulp weight to be prepared, the additional amount of the crudefiber crop raw material are the 3.5-5.5% of pulp weight to be prepared, institute
Water is stated as surplus, in the step (1) enzyme cold dome treatment process, the time of immersion is 12-24h.
8. based on the cellulose viscose manufacturing technique of hemp dissolving pulp according to requiring 2, it is characterized in that: the metal chelating agent includes
EDTA-2Na, one or both of citric acid；The wetting and penetrating agent includes nonionic surfactant, the multi-functional place
Reason auxiliary agent includes one or both of nonionic surfactant, anionic surfactant, and the enhancing wetting agent is non-
Ionic surface active agent, the toughener are improved plant starch binder, and the dispersion defrother is special silicone grease water dispersion
Agent.
9. based on the cellulose viscose manufacturing technique of hemp dissolving pulp according to requiring 5, it is characterized in that: the degumming composite enzyme by
It is prepared following weight percentage components:
Zytase: 6%-9%；
Cellulase: 2%-5%；
Pectase: 20%-25%；
Chelated dispersants: 35%-44%；
Inhibitor: 16%-34%；
Nonionic polymer surfactant: 1%-3%.
10. based on the cellulose viscose manufacturing technique of hemp dissolving pulp according to requiring 6, it is characterized in that: the oxygenic bleaching aids by
It is prepared following weight percentage components:
Anionic surfactant: 15%-20%；
Nonionic surfactant: 4%-5%；
Solid oxygen: 25%-30%；
Chelated dispersants: 5%-10%；
Defoaming agent: 1%-2%；
Metasilicate pentahydrate sodium: 40%-45%.
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| CN111607898A (en) * | 2020-04-26 | 2020-09-01 | 马建伟 | Production process of high-performance composite material based on China hemp fibers |
| CN113062138A (en) * | 2021-04-22 | 2021-07-02 | 山东银鹰股份有限公司 | Preparation method of pulp for preparing viscose fiber from seed hemp |
| CN116200837A (en) * | 2023-03-11 | 2023-06-02 | 山东银鹰化纤有限公司 | China hemp fiber for regenerated seeds and preparation method thereof |
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