CN104928786A - Preparation process of semi-dull high-strength low-elongation viscose fibers - Google Patents

Abstract

The invention provides a preparation process of semi-dull high-strength low-elongation viscose fibers. The preparation process comprises the following steps: firstly immersing and pressing a pulp raw material, then removing an alkaline solution to obtain alkali cellulose, then crushing, kneading and de-polymerizing, by adding pure oxygen, the alkaline cellulose to obtain methylcellulose, yellowing, dissolving, filtering, curing and defoaming the methylcellulose to obtain a spinning solution, charging a dulling agent into the spinning solution to obtain a mixed solution, spinning stretching, refining and drying the mixed solution to obtain the semi-dull high-strength low-elongation viscose fibers. The viscose fibers produced in the preparation process are of a novel fiber type different from ordinary viscose fibers and modal fibers, the product of the viscose fibers not only has the fiber characteristics of the modal fibers such as high strength and low elongation, but also has higher skin adaptability compared with cotton fibers and can effectively substitute the existing differentiated viscose fibers, while the processing performance of a downstream procedure of the viscose cellulose is improved, the development and industry upgrading of novel downstream textile products can be promoted, and the prepared semi-dull high-strength low-elongation viscose fibers can be used for producing various fiber fabrics.

Description

The preparation technology of the high-strength flatness viscose of a kind of half delustring

Technical field

The present invention relates to viscose technical field, particularly the preparation technology of the high-strength flatness viscose of a kind of half delustring.

Background technology

Textile fiber material is mainly divided into the natural fabric raw material for representative such as cotton, numb, the petroleum base fibrous raw material being representative with terylene, acrylic fibers etc., and be the bio-based fibrous raw material such as sky silk, copper ammonia fibre, viscose that raw material regenerates with natural cellulosic materials.Cotton fiber obtains great fame because of qualities such as it are comfortable, soft, ventilative, next to the skin, the market share of about 36% is accounted in whole textile fabric market, but common cotton fiber needs a large amount of water resources and chemical substance because of it, nutritional labeling in taken in excess soil, and whole world various countries ensure that population in the world staple food supply reduces the reasons such as cotton planting soil erosion and makes the plantation of cotton be restricted, cotton fiber material is in short supply, can not meet the needs that people's living standard is growing.Short rayon fiber belongs to native cellulose regenerated fiber, and it not only has the characteristic of cotton fiber, and has the certain advantages of the silk that cotton fiber does not possess; Hygroscopic capacity, then up to 13 ~ 15%, exceeds 6 ~ 7% than cotton fiber, wears more comfortable; The beautiful property that dyes more is better than cotton fiber; Soft, plentiful, smooth, there is the gloss as excellent drapability and silk; By artificially processing and new capability can being given, in gloss, chromatogram, function and required fiber number etc., exceed natural fabric.Short rayon fiber is because of its natural attribute, and the waste and old gurry of its goods can natural degradation, is a kind of environmental protection fiber of function admirable; In addition, short rayon fiber do not play the natural cotton fiber attributes such as electrostatic, sucting wet air permeability, snugness of fit, have very strong substituting to cotton fiber.

Viscose take native cellulose as raw material, makes soluble cellulose sulphonic acid ester through operations such as alkalization, aging, sulfonation, then is dissolved in sig water and makes viscose glue, makes through wet spinning.Adopt different raw materials and spinning technique, common viscose fiber, Modal fibre, differential viscose etc. can be obtained respectively.The fabric fastness that common viscose fiber knits system is poor, and washing shrinkage is higher, elasticity and ABRASION RESISTANCE poor, dress after yielding.Compared with common viscose fiber, Modal fibre has high wet modulus, high strength and low wet expansion, and its density is greater than common viscose fiber, and chance water volume expansion rate is less than common viscose fiber, and washing shrinkage is low; There is good very thin degree, thinner yarn can be spun; Have higher degree of crystallinity and the degree of orientation, make fabric hand fine and smooth soft, skin-friendly is strong, comfortable and easy to wear.Also because Modal fibre has the raw material that above-mentioned advantage makes Modal fibre, the cost of production technology etc. is greatly higher than common viscose fiber; Secondly, the fabric of Modal fibre formation is soft, exoskeletal, conformality is bad, because the fibrillation of Modal fibre is inclined to, once friction, very easily cause fabric napping, balling-up, affect the outward appearance of fabric, in addition, Modal fibre is used in the production of underwear mostly, and products application is limited, therefore can meet people to flexibility and comfortableness demand, the fabric of formation can be made again to have fine conformality, and the fiber product that production cost is low is necessary.

One section of application number be 200910098209.5 Chinese patent disclose a kind of method for manufacturing modal fiber, pass through quaternization successively, experienced reaction, yellow is reacted, the dissolving of viscose glue, the filtration of viscose glue, the deaeration of viscose glue, the maturation of viscose glue, wet spinning, drawing-off and other associated process steps, the cellulose pulp adopting the fine content <95% of first is raw material, use the common equipment that common viscose staple fibre is produced, the special process formula adopting technology controlling and process simple and practical and spinning drawing mode, produce the Modal fibre that can meet international standards.

Based on above-mentioned situation, be the sustainable development promoting viscose industry, producing viscose that is differential, functionalization has become current industry and has newly marked.Application number is that the Chinese patent of CN201010011519.1 discloses a kind of polynosic fibre and production method thereof, be characterised in that it to be mixed with rayon spinning solution by bacteria cellulose and makes viscose, wherein, the content of bacteria cellulose in viscose is 1% ~ 10%.The intensity of the polynosic fibre of this patent adds, but its line density and common viscose fiber are substantially the same, the demand of downstream product to flexibility can not be better met, and this invention adopts bacteria cellulose as one of raw material, at present, bacteria cellulose is mainly used in biological medicine material, it obtains complex process, productive rate is low, cost is higher, so adopt bacteria cellulose to mix the raw material of the high-intensity fiber as this invention with viscose, increase cost greatly, limit large-scale industrialization application.

The production method of a patent document CN102296373A(superfine high-strength high-modulus viscose fiber, 2011.12.28) disclose a kind of viscose that a kind of even structure, fibre strength and modulus exceed conventional variety more than 50%, the fibre strength of obtained viscose be 0.44 ~ 0.78dtex, dry strong >=3.1cN/dtex(li ox/dtex), wet strong >=2.1cN/dtex, wet modulus >=0.5cN/dtex, whiteness >=82.0%.

The high white powerful fine denier viscose staple fiber of patent document CN1632189(mono-kind and production technology thereof, 2005.06.29) short rayon fiber that a kind of fiber number is thin, intensity is high is disclosed, compared with common viscose fiber, there is the advantages such as intensity is high, ABRASION RESISTANCE is strong, feel is fine and smooth, anti-fold, resistance to repeatedly distortion by the garment material of its processing, also can be used for weaving high grade yarn fabric products.

Patent document CN102251301A(production process of ultrafine-denier high-strength viscose fibers, 2011.11.23) disclose the preparation method of the viscose that a kind of fiber number is low, intensity is high, can obtain fiber number is the viscose that 1.11 dtexs and intensity are greater than 2.9 cN/dtex.

Only above-mentioned disclosed patent document can be known, for obtained differential, the viscose of functionalization, prior art is all that the mode by changing production technology realizes, wherein, include raw material, change of the shaping and technological parameter of viscose glue etc., the viscose obtained comparatively common viscose fiber has all carried out suitable optimization in fiber number and intensity, but for day by day fierce market competition, differential viscose does not meet exploitation and the industrial upgrading of downstream new textile to a greater extent, especially the same sky silk taking natural cellulosic materials as raw material and regenerate, model, the development of the fibrous raw materials such as copper ammonia fibre, the occupation rate of market of viscose is reduced increasingly.As: the preparation method of patent document CN101130885(fiber crops material viscose and the numb material viscose of preparation, 2008.02.27) a kind of viscose and the preparation technology thereof that utilize numb material plant production is disclosed, technique is simple, supplies consumption is low, and the numb material viscose produced has excellent whiteness, the performance such as intensity and elongate fiber, the numb material viscose prepared by this technique meets dry fracture strength >=1.820 cN/dtex, wet breaking strength >=1.12 cN/dtex, dry elongation at break >=15.4%, line density deviation ratio ± 6.00%, length variation rate ± 6.00%, overcut fibre rate≤1.0%, over-length fibre≤18.0mg/100g, fault≤11mg/100g, residual sulphur≤18.0mg/100g.

For this reason, we need to find one to be different from natural fabric raw material and petroleum base fibrous raw material, performance is better than again the New Viscose Fibre of differential viscose, the requirement of people to natural prodcuts (as: Modal fibre) can not only be met, industrialized continuous production can also be applicable to, for enterprise brings larger economic benefit, certainly, this is also the inexorable trend of viscose industry energy sustainable development.

Summary of the invention

The object of the present invention is to provide a kind of preparation method of high-strength flatness viscose, this preparation method take pulp as raw material, prepared by viscose glue, viscose is obtained after spinning technique and post processing, in production process, still remain secondary response microscope sectional area, and the ectonexine area ratio at this interface is obviously different from the secondary response vestige of Modal fibre and common viscose fiber, ensure that the viscose prepared has high-strength, the feature of flatness, the viscose prepared by this technique is different from traditional viscose product and cotton is fine, there is the index system being different from common viscose fiber and Modal fibre, it is high-strength that its product not only shows Modal fibre, the fiber characteristics of flatness, also show the skin-friendly that more cotton fibre is stronger, can effectively substitute existing differential viscose, while raising viscose lower procedure processing characteristics, exploitation and the industrial upgrading of downstream new textile can also be promoted, there is good social benefit.Also there is suitable water imbibition and significant fiber skin-friendly simultaneously.

For solving the problems of the technologies described above, the present invention is achieved through the following technical solutions.

Present invention also offers the preparation technology of the high-strength flatness viscose of a kind of half delustring, described step of preparation process is as follows:

The method first pulp material is removed alkali lye after dipping, squeezing to obtain alkali cellulose, then alkali cellulose is fallen to gather obtain methylcellulose through pulverizing, rubbing, orientation, methylcellulose obtains cellulose sulfonate through yellow again, filtration after cellulose sulfonate solubilizer dissolves, maturation, deaeration obtain spinning solution, spinning solution add delustering agent through spinning drawing, refining, dry to obtain viscose of the present invention.

For material pulp: the degree of polymerization of pulp material is 650 ~ 1200.

Pulp can adopt the one or more kinds of combinations in cotton pulp, bamboo pulp, wood pulp, jute pulp.

In order to better implement the present invention, the present invention illustrates preparation method.

A preparation method for half delustring viscose, described method step is as follows:

A, to be impregnated in by cellulose slurry congee and be equipped with in the treating tank of soda bath, after being uniformly mixed, be mixed with the slurry congee (mass percent) that concentration is 3-6%, wherein, dipping uses concentration of lye 110-240g/L, temperature 30-60 DEG C, and dip time is 50-90 minute; Known by actual production, when flooding, if the too high meeting of concentration of lye makes later stage cellulose sulfonic acid fat solubility reduce, cause viscose filtration difficulty, the too low meeting of concentration of lye makes pulp puffed degree too high, squeezing difficulty; It is poly-fast that the too high meeting of alkali liquid temperature causes cellulose to fall, and accelerate side reaction, affect viscose filtration, temperature is too low, and pulp puffed degree is high, squeezing difficulty.It is 110-240g/L, temperature 30-60 DEG C that this processing step controls naoh concentration, ensures that the later stage filters and effectively the carrying out of squeezing process, adopts the impregnation process of this step can improve the content of methylcellulose, production alkali cellulose.

B, flooded after, the slurry congee in treating tank is delivered to squeezer by conveyance conduit and carries out expression separation and obtain alkali cellulose, wherein squeezing multiple is 2.2-2.8.The content squeezing the fine first fibre of alkali in the alkali cellulose obtained is 29%-31%%, the content of the fine alkali of alkali is 16 ± 1%, and in alkali lye, half fine Han Liang≤10g/L, prepares alkali cellulose data with traditional viscose and compare, the alkali cellulose that the present invention obtains half is fine low, and product strength is high.

The material wherein squeezed out is divided into two parts, and a part is mingled with the alkali lye of fiber, impurity, and another part is the solid-state and liquid mixture (i.e. alkali cellulose) being forced out excessive moisture.So by squeezing by being mingled with fiber, the alkali lye of impurity is separated with alkali cellulose;

Be mingled with fiber, impurity alkali lye by filter net type vacuum adsorption machine, fiber and clean alkali lye separation and recovery, remove unnecessary hemicellulose, wherein filter screen adopts 60-120 order, and vacuum is-(0.1-0.4) MPa;

In addition, slurry congee can first grind before squeezing, concrete, can be ground, milling time 10-40 second by a grinder be arranged in the connecting pipe for the treatment of tank and squeezer; Can continue like this to generate alkali cellulose, the impurity such as stripping hemicellulose, lignin, simultaneous grinding can carry out shredding, dispersion to alkali cellulose, thus improves alkalization speed and alkalization rate.

Alkali cellulose is pulverized, rubbing: pulverize squeezing the alkali cellulose fiber obtained through pulverizer, degree of grinding 120-180g/L, carry out obtaining temperature 30-60 DEG C after rubbing process through kneader twin screw device after pulverizing, concentration is the slurry congee of 30-40%, and pulverizing, rubbing can make fiber sub-wire, brooming, reach the cell membrane destroying cellulose fibre, remove the Small molecular in cellulose, thus improve fibrin reaction performance, improve cellulose in conjunction with alkali content, alkali cellulose content reaches 6-8%;

C, the alkali cellulose that step B is prepared add alkali lye be mixed to form concentration be 4-8% starch congee, and be transported to orientation and fall poly-reactor, add the pure oxygen of the 2-10% of reactor volume in reactor, carry out orientation and fall poly-reaction, reaction time 30-60min, in this step, add pure oxygen to carry out oxidation and fall poly-, fall poly-after, the alkali cellulose degree of polymerization reduces to 400-600 by 650-1200, in alkali cellulose, the fine purity of first reaches 98.0-98.5%, can improve 2-3% than traditional handicraft.Orientation is fallen poly-fall more experienced than tradition and is gathered minimizing first fibre loss 3-5%, and molecule falls poly-more even, abundant; Alkali lye adopts NaOH, and concentration is 140-200g/l;

D, the alkali cellulose prepared by step C are delivered in xanthating machine and are reacted with carbon disulfide, and wherein the addition of carbon disulfide is the 25-37% of the fine content of first in alkali cellulose, and the yellow reaction time is 45-50 minute, and temperature is 20-30 DEG C; When practical application, carbon disulfide addition is very few, and yellow reaction is incomplete, filtration difficulty; Carbon disulfide addition is too high, and yellow overreact, accessory substance is more.

The cellulose sulfonate obtained through yellow reaction mixes by a certain percentage with solvent again, stir, grinding, final dissolving obtains cellulose sulfonate solution, the addition of solvent with obtained cellulose sulfonate concentration for 9.0-10.0% is as the criterion, dissolving the solvent used is NaOH, sodium sulfite aqueous solution, its concentration is respectively 25-45 g/L, 5-10 g/L, solution temperature 10-20 DEG C, dissolution time 30-50min, cellulose sulfonate solution more after filtration, deaeration, maturation, final obtained viscosity is 40-45s, degree of ripeness 9.5-12ml, methylcellulose content 8.8-9.0%, containing the spinning solution of alkali 4.5-4.8%, according to the requirement of product to whiteness, add delustering agent mix before spinning solution is sent to spinning machine spinning by injection, delustering agent can select titanium dioxide, is mixed with the aqueous solution use that concentration is 10-15%.

,spinning machine spinning delivered to by the spinning solution that step D is obtained, spinning adopts many baths, low acid, less salt wet spinning technology, specific as follows: by spinning machine shower nozzle extruding spinning liquid, then spinning solution enters a bath and forms tow after one drawing-off, tow through a bath sends into two baths through one drawing machine, three baths sent into by Zai Jing bis-road drawing machine, and the tow after three baths delivers to refinery practice by three road drawing machines; Refining post-drying obtains half delustring viscose;

The spinning coagulation bath that wherein can adopt is composed as follows: a bath consists of: sulfuric acid 90-120g/L, zinc sulfate 8-15g/L, sodium sulphate 220-280g/L, one bath temperature is 40-50 DEG C, acid bath drop: 3-5g/L, two bath composition: temperature 80-90 DEG C, sulfuric acid 18-22g/L, three baths are sulfuric acid, and its temperature is 80-90 DEG C, pH value 1-3;

H, drawing-off: can to adopt step by step, high drawing-off technology, wherein total draft rate controls: 150-200%, and (drawing-off is too high, lousiness is many, and drawing-off is low, and intensity is low,) to be rate be in shower nozzle drawing-off: 50-100%, (drawing-off is low, occurs doubling fault, too high, intensity declines), one degree of draft is: 40-60%, and two road degree of drafts are: 5-15%, (drawing-off is too high, and lousiness is many; Drawing-off is low, and intensity declines), the degree of draft of three road drawing machines is 5 ~ 15%.

Wherein refining process comprises: by strand through desulfurization, bleach, oil after obtain half delustring viscose, benign environment is taked to carry out desulfurization, bleaching, reduce post processing to damage strand strength and elongation, desulfurizing agent is vulcanized sodium and the mixing of sodium carbonate, the concentration of vulcanized sodium is 4-8 g/L, sodium carbonate 1-4 g/L, desulfurization temperature 50-55 DEG C, time 2-3min; Adopt vulcanized sodium as desulfurizing agent, comparatively NaOH, sodium sulfite are gentleer, during sodium carbonate is used for and the sulfuric acid that brings of strand.

Adopt hydrogen peroxide bleaching, hydrogen peroxide concentration is 0.3-0.6g/L, temperature 50-55 DEG C, and bleaching time is 1-2min, and comparatively the bleaching agent such as clorox is gentleer for hydrogen peroxide;

Oiling treatment: the finish addition of oiling treatment is 7-9g/l, and finish temperature is 50-55 DEG C, reconciles strand pH value after oiling treatment within the scope of 6.5-7; Within the scope of this pH, finished product strand strength and elongation can not affect, can by washing, multiple-effect acid (organic acid) adjust ph.

Dry: Tumble Dry, bake out temperature 75-115 DEG C, after oven dry, obtains finished product.

beneficial effect:

1, compared with common viscose fiber of the prior art, Modal fibre, differential viscose, half delustring viscose of the present invention, its fiber product intensity can reach 3.6cn/dtex, its rheobase instinct and Modal fibre match in excellence or beauty, higher than common viscose fiber intensity by about 30%, simultaneously its wet elongation at break is lower than Modal fibre, make its fabric comparatively Modal fibre fabric have more conformality; The present invention half delustring viscose has more suitably water swelling rate, makes its skin-friendly more be better than Modal fibre; Also more soft; Product moisture absorption, good permeability, pro-skin is comfortable, is better than model, dyes with under process conditions, and inhale color depth than model, dye-uptake is higher, uniformity is better, and finished product COLOR FASTNESS is good.Meet downstream product to intensity, skin-friendly, the multiple requesting of flexibility, obtains compared with the viscose that partial properties improves with prior art by feedstock optimization and process optimization, viscose product quality of the present invention has had the lifting of matter, is new products innovation.

Viscose of the present invention has the secondary response interface different from common viscose fiber and Modal fibre, fibre section is done after fiber is dyed, the fibre section of the viscose that the present invention relates to shows clear, obvious secondary response microscope sectional area, and the inclined internal layer in interface, ratio is moderate, inside and outside layer " area " ratio is respectively (40 ~ 70): (30 ~ 60), ensure that this viscose product has feature that is high-strength, flatness, also have suitable water imbibition, fiber skin-friendly has significant advantage simultaneously.

The inventive method is raw materials for production with natural cellulosic materials, and the viscose prepared is the same with cotton fibre, Modal fibre etc., is degradable fibrous material, meets the requirement of people to environmental protection.

2, the present invention is reasonable in design, in the production process of identical viscose product, the aspects such as the present invention chooses from raw material, preparation process amelioration, the production cost of the reduction viscose product of high degree, it is lower than model requirement that product of the present invention prepares the fine content of first, therefore can reduce pulp consumption, reduce cost of material; The acid bath composition that the present invention optimizes and draft process, the controling parameters of each process of overall balance can be accomplished, and it is appropriate, its price is low 4000 ~ 5000 yuan/ton compared with Modal fibre, significantly can reduce downstream raw material use cost, can be used for that family is spun, nonwoven fabric etc., particularly underwear and facial mask, hygenic towelette etc., for down-stream enterprises such as spinning, weave cotton cloth brings more high added value and wide market prospects, the market competitiveness of remarkable enterprise.

3, for guaranteeing that high-strength flatness viscose secondary response interface has suitable cortex, sandwich layer ratio, the present invention, from technology, has accomplished improvement acid bath technique, as reduced sulfuric acid concentration, sluggish, improves skin thickness; Change viscose glue index, as viscose ripening degree, the fine index such as content, alkali content of first.

4, compared with adhering process of the prior art, the alkali cellulose hemicellulose level that the present invention obtains is low, we know: hemicellulose refers to that the degree of polymerization is at the beta cellulose of 50 ~ 200 and the gamma-cellulose of degree of polymerization < 50, as long as the impact of hemicellulose has the following aspects: a. affects the uniformity of alkali cellulose; B. ageing time is extended; C. the yellowing rate of hemicellulose is more fine than first fast, consumes a certain amount of carbon disulfide, causes alkali cellulose esterification to reduce, and the solubility of sulphonic acid ester reduces; D. affect the filtration of viscose glue, the solubility of sulphonic acid ester reduces, and the potential aldehyde radical of its end is oxidized to metal ion in carboxyl and ash content as ferrous ion, manganese ion, calcium ion, magnesium ion, form the complex compound that viscosity is extremely strong, cause viscose filtration difficulty, yield poorly; E. hemicellulose is more, and the physical and mechanical properties of viscose is poorer.The present invention passes through grinding mill, can grind the slurry congee sending into squeezer in advance, milling time is 10 ~ 40s, by the slurry congee after grinding with after squeezer squeezing, be separated and obtain mixed alkali liquor and alkali cellulose, containing hemicellulose and other impurity in mixed alkali liquor, pulverize through pulverizer, the multiple of squeezing is 2.2 ~ 2.8, degree of grinding is 120-180g/L, the present invention passes through tube mill, can roll the slurry congee sending into squeezer in advance, pass through mechanism, fiber can be carried out tearing and discongesting, to improve the reactivity worth of slurry congee, ensure carrying out smoothly of viscose production, prepare alkali cellulose data with traditional viscose to compare, alkali cellulose half fibre that the present invention obtains is lower, half fine Han Liang≤10g/L, product strength is higher.

5, the present invention is through large quantity research, directed degrading and polymerizing technology is adopted to replace traditional experienced technique first, and draw and specifically fall poly-parameter, add oxygen by the present invention to carry out oxidation and fall poly-, fall after gathering, the alkali cellulose degree of polymerization reduces to 400-600 by 650-1200, and the fine purity of first reaches 98.0-98.5%, and the fine content of first can improve 2-3% than traditional handicraft.Than traditional experienced technique minimizing first fibre loss 3-5%, molecule falls poly-more even, abundant; Reduce production cost.

6, yellow of the present invention and spinning technique more environmental protection, energy-conservation, in large-scale industrial production, during model production yellow, carbon disulfide consumption is up to about 35% (calculating with the fine content of first), and carbon disulfide consumption only about 30% (fine to first) during yellow of the present invention, can effectively reduce costs and reduce air pollution;

During model spinning, acid bath adopts high zinc sulfate, low sodium sulphate to combine, and it is serious that high zinc sulfate can lead heavy metal pollution of water body, and low sodium sulphate then can cause its acid bath evaporation crystallization energy consumption high.The present invention is compatibility acid bath composition again, as a bath adopts sulfuric acid 90-120g/L, zinc sulfate 8-15g/L, sodium sulphate 220-280g/L forms, while guarantee acid bath effect, overturn the high zinc sulfate of traditional acid bath, the constituent of low sodium sulphate completely, avoid the problem of heavy metal pollution of water body and acid bath evaporation crystallization;

7, in spinning technique of the present invention, tow is by many baths, low acid, less salt wet spinning technology, simultaneously, in conjunction with step by step, high drawing-off technology carries out spinning, one degree of draft is 50 ~ 100%, two road degree of drafts be 40 ~ 60%, three road degree of drafts is 5 ~ 15%, is more conducive to the fragility improving fiber, the degree of stretching of fiber is improved, show: produce the intensity >=0.55cN/dtex needed for 5% percentage elongation under wet condition, dry elongation at break is 11.0 ~ 16.0%.Viscose comparatively Modal fibre has more spinnability, and therefore spin scooter about 50 meters/minutes, and model only has about 30 meters/minutes, production efficiency is high, reduces production cost.

Accompanying drawing explanation

Fig. 1 is the fibre section cross section of high-strength flatness viscose of the present invention.

Fig. 2 is the fibre section cross section of model.

Fig. 3 is the fibre section cross section of sky silk.

Detailed description of the invention

The present invention is described in detail below in conjunction with specific embodiment.

It should be noted that, it is all exemplary for below describing in detail, be intended for the requested to provide further explanation of the invention, except as otherwise noted, all technology used herein and scientific terminology have the identical meanings usually understood with general technical staff of the technical field of the invention.

The each desired value of following examples of the present invention measures by following standard, is applicable to the mensuration that linear density range is 0.8dtex ~ 1.67dtex viscose:

Index determining: the assay method of dry fracture strength is GB/T 14337, the assay method of wet breaking strength is GB/T 14337, the intensity produced under wet condition needed for 5% percentage elongation is completed by GB/T 14337, the assay method of dry elongation at break is GB/T 14337, the assay method of line density deviation ratio is GB/T 14335, the assay method of length variation rate is GB/T 14336, the assay method of overcut fibre rate is GB/T 14336, the assay method of over-length fibre is GB/T 14336, the assay method of fault is GB/T 14339, the assay method of whiteness is FZ/T 50013, the assay method of residual sulphur is FZ/T 50014, the assay method of radial water swelling capacity is GB/T 6503.

Embodiment 1

The preparation technology of the high-strength flatness viscose of a kind of half delustring, described processing step is as follows: first pulp material is removed alkali lye after dipping, squeezing and obtain alkali cellulose, then by alkali cellulose through pulverize, crumple, add pure oxygen orientation fall poly-after obtain methylcellulose, methylcellulose obtains cellulose sulfonate through yellow again, filtration after cellulose sulfonate solubilizer dissolves, maturation, deaeration obtain spinning solution, and spinning solution adds delustering agent and obtain the high-strength flatness viscose of half delustring after spinning drawing, refining, oven dry.Grab sample detection perform index, the half delustring viscose of the present embodiment has following train diagram adjusting:

Dry fracture strength is 3.12 cN/dtex, and wet breaking strength is 1.65cN/dtex,

The intensity produced under wet condition needed for 5% percentage elongation is 0.55cN/dtex,

Dry elongation at break 19.0%, wet elongation at break 21.0%,

Degree of crystallinity is 40%, and radial water swelling capacity is 22%, dulling agent content 0.1%,

Line density deviation ratio is-11.0%, and residual sulphur is 8.0mg/100g,

Length variation rate is-11.0%, overcut fibre rate 0.48%, and whiteness is 84.1%,

Over-length fibre is 4.0mg/100g, and fault is 3.8.0mg/100g.

Embodiment 2

The half delustring viscose of the present embodiment and the difference of embodiment 1 are: the present embodiment has following index:

Dry fracture strength is 3.15 cN/dtex, and wet breaking strength is 1.67cN/dtex,

The intensity produced under wet condition needed for 5% percentage elongation is 0.54cN/dtex,

Dry elongation at break is 18.9%, and wet elongation at break is 20.8%,

Degree of crystallinity 40%, radial water swelling capacity is 22.5%, dulling agent content 0.3%,

Whiteness 84.6%, line density deviation ratio is-10.0%, and residual sulphur is 8.0mg/100g,

Length variation rate is+10.0%, and overcut fibre rate is 0.5%,

Over-length fibre is 4.0mg/100g, and fault is 4.0mg/100g.

Embodiment 3

The half delustring viscose of the present embodiment and the difference of embodiment 1 are: the present embodiment has following index:

Dry fracture strength is 3.25 cN/dtex, and wet breaking strength is 1.7.cN/dtex,

The intensity produced under wet condition needed for 5% percentage elongation is 0.60cN/dtex,

Dry elongation at break is 17.5%, and wet elongation at break is 18.0%,

Degree of crystallinity 43%, radial water swelling capacity is 22.8%, dulling agent content 0.75%,

Whiteness 84.6%, line density deviation ratio is-5.0%, and residual sulphur is 6.8mg/100g,

Length variation rate is-5.0%, and overcut fibre rate is 0.45%,

Over-length fibre is 3.8mg/100g, and fault is 1.0mg/100g.

Embodiment 4

The difference of the present embodiment and embodiment 1 is: the present embodiment further determined that the degree of polymerization and preferred raw material type of preparing pulp material used, obtain through practical studies, the degree of polymerization of pulp material is better with 800 ~ 1200, pulp material adopts the one or more kinds of arbitrary proportion combinations in cotton pulp, bamboo pulp, wood pulp, jute pulp better, this enforcement select the degree of polymerization be 650 ~ 1200 cotton pulp and bamboo pulp, used in combination in the ratio of 1:1.The fiber sampling and measuring index obtained by the present embodiment.

Embodiment 5

In order to better implement the present invention, the present invention improves the preparation method of the present invention half delustring viscose further, and its concrete steps are as follows:

A: be impregnated in by pulp material and be equipped with in the treating tank of alkali lye, makes the slurry congee that concentration is 3% by grinder after being ground; Pulp material adopt the degree of polymerization be 650 ~ 1200 bamboo pulp and wood pulp used in combination in the ratio of 1:1;

B: squeezer delivered to by the slurry congee that steps A is obtained, delivers to pulverizer and pulverizes after squeezing, obtains alkali cellulose, this alkali cellulose is delivered to kneading machine, obtains the slurry congee that concentration is 30% after process;

C: deliver to reactor after mix with alkali lye by slurry congee obtained for step B, add pure oxygen in the reactor, fall poly-after the acquisition degree of polymerization be 400 ~ 600, first fibre purity is the alkali cellulose of 98.0 ~ 98.5%;

D: the alkali cellulose that step C is obtained delivers to xanthating machine, adds carbon disulfide in xanthating machine, after yellow reaction, the cellulose sulfonate that chrysanthemum is obtained by reacting and dissolution with solvents, obtained concentration is the cellulose sulfonate solution of 9.0%;

E: by cellulose sulfonate solution obtained for step D after filtration, deaeration, obtain spinning solution after maturation, spinning solution adds delustering agent obtained viscose after spinning drawing, refining, oven dry.

Embodiment 6

The difference of the present embodiment and embodiment 5 is, the present embodiment further improves dipping, grinding technics, and adopt the sodium hydroxide solution of concentration 110g/L during dipping, the temperature of steeping liquor is 30 DEG C, and dip time is 50min.It is 4% that the slurry congee concentration made after grinding controls.

Embodiment 7

Be with the difference of embodiment 5, grinder is arranged on the pipeline of connection treating tank and squeezer by the present embodiment, slurry congee has flooded and has ground, milling time is 10s, it is 5% that slurry congee concentration obtained after grinding controls, and the temperature of slurry congee controls to be 30 DEG C, and the connecting pipe for the treatment of tank and squeezer establishes grinder, easy to operate, efficiency is high.

Embodiment 8:

The difference of the present embodiment and embodiment 5 is: the present embodiment further improves squeezing process and disintegrating process, and determine pressing temperature, squeezing multiple and degree of grinding, the pressing temperature of the present embodiment is 57 DEG C; Squeezing multiple is 2.2; Degree of grinding is 120g/L

The slurry congee concentration that the present embodiment grinding obtains controls to be 6%, and after squeezing, obtained congee concentration of starching controls to be 35%

Embodiment 9

The difference of the present embodiment and embodiment 5 is: the present embodiment further improves degrading and polymerizing technology: determine lye type and concentration thereof, the addition of pure oxygen, the time of poly-reaction falls, the alkali lye of the present embodiment adopts concentration to be the sodium hydroxide solution of 140g/l, pure oxygen addition is 2% of reactor volume, and falling the poly-reaction time is 30min.

Embodiment 10:

The difference of the present embodiment and embodiment 5 is: the present embodiment further improves yellow technique, determine the addition of carbon disulfide in yellow reaction, the yellow reaction time, yellow temperature, the present embodiment yellow reaction carbon disulfide addition is 30% of the fine content of first in the alkali cellulose obtained after squeezing disintegrating process, the yellow time is 45min, and yellow reaction temperature is 20 DEG C.

Embodiment 11

The difference of the present embodiment and embodiment 5 is: the present embodiment further improves the dissolution process of the cellulose sulfonate obtained after yellow is reacted, determine dissolving solvent, solution temperature and dissolving required time, the mixing of the present embodiment solvent is concentration to be 25 g/L sodium hydroxide solutions and concentration the be sodium sulfite aqueous solution of 5 g/L, solution temperature is 10 DEG C, and dissolution time is 30min.

Embodiment 12

The difference of the present embodiment and embodiment 5 is: the present embodiment further improves spinning drawing technique, determines coagulating bath technical parameter, drafting step parameter that in spinning concrete steps and spinning process, acid bath uses.The spinning drawing technique of the present embodiment is as follows:

F: by cellulose sulfonate solution after filtration, deaeration, deliver to spinning machine after maturation, after a bath, form tow by the shower nozzle extruding spinning thread of spinning machine, the coagulating bath that a described bath uses comprises the zinc sulfate of the sulfuric acid of 90g/L, the sodium sulphate of 220g/L and 8g/L;

G: the tow after a bath sends into two baths by one drawing machine, the coagulating bath that described two baths use comprises the sulfuric acid of 18g/L, and the degree of draft of described one drawing machine is 50%;

H: the tow after two baths sends into three baths by two road drawing machines, the coagulating bath that described three baths use comprises the sulfuric acid that pH value is 1, and the degree of draft of described two road drawing machines is 40%;

I: the tow after three baths delivers to post processing part by three road drawing machines, and the degree of draft of described three road drawing machines is 5%.

A described bath temperature is 40 DEG C, two bath temperatures are 80 DEG C, three bath temperatures are 80 DEG C.

Embodiment 13

The difference of the present embodiment and embodiment 5 is, the present embodiment further improves refinery practice, refining comprises desulfurization that the tow that formed spinning drawing carries out, bleaches and oil, and the desulfurizing agent that described desulfurization uses is made up of the sodium carbonate of concentration to be the vulcanized sodium of 4g/L and concentration be 1g/L; The hydrogen peroxide that the bleaching agent that described bleaching uses is concentration 0.3g/L; The described finish addition used that oils is 7g/L, and after oiling, the pH value of tow is 6.5.

Described desulfurization temperature is 50 DEG C, and desulfurization time is 2min; Described bleaching temperature is 50 DEG C, and bleaching time is 1min; The temperature of described finish is 50 DEG C.

Embodiment 14

The present embodiment be with the difference of embodiment 5, the present embodiment further improves stoving process, and the oven dry of the present embodiment is that tow refining obtained makes to Tumble Dry, and bake out temperature is 75 DEG C.

Embodiment 15

In order to better implement the present invention, the present embodiment provides the preferred preparation method of viscose of the present invention further,

Described method step is as follows:

A, dipping: smashed by pulp material, impregnated in and be equipped with in the treating tank of soda bath, after being uniformly mixed, is mixed with the slurry congee that concentration is 4%, and wherein, dipping uses concentration of lye 150g/L, temperature 40 DEG C, and dip time is 60 minutes; Material pulp: adopt that the degree of polymerization is the cotton pulp of 650-1200, bamboo pulp, wood pulp use with the ratio combination of 1:2:1.

B, flooded after, the slurry congee in treating tank is sent to be arranged on and connects treating tank and the ducted grinder of squeezer and grind, grind after 20 seconds; Be delivered to squeezer by conveyance conduit to carry out expression separation and obtain alkali cellulose, wherein squeezing multiple is 2.5, and pressing temperature is 60 DEG C.Pulverize squeezing the alkali cellulose fiber obtained through pulverizer, degree of grinding 140g/L, carrying out the obtained temperature of rubbing process through kneader twin screw device after pulverizing is 40 DEG C, concentration is the slurry congee of 32%, and rubbing process can make fiber sub-wire, brooming, reaches the cell membrane destroying cellulose fibre, remove the Small molecular in cellulose, thus improve fibrin reaction performance, improve cellulose in conjunction with alkali content, alkali cellulose content reaches 6-8%;

In order to regain alkali lye, in the present embodiment, squeeze out point to be mingled with fiber, impurity alkali lye by filter net type vacuum adsorption machine, fiber and clean alkali lye separation and recovery, remove unnecessary hemicellulose, wherein filter screen adopts 60 orders, and vacuum is-0.2MPa;

C, the slurry congee prepared by step B add alkali lye to be mixed to form concentration are 6% slurry congee, and are transported to orientation and fall poly-reactor, add the pure oxygen of 5% of reactor volume, carry out orientation and fall poly-reaction, reaction time 50min in reactor; In this step, add pure oxygen and carry out oxidation and fall poly-, fall poly-after, the alkali cellulose degree of polymerization reduces to 400-600 by 650-1200, and in alkali cellulose, the fine purity of first reaches 98.0-98.5%, can improve 2-3% than traditional handicraft.Orientation is fallen poly-fall more experienced than tradition and is gathered minimizing first fibre loss 3-5%, and molecule falls poly-more even, abundant; Alkali lye adopts NaOH, and concentration is 160g/l;

D, by step C through falling poly-after alkali cellulose add in xanthating machine and react with carbon disulfide, wherein the addition of carbon disulfide is 28% of the fine content of first in alkali cellulose, and the yellow time is 48 min, and yellow reaction temperature is 25 DEG C, rear obtained cellulose sulfonate has been reacted in yellow, then cellulose sulfonate and solvent are carried out mix and blend by a certain percentage, grinding, final dissolving obtains cellulose sulfonate solution, the addition of solvent is 9.5% to be as the criterion with obtained cellulose sulfonate concentration, solvent is sodium hydrate aqueous solution and sodium sulfite aqueous solution mixed liquor, its concentration is respectively 30 g/L, 8 g/L, solution temperature is 15 DEG C, dissolution time is 35min, cellulose sulfonate solution more after filtration, deaeration, maturation, final obtained viscosity is 40-45s, degree of ripeness is 9.5-12ml, methylcellulose content is 8.8-9.0%, be the spinning solution of 4.5-4.8% containing alkali,

According to the requirement of product, add delustering agent mix before spinning solution is sent to spinning machine spinning by injection, delustering agent can select titanium dioxide, is mixed with the aqueous solution use that concentration is 12%;

E, spinning solution obtained for step (D) is delivered to spinning machine, by spinning machine shower nozzle extruding spinning liquid, then spinning solution enters a bath and forms tow after one drawing-off, tow through a bath sends into two baths through one drawing machine, three baths sent into by Zai Jing bis-road drawing machine, and the tow after three baths delivers to refinery practice by three road drawing machines;

The coagulation bath composition of the spinning acid bath wherein used is as follows: a bath consists of: sulfuric acid 90g/L, zinc sulfate 8g/L, sodium sulphate 220g/L, and a bath temperature is 40 DEG C, acid bath drop is 3g/L, two bath compositions: temperature is 80 DEG C, sulfuric acid 18g/L, three baths are sulfuric acid, and its temperature is 80 DEG C, pH value 1;

Wherein draft process adopt step by step, high drawing-off technology, wherein total draft rate controls: 150%, and to be rate be in shower nozzle drawing-off: 50%, and one degree of draft is: 40%, two road degree of drafts are: the degree of draft of 5%, three road drawing machines is 5%.

Wherein refinery practice be by strand through desulfurization, bleach, oil after obtain half delustring viscose, the present embodiment takes benign environment to carry out desulfurization, bleaching, reduce post processing strand strength and elongation is damaged;

Wherein desulfurizing agent is vulcanized sodium and the mixing of sodium carbonate, and the concentration of vulcanized sodium is 4 g/L, sodium carbonate 1 g/L, and desulfurization temperature is 50 DEG C, and the time is 2min; Adopt vulcanized sodium as desulfurizing agent, comparatively NaOH, sodium sulfite are gentleer, during sodium carbonate is used for and the sulfuric acid that brings of strand;

Adopt hydrogen peroxide bleaching: hydrogen peroxide concentration is 0.3g/L, and temperature is 50 DEG C, and bleaching time is 1min, comparatively the bleaching agent such as clorox is gentleer for hydrogen peroxide;

Oiling treatment: finish addition is 7g/l, and finish temperature is 50 DEG C, regulates the pH value of strand to be 6.5 after oiling treatment.PH value is 6.5, and finished product strand strength and elongation can not affect.PH can be regulated by washing;

Dry: the strand after refining Tumblies Dry, and bake out temperature is 75 DEG C, after oven dry, obtains product.The each desired value of sampling and measuring product.

Embodiment 16

The difference of the present embodiment and embodiment 15 is:

Raw material is distinguished: the pulp material of the present embodiment adopts the cotton pulp of degree of polymerization 650-1200, bamboo pulp, wood pulp, jute pulp to use with the ratio combination of 1:2:2:1.

Process distinction:

Be 6% in dipping time control slurrying congee concentration, alkali lye naoh concentration is 200g/L, and alkali liquid temperature is 50 DEG C, and dip time is 70 minutes.

Squeezing multiple during squeezing is 2.7, and pressing temperature is 61 DEG C, and milling time is 30 seconds;

During pulverizing, control degree of grinding be 120-180g/L, pulverize after slurry congee concentration control be 38%, temperature is 45 DEG C;

Alkali cellulose after rubbing adds alkali lye, and to be mixed to form concentration be 7% slurry congee;

When falling poly-, pure oxygen addition is 5% of reactor volume, and the reaction time is 45min, and alkali lye naoh concentration is 180g/l;

During yellow, the addition of carbon disulfide is 25% of the fine content of first in alkali cellulose, and the yellow time is 50 minutes, and yellow reaction temperature is 30 DEG C.

The dissolving of cellulose sulfonate: the addition of solvent is 10.0% to be as the criterion with obtained cellulose sulfonate concentration, the mixing of solvent to be concentration the be 40 g/L NaOH water aqueous solution and 10 g/L sodium sulfite aqueous solutions, solution temperature is 20 DEG C, and dissolution time is 50min

Spinning a: bath consists of: sulfuric acid 110g/L, zinc sulfate 12g/L, sodium sulphate 260g/L, and temperature is 45 DEG C; Acid bath drop is 4g/L; Two bath compositions: temperature is 85 DEG C, sulfuric acid 20g/L, three baths are sulfuric acid, and its temperature is 85 DEG C, pH value 2;

Drawing-off: wherein total draft rate controls is 180%, and shower nozzle drawing-off is rate is 80%, the degree of draft of one degree of draft to be 50%, two road degree of drafts be 10%, three road drawing machines is 10%.

Concise: the concentration of vulcanized sodium is 6 g/L, and concentration of sodium carbonate is 2 g/L, and desulfurization temperature is 52 DEG C, and the time is 2.5min; Bleaching hydrogen peroxide concentration is 0.5g/L, and temperature is 53 DEG C, and bleaching time is 2min, oiling treatment, and the finish addition oiled is 8g/l, and finish temperature is 52 DEG C.Reconciling strand pH value after oiling is 6.8; Strand pH value is regulated by organic acid,

Dry: Tumble Dry, bake out temperature is 85 DEG C, after oven dry, each desired value of sampling and measuring.

Embodiment 17

The difference of the present embodiment and embodiment 16 is:

Raw material is distinguished: the pulp material of the present embodiment adopts the degree of polymerization to be the cotton pulp of 650-1200;

Process distinction:

Be 3% in dipping time control slurrying congee concentration, alkali lye naoh concentration is 180g/L, and alkali liquid temperature is 60 DEG C, and dip time is 80 minutes.

Squeezing multiple during squeezing is 2.8, and pressing temperature is 63 DEG C, and milling time is 40 seconds;

During pulverizing, control degree of grinding be 180g/L, pulverize after slurry congee concentration control be 40%, temperature is 60 DEG C;

Alkali cellulose after rubbing adds alkali lye, and to be mixed to form concentration be 8% slurry congee;

When falling poly-, pure oxygen addition is 10% of reactor volume, and the reaction time is 60min, and alkali lye naoh concentration is 200g/l;

During yellow reaction, the addition of carbon disulfide is 37% of the fine content of first in alkali cellulose, and the yellow time is 45-50 minute, and yellow reaction temperature is 30 DEG C.

The dissolving of cellulose sulfonate: the addition of solvent is 9.5% to be as the criterion with obtained cellulose sulfonate concentration, the mixing of solvent to be concentration the be 45 g/L NaOH water aqueous solution and 10 g/L sodium sulfite aqueous solutions, solution temperature is 20 DEG C, and dissolution time is 50min

Spinning a: bath consists of: sulfuric acid 120g/L, zinc sulfate 15g/L, sodium sulphate 280g/L, and temperature is 50 DEG C; Acid bath drop is 5g/L; Two bath compositions: temperature is 90 DEG C, sulfuric acid 22g/L, three baths are sulfuric acid, and its temperature is 90 DEG C, pH value 3;

Drawing-off: wherein total draft rate controls is 200%, and shower nozzle drawing-off is rate is 100%, the degree of draft of one degree of draft to be 60%, two road degree of drafts be 15%, three road drawing machines is 15%.

Concise: the concentration of vulcanized sodium is 8 g/L, and concentration of sodium carbonate is 4 g/L, and desulfurization temperature is 55 DEG C, and the time is 3min; Bleaching hydrogen peroxide concentration is 0.6g/L, and temperature is 55 DEG C, and bleaching time is 2min, oiling treatment, and the finish addition oiled is 9g/l, and finish temperature is 55 DEG C.Reconciling strand pH value after oiling is 7; Strand pH value can be regulated by washing, multiple-effect acid (organic acid),

Dry: Tumble Dry, bake out temperature is 115 DEG C, after oven dry, each desired value of sampling and measuring.

Embodiment 18

The difference of the present embodiment and embodiment 16 is:

Raw material is distinguished: the pulp material of the present embodiment adopts the degree of polymerization to be the bamboo pulp of 650-1200.

Process distinction:

Be 4.5% in dipping time control slurrying congee concentration, alkali lye naoh concentration is 150g/L, and alkali liquid temperature is 48 DEG C, and dip time is 75 minutes.

Squeezing multiple during squeezing is 2.5, and pressing temperature is 60 DEG C, and milling time is 25 seconds;

During pulverizing, control degree of grinding be 120-180g/L, pulverize after slurry congee concentration control be 35%, temperature is 45 DEG C;

Alkali cellulose after rubbing adds alkali lye, and to be mixed to form concentration be 5% slurry congee;

When falling poly-, pure oxygen addition is 8% of reactor volume, and the reaction time is 45min, and alkali lye naoh concentration is 190g/l;

During yellow reaction, the addition of carbon disulfide is 35.5% of the fine content of first in alkali cellulose, and the yellow time is 45 minutes, and yellow reaction temperature is 25 DEG C.

The dissolving of cellulose sulfonate: the addition of solvent is 9.5% to be as the criterion with obtained cellulose sulfonate concentration, the mixed liquor of solvent to be concentration the be 35 g/L NaOH water aqueous solution and 7.5 g/L sodium sulfite aqueous solutions, solution temperature is 15 DEG C, and dissolution time is 40min

Spinning a: bath consists of: sulfuric acid 110g/L, zinc sulfate 12g/L, sodium sulphate 240g/L, and temperature is 45 DEG C; Acid bath drop is 4g/L; Two bath compositions: temperature is 85 DEG C, sulfuric acid 20g/L, three baths are sulfuric acid, and its temperature is 85 DEG C, pH value 2.5;

Drawing-off: wherein total draft rate controls is 170%, and shower nozzle drawing-off is rate is 75%, the degree of draft of one degree of draft to be 55%, two road degree of drafts be 12%, three road drawing machines is 12%.

Concise: the concentration of vulcanized sodium is 6 g/L, and concentration of sodium carbonate is 3 g/L, and desulfurization temperature is 54 DEG C, and the time is 3min; Bleaching hydrogen peroxide concentration is 0.5g/L, and temperature is 52 DEG C, and bleaching time is 2min, oiling treatment, and the finish addition oiled is 7g/l, and finish temperature is 50 DEG C.Reconciling strand pH value after oiling is 7; Strand pH value can be regulated by washing, multiple-effect acid (organic acid),

Dry: Tumble Dry, bake out temperature is 100 DEG C, after oven dry, each desired value of sampling and measuring.

Embodiment 19

The difference of the present embodiment and embodiment 16 is:

Raw material is distinguished: the pulp material of the present embodiment adopts the cotton pulp of 650-1200, bamboo pulp, wood pulp, jute pulp used in combination in the ratio of 2:3:1:3.

Process distinction:

Be 5% in dipping time control slurrying congee concentration, alkali lye naoh concentration is 140g/L, and alkali liquid temperature is 50 DEG C, and dip time is 65 minutes.

Squeezing multiple during squeezing is 2.6, and pressing temperature is 60 DEG C, and milling time is 40 seconds;

During pulverizing, control degree of grinding be 160g/L, pulverize after slurry congee concentration control be 33%, temperature is 50 DEG C;

Alkali cellulose after rubbing adds alkali lye, and to be mixed to form concentration be 6.5% slurry congee;

When falling poly-, pure oxygen addition is 4% of reactor volume, and the reaction time is 40min, and alkali lye naoh concentration is 160g/l;

During yellow, the addition of carbon disulfide is 33% of the fine content of first in alkali cellulose, and the yellow time is 48 minutes, and yellow reaction temperature is 24 DEG C.

The dissolving of cellulose sulfonate: the addition of solvent is 9.0% to be as the criterion with obtained cellulose sulfonate concentration, the mixing of solvent to be concentration the be 40 g/L NaOH water aqueous solution and 5 g/L sodium sulfite aqueous solutions, solution temperature is 17 DEG C, and dissolution time is 40min

Spinning a: bath consists of: sulfuric acid 115g/L, zinc sulfate 13g/L, sodium sulphate 260g/L, and temperature is 40 DEG C; Acid bath drop is 4.5g/L; Two bath compositions: temperature is 82 DEG C, sulfuric acid 21g/L, three baths are sulfuric acid, and its temperature is 85 DEG C, pH value 1.5;

Drawing-off: wherein total draft rate controls is 190%, and shower nozzle drawing-off is rate is 80%, the degree of draft of one degree of draft to be 50%, two road degree of drafts be 7%, three road drawing machines is 7%.

Concise: the concentration of vulcanized sodium is 5 g/L, and concentration of sodium carbonate is 3 g/L, and desulfurization temperature is 55 DEG C, and the time is 3min; Bleaching hydrogen peroxide concentration is 0.5g/L, and temperature is 50 DEG C, and bleaching time is 1.5min, oiling treatment, and the finish addition oiled is 9g/l, and finish temperature is 53 DEG C.Reconciling strand pH value after oiling is 7; Strand pH value can be regulated by washing,

Dry: Tumble Dry, bake out temperature is 90 DEG C, after oven dry, each desired value of sampling and measuring.

By measuring each desired value of viscose that embodiment 1-19 obtains, embodiment 1-7 data statistics concluded in table 1 below, embodiment 8-14 statistical induction is at table 2, and embodiment 15-19 statistical induction in table 3;

Table 4 for viscose of the present invention with and common viscose fiber, Modal fibre, differential viscose (CN102296373A documents 1, CN1632189 documents 2, CN102251301A documents 3) correction data:

Table 1

Table 2

Table 3

Table 4

From upper table 1,2, the data of 3 and 4, viscose of the present invention has and is different from common viscose fiber, Modal fibre, the new index system of the novelty of differential viscose, effectively can substitute the Modal fibre of high cost, while raising viscose lower procedure processing characteristics, exploitation and the industrial upgrading of downstream new textile can also be promoted, there is good economic benefit and social benefit.

Embodiment 20

Secondary response interface is inhaled look ability difference according to fiber cross section to dyestuff and is formed, the i.e. cortex of fiber and sandwich layer, cortex is little to dyestuff suction look ability, dyes partially shallow, and sandwich layer is large to dyestuff suction look ability, color is partially dark, cortex has the higher degree of orientation, and cortex is more, and fracture strength is higher, and sandwich layer is more, water swelling capacity is higher; Therefore the present embodiment is by any one viscose of gained in embodiment 1-19, does fibre section after common viscose fiber, the dyed process of model viscose, and amplify 2000 times of observations under the microscope, section statining result is as following table 5;

Table 5

From upper table 5, common viscose fiber (sky silk) dyed process, as shown in Figure 3, its fiber inner, middle and outer layer obtains color depth, shallowly to differ greatly, outer obviously partially shallow, middle level and internal layer are partially dark, there is secondary response interface, but interface is partially outer,, the sandwich layer and cortex " area " ratio that measure fiber are (90 ~ 95): (5 ~ 10), the inclined internal layer of ratio, ectonexine ratio is not enough to ensure that fiber has feature that is high-strength, flatness, and fiber is yielding.

Fibre section is done after Modal fibre dyeing, examine under a microscope, as shown in Figure 2, without secondary response interface, viscose of the present invention and Modal fibre are under equal dyeing condition, and viscose of the present invention inhales color depth than model, and dye-uptake is high, uniformity is better, and the COLOR FASTNESS of finished product is good.

As shown in Figure 1, the color of its fiber inner, middle and outer layer of viscose of the present invention is dark, shallow to differ greatly, outer and middle level is partially shallow, and internal layer is obviously partially dark, there is clear, obvious secondary response interface, measuring microscope sectional area, sandwich layer, cortex " area " ratio are (40 ~ 70): (30 ~ 60), and ratio is moderate, therefore viscose of the present invention is compared with common viscose fiber, have feature that is high-strength, flatness, also have suitable water imbibition, fiber skin-friendly has significant advantage simultaneously.

Embodiment 21

The Denier range of the high-strength flatness viscose of half delustring prepared according to the inventive method and other indication ranges are comparatively wide, therefore, in practical application, according to the difference of the indication range that it has, different field can be applied to respectively, for the production of different products

As: 1, have: fiber number (D) 0.8 ~ 1.5

Dry fracture strength >=3.15 cN/dtex, wet breaking strength >=1.70cN/dtex,

Intensity >=the 0.6cN/dtex needed for 5% percentage elongation is produced under wet condition,

Wet elongation at break 16 ~ 21%, dry elongation at break 15.0 ~ 19.0%,

Radial water swelling capacity 22 ~ 26%, degree of crystallinity 40 ~ 45%.

The dry ultimate strength coefficient of variation≤12, line density deviation ratio≤± 2.0%,

Residual sulphur≤7.0mg/100g, length variation rate≤± 3.0%,

Overcut fibre rate≤0.5%, over-length fibre≤1.0mg/100g,

Whiteness >=84%, the viscose of the index system of fault≤1.0mg/100g mainly applies to tight SEILE textile field, produces high sth. made by twisting, high grade yarn product, with the high domain requirements such as high sth. made by twisting that are applicable to of product strength for feature.As half delustring viscose of embodiment 5,6,7,9,11 etc.

2, have: fiber number (D) 0.8 ~ 1.5

Dry fracture strength >=3.20 cN/dtex, wet breaking strength >=1.70cN/dtex,

Intensity >=the 0.6cN/dtex needed for 5% percentage elongation is produced under wet condition,

Wet elongation at break 16 ~ 21%, dry elongation at break 13.0 ~ 16.0%,

Radial water swelling capacity 22 ~ 26%, degree of crystallinity 40 ~ 45%,

The dry ultimate strength coefficient of variation≤12, line density deviation ratio≤± 2.0%,

Residual sulphur≤7.0mg/100g, length variation rate≤± 3.0%,

Overcut fibre rate≤0.5%, over-length fibre≤1.0mg/100g,

Whiteness >=84%, the viscose of the index system of fault≤1.0mg/100g mainly applies to produce underwear, high-grade shuttle-woven fabric field, and with product feel silk sliding softness, comfortable pro-skin, and finished textile product good stability of the dimension is feature.As embodiment 12,13,15,17,19 etc.

3, have: fiber number (D) 0.8 ~ 1.5

Dry fracture strength >=3.10 cN/dtex, wet breaking strength >=1.60cN/dtex,

Intensity >=the 0.55cN/dtex needed for 5% percentage elongation is produced under wet condition,

Wet elongation at break 16 ~ 21%, dry elongation at break 12 ~ 14.5%,

Radial water swelling capacity 22 ~ 26%, degree of crystallinity 40-45%,

The dry ultimate strength coefficient of variation≤12, line density deviation ratio≤± 2.0%,

Residual sulphur≤7.0mg/100g, length variation rate≤± 3.0%,

Overcut fibre rate≤0.5%, over-length fibre≤1.0mg/100g,

Whiteness >=84%, the viscose of the index system of fault≤1.0mg/100g mainly applies to mainly apply to jean field, with light, soft, and finished textile product modification little be feature.As embodiment 16,18 etc.

Claims (20)

1. the preparation technology of the high-strength flatness viscose of one and half delustrings, it is characterized in that: described processing step is as follows: first pulp material is removed alkali lye after dipping, squeezing and obtain alkali cellulose, then by alkali cellulose through pulverize, crumple, add pure oxygen orientation fall poly-after obtain methylcellulose, methylcellulose obtains cellulose sulfonate through yellow again, filtration after cellulose sulfonate solubilizer dissolves, maturation, deaeration obtain spinning solution, and spinning solution adds delustering agent and obtain the high-strength flatness viscose of half delustring after spinning drawing, refining, oven dry.

2. the preparation method of a kind of half delustring viscose according to claim 1, is characterized in that: the degree of polymerization of described pulp material is 650 ~ 1200.

3. the preparation technology of the high-strength flatness viscose of a kind of half delustring according to claim 1, is characterized in that: described pulp material is the one or more kinds of combinations in cotton pulp, bamboo pulp, wood pulp, jute pulp.

4. the preparation technology of the high-strength flatness viscose of a kind of half delustring according to any one of claim 1-3, is characterized in that: the step of described preparation technology is as follows:

A: be impregnated in by pulp material and be equipped with in the treating tank of alkali lye, makes the slurry congee that concentration is 3 ~ 6% by grinder after being ground;

B: squeezer delivered to by the slurry congee that steps A is obtained, delivers to pulverizer and pulverizes after squeezing, obtains alkali cellulose, this alkali cellulose is delivered to kneading machine, obtains the slurry congee that concentration is 30 ~ 40% after process;

C: deliver to reactor after mix with alkali lye by slurry congee obtained for step B, adds pure oxygen in the reactor and carries out orientation and fall poly-, fall poly-after the acquisition degree of polymerization be 400 ~ 600, first fibre purity is the alkali cellulose of 98.0 ~ 98.5%;

D: the alkali cellulose that step C is obtained delivers to xanthating machine, adds carbon disulfide in xanthating machine, after yellow reaction, the cellulose sulfonate that chrysanthemum is obtained by reacting and dissolution with solvents, obtained concentration is the cellulose sulfonate solution of 9.0 ~ 10.0%;

E: by cellulose sulfonate solution obtained for step D after filtration, deaeration, obtain spinning solution after maturation, spinning adds delustering agent obtained viscose after spinning drawing and refining, oven dry.

5. the preparation technology of the high-strength flatness viscose of a kind of half delustring according to claim 4, it is characterized in that: in described steps A, described alkali lye is the sodium hydroxide solution of concentration 110 ~ 240g/L, and the temperature of steeping liquor is 30 ~ 60 DEG C, and dip time is 50 ~ 90min.

6. the preparation technology of the high-strength flatness viscose of a kind of half delustring according to claim 4, is characterized in that: in described steps A, and described grinder is located in the pipeline of connection treating tank and squeezer.

7. the preparation technology of the high-strength flatness viscose of a kind of half delustring according to claim 4, is characterized in that: in described steps A, and the temperature of described slurry congee is 30 ~ 60 DEG C, and the milling time of described grinder is 10 ~ 40s.

8. the preparation technology of the high-strength flatness viscose of a kind of half delustring according to claim 4, is characterized in that: in described step B, and the pressing temperature of described squeezer is 57 ~ 63 DEG C, squeezing multiple is 2.2 ~ 2.8.

9. the preparation technology of the high-strength flatness viscose of a kind of half delustring according to claim 4, is characterized in that: in described step B, and the degree of grinding of described pulverizer is 120 ~ 180g/L.

10. the preparation method of a kind of half delustring viscose according to claim 4, it is characterized in that: in described step C, described alkali lye is the sodium hydroxide solution of concentration 140 ~ 200g/l, in reactor, the addition of pure oxygen is 2 ~ 10% of reactor volume, falls the poly-reaction time to control at 30 ~ 60min.

The preparation technology of the high-strength flatness viscose of 11. a kind of half delustring according to claim 4, is characterized in that: in described step D, and the addition of carbon disulfide is 35 ~ 37% of the fine content of first in the alkali cellulose that obtains of step B.

The preparation technology of the high-strength flatness viscose of 12. a kind of half delustring according to claim 4, it is characterized in that: in described step D, the described yellow reaction time controls at 45 ~ 50min, and yellow reaction temperature is 20 ~ 30 DEG C.

The preparation technology of the high-strength flatness viscose of 13. a kind of half delustring according to claim 4, it is characterized in that: in described step D, described dissolving is carried out mixing, stir and grinding at cellulose sulfonate and solvent, the sodium sulfite aqueous solution of described solvent comprises concentration to be 25 ~ 45 g/L sodium hydroxide solution aqueous solution and concentration be 5 ~ 10 g/L.

The preparation technology of the high-strength flatness viscose of 14. a kind of half delustring according to claim 4, it is characterized in that: in described step D, described solution temperature is 10 ~ 20 DEG C, and dissolution time is 30 ~ 50min.

The preparation technology of the high-strength flatness viscose of 15. a kind of half delustring according to claim 4, it is characterized in that: in described step e, described spinning drawing step is as follows:

F: by cellulose sulfonate solution after filtration, deaeration, deliver to spinning machine after maturation, after a bath, form tow by the shower nozzle extruding spinning thread of spinning machine, the coagulating bath that a described bath uses comprises the zinc sulfate of the sulfuric acid of 90 ~ 120g/L, the sodium sulphate of 220 ~ 280g/L and 8 ~ 15g/L;

G: the tow after a bath sends into two baths by one drawing machine, the coagulating bath that described two baths use comprises the sulfuric acid of 18 ~ 22g/L, and the degree of draft of described one drawing machine is 50 ~ 100%;

H: the tow after two baths sends into three baths by two road drawing machines, the coagulating bath that described three baths use comprises the sulfuric acid that pH value is 1 ~ 3, and the degree of draft of described two road drawing machines is 40 ~ 60%;

I: the tow after three baths delivers to post processing part by three road drawing machines, and the degree of draft of described three road drawing machines is 5 ~ 15%.

The preparation technology of the high-strength flatness viscose of 16. a kind of half delustring according to claim 15, it is characterized in that: in described spinning drawing step, a described bath temperature is 40 ~ 50 DEG C, two bath temperatures are 80 ~ 90 DEG C, three bath temperatures are 80 ~ 90 DEG C.

The preparation technology of the high-strength flatness viscose of 17. a kind of half delustring according to claim 4, it is characterized in that: in described step e, described refining comprises desulfurization that the tow that formed spinning drawing carries out, bleaches and oil, and the desulfurizing agent that described desulfurization uses is made up of the sodium carbonate of concentration to be the vulcanized sodium of 4 ~ 8g/L and concentration be 1 ~ 4g/L; The hydrogen peroxide that the bleaching agent that described bleaching uses is concentration 0.3 ~ 0.6g/L; The described finish addition used that oils is 7 ~ 9g/L, and after oiling, the pH value of tow is 6.5 ~ 7.

The preparation technology of the high-strength flatness viscose of 18. a kind of half delustring according to claim 17, it is characterized in that: described desulfurization temperature is 50 ~ 55 DEG C, desulfurization time is 2 ~ 3min; Described bleaching temperature is 50 ~ 55 DEG C, and bleaching time is 1 ~ 2min; The temperature of described finish is 50 ~ 55 DEG C.

The preparation technology of the high-strength flatness viscose of 19. a kind of half delustring according to claim 4, it is characterized in that: in described step e, described oven dry is that tow refining obtained makes to Tumble Dry, and bake out temperature is 75 ~ 115 DEG C.

The preparation technology of the high-strength flatness viscose of 20. a kind of half delustring according to claim 1, is characterized in that: described half delustring high-strength flatness viscose has following performance indications:

Dry fracture strength >=3.10 cN/dtex, wet breaking strength >=1.60cN/dtex,

Intensity >=the 0.55cN/dtex needed for 5% percentage elongation is produced under wet condition,

Dry elongation at break 11.0 ~ 19.0%, wet elongation at break 16.0 ~ 21.0%,

Degree of crystallinity 40 ~ 45.0%, radial water swelling capacity 22 ~ 26%, dulling agent content 0.1-0.75%.