CN104846462B - Superfine semi-dull high-strength low-elongation viscose fiber and preparation method thereof - Google Patents
Superfine semi-dull high-strength low-elongation viscose fiber and preparation method thereof Download PDFInfo
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Abstract
The invention provides a superfine semi-dull high-strength low-elongation viscose fiber and a preparation method thereof, wherein the viscose fiber is obtained by sequentially carrying out dipping, grinding, squeezing and crushing, kneading, polymerization reduction, yellowing, dissolving, filtering, defoaming, ripening, spinning and drafting and post-treatment on pulp raw materials, and has the following indexes: the fineness is 0.8-1.11dtex, the dry breaking strength is more than or equal to 3.10 cN/dtex, the wet breaking strength is more than or equal to 1.60cN/dtex, the strength required for generating 5% elongation in a wet state is more than or equal to 0.55cN/dtex, and the dry breaking elongation is 11.0-19.0%. The superfine high-strength low-elongation viscose fiber is a novel fiber variety realized by technical innovation, has an index system different from common viscose fibers and modal fibers, not only shows the fiber characteristics of the modal fibers such as high strength and low elongation, but also shows stronger skin-friendly performance compared with cotton fibers, can effectively replace the existing differential viscose fiber, and can promote the development and industrial upgrading of downstream novel textiles while improving the downstream process processability of the viscose fiber.
Description
Technical field
The present invention relates to viscose rayon technical field, in particular to a kind of superfine type high-strength flatness viscose glue semi-dull it is fine and its
Preparation method.
Background technique
Textile fiber material is broadly divided into the natural fiber raw material with cotton, fiber crops etc. for representative, with terylene, acrylic fibers etc. for representative
Petroleum base fibrous raw material, and using natural cellulosic materials as tencel, copper ammonia fiber, viscose rayon etc. made of raw material regeneration
Biology base fibrous raw material.Cotton fiber obtains great fame due to its quality such as comfortable, soft, ventilative, personal, in entire textile fabric market
In account for about 36% the market share, however common cotton fiber needs a large amount of water resource and chemical substance, taken in excess soil because of it
In nutritional ingredient and whole world various countries be guarantee population in the world staple food supply and reduce the reasons such as cotton planting soil erosion
So that the plantation of cotton is restricted, cotton fiber material is in short supply, is not able to satisfy the growing needs of people's living standard.Viscose glue
Short fine category native cellulose regenerated fiber, it not only possesses the characteristic of cotton fiber, and possesses the portion for the silk that cotton fiber does not have
Divide advantage；Hygroscopic capacity is then up to 13~15%, is higher by 6~7% than cotton fiber, wears more comfortable；It dyes beautiful property and is better than cotton
Fiber；It is soft, plentiful, smooth, with the gloss as excellent drapability and silk；It is new by artificially processing and can assign
Performance, gloss, chromatography, function and it is required in terms of be more than natural fiber.Short rayon fiber because of its natural attribute,
The waste and old gurry of product can natural degradation, be a kind of environmental protection fiber of function admirable；In addition, short rayon fiber do not rise electrostatic,
The natural cotton fibers attribute such as sucting wet air permeability, snugness of fit has cotton fiber very strong alternative.
Soluble cellulose sulfonic acid is made using native cellulose as raw material, through processes such as alkalization, aging, sulfonation in viscose rayon
Ester, is re-dissolved in sig water and viscose glue is made, and is made through wet spinning.Using different raw material and spinning technique, can obtain respectively
To common viscose fiber, Modal fibre, differential viscose rayon etc..The fabric fastness that common viscose fiber weaves is poor, contracting
Water rate is higher, and elasticity and wearability are poor, easily-deformable after dress.Compared with common viscose fiber, Modal fibre has high humidity
Modulus, high intensity and low humidity elongation, density are greater than common viscose fiber, meet water volume expansion rate and compare common viscose fiber
Small, washing shrinkage is low；With preferable degree of fineness, thinner yarn can be spun；Crystallinity and the degree of orientation with higher so that fiber hand
Sense is fine and smooth soft, and skin-friendly is strong, comfortable and easy to wear.Also because Modal fibre has the above advantages the former material so that Modal fibre
Material, the cost of production technology etc. are greatly higher than common viscose fiber；Secondly, the fabric that Modal fibre is formed is soft, it is bone-free
Frame, conformality is bad, and since the fibrillation of Modal fibre is inclined to, one is rubbed, easily causes fabric raising, and pilling influences
The appearance of fabric, in addition, Modal fibre is used in the production of underwear mostly, products application is limited, therefore is both able to satisfy people couple
Flexibility and comfort demand, and can make the fabric to be formed that there is fine conformality, the low fiber product of production cost is that have very much
It is necessary.
One application No. is 200910098209.5 Chinese patents to disclose a kind of method for manufacturing modal fiber, successively
By quaternization, experienced reaction, yellow reaction, the dissolution of viscose glue, the filtering of viscose glue, the deaeration of viscose glue, the maturation of viscose glue, wet
Method spinning, drawing-off and other associated process steps use the cellulose pulp of first fibre content < 95% for raw material, using common viscous
The commonly used equipment of glue staple fiber production, using the simple and practical special process formula of technology controlling and process and spinning drawing mode, manufacture
The Modal fibre that can be met international standards out.
Based on the above situation, it is the sustainable development for promoting viscose rayon industry, produces differential, functionalization viscose rayon
Current industry is had become newly to mark.Application No. is the Chinese patents of CN201010011519.1 to disclose a kind of polynosic fibre
And its production method, it is characterized in that it is mixed with rayon spinning solution by bacteria cellulose and viscose rayon is made, wherein bacterium
Content of the cellulose in viscose rayon is 1% ~ 10%.The intensity of the polynosic fibre of the patent increases, but its line
Density is essentially the same with common viscose fiber, cannot better meet demand of the downstream product to flexibility, and the invention uses
Bacteria cellulose is as one of raw material, currently, bacteria cellulose is mainly used in biological medicine material, it is multiple to obtain technique
It is miscellaneous, low yield, higher cost, so mixing with viscose rayon the former material of the high-intensity fiber as the invention using bacteria cellulose
Material, greatly increases cost, limits large-scale industrialization application.
A kind of production method of superfine high-strength high-modulus viscose fiber of patent document CN102296373A(, 2011.12.28) it is public
A kind of viscose rayon that a kind of uniform structure, fibre strength and modulus are higher by 50% or more conventional variety is opened, viscose glue obtained is fine
The fibre strength of dimension is 0.44~0.78dtex, dry strong >=3.1cN/dtex(lis of ox/dtex), it is wet strong >=2.1cN/dtex, wet
Modulus >=0.5cN/dtex, whiteness >=82.0%.
A kind of high white strength fine denier viscose staple fiber of patent document CN1632189(and its production technology, 2005.06.29)
The short rayon fiber that a kind of fiber number is thin, intensity is high is disclosed, it is strong compared with having for common viscose fiber by the garment material of its processing
The advantages that degree is high, wearability is strong, feel is fine and smooth, wrinkle resistance, resistance to multiple deformation, it may also be used for weaving high grade cotton yarn fabric products.
A kind of production process of ultrafine-denier high-strength viscose fibers of patent document CN102251301A(, 2011.11.23) it discloses
A kind of preparation method for the viscose rayon that fiber number is low, intensity is high, can get fiber number is that 1.11 dtexs and intensity are greater than 2.9 cN/
The viscose rayon of dtex.
Only the above-mentioned published patent document can be known, for differential, functionalization viscose rayon is made, the prior art is equal
It is to be realized by way of changing production technology, wherein include raw material, viscose glue molding and its change of technological parameter
Etc., the viscose rayon of acquisition has carried out appropriate optimization compared with common viscose fiber in fiber number and intensity, but for increasingly swashing
For strong market competition, there is no the exploitations and production that meet downstream new textile to a greater extent for differential viscose rayon
Industry upgrading, it is especially equally former using natural cellulosic materials as fibers such as tencel, Modal, copper ammonia fiber made of raw material regeneration
The development of material, so that the occupation rate of market of viscose rayon reduces increasingly.Such as: patent document CN101130885(fiber crops material viscose rayon
Preparation method and preparation numb material viscose rayon, 2008.02.27) to disclose a kind of viscose glue using numb material plant production fine
Dimension and its preparation process, simple process, supplies consumption is low, and the numb material viscose rayon produced has excellent whiteness, intensity
Breaking strength >=1.820 cN/ are done with performances, the numb material viscose rayon satisfactions prepared by the technique such as elongate fibers
Dtex, wet breaking strength >=1.12 cN/dtex, dry elongation at break >=15.4%, line density deviation ratio ± 6.00%, length are inclined
Rate ± 6.00%, overlength fiber rate≤1.0%, over-length fibre≤18.0mg/100g, fault≤11mg/100g, residual sulphur≤
18.0mg/100g。
Thus, it would be desirable to find one kind and be different from natural fiber raw material and petroleum base fibrous raw material, performance is better than difference again
Not Hua viscose rayon New Viscose Fibre, be not only able to satisfy requirement of the people to natural prodcuts (such as: Modal fibre), moreover it is possible to
Suitable for industrialized continuous production, biggish economic benefit is brought for enterprise, certainly, this is also that viscose rayon industry can continue
The inexorable trend of development.
Summary of the invention
The purpose of the present invention is to provide a kind of superfine type high-strength flatness viscose rayon semi-dull, which is different from
Traditional viscose rayon product and cotton are fine, are the tencel kinds realized by technological innovation, have and are different from common viscose glue
The index system of fiber and Modal fibre, product not only show that Modal fibre is high-strength, fiber characteristics of flatness, also
It shows compared with the fine stronger skin-friendly of cotton, existing differential viscose rayon can be effectively substituted, in the case where improving viscose rayon
While swimming process processing performance, moreover it is possible to promote the exploitation and industrial upgrading of downstream new textile, there is good society's effect
Benefit.
Another object of the present invention is to provide a kind of preparation methods of superfine type high-strength flatness viscose rayon semi-dull, originally
Preparation method as a raw material for production, by the way that viscose rayon is made after viscose glue preparation, spinning technique and post-processing, was produced with raw material
Cheng Zhong still remains secondary response microscope sectional area, and the ectonexine area ratio at the interface is clearly distinguishable from Modal fibre
The secondary response trace of peacekeeping common viscose fiber, it is ensured that the product has the characteristics that high-strength, flatness, while also having suitably
Water imbibition and significant fiber skin-friendly.
In order to solve the above technical problems, the invention is realized by the following technical scheme.
Superfine type high-strength flatness viscose rayon semi-dull, the viscose rayon have following performance indicators:
Fiber number is 0.8~1.11 dtex, does breaking strength >=3.10 cN/dtex, wet breaking strength >=1.60cN/
Dtex,
Intensity >=0.55cN/dtex needed for 5% elongation is generated under wet condition,
Dry elongation at break 11.0~19.0%, wet elongation at break 16.0~21.0%,
Crystallinity 40~45.0%, dulling agent content 0.1-75%, radial water swelling capacity 22~26%.
Further, the viscose rayon semi-dull also has following indexs:
Line density deviation ratio≤± 11.0%, residual sulphur≤12mg/100g,
Length variation rate≤± 11.0%, overlength fiber rate≤0.5%,
Over-length fibre≤4.0mg/100g, whiteness >=84%, fault≤4.0mg/100g.
The present invention also provides the preparation method of superfine type high-strength flatness viscose rayon semi-dull, this method is first by pulp
Raw material removes lye after impregnating, squeezing and obtains alkali cellulose, then gathers alkali cellulose through crushing, rubbing, drop and obtains first
Base cellulose, methylcellulose are made cellulose sulfonate through yellow again, filter after the dissolution of cellulose sulfonate solubilizer, is ripe
Be made spinning solution at, deaeration, spinning solution be added delustering agent through spinning drawing, refining, dry to obtain viscose rayon of the present invention.
For material pulp: the degree of polymerization of pulp material is 650~1200, and advantage is: needle pulp fibres length 2~
3mm, intensity are high.
Pulp can be combined using one of cotton pulp, bamboo pulp, wood pulp, jute pulp or two or more arbitrary proportions.
For the better implementation present invention, the present invention illustrates preparation method.
The preparation method of superfine type high-strength flatness viscose rayon semi-dull, the method comprises the following steps:
A, cellulose slurry congee is impregnated in the treating tank equipped with soda bath, after being stirred, being configured to concentration is 3-
6% slurry congee (mass percent), wherein it impregnates and uses concentration of lye 110-240g/L, 30-60 DEG C of temperature, dip time 50-
90 minutes；Known by actual production, in dipping, if the excessively high meeting of concentration of lye is so that later period cellulose sulfonic acid rouge solubility drops
It is low, cause viscose filtration difficult, concentration of lye is too low to make pulp puffed degree excessively high, and squeezing is difficult；Alkali liquid temperature is excessively high to lead
It causes cellulose drop poly- fast, accelerates side reaction, influence viscose filtration, temperature is too low, and pulp puffed degree is high, and squeezing is difficult.This technique
Step control naoh concentration be 110-240g/L, 30-60 DEG C of temperature, guarantee the later period filtering and squeezing process it is effective into
Row can improve the content of methylcellulose using the impregnation of this step, produce alkali cellulose.
B, after the completion of dipping, the slurry congee in treating tank is delivered to squeezer progress expression separation by conveyance conduit and is obtained
Alkali cellulose, wherein squeezing multiple is 2.2-2.8.The content for squeezing alkali fibre first fibre in obtained alkali cellulose is 29%-31%%,
The content of alkali fibre alkali is 16 ± 1%, and half fiber Han Liang≤10g/L in lye prepares alkali cellulose data ratio with traditional viscose rayon
Compared with alkali cellulose half fiber produced by the present invention is low, and product strength is high.
The substance wherein squeezed out is divided into two parts, and a part is mingled with the lye of fiber, impurity, and another part is to be pressed
The solid-state of excessive moisture and the mixture (i.e. alkali cellulose) of liquid are gone out.So fiber, impurity will be mingled with by squeezing
Lye and alkali cellulose separation；
It is mingled with the lye of fiber, impurity by filter net type vacuum adsorption machine, fiber and clean lye is separated and recovered,
Extra hemicellulose is removed, wherein strainer uses 60-120 mesh, and vacuum degree is-(0.1-0.4) MPa；
In addition, slurry congee can first be ground before squeezing, specifically, can be mounted on treating tank and squeezing by one
Grinder in the connecting pipe of machine is ground, and milling time 10-40 seconds；It can continue to generate alkali cellulose, dissolution in this way
The impurity such as hemicellulose, lignin, simultaneous grinding can carry out shredding, dispersion to alkali cellulose, to improve alkalization speed and alkali
Rate.
Alkali cellulose is crushed, is crumpled: obtained alkali cellulose fiber will be squeezed and crushed through pulverizer, degree of grinding 120-
180g/L obtains 30-60 DEG C of temperature after kneader twin screw device carries out rubbing processing after crushing, concentration is the slurry of 30-40%
Congee, crushing, rubbing can make fiber sub-wire, brooming, reach the cell wall for destroying cellulose fibre, remove small point in cellulose
Son improves cellulose combination alkali content to improve fibrin reaction performance, and alkali cellulose content reaches 6-8%；
C, lye is added to be mixed to form concentration by the alkali cellulose that step B is prepared is that 4-8% starches congee, and is transported to and determines
To poly- reactor is dropped, the pure oxygen of the 2-10% of reactor volume is added in reactor, is oriented the poly- reaction of drop, reaction time 30-
60min is added pure oxygen and aoxidize dropping and gather, after drop is poly-, the alkali cellulose degree of polymerization is reduced to 400- by 650-1200 in this step
600, first fibre purity reaches 98.0-98.5% in alkali cellulose, and 2-3% can be improved than traditional handicraft.Orientation drop is poly- more experienced than tradition
The poly- first fibre that reduces of drop loses 3-5%, and molecule drop is gathered more uniform, abundant；Lye uses sodium hydroxide, concentration 140-200g/L；
D, the step C alkali cellulose being prepared is sent into xanthating machine and is reacted with carbon disulfide, wherein curing
The additional amount of carbon is the 25-37% of first fibre content in alkali cellulose, and the yellow reaction time is 45-50 minutes, temperature 20-30
℃；In practical application, carbon disulfide additional amount is very few, yellow reaction is incomplete, filtration difficulty；Carbon disulfide additional amount mistake
Height, yellow overreact, by-product are more.
It mixed, stirred, ground by a certain percentage with solvent again through yellow reaction cellulose sulfonate obtained, finally
Dissolve be made cellulose sulfonate solution, the additional amount of solvent be subject to cellulose sulfonate concentration obtained be 9.0-10.0%,
Dissolving the solvent used is sodium hydroxide, sodium sulfite aqueous solution, and concentration is respectively 25-45 g/L, 5-10 g/L, dissolution temperature
10-20 DEG C, dissolution time 30-50min of degree, cellulose sulfonate solution are using filter, deaeration, maturation, finally obtained viscosity
The spinning solution of 40-45s, degree of ripeness 9.5-12ml, methylcellulose content 8.8-9.0%, the 4.5-4.8% containing alkali；According to product dialogue
The requirement of degree is added delustering agent by injection method before spinning solution is sent to spinning machine spinning and is uniformly mixed, and delustering agent can choose
Titanium dioxide is configured to the aqueous solution that concentration is 10-15% and uses.
, spinning solution made from step D sent to spinning machine spinning, spinning is using more baths, low acid, less salt wet spinning skill
Art, specific as follows: by spinning machine spray head extruding spinning liquid, then spinning solution forms tow into a bath after one of drawing-off,
Tow by a bath is sent into two baths through one of drafting machine, and bis- drafting machine of Zai Jing is sent into three baths, and the tow after three baths is by three
Drafting machine is sent to refinery practice；Viscose rayon semi-dull is dried to obtain after refining；
The spinning coagulation bath composition that can wherein use is as follows: a bath composition are as follows: sulfuric acid 90-120g/L, zinc sulfate 8-
15g/L, sodium sulphate 220-280g/L, a bath temperature are 40-50 DEG C, acid bath drop: 3-5g/L, two bath compositions: temperature 80-90
DEG C, sulfuric acid 18-22g/L, three baths are sulfuric acid, and temperature is 80-90 DEG C, pH value 1-3；
H, drawing-off: can using step by step, high drawing-off technology, wherein total draft rate control exists: 150-200%, (drawing-off is excessively high,
Lousiness is more, and drawing-off is low, and intensity is low) spray head drawing-off be rate are as follows: 50-100%, (drawing-off is low, occur and silk fault, it is excessively high, under intensity
Drop), one of degree of draft are as follows: 40-60%, two degree of drafts are as follows: 5-15%, (drawing-off is excessively high, and lousiness is more；Drawing-off is low, intensity decline),
The degree of draft of three drafting machines is 5~15%.
Wherein refining process include: by strand by desulfurization, bleach, oil after obtain viscose rayon semi-dull, take temperature
Desulfurization, bleaching are carried out with environment, post-processing is reduced and strand strength and elongation is damaged, desulfurizing agent is the mixed of vulcanized sodium and sodium carbonate
It closes, the concentration of vulcanized sodium is 4-8 g/L, sodium carbonate 1-4 g/L, 50-55 DEG C of desulfurization temperature, time 2-3min；Using vulcanized sodium
Milder compared with sodium hydroxide, sodium sulfite as desulfurizing agent, sodium carbonate is for neutralizing strand bring sulfuric acid.
Using hydrogen peroxide bleaching, hydrogen peroxide concentration 0.3-0.6g/L is 50-55 DEG C of temperature, bleaching time 1-2min, double
Oxygen water is milder compared with bleaching agents such as sodium hypochlorite；
Oiling treatment: the oil agent addition of oiling treatment is 7-9g/L, and finish temperature is 50-55 DEG C, is adjusted after oiling treatment
Strand pH value is solved within the scope of 6.5-7；Within the scope of the pH, finished product strand strength and elongation be will not influence, and can pass through washing, multiple-effect
Sour (organic acid) adjusts pH value.
Drying: it Tumblies Dry, 75-115 DEG C of drying temperature, after drying, obtains finished product.
The utility model has the advantages that
1, compared with common viscose fiber in the prior art, Modal fibre, differential viscose rayon, of the invention half
Delustring viscose rayon, fiber product intensity is up to 3.6cn/dtex, and rheobase instinct matches in excellence or beauty with Modal fibre, than common
Viscose fiber strength is high by 30% or so, while its wet elongation at break is lower than Modal fibre, knits its fabric compared with Modal fibre
Object has more conformality；Present invention viscose rayon semi-dull has more suitable water swelling rate, its skin-friendly is made to be better than Modal
Fiber；Also more soft；Product moisture absorption, good permeability, pro-skin is comfortable, compares Modal with dyeing under process conditions better than Modal
Color depth is inhaled, dye-uptake is higher, uniformity is more preferable, finished product good color fastness.Meet downstream product to intensity, skin-friendly, flexibility
Multiple requesting, in the prior art by feedstock optimization with process optimization obtain partial properties improvement viscose rayon compared with, this
The viscose rayon product quality of invention is improved, and is new products innovation.
Viscose rayon of the present invention has the secondary response interface different from common viscose fiber and Modal fibre,
Fiber is done into fibre section after dyeing, the fibre section of viscose rayon of the present invention is shown clear, apparent two
Secondary response microscope sectional area, and the inclined internal layer in interface, ratio is moderate, and inside and outside layer " area " ratio is respectively (40~70): (30
~60), it is ensured that the viscose rayon product has the characteristics that high-strength, flatness, while also having water imbibition appropriate, fiber pro-skin
Property have significant advantage.
The method of the present invention is the viscose rayon and cotton fibre, the not generation that prepare using natural cellulosic materials as raw materials for production
Your fiber etc. is the same, is degradable fibrous material, meets requirement of the people to environmental protection.
2, the present invention has rational design, and in the production process of identical viscose rayon product, the present invention chooses from raw material, prepares
Process modification etc., the production cost of the reduction viscose rayon product of high degree, product of the present invention prepare first fibre content ratio
Modal requirement is low, therefore can reduce pulp dosage, reduces cost of material；The acid bath composition and draft process that the present invention optimizes,
It can accomplish the control parameter of each process of overall balance, and appropriate, price is low 4000 compared with Modal fibre
~5000 yuan/ton, downstream raw material use cost can be greatly lowered, can be used for home textile, non-woven fabrics etc., especially underwear and face
Film, hygenic towelette etc. bring more high added value and vast market prospect for down-stream enterprises such as spinning, woven fabrics, are obviously improved enterprise
The market competitiveness.
3, to ensure that high-strength flatness viscose rayon secondary response interface has a suitable cortex, sandwich layer ratio, the present invention from
Technology is set out, and has accomplished improvement acid bath technique, such as reduces sulfuric acid concentration, and reaction slowly, improves skin thickness；Change viscose glue
Index, such as viscose ripening degree, first fibre content, alkali content index.
4, compared with adhering process in the prior art, alkali cellulose hemicellulose level produced by the present invention is low, we
Know: hemicellulose refers to the degree of polymerization in 50~200 beta cellulose and the gamma-cellulose of degree of polymerization < 50, the shadow of hemicellulose
As long as sound has the following aspects: the uniformity of a. influence alkali cellulose；B. extend ageing time；C. the yellow speed of hemicellulose
Degree is more fine than first fast, consumes a certain amount of carbon disulfide, and alkali cellulose esterification is caused to reduce, and the solubility of sulphonic acid ester reduces；D. shadow
The filtering of viscose glue is rung, the solubility of sulphonic acid ester reduces, and the potential aldehyde radical in end is oxidized to the metal ion in carboxyl and ash content
Such as: ferrous ion, manganese ion, calcium ion, magnesium ion form the extremely strong complex compound of viscosity, cause viscose filtration difficult, yield
It is low；E. hemicellulose is more, and the physical mechanical property of viscose rayon is poorer.The present invention can in advance press feeding by grinding mill
The slurry congee of crusher is ground, and milling time is 10~40s, and after the slurry congee after grinding is squeezed with squeezer, separation is mixed
Lye and alkali cellulose are closed, contains hemicellulose and other impurities in mixed alkali liquor, is crushed through pulverizer, the multiple of squeezing is
2.2~2.8, degree of grinding 120-180g/L, the present invention can in advance carry out the slurry congee for being sent into squeezer by tube mill
It rolls, by mechanism, can fiber be torn and be discongested, to improve the reactivity worth of slurry congee, guarantee that viscose rayon is raw
What is produced goes on smoothly, and compared with preparing alkali cellulose data with traditional viscose rayon, alkali cellulose half fiber produced by the present invention is lower,
Half fiber Han Liang≤10g/L, product strength are higher.
5, the present invention passes through numerous studies, replaces the experienced technique of tradition using orientation degrading and polymerizing technology for the first time, and obtains specific
It orients and drops poly- parameter, oxygen is added through the invention and aoxidize dropping and gathers, after drop is poly-, the alkali cellulose degree of polymerization is dropped by 650-1200
For 400-600, first fibre purity reaches 98.0-98.5%, and 2-3% can be improved than traditional handicraft in first fibre content.Technique more experienced than tradition
It reduces first fibre and loses 3-5%, molecule drop is gathered more uniform, abundant；Reduce production cost.
6, yellow of the invention and spinning technique are more environmentally friendly, energy saving, and in large-scale industrial production, Modal produces yellow
When carbon disulfide dosage be up to 35% or so (being calculated with first fibre content), and carbon disulfide dosage only 30% when yellow of the present invention
Left and right (to first fibre), can effectively reduce cost and reduces air pollution；
Acid bath is combined using high zinc sulfate, low sodium sulphate when Modal spinning, and high zinc sulfate can lead heavy metal pollution of water body
Seriously, it is high then to will lead to its acid bath evaporation crystallization energy consumption for low sodium sulphate.Again compatibility acid bath forms the present invention, and a such as bath uses
Sulfuric acid 90-120g/L, zinc sulfate 8-15g/L, sodium sulphate 220-280g/L composition are run completely while guaranteeing acid bath effect
The high zinc sulfate of traditional acid bath, the constituent of low sodium sulphate have been covered, heavy metal pollution of water body and acid bath evaporation crystallization are avoided
The problem of；
7, in spinning technique of the invention, tow by mostly bath, it is low acid, less salt wet spinning technology, meanwhile, in conjunction with by
Grade, high drawing-off technology carry out spinning, and it be 40~60%, three degree of drafts is 5 that one of degree of draft, which is 50~100%, two degree of drafts,
~15%, it is more advantageous to the brittleness for improving fiber, the elongation of fiber is improved, shows: generating 5% elongation under wet condition
Required intensity >=0.55cN/dtex, dry elongation at break are 11.0~16.0%.Viscose rayon more can compared with Modal fibre
The property spun, therefore 50 meters of scooter or so/minute is spun, and Modal only has 30 meters or so/minute, high production efficiency, reduces production
Cost；
Detailed description of the invention
Fig. 1 is the fibre section cross section of superfine type of the present invention high-strength flatness viscose rayon semi-dull.
Fig. 2 is the fibre section cross section of Modal.
Fig. 3 is the fibre section cross section of tencel.
Specific embodiment
The present invention will be described in detail combined with specific embodiments below.
It is noted that described further below be all exemplary, it is intended to provide further the required present invention
Bright, unless otherwise indicated, all technical and scientific terms used herein has the common skill with the technical field of the invention
The normally understood identical meanings of art personnel.
Following standards are pressed in each index value measurement of following embodiment of the present invention, be suitable for linear density range be 0.8dtex~
The measurement of 1.67dtex viscose rayon:
Index determining: the measuring method of dry breaking strength is GB/T 14337, and the measuring method of wet breaking strength is GB/T
14337, intensity needed for generating 5% elongation under wet condition is completed by GB/T 14337, the measurement of dry elongation at break
Method is GB/T 14337, and the measuring method of line density deviation ratio is GB/T 14335, and the measuring method of length variation rate is GB/
T 14336, the measuring method of overlength fiber rate are GB/T 14336, and the measuring method of over-length fibre is GB/T 14336, fault
Measuring method be GB/T 14339, the measuring method of whiteness is FZ/T 50013, and the measuring method of residual sulphur is FZ/T 50014,
The measuring method of radial water swelling capacity is GB/T 6503.
Embodiment 1
Pulp material is successively crushed through dipping, grinding, squeezing, rubbing, drop are poly-, yellow, dissolution, filtering, deaeration, ripe
At, delustering agent, spinning drawing, refining, drying reason is added after obtain viscose rayon semi-dull, the viscose glue semi-dull of the present embodiment is fine
Dimension has following train diagram adjustings:
Fiber number be 1.1 dtex, do breaking strength be 3.12 cN/dtex, wet breaking strength 1.65cN/dtex,
Intensity needed for generating 5% elongation under wet condition is 0.55cN/dtex,
Dry elongation at break 19.0%, wet elongation at break 21.0%,
Crystallinity is 40%, and radial water swelling capacity is 22%, dulling agent content 0.10%,
Line density deviation ratio is -11.0%, and residual sulphur is 12mg/100g,
Length variation rate is -11.0%, overlength fiber rate 0.48%, whiteness 84.1%,
Over-length fibre is 4.0mg/100g, fault 3.8mg/100g.
Embodiment 2
The superfine type of the present embodiment high-strength flatness viscose rayon semi-dull the difference from embodiment 1 is that: the present embodiment tool
There are following indexs:
Fiber number be 1.08 dtex, do breaking strength be 3.10 cN/dtex, wet breaking strength 1.67cN/dtex,
Intensity needed for generating 5% elongation under wet condition is 0.54cN/dtex,
Dry elongation at break is 18.9%, and wet elongation at break is 20.8%,
Crystallinity 40%, radial water swelling capacity be 22%, dulling agent content 0.75%,
Whiteness 84.6%, line density deviation ratio are -9.0%, and residual sulphur is 11mg/100g,
Length variation rate is+8.0%, and overlength fiber rate is 0.5%,
Over-length fibre is 2.2mg/100g, fault 4.0mg/100g.
Embodiment 3
For the better implementation present invention, it is viscous that the present embodiment further provides superfine type of the invention high-strength flatness semi-dull
The specific preparation method of glue fiber, and measure performance indicator.
A kind of preparation method of viscose rayon semi-dull: being that pulp material is removed lye to obtain after impregnating, squeezing
Alkali cellulose；The alkali cellulose being prepared removes lye after crushing, rubbing, drop are poly- and obtains methylcellulose；It is made
Cellulose sulfonate is made through yellow in methylcellulose；Be made cellulose sulfonate solubilizer dissolution after filtering, maturation, take off
Spinning solution is made in bubble；Spinning solution obtained is sent to spinning machine spinning after delustering agent is added, drawing-off obtains tow, and tow is by essence
Viscose rayon of the present invention is obtained after refining, drying.Sampling, according to each index of said determination standard test.
Embodiment 4
The present embodiment and the difference of embodiment 3 are: the present embodiment further determined preparation pulp material used
The degree of polymerization and preferred raw material type, obtain through practical studies, and the degree of polymerization of pulp material is preferable with 800~1200, pulp
Raw material is preferable using one of cotton pulp, bamboo pulp, wood pulp, jute pulp or the combination of two or more arbitrary proportions, this implementation is selected
The cotton pulp and bamboo pulp that the degree of polymerization is 650~1200, are used in mixed way in the ratio of 1:1.Fiber made from the present embodiment is sampled and is surveyed
Determine index.
Embodiment 5
For the better implementation present invention, it is fine that the present invention is further improved superfine type of the present invention high-strength flatness viscose glue semi-dull
The preparation method of dimension, the specific steps of which are as follows:
A: pulp material is impregnated in the treating tank equipped with lye, and the slurry that concentration is 3% is made after being ground by grinder
Congee；Pulp material uses the degree of polymerization to be used in mixed way for 650~1200 bamboo pulp and wood pulp in the ratio of 1:1；
B: slurry congee made from step A is sent to squeezer, send after squeezing to pulverizer and is crushed, obtains alkali fiber
The alkali cellulose is sent to kneading machine, the slurry congee that concentration is 30% is obtained after processing by element；
C: sending after slurry congee made from step B is mixed with lye to reactor, and pure oxygen is added in the reactor, obtains after drop is poly-
Obtain the alkali cellulose that the degree of polymerization is 400~600, first fibre purity is 98.0~98.5%；
D: alkali cellulose made from step C is sent to xanthating machine, carbon disulfide is added in xanthating machine, is reacted through yellow
Afterwards, the cellulose sulfonate and solvent yellow reacted dissolves, and the cellulose sulfonate solution that concentration is 9.0% is made；
E: cellulose sulfonate solution made from step D is obtained into spinning solution after filtering, deaeration, maturation, spinning solution adds
Enter delustering agent and viscose rayon is made after spinning drawing, refining, drying.
Embodiment 6
The present embodiment and the difference of embodiment 5 be, the present embodiment further improves dipping, grinding technics, when dipping
Using the sodium hydroxide solution of concentration 110g/L, the temperature of steeping liquor is 30 DEG C, dip time 50min.It is made after grinding
Slurry congee concentration control be 4%.
Embodiment 7
Difference with embodiment 5 is that the present embodiment grinder is arranged on the pipeline of connection treating tank and squeezer,
Slurry congee dipping is completed to be ground, and milling time 10s, slurry congee concentration obtained control is 5% after grinding, starches the temperature control of congee
30 DEG C are made as, grinder is set in the connecting pipe for the treatment of tank and squeezer, it is easy to operate, it is high-efficient.
Embodiment 8:
The present embodiment and the difference of embodiment 5 are: the present embodiment further improves squeezing process and disintegrating process, really
Pressing temperature, squeezing multiple and degree of grinding are determined, the pressing temperature of the present embodiment is 57 DEG C；Squeezing multiple is 2.2；Degree of grinding is
120g/L
The present embodiment grinding slurry congee concentration control obtained is 6%, and it is 35% that slurry congee concentration control is made after squeezing
Embodiment 9
The present embodiment and the difference of embodiment 5 are: the present embodiment further improves degrading and polymerizing technology: lye kind has been determined
The time of poly- reaction drops in class and its concentration, the additional amount of pure oxygen, and the lye of the present embodiment uses concentration for the hydroxide of 140g/L
Sodium solution, pure oxygen additional amount are the 2% of reactor volume, and dropping the poly- reaction time is 30min.
Embodiment 10:
The present embodiment and the difference of embodiment 5 are: the present embodiment further improves yellow technique, it is determined that yellow is anti-
The additional amount of middle carbon disulfide is answered, in the yellow reaction time, yellow temperature, it is warp that carbon disulfide additional amount is reacted in the present embodiment yellow
30% of first fibre content in alkali cellulose obtained is squeezed after disintegrating process, the yellow time is 45min, and yellow reaction temperature is 20
℃。
Embodiment 11
The present embodiment is with the difference of embodiment 5: the present embodiment is further improved reacted through yellow after obtained fibre
Tie up the dissolution process of plain sulphonic acid ester, it is determined that the time required to dissolution solvent, solution temperature and dissolution, the present embodiment solvent is dense
The mixing for the sodium sulfite aqueous solution that degree is 25 g/L sodium hydroxide solutions and concentration is 5 g/L, solution temperature are 10 DEG C, dissolution
Time is 30min.
Embodiment 12
The present embodiment and the difference of embodiment 5 are: the present embodiment further improves spinning drawing technique, it is determined that spins
Silk specific steps and spinning process in acid bath use coagulating bath technical parameter, drafting step parameter.The spinning of the present embodiment is led
Stretching process is as follows:
F: cellulose sulfonate solution is sent after filtering, deaeration, maturation to spinning machine, is squeezed out and is spun by the spray head of spinning machine
Silk thread forms tow after a bath, the coagulating bath that a bath uses include the sulfuric acid of 90g/L, 220g/L sodium sulphate and
The zinc sulfate of 8g/L；
G: the tow after a bath is sent into two baths by one of drafting machine, and the coagulating bath that two bath uses includes 18g/L's
Sulfuric acid, the degree of draft of one of drafting machine are 50%；
H: the tow after two baths is sent into three baths by two drafting machines, and it is 1 that the coagulating bath that three bath uses, which includes pH value,
Sulfuric acid, the degree of draft of two drafting machine is 40%；
I: the tow after three baths is sent by three drafting machines to post-processing part, and the degree of draft of three drafting machine is
5%。
One bath temperature is 40 DEG C, two bath temperatures are 80 DEG C, three bath temperatures are 80 DEG C.
Embodiment 13
The present embodiment and the difference of embodiment 5 are that the present embodiment further improves refinery practice, and refining includes to spinning
The desulfurization for the tow progress that filament drafting is formed is bleached and is oiled, the vulcanization that the desulfurizing agent that the desulfurization uses is 4g/L by concentration
The sodium carbonate that sodium and concentration are 1g/L forms；The hydrogen peroxide bleached the bleaching agent used and be concentration 0.3g/L；It is described to oil
The oil agent addition used is 7g/L, and the pH value of tow is 6.5 after oiling.
The desulfurization temperature is 50 DEG C, desulfurization time 2min；The bleaching temperature is 50 DEG C, and bleaching time is
1min；The temperature of the finish is 50 DEG C.
Embodiment 14
The present embodiment is that the present embodiment further improves stoving process, the present embodiment with the difference with embodiment 5
Drying is will to refine obtained tow using drying machine drying, and drying temperature is 75 DEG C.
Embodiment 15
For the better implementation present invention, the present embodiment further provides superfine type of the present invention high-strength flatness viscose glue semi-dull
The preferred preparation method of fiber,
The method comprises the following steps:
A, it impregnates: pulp material being smashed, is impregnated in the treating tank equipped with soda bath, after being stirred, is configured to
The slurry congee that concentration is 4%, wherein dipping concentration of lye 150g/L, 40 DEG C of temperature, dip time is 60 minutes；Material pulp:
Using the degree of polymerization is that cotton pulp, bamboo pulp, the wood pulp of 650-1200 is applied in combination with the ratio of 1:2:1.
B, after the completion of dipping, the slurry congee in treating tank is sent to and is mounted on connection treating tank and grinding in squeezer pipeline
Grinding machine is ground, after grinding 20 seconds；Squeezer progress expression separation, which is delivered to, by conveyance conduit obtains alkali cellulose, wherein
Squeezing multiple is 2.5, and pressing temperature is 60 DEG C.The alkali cellulose fiber that squeezing obtains is crushed through pulverizer, degree of grinding 140g/
L carries out rubbing to handle obtained temperature being 40 DEG C, the slurry congee that concentration is 32%, rubbing processing after crushing through kneader twin screw device
It can make fiber sub-wire, brooming, reach the cell wall for destroying cellulose fibre, the small molecule in cellulose be removed, to improve
Fibrin reaction performance, improves cellulose combination alkali content, and alkali cellulose content reaches 6-8%；
In order to withdraw lye, in the present embodiment, it is true that dividing for squeezing out is mingled with fiber, the lye of impurity passes through filter net type
Suction random separates and recovers fiber and clean lye, removes extra hemicellulose, and wherein strainer uses 60 mesh, vacuum
Degree is -0.2MPa；
C, lye is added to be mixed to form concentration by the slurry congee that step B is prepared is 6% slurry congee, and it is poly- to be transported to orientation drop
5% pure oxygen of reactor volume is added in reactor for reactor, is oriented the poly- reaction of drop, reaction time 50min；In the step
In rapid, pure oxygen is added and aoxidize dropping and gathers, after drop is poly-, the alkali cellulose degree of polymerization is reduced to 400-600, alkali cellulose by 650-1200
Middle first fibre purity reaches 98.0-98.5%, and 2-3% can be improved than traditional handicraft.It is fine that the poly- poly- reduction first of drop more experienced than tradition drops in orientation
3-5% is lost, molecule drop is gathered more uniform, abundant；Lye uses sodium hydroxide, concentration 160g/L；
D, the alkali cellulose by step C after dropping and gathering is added in xanthating machine reacts with carbon disulfide, wherein two sulphur
The additional amount for changing carbon is 28% of first fibre content in alkali cellulose, and the yellow time is 48 min, and yellow reaction temperature is 25 DEG C；It is yellow
Change and cellulose sulfonate is made after the reaction was completed, then cellulose sulfonate and solvent are mixed by a certain percentage,
Cellulose sulfonate solution is made in grinding, final dissolve, and the additional amount of solvent is with cellulose sulfonate concentration obtained for 9.5%
Subject to, solvent is sodium hydrate aqueous solution and sodium sulfite aqueous solution mixed liquor, and concentration is respectively 30 g/L, 8 g/L, dissolution
Temperature is 15 DEG C, dissolution time 35min, and cellulose sulfonate solution is using filter, deaeration, maturation, finally obtained viscosity
The spinning solution that 40-45s, degree of ripeness 9.5-12ml, methylcellulose content be 8.8-9.0%, is 4.5-4.8% containing alkali；
According to the requirement of product, delustering agent is added by injection method before spinning solution is sent to spinning machine spinning and is uniformly mixed,
Delustering agent can choose titanium dioxide, is configured to the aqueous solution that concentration is 12% and uses；
E, spinning solution made from step (D) is sent to spinning machine, by spinning machine spray head extruding spinning liquid, then spinning solution is passed through
It crosses after one of drawing-off and forms tow into a bath, the tow by a bath is sent into two baths, bis- drawing-off of Zai Jing through one of drafting machine
Machine is sent into three baths, and the tow after three baths is sent by three drafting machines to refinery practice；
The coagulation bath composition of spinning acid bath used in it is as follows: a bath composition are as follows: sulfuric acid 90g/L, zinc sulfate 8g/L, sulphur
Sour sodium 220g/L, a bath temperature are 40 DEG C, and acid bath drop is 3g/L, and two bath compositions: temperature is 80 DEG C, sulfuric acid 18g/L, and three baths are
Sulfuric acid, temperature are 80 DEG C, pH value 1；
Wherein draft process using step by step, high drawing-off technology, wherein total draft rate control exists: 150%, spray head drawing-off be rate
Are as follows: 50%, one of degree of draft are as follows: 40%, two degree of drafts are as follows: 5%, the degree of draft of three drafting machines is 5%.
Wherein refinery practice be by strand by desulfurization, bleach, oil after obtain viscose rayon semi-dull, the present embodiment is adopted
It takes benign environment to carry out desulfurization, bleaching, reduces post-processing and strand strength and elongation is damaged；
Wherein desulfurizing agent is the mixing of vulcanized sodium and sodium carbonate, and the concentration of vulcanized sodium is 4 g/L, 1 g/L of sodium carbonate, desulfurization
Temperature is 50 DEG C, time 2min；Using vulcanized sodium as desulfurizing agent, sodium carbonate milder compared with sodium hydroxide, sodium sulfite
For neutralizing strand bring sulfuric acid；
Use hydrogen peroxide bleaching: hydrogen peroxide concentration 0.3g/L, temperature be 50 DEG C, bleaching time 1min, hydrogen peroxide compared with
The bleaching agents such as sodium hypochlorite are milder；
Oiling treatment: oil agent addition 7g/L, finish temperature are 50 DEG C, and the pH value that strand is adjusted after oiling treatment is
6.5.PH value is 6.5, and finished product strand strength and elongation will not influence.PH can be adjusted by washing；
Drying: the strand after refining Tumblies Dry, and drying temperature is 75 DEG C, after drying, obtains product.It is measured by sampling
Each index value of product.
Embodiment 16
The present embodiment and the difference of embodiment 15 are:
Raw material difference: the pulp material of the present embodiment use the cotton pulp of degree of polymerization 650-1200, bamboo pulp, wood pulp, jute pulp with
The ratio of 1:2:2:1 is applied in combination.
Process distinction:
It is 6% in dipping time control slurrying congee concentration, lye naoh concentration is 200g/L, and alkali liquid temperature is 50 DEG C, dipping
Time is 70 minutes.
Squeezing multiple when squeezing is 2.7, and pressing temperature is 61 DEG C, and milling time is 30 seconds；
When crushing, control degree of grinding is 120-180g/L, the control of smashed slurry congee concentration is 38%, and temperature is 45 DEG C；
It is 7% slurry congee that alkali cellulose after rubbing, which is added lye and is mixed to form concentration,；
When dropping poly-, pure oxygen additional amount is the 5% of reactor volume, and reaction time 45min, lye naoh concentration is
180g/L；
When yellow, the additional amount of carbon disulfide is 25% of first fibre content in alkali cellulose, and the yellow time is 50 minutes, yellow
Changing reaction temperature is 30 DEG C.
The dissolution of cellulose sulfonate: the additional amount of solvent be subject to cellulose sulfonate concentration obtained be 10.0%, it is molten
Agent is the mixing that concentration is 40 g/L sodium hydroxide water aqueous solutions and 10 g/L sodium sulfite aqueous solutions, and solution temperature is 20 DEG C,
Dissolution time is 50min,
Spinning: a bath composition are as follows: sulfuric acid 110g/L, zinc sulfate 12g/L, sodium sulphate 260g/L, temperature are 45 DEG C；Acid bath is fallen
Difference is 4g/L；Two bath compositions: temperature is 85 DEG C, and sulfuric acid 20g/L, three baths are sulfuric acid, and temperature is 85 DEG C, pH value 2；
Drawing-off: wherein the control of total draft rate is 180%, and spray head drawing-off is that rate is 80%, and one of degree of draft is 50%, and two lead
Stretching rate is 10%, and the degree of draft of three drafting 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 is 0.5g/L with hydrogen peroxide concentration, and temperature is 53 DEG C, bleaching time 2min, oiling treatment, the oil to oil
Agent additional amount is 8g/L, and finish temperature is 52 DEG C.It is 6.8 that strand pH value is reconciled after oiling；Strand pH value is adjusted by organic acid,
Drying: Tumbleing Dry, and drying temperature is 85 DEG C, and after drying, each index value is measured by sampling.
Embodiment 17
The present embodiment and the difference of embodiment 16 are:
Raw material difference: the pulp material of the present embodiment uses the degree of polymerization for the cotton pulp of 650-1200；
Process distinction:
It is 3% in dipping time control slurrying congee concentration, lye naoh concentration is 180g/L, and alkali liquid temperature is 60 DEG C, dipping
Time is 80 minutes.
Squeezing multiple when squeezing is 2.8, and pressing temperature is 63 DEG C, and milling time is 40 seconds；
When crushing, control degree of grinding is 180g/L, the control of smashed slurry congee concentration is 40%, and temperature is 60 DEG C；
It is 8% slurry congee that alkali cellulose after rubbing, which is added lye and is mixed to form concentration,；
When dropping poly-, pure oxygen additional amount is the 10% of reactor volume, and reaction time 60min, lye naoh concentration is
200g/L；
When yellow is reacted, the additional amount of carbon disulfide is 37% of first fibre content in alkali cellulose, and the yellow time is 45-50
Minute, yellow reaction temperature is 30 DEG C.
The dissolution of cellulose sulfonate: the additional amount of solvent be subject to cellulose sulfonate concentration obtained be 9.5%, it is molten
Agent is the mixing that concentration is 45 g/L sodium hydroxide water aqueous solutions and 10 g/L sodium sulfite aqueous solutions, and solution temperature is 20 DEG C,
Dissolution time is 50min,
Spinning: a bath composition are as follows: sulfuric acid 120g/L, zinc sulfate 15g/L, sodium sulphate 280g/L, temperature are 50 DEG C；Acid bath is fallen
Difference is 5g/L；Two bath compositions: temperature is 90 DEG C, and sulfuric acid 22g/L, three baths are sulfuric acid, and temperature is 90 DEG C, pH value 3；
Drawing-off: wherein the control of total draft rate is 200%, and spray head drawing-off is that rate is 100%, and one of degree of draft is 60%, and two lead
Stretching rate is 15%, and the degree of draft of three drafting 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, time 3min；
Bleaching is 0.6g/L with hydrogen peroxide concentration, and temperature is 55 DEG C, bleaching time 2min, oiling treatment, the oil agent addition to oil
For 9g/L, finish temperature is 55 DEG C.It is 7 that strand pH value is reconciled after oiling；Silk can be adjusted by washing, multiple-effect sour (organic acid)
PH value,
Drying: Tumbleing Dry, and drying temperature is 115 DEG C, and after drying, each index value is measured by sampling.
Embodiment 18
The present embodiment and the difference of embodiment 16 are:
Raw material difference: the pulp material of the present embodiment uses the degree of polymerization for the bamboo pulp of 650-1200.
Process distinction:
It is 4.5% in dipping time control slurrying congee concentration, lye naoh concentration is 150g/L, and alkali liquid temperature is 48 DEG C, leaching
The stain time is 75 minutes.
Squeezing multiple when squeezing is 2.5, and pressing temperature is 60 DEG C, and milling time is 25 seconds；
When crushing, control degree of grinding is 120-180g/L, the control of smashed slurry congee concentration is 35%, and temperature is 45 DEG C；
It is 5% slurry congee that alkali cellulose after rubbing, which is added lye and is mixed to form concentration,；
When dropping poly-, pure oxygen additional amount is the 8% of reactor volume, and reaction time 45min, lye naoh concentration is
190g/L；
When yellow is reacted, the additional amount of carbon disulfide is 35.5% of first fibre content in alkali cellulose, and the yellow time is 45
Minute, yellow reaction temperature is 25 DEG C.
The dissolution of cellulose sulfonate: the additional amount of solvent be subject to cellulose sulfonate concentration obtained be 9.5%, it is molten
Agent is the mixed liquor that concentration is 35 g/L sodium hydroxide water aqueous solutions and 7.5 g/L sodium sulfite aqueous solutions, solution temperature 15
DEG C, dissolution time 40min,
Spinning: a bath composition are as follows: sulfuric acid 110g/L, zinc sulfate 12g/L, sodium sulphate 240g/L, temperature are 45 DEG C；Acid bath is fallen
Difference is 4g/L；Two bath compositions: temperature is 85 DEG C, and sulfuric acid 20g/L, three baths are sulfuric acid, and temperature is 85 DEG C, pH value 2.5；
Drawing-off: wherein the control of total draft rate is 170%, and spray head drawing-off is that rate is 75%, and one of degree of draft is 55%, and two lead
Stretching rate is 12%, and the degree of draft of three drafting 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, time 3min；
Bleaching is 0.5g/L with hydrogen peroxide concentration, and temperature is 52 DEG C, bleaching time 2min, oiling treatment, the oil agent addition to oil
For 7g/L, finish temperature is 50 DEG C.It is 7 that strand pH value is reconciled after oiling；Silk can be adjusted by washing, multiple-effect sour (organic acid)
PH value,
Drying: Tumbleing Dry, and drying temperature is 100 DEG C, and after drying, each index value is measured by sampling.
Embodiment 19
The present embodiment and the difference of embodiment 16 are:
Raw material difference: the pulp material of the present embodiment presses 2:3:1:3 using the cotton pulp of 650-1200, bamboo pulp, wood pulp, jute pulp
Ratio be used in mixed way.
Process distinction:
It is 5% in dipping time control slurrying congee concentration, lye naoh concentration is 140g/L, and alkali liquid temperature is 50 DEG C, dipping
Time is 65 minutes.
Squeezing multiple when squeezing is 2.6, and pressing temperature is 60 DEG C, and milling time is 40 seconds；
When crushing, control degree of grinding is 160g/L, the control of smashed slurry congee concentration is 33%, and temperature is 50 DEG C；
It is 6.5% slurry congee that alkali cellulose after rubbing, which is added lye and is mixed to form concentration,；
When dropping poly-, pure oxygen additional amount is the 4% of reactor volume, and reaction time 40min, lye naoh concentration is
160g/L；
When yellow, the additional amount of carbon disulfide is 33% of first fibre content in alkali cellulose, and the yellow time is 48 minutes, yellow
Changing reaction temperature is 24 DEG C.
The dissolution of cellulose sulfonate: the additional amount of solvent be subject to cellulose sulfonate concentration obtained be 9.0%, it is molten
Agent is the mixing that concentration is 40 g/L sodium hydroxide water aqueous solutions and 5 g/L sodium sulfite aqueous solutions, and solution temperature is 17 DEG C, molten
The solution time is 40min,
Spinning: a bath composition are as follows: sulfuric acid 115g/L, zinc sulfate 13g/L, sodium sulphate 260g/L, temperature are 40 DEG C；Acid bath is fallen
Difference is 4.5g/L；Two bath compositions: temperature is 82 DEG C, and sulfuric acid 21g/L, three baths are sulfuric acid, and temperature is 85 DEG C, pH value 1.5；
Drawing-off: wherein the control of total draft rate is 190%, and spray head drawing-off is that rate is 80%, and one of degree of draft is 50%, and two lead
Stretching rate is 7%, and the degree of draft of three drafting 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, time 3min；
Bleaching is 0.5g/L with hydrogen peroxide concentration, and temperature is 50 DEG C, bleaching time 1.5min, and oiling treatment, the finish to oil is added
Amount is 9g/L, and finish temperature is 53 DEG C.It is 7 that strand pH value is reconciled after oiling；Strand pH value can be adjusted by washing,
Drying: Tumbleing Dry, and drying temperature is 90 DEG C, and after drying, each index value is measured by sampling.
Each index value of viscose rayon obtained by measuring embodiment 1-19, embodiment 1-7 data statistics is summarized in down
In table 1, embodiment 8-14 statistical induction is in table 2, and embodiment 15-19 statistical induction is in table 3；
Table 4 is superfine type of the present invention high-strength flatness viscose rayon semi-dull and common viscose fiber, Modal fibre, difference
It is right to change viscose rayon (CN102296373A documents 1, CN1632189 documents 2, CN102251301A documents 3)
Than data:
Table 1
Table 2
Table 3
Table 4
By the data of upper table 1,2,3 and 4 it is found that viscose rayon of the invention, which has, is different from common viscose fiber, not generation
That fiber, the innovative new index system of differential viscose rayon, can effectively substitute high-cost Modal fibre, mention
While high viscose rayon downstream process processing performance, moreover it is possible to which the exploitation and industrial upgrading for promoting downstream new textile have
Good economic benefit and social benefit.
Embodiment 20
Secondary response interface is to inhale color ability to dyestuff according to fiber cross section to be differently formed, i.e. the cortex and core of fiber
Layer, cortex are small to dyestuff suction color ability, and dyeing is partially shallow, and sandwich layer is big to dyestuff suction color ability, and color is partially deep, and cortex is with higher
The degree of orientation, cortex is more, and breaking strength is higher, and sandwich layer is more, and water swelling capacity is higher；Therefore the present embodiment is by embodiment 1-19
Any one viscose rayon of middle gained, common viscose fiber, Modal viscose rayon do fibre section after dyeing is handled, aobvious
Amplify 2000 times of observations under micro mirror, is sliced coloration result such as the following table 5；
Table 5
By upper table 5 it is found that common viscose fiber (tencel) is handled through dyeing, as shown in figure 3, its fiber inner, middle and outer layer obtains
Color depth shallowly differs greatly, and outer layer is obviously partially shallow, and middle layer and internal layer are partially deep, there are secondary response interface, but the inclined outer layer in interface, it surveys
The sandwich layer and cortex " area " ratio for determining fiber are (90~95): (5~10), the inclined internal layer of ratio, ectonexine ratio are not enough to protect
Card fiber has the characteristics that high-strength, flatness, fiber are easily-deformable.
Fibre section is done after Modal fibre dyeing, is observed under the microscope, as shown in Fig. 2, without secondary response interface, this
For the viscose rayon and Modal fibre of invention under same dyeing condition, viscose rayon of the invention inhales color depth than Modal, on
Dye rate is high, and uniformity is more preferable, and the good color fastness of finished product.
As shown in Figure 1, the color of its fiber inner, middle and outer layer of viscose rayon of the present invention is deep, shallowly differs greatly, outer layer is in
Layer is partially shallow, and internal layer is obviously partially deep, there are clear, apparent secondary response interface, measuring microscope sectional area, and, sandwich layer, cortex
" area " ratio is (40~70): (30~60), ratio is moderate, therefore viscose rayon of the invention is compared with common viscose fiber,
Have the characteristics that high-strength, flatness, while also there is water imbibition appropriate, fiber skin-friendly has significant advantage.
Embodiment 21
The Denier range and other indication ranges of viscose rayon semi-dull of the present invention are wider, therefore, are actually answering
With, viscose rayon semi-dull can be used for producing different products respectively according to the difference of its indication range having,
1,0.8~1.11 dtex of fiber number (D) is included
Dry breaking strength >=3.15 cN/dtex, wet breaking strength >=1.70cN/dtex,
Intensity >=0.6cN/dtex needed for 5% elongation is generated under wet condition,
Wet elongation at break 16~21%, dry elongation at break 15.0~19.0%,
Radial water swelling capacity 22~26%, 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%,
Overlength fiber rate≤0.5%, over-length fibre≤1.0mg/100g,
Whiteness >=84%, the viscose rayon of fault≤1.0mg/100g index system mainly apply to close SEILE textile neck
Domain, the high twirl of production, high grade cotton yarn product, characterized by product strength height is suitable for the domain requirements such as high twirl.Such as embodiment 6,7,9
Viscose rayon semi-dull.
2,0.8~1.11 dtex of fiber number (D) is included
Dry breaking strength >=3.20 cN/dtex, wet breaking strength >=1.70cN/dtex,
Intensity >=0.6cN/dtex needed for 5% elongation is generated under wet condition,
Wet elongation at break 16~21%, dry elongation at break 13.0~16.0%,
Radial water swelling capacity 22~26%, 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%,
Overlength fiber rate≤0.5%, over-length fibre≤1.0mg/100g,
Whiteness >=84%, the viscose rayon of fault≤1.0mg/100g index system mainly apply to produce underwear, top grade
Shuttle-woven fabric field is characterized with sliding soft, the comfortable pro-skin of product feel silk and finished textile product good stability of the dimension.Strictly according to the facts
Apply example 7,8,12,17,19 etc..
3,0.8~1.11 dtex of fiber number (D) is included
Dry breaking strength >=3.10 cN/dtex, wet breaking strength >=1.60cN/dtex,
Intensity >=0.55cN/dtex needed for 5% elongation is generated under wet condition,
Wet elongation at break 16~21%, dry elongation at break 12~14.5%,
Radial water swelling capacity 22~26%, 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%,
Overlength fiber rate≤0.5%, over-length fibre≤1.0mg/100g,
The viscose rayon of whiteness >=84%, fault≤1.0mg/100g index system is raw in mainly applying to denim fabric
Production field is characterized so that bright, soft and finished textile product modification is small.Such as embodiment 6,12,17,19.
Claims (16)
1. superfine type high-strength flatness viscose rayon semi-dull, it is characterised in that: the viscose rayon has following performance indicators:
Fiber number is 0.8~1.11dtex, dry breaking strength >=3.10 cN/dtex, wet breaking strength >=1.60cN/dtex,
Intensity >=0.55cN/dtex needed for 5% elongation is generated under wet condition,
Dry elongation at break 11.0~19.0%, wet elongation at break 16.0~21.0%,
Crystallinity 40~45.0%, radial water swelling capacity 22~26%
Dulling agent content 0.1-0.75%；
The superfine type high-strength flatness viscose rayon semi-dull is prepared by following step:
A: pulp material is impregnated in the treating tank equipped with lye, and the slurry congee that concentration is 3~6% is made after being ground by grinder；
B: slurry congee made from step A being sent to squeezer, send after squeezing to pulverizer and is crushed, obtains alkali cellulose, will
The alkali cellulose is sent to kneading machine, and the slurry congee that concentration is 30~40% is obtained after processing；
C: sending after slurry congee made from step B is mixed with lye to reactor, and pure oxygen is added in the reactor, is gathered after drop is poly-
It is right be 400~600, the alkali cellulose that first fibre purity is 98.0~98.5%；
D: alkali cellulose made from step C being sent to xanthating machine, carbon disulfide is added in xanthating machine, will after yellow is reacted
The cellulose sulfonate and solvent that yellow is reacted dissolve, and the cellulose sulfonate solution that concentration is 9.0~10.0% is made；
E: cellulose sulfonate solution made from step D is obtained into spinning solution after filtering, deaeration, maturation, delustring is added in spinning
Viscose rayon is made after spinning drawing and refining, drying in agent；In the step C, the lye be concentration 140~
The sodium hydroxide solution of 200g/L, the additional amount of pure oxygen is the 2~10% of reactor volume in reactor, drops poly- reaction time control
System is in 30~60min；In the step E, steps are as follows for the spinning drawing:
F: cellulose sulfonate solution is sent after filtering, deaeration, maturation to spinning machine, thin by the spray head extruding spinning of spinning machine
Tow is formed after flowing through a bath, the coagulating bath that a bath uses includes the sulfuric acid of the sulfuric acid of 90~120g/L, 220~280g/L
The zinc sulfate of sodium and 8~15g/L；
G: the tow after a bath is sent into two baths by one of drafting machine, and the coagulating bath that two bath uses includes 18~22g/L's
Sulfuric acid, the degree of draft of one of drafting machine are 50~100%；
H: the tow after two baths is sent into three baths by two drafting machines, and it is 1~3 that the coagulating bath that three bath uses, which includes pH value,
Sulfuric acid, the degree of draft of two drafting machine are 40~60%；
I: the tow after three baths is sent by three drafting machines to post-processing part, and the degree of draft of three drafting machine is 5~
15%。
2. the preparation method of superfine type high-strength flatness viscose rayon semi-dull according to claim 1, it is characterised in that: institute
The degree of polymerization for stating pulp material is 650~1200.
3. superfine type high-strength flatness viscose rayon semi-dull according to claim 1, it is characterised in that: the pulp is former
Material is the combination of one of cotton pulp, bamboo pulp, wood pulp, jute pulp or two or more arbitrary proportions.
4. superfine type high-strength flatness viscose rayon semi-dull according to claim 1, it is characterised in that: in the step
In A, the lye is the sodium hydroxide solution of 110~240g/L of concentration, and the temperature of steeping liquor is 30~60 DEG C, when dipping
Between be 50~90min.
5. superfine type high-strength flatness viscose rayon semi-dull according to claim 1, it is characterised in that: in the step
In A, the grinder is set in the pipeline of connection treating tank and squeezer.
6. superfine type high-strength flatness viscose rayon semi-dull according to claim 1, it is characterised in that: in the step
In A, the temperature of the slurry congee is 30~60 DEG C, and the milling time of the grinder is 10~40s.
7. superfine type high-strength flatness viscose rayon semi-dull according to claim 1, it is characterised in that: in the step
In B, the pressing temperature of the squeezer is 57~63 DEG C, squeezing multiple is 2.2~2.8.
8. superfine type high-strength flatness viscose rayon semi-dull according to claim 1, it is characterised in that: in the step
In B, the degree of grinding of the pulverizer is 120~180g/L.
9. superfine type high-strength flatness viscose rayon semi-dull according to claim 1, it is characterised in that: in the step
In D, the additional amount of carbon disulfide is 35~37% of first fibre content in alkali cellulose made from step B.
10. superfine type high-strength flatness viscose rayon semi-dull according to claim 1, it is characterised in that: in the step
In rapid D, in 45~50min, yellow reaction temperature is 20~30 DEG C for the yellow reaction time control.
11. superfine type high-strength flatness viscose rayon semi-dull according to claim 1, it is characterised in that: in the step
In rapid D, the dissolution is that cellulose sulfonate is mixed, stirred and ground with solvent, and the solvent includes concentration
The sodium sulfite aqueous solution for being 5~10 g/L for 25~45 g/L sodium hydrate aqueous solutions and concentration.
12. superfine type high-strength flatness viscose rayon semi-dull according to claim 1, it is characterised in that: in the step
In rapid D, the solution temperature is 10~20 DEG C, and dissolution time is 30~50min.
13. superfine type high-strength flatness viscose rayon semi-dull according to claim 1, it is characterised in that: in the spinning
In filament drafting step, a bath temperature is 40~50 DEG C, two bath temperatures are 80~90 DEG C, three bath temperatures are 80~90 DEG C.
14. superfine type high-strength flatness viscose rayon semi-dull according to claim 1, it is characterised in that: in the step
In rapid E, the refining includes the desulfurization carried out to the tow that spinning drawing is formed, bleaches and oil, what the desulfurization used
The sodium carbonate that the vulcanized sodium and concentration that desulfurizing agent is 4~8g/L by concentration are 1~4g/L forms；It is described to bleach the bleaching agent used
For the hydrogen peroxide of 0.3~0.6g/L of concentration；The oil agent addition used that oils is 7~9g/L, the pH value of tow after oiling
It is 6.5~7.
15. superfine type high-strength flatness viscose rayon semi-dull according to claim 14, it is characterised in that: the desulfurization
Temperature is 50~55 DEG C, and desulfurization time is 2~3min；The bleaching temperature is 50~55 DEG C, and bleaching time is 1~2min；
The temperature of the finish is 50~55 DEG C.
16. superfine type high-strength flatness viscose rayon semi-dull according to claim 1, it is characterised in that: in the step
In rapid E, the drying is will to refine obtained tow using drying machine drying, and drying temperature is 75~115 DEG C.
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