CN104846453B - Superfine viscose fiber and preparation method thereof - Google Patents
Superfine viscose fiber and preparation method thereof Download PDFInfo
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- CN104846453B CN104846453B CN201510275873.8A CN201510275873A CN104846453B CN 104846453 B CN104846453 B CN 104846453B CN 201510275873 A CN201510275873 A CN 201510275873A CN 104846453 B CN104846453 B CN 104846453B
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- 229920000297 Rayon Polymers 0.000 title claims abstract description 182
- 239000000835 fiber Substances 0.000 title claims abstract description 165
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000009987 spinning Methods 0.000 claims abstract description 49
- 229920000742 Cotton Polymers 0.000 claims abstract description 26
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 238000000227 grinding Methods 0.000 claims abstract description 16
- 238000004090 dissolution Methods 0.000 claims abstract description 15
- 238000004898 kneading Methods 0.000 claims abstract description 10
- 238000007598 dipping method Methods 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 141
- 229920002678 cellulose Polymers 0.000 claims description 109
- 239000001913 cellulose Substances 0.000 claims description 109
- 239000003513 alkali Substances 0.000 claims description 105
- 239000000243 solution Substances 0.000 claims description 71
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 54
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 48
- 239000002002 slurry Substances 0.000 claims description 41
- 238000006477 desulfuration reaction Methods 0.000 claims description 35
- 230000023556 desulfurization Effects 0.000 claims description 35
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 35
- 239000000463 material Substances 0.000 claims description 34
- 238000001035 drying Methods 0.000 claims description 30
- 239000002904 solvent Substances 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 26
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 22
- 230000001112 coagulating effect Effects 0.000 claims description 22
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 22
- 238000006116 polymerization reaction Methods 0.000 claims description 20
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 18
- 238000004061 bleaching Methods 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 16
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- 239000003921 oil Substances 0.000 claims description 15
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- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 230000035484 reaction time Effects 0.000 claims description 13
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- 229920001131 Pulp (paper) Polymers 0.000 claims description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 12
- 230000035800 maturation Effects 0.000 claims description 11
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 11
- 235000010265 sodium sulphite Nutrition 0.000 claims description 11
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 10
- 229910052708 sodium Inorganic materials 0.000 claims description 10
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- 238000003825 pressing Methods 0.000 claims description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- 150000004679 hydroxides Chemical class 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 29
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- 238000011161 development Methods 0.000 abstract description 5
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- 238000003556 assay Methods 0.000 description 11
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- 229920000433 Lyocell Polymers 0.000 description 10
- 230000008859 change Effects 0.000 description 10
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 8
- 229960001763 zinc sulfate Drugs 0.000 description 8
- 229910000368 zinc sulfate Inorganic materials 0.000 description 8
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 7
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- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 description 4
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- 238000005213 imbibition Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 240000007594 Oryza sativa Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 229920004933 Terylene® Polymers 0.000 description 3
- 238000007380 fibre production Methods 0.000 description 3
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- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 208000019901 Anxiety disease Diseases 0.000 description 2
- 244000007853 Sarothamnus scoparius Species 0.000 description 2
- 239000005708 Sodium hypochlorite Substances 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
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- 150000003384 small molecules Chemical class 0.000 description 2
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-N sulfonic acid Chemical compound OS(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-N 0.000 description 2
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- 229920002972 Acrylic fiber Polymers 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 240000000731 Fagus sylvatica Species 0.000 description 1
- 235000004994 Fagus sylvatica subsp sylvatica Nutrition 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 206010016590 Fibrin deposition on lens postoperative Diseases 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical group [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000003287 bathing Methods 0.000 description 1
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- Artificial Filaments (AREA)
Abstract
The invention discloses a superfine viscose fiber and a preparation method thereof, the viscose fiber is prepared by pulp raw materials through dipping, grinding, squeezing and crushing, kneading, pure oxygen precipitation, yellowing, dissolution, filtration, defoaming, ripening, spinning drafting and post-treatment in sequence, and the viscose fiber satisfies the following requirements: the fineness is 0.88-1.11D, the dry breaking strength is more than or equal to 3.20 cN/dtex, and the wet breaking strength is more than or equal to 1.60 cN/dtex. The 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, shows the fiber characteristics of the modal fibers such as high strength and low elongation, has stronger skin-friendly performance than cotton fibers, can effectively replace the existing differential viscose fiber, improves the processability of the downstream process of the viscose fiber, and can promote the development and industrial upgrading of downstream novel textiles.
Description
Technical field
A kind of superfine type viscose rayon of the present invention and preparation method thereof is related to field, and in particular to superfine type viscose staple fibre
The technology controlling and process of kind and preparation method thereof, belongs to the innovation of viscose staple fibre and cellulose fibre production technical field.
Background technology
Current textile fiber material is broadly divided into the natural fiber raw material with cotton, fiber crops etc. for representative, is with terylene, acrylic fibers etc.
The petroleum base fibrous raw material of representative, and the bio-based fiber such as the viscose rayon regenerated by raw material of natural cellulosic materials
Raw material.At present, with rare and human resources the anxiety of land resource, sown areas of cotton are in downward trend year by year, cotton
Product can not meet people's living standard it is growing the need for；And the increasingly reduction and people with petroleum reserves are to weaving
Product comfortableness, feature, the continuous enhancing of environment-friendly type consciousness, the viscose rayon produced by raw material of recyclability resource is increasingly
Many is taken seriously.For viscose rayon, as natural regeneration fiber, the quality of its existing natural fiber has excellent again
Good machinability, its structure composition is similar to cotton, not only with hygroscopicity height, good permeability, comfortable and easy to wear, easy dyeing, resistance to
The high temperatures multifrequency nature such as strong, meanwhile, there is the unexistent drapability of cotton and flexibility again, certainly, due to viscose rayon tool
These standby excellent properties, develop very rapid, the particularly viscose rayon scale of common variety drastically swollen in recent years
Swollen, this phenomenon causes raw material supply anxiety, and market harmful competition is fierce, at the same time, more limits downstream Novel Spinning
The exploitation of fabric and industrial upgrading.
Based on above-mentioned situation, to promote the sustainable development of viscose rayon industry, differential, functionalization viscose rayon is produced
Newly marked as current industry.Patent document CN102296373A（A kind of production method of superfine high-strength high-modulus viscose fiber,
2011.12.28）Disclose a kind of viscose glue fibre that a kind of even structure, fibre strength and modulus are higher by conventional variety more than 50%
Dimension, the fibre strength of obtained viscose rayon is 0.44~0.78dtex, does strong >=3.1cN/dtex（Li ox/dtex）, it is wet strong
>=2.1cN/dtex, wet modulus >=0.5cN/dtex, whiteness >=82.0%.
Patent document CN100359050C（A kind of high white strength fine denier viscose staple fiber and its production technology,
2005.06.29）The short rayon fiber that a kind of fiber number is thin, intensity is high is disclosed, by the garment material of its processing compared with common viscose fiber
For have the advantages that intensity is high, wearability is strong, feel is fine and smooth, anti-fold, resistance to multiple deformation, it may also be used for weaving high grade cotton yarn
Fabric products.
Patent document CN102251301A（A kind of production process of ultrafine-denier high-strength viscose fibers, 2011.11.23）Disclose
A kind of preparation method for the viscose rayon that fiber number is low, intensity is high, it is that 1.11 dtexs and intensity are more than 2.9 cN/ that can obtain fiber number
Dtex viscose rayon.
Patent document only disclosed above can know that, for differential, functionalization viscose rayon is made, prior art is equal
It is to be realized by way of changing production technology, wherein, include raw material, viscose glue shaping 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, differential viscose rayon does not meet the exploitation and production of downstream new textile to a greater extent
Industry is upgraded, and the fiber such as especially same tencel, Modal, CUP regenerated by raw material of natural cellulosic materials is former
The development of material so that the occupation rate of market of viscose rayon is reduced increasingly.Such as：Patent document CN101130885（Numb material viscose rayon
Preparation method and preparation numb material viscose rayon, 2008.02.27）Disclose a kind of viscose glue using numb material plant production fine
Dimension and its preparation technology, technique are simple, and supplies consumption is low, and the numb material viscose rayon of production has excellent whiteness, intensity
With the performance such as elongate fiber, the numb material viscose rayon prepared by the technique meets the cN/ of dry fracture strength >=1.820
Dtex, the cN/dtex of wet breaking strength >=1.12, dry elongation at break >=15.4%, line density deviation ratio ± 6.00%, length is inclined
Rate ± 6.00%, overlength fiber rate≤1.0%, over-length fibre≤18.0mg/100g, fault≤11mg/100g, residual sulphur≤
18.0mg/100g。
By taking Modal fibre as an example, it is known that Modal fibre is using European beech as raw material, it is made after wooden slurries
It is made by special spinning technique, belongs to natural fiber raw material together as cotton, the whole of Modal fibre produced
There is no any pollution in journey, it dry strong close to terylene is wet to improve many than common viscose fiber by force, whether light
Pool, flexibility, hygroscopicity, dyeability, dyefastness are superior to Pure cotton Product, the fabric made with it, not show only one
Silk face gloss is planted, feels with more pleasant soft touch and pendency sense and fabulous endurable performance, is a kind of preferable ring
Protect fiber type cellulose fiber.But because Modal fibre textile technology is costly, the Modal circulated on the market substantially belongs to
Modal and cotton blend, or directly take viscose glue（People cotton）Fiber pretends to be Modal.
Therefore, we, which need to find one kind, is different from natural fiber raw material and petroleum base fibrous raw material, performance is again better than poor
Not Hua viscose rayon New Viscose Fibre, people can not only be met to natural prodcuts（Such as：Modal fibre）Requirement, moreover it is possible to
It is that enterprise brings larger economic benefit suitable for industrialized continuous production, certainly, this is also that viscose rayon industry can continue
The inexorable trend of development.
The content of the invention
It is an object of the invention to provide a kind of superfine type viscose rayon, the viscose rayon is different from traditional viscose rayon production
Product and cotton are fine, are the tencel kinds realized by technological innovation, with being different from common viscose fiber and Modal is fine
The index system of dimension, its product not only shows that Modal fibre is high-strength, flatness fiber characteristics, also shows fine compared with cotton
Stronger skin-friendly, can effectively substitute existing differential viscose rayon, improve viscose rayon lower procedure processing characteristics
While, moreover it is possible to promote exploitation and the industrial upgrading of downstream new textile, with good social benefit.
Another object of the present invention is to provide a kind of preparation method of superfine type viscose rayon, this preparation method is with pulp
Raw material is prepared by viscose glue, is made in viscose rayon, production process after spinning technique and post processing, still protected as raw materials for production
Secondary response microscope sectional area has been stayed, and the ectonexine area ratio at the interface is clearly distinguishable from Modal fibre and common viscous
The secondary response vestige of glue fiber, it is ensured that the characteristics of product has high-strength, flatness, at the same also have appropriate water imbibition with
And significant fiber skin-friendly.
The present invention is achieved through the following technical solutions：A kind of superfine type viscose rayon and preparation method thereof, described viscose glue
Fiber is using pulp material is impregnated successively, grinding, squeezing are crushed, rubbing, pure oxygen drop poly-, yellow, dissolving, filtering, deaeration, ripe
It is made after into, spinning drawing and post processing, the viscose rayon is met：
0.88~1.11D of fiber number, does the cN/dtex of fracture strength >=3.20, wet breaking strength >=1.60cN/dtex,
Intensity >=0.55cN/dtex needed for 5% elongation is produced under wet condition,
Dry elongation at break 12.0~17.5%, wet elongation at break 18.0~21.0%,
Crystallinity 40.0~45.0%, radial water swelling capacity 22~26%.
The fiber number of viscose rayon of the present invention belongs to plain edition viscose rayon product between 0.88~1.11D, tool
There is high-strength, flatness product performance, while also having high water absorption characteristic, imparting product has very strong skin-friendly, is much better than
Modal, is the great innovation of viscose staple fibre and cellulose fibre production technical field slightly better than natural cotton.
Further, described high-strength flatness viscose rayon is also met：
Line density deviation ratio≤± 4.0%, whiteness >=83%,
Residual sulphur≤12.0mg/100g, length variation rate≤± 6.0%,
Overlength fiber rate≤0.5%, over-length fibre≤4.0mg/100g,
Fault≤4.0mg/100g, dry ultimate strength mutation coefficient 18%.
Described pulp material includes the combination of the one or two kinds of and the above in cotton pulp, bamboo pulp, wood pulp, jute pulp,
During practical application, cotton pulp, bamboo pulp, wood pulp, jute pulp can be mixed in any proportion.
The invention also provides a kind of preparation method for having a high-strength flatness viscose rayon of light type, comprise the following steps：
A：By pulp material soda-dip, then ground, squeezing crush, rub after slurry congee is made；
B：Reactor is sent into after slurry congee is mixed with alkali lye, is dropped using pure oxygen and obtains alkali cellulose after gathering；
C：The cellulose sulfonate that alkali cellulose is obtained with carbon disulfide reaction is dissolved using solvent, cellulose sulfonic acid is obtained
Ester solution；
D：Spinning solution is made in cellulose sulfonate solution after filtering, deaeration, maturation, then by the spinning solution of acquisition through spinning
High-strength flatness viscose rayon is made after filament drafting and post processing.
In the production process of product, fibrous inside molding structure leaves obvious secondary response indication character, still protects
Stayed secondary response microscope sectional area, fibre section will be done after viscose fiber staining of the present invention, with common viscose glue
During the stained slice contrast of fiber and Modal fibre, it is found that it reacts, and vestige is high-visible, and interface ratio is moderate, really
The characteristics of product has high-strength, flatness is protected, while also having appropriate water imbibition, fiber skin-friendly has significant advantage.
Above-mentioned secondary response microscope interface is inhaled color ability difference to dyestuff according to fiber cross section and formed, i.e. fiber
Cortex, sandwich layer.Cortex is few to dyestuff suction color, dyes partially shallow；Sandwich layer inhales color ability to dyestuff greatly, and color is partially deep.Cortex has
The higher degree of orientation, cortex is more, and fracture strength is high, and sandwich layer is more, and water swelling capacity is high, from viscose rayon of the present invention
Speech, its fibrocortex is more, and fibre strength is improved so as to effective.
In described step A, the degree of polymerization is 650~1,200 110~240g/L of pulp material concentration hydroxide
Sodium solution impregnates 50~90min, then ground, squeezing crush, rub after be made slurry congee, the concentration of slurry congee is 30~40%.
Step A can be specifically summarized as follows：
1）The degree of polymerization is firstly placed to feed on the machine dregs of rice for 650~1200 pulp material, sets after certain rate of feeding, such as
40kg/min, is added to equipped with alkali lye（110~240g/L of concentration sodium hydroxide solution）Treating tank in, dipping 50~
90min, is ground by grinder and the slurry congee that concentration is 3~6% is made after 10~40s, the purpose of grinding is to fibre by mechanism
Dimension carries out shredding and scattered, so as to improve the alkalization speed and alkalization rate of cellulose；
2）3~6% slurry congee is sent to squeezer, and pulverizer is delivered to after squeezing and is crushed, and it is 29 to obtain the fine content of first
~31%, alkali content is 15~17% alkali cellulose, in this step, and squeezing function removes unnecessary alkali lye, the pressure of squeezer
Squeeze temperature be 57~63 DEG C, squeezing multiple be 2.2~2.8, the degree of grinding of pulverizer is that half fibre contains in 120~180g/L, alkali lye
Amount control prepares alkali cellulose data with traditional viscose rayon and compared in 10g/L, and alkali cellulose produced by the present invention half is fine
Low, product strength is high, and the processing mode of the alkali lye is to use the mesh of filter screen 60~120, vacuum -0.4~-0.1MPa filter
Alkali fiber is reclaimed after removing hemicellulose unnecessary in alkali lyeElement, kneading machine uses twin screw device, can make fiber sub-wire, broom
Change, reach the effect of destruction cellulose fibre cell membrane, the small molecule in cellulose is removed, so as to improve cellulose reactive
Can, cellulose combination alkali content is improved, 6~8% are reached（Mass percent）；
3）The alkali cellulose is delivered into kneading machine, the slurry congee that concentration is 30~40% is obtained after processing.
In described step B, slurry congee is sent into after being mixed with concentration for 140~200g/L sodium hydroxide solution to react
Device, the addition that pure oxygen in the alkali cellulose for obtaining that the degree of polymerization is 400~600 after gathering, reactor is dropped using pure oxygen is 2~10%,
Poly- reaction time control is dropped in 30~60min.
In stepb, the purpose of addition pure oxygen is that oxidation drop is poly-, and after gathering through drop, the alkali cellulose degree of polymerization is by 650~1200
400~600 are reduced to, first fibre purity is 98.0~98.5%, and first fibre purity is higher, 2~3%, orientation drop can be improved than traditional handicraft
Poly- drop more experienced than tradition gathers reduction first fibre loss 3~5%, and molecule drop is gathered more uniformly, fully.
In described step C, described solvent be 25~45 g/L sodium hydroxide solutions including concentration and concentration be 5~
10 g/L sodium sulfite aqueous solution；The addition of carbon disulfide be the fine content of first in alkali cellulose made from step B 25~
37%, the concentration of the cellulose sulfonate solution of acquisition is 9.0~10.0%.
Step C can be specifically summarized as follows：
1）Alkali cellulose made from step B is sent to xanthating machine, and the fine content 25 of first in alkali cellulose is added in xanthating machine
~37% carbon disulfide, in practical application, carbon disulfide addition is very few, yellow reaction is incomplete, filtration difficulty；Two sulphur
Change carbon addition is too high, and yellow overreact, accessory substance is more；
2）After being reacted through yellow, obtained cellulose sulfonate is reacted into yellow and dissolved with solvent, be made concentration be 9.0~
10.0% cellulose sulfonate solution, dissolving is that cellulose sulfonate is mixed with solvent, stirred and is ground, dissolving temperature
Spend for 10~20 DEG C, dissolution time is 30~50min.
For the further product performance for improving viscose rayon, the present invention is also improved spinning drawing technique, is wrapped
Include low sour high salt and relax acid bath technique and high stretching spinning modeling technique etc., be in particular in, in described step D, spinning drawing
Step is as follows：
E：Cellulose sulfonate solution is delivered into spinning-drawing machine after filtering, deaeration, maturation, is extruded and spun by the shower nozzle of spinning-drawing machine
Silk thread forms tow after being bathed through one, and coagulating bath that a bath is used includes 90~120g/L sulfuric acid, 220~280g/L
The zinc sulfate of sodium sulphate and 8~15g/L a, bath temperature is 40~50 DEG C；
F：Tow after being bathed through one is sent into two by one of drafting machine and bathed, and the coagulating bath that two bath is used includes 18~22g/
L sulfuric acid, the degree of draft of one of drafting machine is 50~100%, and two bath temperatures are 80~90 DEG C；
G：Tow after being bathed through two is bathed by two road drafting machine feedings three, and it is 1 that the coagulating bath that three bath is used, which includes pH value,
~3 sulfuric acid, the degree of draft of two road drafting machine is 40~60%, and three bath temperatures are 80~90 DEG C；
H：Tow after being bathed through three delivers to post processing part by three road drafting machines, and the degree of draft of three road drafting machine is 5
~15%.
As described above, the present invention is using three bath wet spinning technologies, viscose glue forms tow after draw-spinning process, it is ensured that
Many secondary responses of fiber, in the process, fibre section can form clearly secondary response microscope interface, fine with improving
Intensity, increase fibrous absorbent speed and the characteristic for increasing fiber water-retaining property are tieed up, in spinning technique, tow passes through one of drawing-off
Machine, two road drafting machines, three road drafting machines are stretched, and are more beneficial for improving the fragility of fiber, are improved the degree of stretching of fiber.
In described step D, post processing includes the desulfurization of the tow progress to spinning drawing formation, bleaches and oil,
The sodium carbonate that the vulcanized sodium and concentration that the desulfurizing agent that the desulfurization is used is 4~8g/L by concentration are 1~4g/L is constituted；The drift
The bleaching agent used in vain is 0.3~0.6g/L of concentration hydrogen peroxide；The finish addition used that oils is 7~9g/L, on
The pH value of tow is 6.5~7 after oil.
The present invention uses gentle sulfur removal technology, reduces the damage of product strength, degree of stretching, in actual use, vulcanization
The more existing sodium hydroxide used of desulfurizing agent, the sodium sulfite of sodium and sodium carbonate composition are gentleer, and sodium carbonate can neutralize tow
After the sulfuric acid brought from acid bath, sulfur removal technology, the pH value of tow is can adjust 8~11；Hydrogen peroxide bleaching agent is compared with sodium hypochlorite
Gentleer Deng bleaching agent, the pH value of viscose rayon prepared by the present invention should be controlled in the range of 6.5~7, can also by washing,
Multiple-effect acid（Organic acid）Mode adjust pH value, within the range, the strength and elongation of viscose final product is unaffected, Qiang Shen
Degree is high.
Further, described desulfurization temperature is 50~55 DEG C, and desulfurization time is 2~3min；Described bleaching temperature is
50~55 DEG C, bleaching time is 1~2min；The temperature of the finish is 50~55 DEG C.
To obtain qualified high-strength flatness viscose rayon product, in the present invention, described post processing also includes drying, institute
The drying stated is that the desulfurization carried out to the tow of spinning drawing formation, the tow bleached and obtained after oiling are dried using dryer
Dry, drying temperature is 75~115 DEG C, after drying, obtains high-strength flatness viscose rayon product, the control of product regain 11~
13.5%。
The present invention compared with prior art, with advantages below and beneficial effect：
（1）Viscose rayon of the present invention is the tencel kind realized by technological innovation, belongs to viscose glue short
The great innovation of fiber and cellulose fibre production technical field, the viscose rayon is different from traditional viscose rayon product and cotton
Fibre, with the index system for being different from common viscose fiber and Modal fibre, fiber number reaches for 0.88~1.11D fibre strength
It is higher by 30% or so than common bio-based chopped fiber intensity to more than 3.2cN/dtex, close to Modal, with Modal fibre
High intensity, low elongation, the characteristics of degradable so that fabric is unlikely to deform, also with compared with cotton is fine, the more preferable moisture absorption of Modal
Property and gas permeability, and soft, smoothly, outward appearance is beautiful, can effectively substitute existing differential viscose rayon, viscous improving
While glue fiber lower procedure processing characteristics, moreover it is possible to promote exploitation and the industrial upgrading of downstream new textile, with good
Economic benefit and social benefit.
（2）The present invention uses low sour high salt using three bath wet spinning technologies, coagulating bath, and reaction condition is gentle, and
Viscose glue forms tow after draw-spinning process, it is ensured that many secondary responses of fiber, viscose rayon of the invention have with it is common
The viscose rayon secondary response interface different with Modal fibre is, it is necessary to which explanation, secondary response interface is horizontal according to fiber
Section inhales what color ability was differently formed to dyestuff, i.e. the cortex and sandwich layer of fiber, and cortex is small to dyestuff suction color ability, and dyeing is inclined
Shallow, sandwich layer inhales color ability to dyestuff greatly, and color is partially deep, and 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；By fiber of the present invention it is dyed after do fibre section, viscose rayon of the present invention
Fibre section is shown clear, obvious secondary response microscope sectional area, sandwich layer, cortex " area " ratio are（40~
70）：（30~60）, ratio is moderate, and the sandwich layer of common viscose fiber and cortex " area " ratio are（90~95）：（5~10）,
The inclined internal layer of ratio, therefore the viscose rayon of the present invention is compared with common viscose fiber, the characteristics of with high-strength, flatness, while also having
There is appropriate water imbibition, fiber skin-friendly has significant advantage；Fibre section is done after Modal fibre dyeing, is seen under the microscope
Examine, no secondary response interface, viscose rayon of the invention and Modal fibre are under equal dyeing condition, and viscose glue of the invention is fine
Dimension inhales color depth than Modal, and dye-uptake is high, and uniformity is more preferable, and the good color fastness of finished product.
（3）To ensure that high-strength flatness viscose rayon secondary response interface has suitable cortex, a sandwich layer ratio, the present invention from
Technology is set out, and has accomplished improvement acid bath technique, such as reduction sulfuric acid concentration, and reaction is slow, improves skin thickness；Change viscose glue
Index, such as viscose ripening degree, the fine content of first, alkali content index.
（4）Compared with adhering process of 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 degree of polymerization ＜ 50 gamma-cellulose, the shadow of hemicellulose
As long as sound has the following aspects：A. the uniformity of alkali cellulose is influenceed；B. ageing time is extended；C. the yellow of hemicellulose is fast
Degree is more fine than first fast, consumes a certain amount of carbon disulfide, causes alkali cellulose esterification reduction, the solubility reduction of sulphonic acid ester；D. shadow
The filtering of viscose glue is rung, the solubility reduction of sulphonic acid ester, the potential aldehyde radical in its end is oxidized to carboxyl and the metal ion in ash content
Such as：Ferrous ion, manganese ion, calcium ion, magnesium ion forms the extremely strong complex compound of viscosity, causes viscose filtration difficult, yield
It is low；E. hemicellulose is more, and the physical and mechanical properties of viscose rayon is poorer.The present invention can be pressed feeding in advance by grinding mill
The slurry congee of crusher is ground, and milling time is 10~40s, after the slurry congee after grinding is squeezed with squeezer, and separation is mixed
Close and contain hemicellulose and other impurities in alkali lye and alkali cellulose, mixed alkali liquor, size-reduced machine is crushed, and the multiple of squeezing is
2.2~2.8, degree of grinding is 120~180g/L, by mechanism, to improve the reactivity worth of slurry congee, it is ensured that viscose rayon is given birth to
That produces is smoothed out.
（5）The inventive method is that using natural cellulosic materials as raw materials for production, the viscose rayon for preparing and cotton be fine, not
Dai Er fibers etc. are the same, are degradable fibrous material, meet requirement of the people to environmental protection.
（6）The pulp material that the present invention is used can choose any one in cotton pulp, bamboo pulp, wood pulp, jute pulp or both with
On mixture can be prepared in any proportion, raw material scope is widely applicable, and technical requirements prepare relatively low, raw material
Cost is relatively low.
（7）The present invention can roll to the slurry congee for sending into squeezer by tube mill, pass through machinery work in advance
With, fiber can be torn and be discongested, to improve the reactivity worth of slurry congee, it is ensured that what viscose rayon was produced is smoothed out, with
Traditional viscose rayon prepares alkali cellulose data and compared, and alkali cellulose produced by the present invention half is fine lower（Half fine content in alkali lye
≤10g/L）, product strength height.
（8）The present invention uses multistage purification, and such as grinding, squeezing is crushed, rubbed, alkali lye cascade utilization, such as respectively in dipping
Before stage, rub alkali lye is added after the stage, cellulose combination alkali content can not only be mentioned, reach the comprehensive utilization ratio for improving alkali lye
Purpose, simultaneously, moreover it is possible to effectively reduce the input cost of auxiliary material alkali lye, reduce the production cost of viscose rayon.
（9）The present invention is ground, squeezing can obtain the fine content 29~31% of first, the alkali fiber of alkali content 15~17% after crushing
Element, the alkali cellulose can be sent directly into viscose rayon production system through rubbing, aoxidizing after drop is gathered, and cellulose viscose manufacturing technique can be adopted
With common process, such as yellow is obtained after viscose glue, then by filtering, maturation, deaeration, spinning to obtain viscose rayon.
（10）In the present invention, alkali cellulose fiber is handled through kneader twin screw device, makes fiber sub-wire, broom
Change, reach the cell membrane of destruction cellulose fibre, remove the small molecule in cellulose, so as to improve fibrin reaction performance, carry
High-cellulose combination alkali content, reaches 6~8%（Mass percent）.
（11）After the oxidized drop of the present invention is poly-, the alkali cellulose degree of polymerization is reduced to 400~600, first fibre purity by 650~1200
Can reach 98.0~98.5%, 2~3% can be improved than traditional handicraft, the poly- drop more experienced than tradition of orientation drop is poly- reduce first it is fine lose 3~
5%, molecule drop is poly- more uniform, abundant, can effectively improve the intensity of viscose rayon product.
（12）The present invention forms tow using three bath wet spinning technologies, viscose glue after draw-spinning process, it is ensured that fine
Many secondary responses of dimension, are compared with the tow of traditional spining technology formation, in the process, and the tow that three bath wet spinnings are obtained is fine
Dimension section can form clearly secondary response microscope interface, i.e.,：Core, cortex " area " ratio are respectively（40~70）：（30~
60）, with the characteristic for improving fibre strength, increase fibrous absorbent speed and increasing fiber water-retaining property.
（13）Yellow of the present invention, spinning technique have environmental protection, the advantage of energy-conservation, two in yellowing processes of the present invention
The consumption of nitric sulfid is 30%（Calculated with the fine content of first）Left and right, carbon disulfide consumption is up to 35% during Modal production yellow
（Calculated with the fine content of first）Left and right, this production technology can effectively reduce cost and reduce air pollution；In Modal spinning
When acid bath combined using high zinc sulfate, low sodium sulphate, 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 crystallize high energy consumption, therefore this technique be related to yellow, spinning technique production cost it is also lower.
（14）In the spinning technique of the present invention, tow by bathing more, low acid, less salt wet spinning technology, meanwhile, with reference to
Step by step, high drawing-off technology carries out spinning, and one of degree of draft is that 50~100%, two road degree of drafts are that 40~60%, three road degree of drafts are
5~15%, it is more beneficial for improving the fragility of fiber, is improved the degree of stretching of fiber, shows：5% is produced under wet condition to extend
Intensity >=0.55cN/dtex needed for rate, dry elongation at break is 13.0~16.0%.
（15）The present invention has gentle sulfur removal technology, can reduce the damage of fiber product intensity, degree of stretching, actually make
The more existing sodium hydroxide used of desulfurizing agent, the sodium sulfite of used time, vulcanized sodium and sodium carbonate composition are gentleer, sodium carbonate energy
Neutralize after the sulfuric acid that tow is brought from acid bath, sulfur removal technology, can adjust the pH value of tow 8~11.
（16）The bleaching agent that the present invention is used is gentle, is more heated compared with bleaching agents such as sodium hypochlorite using hydrogen peroxide bleaching agent
With the pH value of viscose rayon prepared by the present invention should be controlled in the range of 6.5~7, can also pass through washing, multiple-effect acid（Organic acid）
Mode adjust pH value, within the range, the strength and elongation of viscose final product is unaffected, and strength and elongation is high.
（17）Influenceed by the aspect of tow intensity and elongation etc., the spinning speed obvious more not generation in present invention process step
Your spinning is higher（Modal spins speed 30m/min, and this technique spins fast 50 m/min）, meanwhile, with reference in spinning drawing technique to acid
The optimization of bath composition and draft process, can accomplish the control parameter of each process of overall balance, and moderately, the present invention
Also have prouctiveness high, effectively reduce the operational characteristic of cost.
（18）The present invention is reasonable in design, in the production process of identical viscose rayon product, and summary raw material is chosen, system
In terms of standby process modification, the production cost of the reduction viscose rayon product of high degree, its price is compared with Modal fibre
It is low 4000~5000 yuan/ton, downstream raw material use cost can be greatly lowered, available for home textile, non-woven fabrics etc., particularly underwear
And facial mask, hygenic towelette etc., to spin, weave cotton cloth etc., down-stream enterprise brings more high added value and wide market prospects, significantly carries
Rise the market competitiveness of enterprise.
Brief description of the drawings
Fig. 1 is the fibre section cross section of high-strength flatness viscose rayon made from the inventive method.
Fig. 2 is the fibre section cross section of Modal.
Fig. 3 is the fibre section cross section of tencel.
Embodiment
Goal of the invention, technical scheme and the beneficial effect of the present invention are described in further detail below.
It is noted that described further below is all exemplary, it is intended to which the required present invention is provided further
Bright, unless otherwise indicated, all technologies used herein and scientific terminology are with the common skill with the technical field of the invention
The identical meanings that art personnel are generally understood that.
The fibrous raw materials such as tencel, Modal, CUP, viscose rayon are regenerated by raw material of natural cellulosic materials
Bio-based fibrous raw material, wherein, with the occupation rate of market highest of viscose rayon, but viscous with common variety in recent years
Glue fiber scale is drastically expanded, and raw material supply is nervous, and the exploitation of downstream new textile and industrial upgrading are progressively restricted,
To overcome this phenomenon, a series of differences by taking patent document CN102296373A, CN100359050C, CN102251301A as an example
Not Hua viscose rayon be suggested, from its disclosed patented technology, this kind of differential viscose rayon be by change production
The mode of technique is realized, but for increasingly fierce market competition, differential viscose rayon do not have the more day of one's doom
The exploitation and the industrial upgrading that meet downstream new textile of degree, especially same regenerated by raw material of natural cellulosic materials and
Into the fibrous raw material such as tencel, Modal, CUP development so that the occupation rate of market of viscose rayon is reduced increasingly.
On the basis of this, the present invention proposes a kind of process for preparing high-strength flatness viscose rayon, and the high-strength flatness prepared glues
Glue fiber product has high-strength, flatness product performance, while also having high-selenium corn characteristic, product skin-friendly outclass Modal
Fiber, slightly better than cotton fiber.
Viscose rayon of the present invention maintains exclusive fibre structure, with high-tenacity in fiber forming process
The characteristics of, its dry fracture strength and wet breaking strength improve 25% or so compared with common viscose fiber, fine with differential viscose glue
Dimension also has significant difference, from product index as can be seen that the product index of high-strength flatness viscose rayon is met：Fiber number 0.88~
1.11D, does the cN/dtex of fracture strength >=3.20, wet breaking strength >=1.60cN/dtex, and differential viscose rayon is with patent
Document is recorded exemplified by CN102296373A, CN100359050C, CN102251301A, and its product index is as follows：
CN102296373A meet the cN/dtex of 0.44~0.78dtex of fiber number, dry fracture strength >=3.10, wet breaking strength >=
2.1cN/dtex；CN100359050C meets the cN/dtex of 0.90~1.40dtex of fiber number, dry fracture strength >=2.50, wet fracture
Intensity >=1.20cN/dtex；CN102251301A meets the cN/dtex of the dtex of fiber number 1.11, intensity >=2.9, from These parameters
As can be seen that the fibre strength of viscose rayon of the present invention is substantially better than existing differential viscose rayon.
High-strength flatness viscose rayon of the present invention is compared with Modal fibre, tencel respectively again, compares other side
Formula is as follows：
Fibre section is done after high-strength flatness viscose rayon, Modal fibre, tencel are dyed respectively, its fibre section is existed
Amplify 2000 times under microscope to be observed, as shown in Figures 1 to 3, Fig. 1 is transversal for the fibre section of high-strength flatness viscose rayon
Face, as shown in figure 1, after the high-strength dyed processing of flatness viscose rayon of the present invention, its fibrocortex, the color point of sandwich layer
Shallow, deep difference is not shown, is differed greatly, cortex is partially shallow, and sandwich layer is substantially partially deep, there is clearly secondary response interface,
Ratio is moderate, it is ensured that the characteristics of product has high-strength, flatness, while also there is appropriate water imbibition, fiber skin-friendly tool
There is significant advantage, wherein, sandwich layer：" area " ratio of cortex is 40~70：30~60.
Fig. 2 is the fibre section sectional view of Modal fibre, as shown in Fig. 2 after the dyed processing of Modal fibre, its
Fibrocortex and the color of sandwich layer are deep, shallow consistent, and without obvious secondary interface, the products characteristics enhance the hydrophobicity of fiber, inhale
Water rate is poor, so that its skin-friendly is deteriorated.
Fig. 3 is the fibre section sectional view of tencel, as shown in figure 3, after the dyed processing of tencel, its fibrocortex and sandwich layer
Color it is deep, shallow consistent, without obvious secondary interface, the products characteristics have the excellent hygroscopicity of plain edition viscose rayon concurrently, soft and smooth
Outside the advantages of elegant property, comfortableness, overcome that common viscose fiber strength is low, especially wet strong low defect, its strength is several
It is close with terylene.
Just because of the said goods characteristic, determine that high-strength flatness viscose rayon of the present invention meets following index：
The cN/dtex of dry fracture strength >=3.20, wet breaking strength >=1.60cN/dtex,
Intensity >=0.55cN/dtex needed for 5% elongation is produced under wet condition,
Dry elongation at break 12.0~17.5%, wet elongation at break 18.0~21.0%,
Crystallinity 40.0~45.0%, radial water swelling capacity 22~26%,
Line density deviation ratio≤± 4.0%, whiteness >=83%,
Residual sulphur≤12.0mg/100g, length variation rate≤± 6.0%,
Overlength fiber rate≤0.5%, over-length fibre≤4.0mg/100g,
Fault≤4.0mg/100g.
These parameters are applied to survey of the linear density range for the viscose rayon of 0.88dtex~1.11dtex high-strength flatness
Fixed, the assay method of dry fracture strength is GB/T 14337, under the assay method of wet breaking strength is GB/T 14337, wet condition
Intensity needed for producing 5% elongation is completed by GB/T 14337, and the assay method of dry elongation at break is GB/T
14337, the assay method of wet elongation at break is GB/T 14337, and the assay method of line density deviation ratio is GB/T 14335,
The assay method of residual sulphur is FZ/T 50014, and the assay method of length variation rate is GB/T 14336, the measure of overlength fiber rate
Method is GB/T 14336, and the assay method of over-length fibre is GB/T 14336, and the assay method of fault is GB/T 14339, in vain
The assay method of degree is FZ/T 50013, and the assay method of radial water swelling capacity is GB/T 6503.
The embodiment of the explanation present invention, certainly, protection of the invention are enumerated with several exemplary embodiments below
Scope is not limited to following examples.
Embodiment 1：
It is of the present invention to there is the high-strength flatness viscose rayon of light type to be to use pulp material impregnated successively, grinding, squeezing
Crush, crumple, pure oxygen drops and is made after poly-, yellow, dissolving, filtering, deaeration, maturation, spinning drawing and post processing, after measured, should
Viscose rayon is met：
Fiber number 0.88D, does fracture strength 3.20 cN/dtex, wet breaking strength 1.60cN/dtex,
The intensity 0.55cN/dtex needed for 5% elongation is produced under wet condition,
Dry elongation at break 12.0%, wet elongation at break 18.0%,
Crystallinity 40.0%, radial water swelling capacity 22%,
Line density deviation ratio -4%, whiteness 83%,
Residual sulphur 12.0mg/100g, length variation rate+0.5%,
Overlength fiber rate 0%, over-length fibre 0mg/100g,
Fault 0.5mg/100g.
Embodiment 2：
The present embodiment and the difference of embodiment 1 are：The pulp material that the present embodiment is used is to use mass ratio for 3：1：
1：1 cotton pulp, bamboo pulp, wood pulp, jute pulp are mixed.After testing, the viscose rayon prepared by the present embodiment meets high
The product performance of strong flatness viscose rayon.
Embodiment 3：
The present embodiment and the difference of embodiment 1 are：The pulp material that the present embodiment is used is to use mass ratio for 4：1
What cotton pulp and bamboo pulp were mixed.After testing, the viscose rayon prepared by the present embodiment meets high-strength flatness viscose rayon
Product performance.
Embodiment 4：
The preparation process that what the present embodiment was related to have the high-strength flatness viscose rayon of light type has steps of：
A：By pulp material soda-dip, then ground, squeezing crush, rub after slurry congee is made；
B：Reactor is sent into after slurry congee is mixed with alkali lye, is dropped using pure oxygen and obtains alkali cellulose after gathering；
C：The cellulose sulfonate that alkali cellulose is obtained with carbon disulfide reaction is dissolved using solvent, cellulose sulfonic acid is obtained
Ester solution；
D：Spinning solution is made in cellulose sulfonate solution after filtering, deaeration, maturation, then by the spinning solution of acquisition through spinning
High-strength flatness viscose rayon is made after filament drafting and post processing.
Embodiment 5：
The present embodiment and the difference of embodiment 4 are：In the step A that the present embodiment is related to, the degree of polymerization is 650 slurry
Dregs of rice raw material concentration 110g/L sodium hydroxide solution impregnates 50min, then ground machine grind, squeeze, crushing, rub after be made
Congee is starched, the concentration of slurry congee is 30%.
Embodiment 6：
The present embodiment and the difference of embodiment 5 are：In the step A that the present embodiment is related to, the degree of polymerization is 1200 slurry
Dregs of rice raw material impregnates 90min with concentration 240g/L sodium hydroxide solution, and the slurry congee that concentration is 6% is made after being ground with grinder, should
Slurry congee is sent to squeezer, and pulverizer is delivered to after squeezing and is crushed, and obtains alkali cellulose, the alkali cellulose is delivered to and rubbed
Machine, obtains the slurry congee that concentration is 40% after processing.
Embodiment 7：
The present embodiment and the difference of embodiment 6 are：In the present embodiment, the pressing temperature of squeezer is 57 DEG C, squeezing
Multiple is set as 2.2；The degree of grinding of pulverizer is 120g/L, and the alkali cellulose obtained after crushing delivers to kneading machine again, after processing
Obtain the slurry congee that concentration is 30%.
Embodiment 8：
The present embodiment and the difference of embodiment 6 are：In the present embodiment, the pressing temperature of squeezer is 63 DEG C, squeezing
Multiple is set as 2.8；The degree of grinding of pulverizer is 180g/L, and the alkali cellulose obtained after crushing delivers to kneading machine again, after processing
Obtain the slurry congee that concentration is 40%.
Embodiment 9：
The present embodiment and the difference of embodiment 4 are：In the step B that the present embodiment is related to, slurry congee is 140g/ with concentration
Reactor is sent into after L sodium hydroxide solution mixing, it is that the fine purity of 400, first is 98.0% that the acquisition degree of polymerization after gathering is dropped using pure oxygen
Alkali cellulose, the addition of pure oxygen is 2% in reactor, drops poly- reaction time control in 30min.
Embodiment 10：
The present embodiment and the difference of embodiment 4 are：In the step B that the present embodiment is related to, slurry congee is 200g/ with concentration
Reactor is sent into after L sodium hydroxide solution mixing, it is that the fine purity of 600, first is 98.5% that the acquisition degree of polymerization after gathering is dropped using pure oxygen
Alkali cellulose, the addition of pure oxygen is 10% in reactor, drops poly- reaction time control in 60min.
Embodiment 11：
The present embodiment and the difference of embodiment 4 are：In the step C that the present embodiment is related to, the addition of carbon disulfide
The 30% of first fibre content in the alkali cellulose made from step B, the concentration of the cellulose sulfonate solution of acquisition is 9.0%, yellow
Reaction time control is in 45min, and yellow reaction temperature is 25 DEG C.
Embodiment 12：
The present embodiment and the difference of embodiment 4 are：In the step C that the present embodiment is related to, solvent is including concentration
25g/L sodium hydroxide solutions and the sodium sulfite aqueous solution that concentration is 10 g/L, solution temperature is 20 DEG C, and dissolution time is
40min。
Embodiment 13：
The present embodiment and the difference of embodiment 11 are：In the step C that the present embodiment is related to, alkali cellulose is in xanthating machine
In occur yellow reaction with carbon disulfide, wherein, the addition of carbon disulfide is the fine content of first in alkali cellulose made from step B
25%, the yellow reaction time should be controlled in 45min, yellow reaction temperature control at 20 DEG C；The fiber obtained after yellow reaction
Plain sulphonic acid ester dissolves with solvent, and course of dissolution is that cellulose sulfonate is mixed with solvent, stirred and is ground, and solvent is then adopted
The sodium sulfite aqueous solution that with concentration be 25g/L sodium hydroxide solutions and concentration is 5g/L, solution temperature is 10 DEG C, dissolution time
For 30min, the cellulose sulfonate solution that concentration is 9.0% is made after dissolving.
Embodiment 14：
The present embodiment and the difference of embodiment 11 are：In the step C that the present embodiment is related to, alkali cellulose is in xanthating machine
In occur yellow reaction with carbon disulfide, wherein, the addition of carbon disulfide is the fine content of first in alkali cellulose made from step B
37%, the yellow reaction time should be controlled in 50min, yellow reaction temperature control at 30 DEG C；The fiber obtained after yellow reaction
Plain sulphonic acid ester dissolves with solvent, and course of dissolution is that cellulose sulfonate is mixed with solvent, stirred and is ground, and solvent is then adopted
The sodium sulfite aqueous solution that with concentration be 45 g/L sodium hydroxide solutions and concentration is 10 g/L, solution temperature is 20 DEG C, dissolving
Time is 50min, and the cellulose sulfonate solution that concentration is 10.0% is made after dissolving.
Embodiment 15：
The present embodiment and the difference of embodiment 4 are：The spinning drawing step that the present embodiment is related to can be specifically summarized as follows：
F：Cellulose sulfonate solution is delivered into spinning-drawing machine after filtering, deaeration, maturation, is extruded and spun by the shower nozzle of spinning-drawing machine
Silk thread forms tow after being bathed through one, the coagulating bath that a bath is used include 90g/L sulfuric acid, 220g/L sodium sulphate and
8g/L zinc sulfate, one bath temperature be set as 40 DEG C, one bath acid bath drop be 3g/L；
G：Tow after being bathed through one is sent into two by one of drafting machine and bathed, and the coagulating bath that two bath is used includes 18g/L's
Sulfuric acid, the degree of draft of one of drafting machine is set as 80 DEG C for the temperature of 50%, two baths；
H：Tow after being bathed through two is bathed by two road drafting machine feedings three, and it is 1 that the coagulating bath that three bath is used, which includes pH value,
Sulfuric acid, the degree of draft of two road drafting machine is set as 80 DEG C for the temperature of 40%, three baths；
I：Tow after being bathed through three delivers to post processing part by three road drafting machines, and the degree of draft of three road drafting machine is
5%。
Embodiment 16：
The present embodiment and the difference of embodiment 15 are：In the present embodiment, the post-processing step tool that the present embodiment is related to
Body can be summarized as follows：The desulfurization that is carried out to the tow of spinning drawing formation, bleach and oil, wherein, the desulfurizing agent that desulfurization is used
The sodium carbonate that the vulcanized sodium and concentration for being 4g/L by concentration are 1g/L is constituted；It is the double of concentration 0.3g/L to bleach the bleaching agent used
Oxygen water；The finish addition used that oils is 7g/L, and the pH value of tow is 6.5 after oiling.
In above-mentioned steps, desulfurization temperature is set as 50 DEG C, and desulfurization time is set as 2min；Bleaching temperature is set as 50
DEG C, bleaching time is set as 1min；The temperature of finish is set as 50 DEG C.
Embodiment 17：
The present embodiment and the difference of embodiment 16 are：The post-processing step that the present embodiment is related to also includes at drying
Reason, drying is that the desulfurization carried out to the tow of spinning drawing formation, the tow bleached and obtained after oiling use drying machine drying,
Drying temperature is 75 DEG C, after drying, obtains high-strength flatness viscose rayon product, in the present embodiment, strong flatness viscose rayon production
The regain of product should be controlled 11%.
Embodiment 18：
The step of preparation process for the high-strength flatness viscose rayon that the present embodiment is related to is as follows：
A：By pulp material（Mass ratio is used for 5：1 cotton pulp and jute pulp is mixed, and its degree of polymerization is 1100）Dipping
In the treating tank equipped with alkali lye, 35 DEG C of dipping temperature, dip time 70min is ground after 30s by tubular type grinder, is made dense
The slurry congee for 5% is spent, wherein, pulp material is made up of wood pulp, and alkali lye is 110~240g/L of concentration sodium hydroxide solution, is obtained
Slurry congee temperature be 30 DEG C；
B：Congee will be starched made from step A and delivers to squeezer, 60 DEG C of pressing temperature of setting, squeezing multiple 2.5 are sent after squeezing
Crushed to pulverizer, set degree of grinding as 160g/L, obtained alkali cellulose, the alkali cellulose is delivered into kneading machine, handled
The slurry congee that concentration is 35% is obtained afterwards；
C：Reactor is delivered to by being starched made from step B after congee is mixed with alkali lye, pure oxygen is added in the reactor, is obtained after drop is poly-
It is the alkali cellulose that the fine purity of 600, first is 98.5% to obtain the degree of polymerization, wherein, alkali lye is molten from concentration 180g/L sodium hydroxide
The addition of pure oxygen is 8% in liquid, reactor, drops poly- reaction time control in 60min；
D：Alkali cellulose made from step C is delivered into xanthating machine, alkali cellulose occurs yellow in xanthating machine with carbon disulfide
Change reaction, wherein, the addition of carbon disulfide is 37% of the fine content of first in alkali cellulose made from step B, when yellow is reacted
Between should control in 50min, the control of yellow reaction temperature is at 30 DEG C, and the cellulose sulfonate and solvent obtained after yellow reaction is molten
Solution, course of dissolution is that cellulose sulfonate is mixed with solvent, stirred and is ground, and solvent then uses concentration for 45 g/L hydrogen
Sodium hydroxide solution and the sodium sulfite aqueous solution that concentration is 7 g/L, solution temperature is 15 DEG C, and dissolution time is 45min, after dissolving
The cellulose sulfonate solution that concentration is 10.0% is made.
E：Cellulose sulfonate solution made from step D is obtained into spinning solution after filtering, deaeration, maturation；
F：The obtained spinning solutions of step E are delivered into spinning-drawing machine, by spinning-drawing machine shower nozzle extruding spinning thread through one bathe after shape
Into tow, the coagulating bath that a bath is used includes the zinc sulfate of 100g/L sulfuric acid, 260g/L sodium sulphate and 12g/L, one
Bath temperature is 50 DEG C, and a bath acid bath drop is 5g/L；
G：Tow after being bathed through one is sent into two by one of drafting machine and bathed, and the coagulating bath that two bath is used includes 20g/L's
Sulfuric acid, the degree of draft of one of drafting machine is 80%, and two bath temperatures are 88 DEG C；
H：Tow after being bathed through two is bathed by two road drafting machine feedings three, and it is 2 that the coagulating bath that three bath is used, which includes pH value,
Sulfuric acid, the degree of draft of two road drafting machine is 58%, and three bath temperatures are 90 DEG C；
I：Tow after being bathed through three delivers to step J by three road drafting machines, and the degree of draft of three road drafting machine is 5%；
J：The tow obtained to step I carries out desulfurization, bleaches and oil, wherein, the desulfurizing agent that desulfurization is used is by concentration
8g/L vulcanized sodium and concentration constitutes for 4g/L sodium carbonate, sets desulfurization temperature as 55 DEG C, desulfurization time is 2min, and bleaching makes
Bleaching agent is concentration 0.5g/L hydrogen peroxide, sets bleaching temperature as 55 DEG C, bleaching time is 2min；Oil the temperature used
The finish for 55 DEG C is spent, its addition is 9g/L, the pH value of tow is 7 after oiling；
K：To using drying machine drying through desulfurization, the tow bleached and obtained after oiling in step J, drying temperature is set as
115 DEG C, after drying, high-strength flatness viscose rayon product is obtained, product regain is controlled 12%.
From above-mentioned production process, this preparation process is not added with delustering agent, and the viscose rayon product of acquisition, which belongs to, light
Type viscose rayon, after testing, the viscose rayon meet the product performance of high-strength flatness viscose rayon.
Embodiment 19：
The step of preparation process for the high-strength flatness viscose rayon that the present embodiment is related to is as follows：
A：By pulp material（Mass ratio is used for 1：3：2 bamboo pulp, wood pulp and jute pulp is mixed, and its degree of polymerization is
650）It is impregnated in the treating tank equipped with alkali lye, 40 DEG C of dipping temperature, dip time 60min grinds 40s by tubular type grinder
Afterwards, the slurry congee that concentration is 5% is made, wherein, pulp material is made up of wood pulp, and alkali lye is concentration 130g/L sodium hydroxide solution,
The temperature of the slurry congee of acquisition is 45 DEG C；
B：Congee will be starched made from step A and delivers to squeezer, 60 DEG C of pressing temperature of setting, squeezing multiple 2.5 are sent after squeezing
Crushed to pulverizer, set degree of grinding as 160g/L, obtained alkali cellulose, the alkali cellulose is delivered into kneading machine, handled
The slurry congee that concentration is 35% is obtained afterwards；
C：Reactor is delivered to by being starched made from step B after congee is mixed with alkali lye, pure oxygen is added in the reactor, is obtained after drop is poly-
It is the alkali cellulose that the fine purity of 500, first is 98.5% to obtain the degree of polymerization, wherein, alkali lye is molten from concentration 190g/L sodium hydroxide
The addition of pure oxygen is 10% in liquid, reactor, drops poly- reaction time control in 60min；
D：Alkali cellulose made from step C is delivered into xanthating machine, alkali cellulose occurs yellow in xanthating machine with carbon disulfide
Change reaction, wherein, the addition of carbon disulfide is 36% of the fine content of first in alkali cellulose made from step B, when yellow is reacted
Between should control in 50min, the control of yellow reaction temperature is at 30 DEG C, and the cellulose sulfonate and solvent obtained after yellow reaction is molten
Solution, course of dissolution is that cellulose sulfonate is mixed with solvent, stirred and is ground, and solvent then uses concentration for 45 g/L hydrogen
Sodium hydroxide solution and the sodium sulfite aqueous solution that concentration is 7 g/L, solution temperature is 20 DEG C, and dissolution time is 50min, after dissolving
The cellulose sulfonate solution that concentration is 9.5% is made.
E：Cellulose sulfonate solution made from step D is obtained into spinning solution after filtering, deaeration, maturation；
F：The obtained spinning solutions of step E are delivered into spinning-drawing machine, by spinning-drawing machine shower nozzle extruding spinning thread through one bathe after shape
Into tow, the coagulating bath that a bath is used includes the zinc sulfate of 110g/L sulfuric acid, 255g/L sodium sulphate and 12g/L, one
Bath temperature is 50 DEG C, and a bath acid bath drop is 5g/L；
G：Tow after being bathed through one is sent into two by one of drafting machine and bathed, and the coagulating bath that two bath is used includes 18g/L's
Sulfuric acid, the degree of draft of one of drafting machine is 80%, and two bath temperatures are 85 DEG C；
H：Tow after being bathed through two is bathed by two road drafting machine feedings three, and it is 2 that the coagulating bath that three bath is used, which includes pH value,
Sulfuric acid, the degree of draft of two road drafting machine is 50%, and three bath temperatures are 85 DEG C；
I：Tow after being bathed through three delivers to step J by three road drafting machines, and the degree of draft of three road drafting machine is 15%；
J：The tow obtained to step I carries out desulfurization, bleaches and oil, wherein, the desulfurizing agent that desulfurization is used is by concentration
6g/L vulcanized sodium and concentration constitutes for 3g/L sodium carbonate, sets desulfurization temperature as 53 DEG C, desulfurization time is 3min, and bleaching makes
Bleaching agent is concentration 0.6g/L hydrogen peroxide, sets bleaching temperature as 55 DEG C, bleaching time is 2min；Oil the temperature used
The finish for 55 DEG C is spent, its addition is 8g/L, the pH value of tow is 6.8 after oiling；
K：To using drying machine drying through desulfurization, the tow bleached and obtained after oiling in step J, drying temperature is set as
115 DEG C, after drying, high-strength flatness viscose rayon product is obtained, product regain is controlled 12%.
From above-mentioned production process, this preparation process is not added with delustering agent, and the viscose rayon product of acquisition, which belongs to, light
Type viscose rayon, after testing, the viscose rayon meet the product performance of high-strength flatness viscose rayon.
Embodiment 20：
The step of preparation process for the high-strength flatness viscose rayon that the present embodiment is related to is as follows：
A：By pulp material（Mass ratio is used for 5：3 bamboo pulps, wood pulp are mixed, and its degree of polymerization is 1050）It is impregnated in dress
Have in the treating tank of alkali lye, 45 DEG C of dipping temperature, dip time 80min, ground by tubular type grinder after 40s, concentration, which is made, is
5.5% slurry congee, wherein, pulp material is made up of wood pulp, and alkali lye is concentration 200g/L sodium hydroxide solution, the slurry congee of acquisition
Temperature be 55 DEG C；
B：Congee will be starched made from step A and delivers to squeezer, 60 DEG C of pressing temperature of setting, squeezing multiple 2.5 are sent after squeezing
Crushed to pulverizer, set degree of grinding as 150g/L, obtained alkali cellulose, the alkali cellulose is delivered into kneading machine, handled
The slurry congee that concentration is 35% is obtained afterwards；
C：Reactor is delivered to by being starched made from step B after congee is mixed with alkali lye, pure oxygen is added in the reactor, is obtained after drop is poly-
It is the alkali cellulose that the fine purity of 480, first is 98.4% to obtain the degree of polymerization, wherein, alkali lye is molten from concentration 180g/L sodium hydroxide
The addition of pure oxygen is 10% in liquid, reactor, drops poly- reaction time control in 60min；
D：Alkali cellulose made from step C is delivered into xanthating machine, alkali cellulose occurs yellow in xanthating machine with carbon disulfide
Change reaction, wherein, the addition of carbon disulfide is 36.5% of the fine content of first in alkali cellulose made from step B, yellow reaction
Time should be controlled in 50min, and the cellulose sulfonate and solvent that the control of yellow reaction temperature is obtained after 30 DEG C, yellow reaction are molten
Solution, course of dissolution is that cellulose sulfonate is mixed with solvent, stirred and is ground, and solvent then uses concentration for 42 g/L hydrogen
Sodium hydroxide solution and the sodium sulfite aqueous solution that concentration is 6g/L, solution temperature is 19 DEG C, and dissolution time is 46min, after dissolving
The cellulose sulfonate solution that concentration is 9.5% is made.
E：Cellulose sulfonate solution made from step D is obtained into spinning solution after filtering, deaeration, maturation；
F：The obtained spinning solutions of step E are delivered into spinning-drawing machine, by spinning-drawing machine shower nozzle extruding spinning thread through one bathe after shape
Into tow, the coagulating bath that a bath is used includes the zinc sulfate of 115g/L sulfuric acid, 235g/L sodium sulphate and 9g/L, a bath
Temperature is 44 DEG C, and a bath acid bath drop is 4.5g/L；
G：Tow after being bathed through one is sent into two by one of drafting machine and bathed, and the coagulating bath that two bath is used includes 21g/L's
Sulfuric acid, the degree of draft of one of drafting machine is 91%, and two bath temperatures are 88 DEG C；
H：Tow after being bathed through two is bathed by two road drafting machine feedings three, and the coagulating bath that three bath is used is including pH value
2.6 sulfuric acid, the degree of draft of two road drafting machine is 52%, and three bath temperatures are 85 DEG C；
I：Tow after being bathed through three delivers to step J by three road drafting machines, and the degree of draft of three road drafting machine is 15%；
J：The tow obtained to step I carries out desulfurization, bleaches and oil, wherein, the desulfurizing agent that desulfurization is used is by concentration
6g/L vulcanized sodium and concentration constitutes for 3.2g/L sodium carbonate, sets desulfurization temperature as 55 DEG C, desulfurization time is 3min, bleaches
The bleaching agent used is concentration 0.6g/L hydrogen peroxide, sets bleaching temperature as 55 DEG C, bleaching time is 2min；Oil what is used
Temperature is 55 DEG C of finish, and its addition is 7g/L, and the pH value of tow is 6.6 after oiling；
K：To using drying machine drying through desulfurization, the tow bleached and obtained after oiling in step J, drying temperature is set as
75 DEG C, after drying, high-strength flatness viscose rayon product is obtained, product regain is controlled 13.5%.
From above-mentioned production process, this preparation process is not added with delustering agent, and the viscose rayon product of acquisition, which belongs to, light
Type viscose rayon, after testing, the viscose rayon meet the product performance of high-strength flatness viscose rayon.
Embodiment 21：
The step of preparation process for the high-strength flatness viscose rayon that the present embodiment is related to is as follows：
A：By pulp material（Wood pulp all is used, its degree of polymerization is 800）It is impregnated in the treating tank equipped with alkali lye, dipping
Temperature 60 C, dip time 90min is ground after 38s by tubular type grinder, and the slurry congee that concentration is 3% is made, wherein, pulp material
It is made up of wood pulp, alkali lye is concentration 160g/L sodium hydroxide solution, and the temperature of the slurry congee of acquisition is 50 DEG C；
B：Congee will be starched made from step A and delivers to squeezer, 63 DEG C of pressing temperature of setting, squeezing multiple 2.3 are sent after squeezing
Crushed to pulverizer, set degree of grinding as 140g/L, obtained alkali cellulose, the alkali cellulose is delivered into kneading machine, handled
The slurry congee that concentration is 38% is obtained afterwards；
C：Reactor is delivered to by being starched made from step B after congee is mixed with alkali lye, pure oxygen is added in the reactor, is obtained after drop is poly-
It is the alkali cellulose that the fine purity of 400, first is 98.4% to obtain the degree of polymerization, wherein, alkali lye is molten from concentration 150g/L sodium hydroxide
The addition of pure oxygen is 3% in liquid, reactor, drops poly- reaction time control in 45min；
D：Alkali cellulose made from step C is delivered into xanthating machine, alkali cellulose occurs yellow in xanthating machine with carbon disulfide
Change reaction, wherein, the addition of carbon disulfide is 25% of the fine content of first in alkali cellulose made from step B, when yellow is reacted
Between should control in 50min, the control of yellow reaction temperature is at 20 DEG C, and the cellulose sulfonate and solvent obtained after yellow reaction is molten
Solution, course of dissolution is that cellulose sulfonate is mixed with solvent, stirred and is ground, and solvent then uses concentration for 45 g/L hydrogen
Sodium hydroxide solution and the sodium sulfite aqueous solution that concentration is 60 g/L, solution temperature is 18 DEG C, and dissolution time is 45min, dissolving
The cellulose sulfonate solution that concentration is 9.3% is made afterwards.
E：Cellulose sulfonate solution made from step D is obtained into spinning solution after filtering, deaeration, maturation；
F：The obtained spinning solutions of step E are delivered into spinning-drawing machine, by spinning-drawing machine shower nozzle extruding spinning thread through one bathe after shape
Into tow, the coagulating bath that a bath is used includes the zinc sulfate of 90g/L sulfuric acid, 220g/L sodium sulphate and 8g/L, a bath
Temperature is 40 DEG C, and a bath acid bath drop is 3g/L；
G：Tow after being bathed through one is sent into two by one of drafting machine and bathed, and the coagulating bath that two bath is used includes 18g/L's
Sulfuric acid, the degree of draft of one of drafting machine is 60%, and two bath temperatures are 90 DEG C；
H：Tow after being bathed through two is bathed by two road drafting machine feedings three, and it is 2 that the coagulating bath that three bath is used, which includes pH value,
Sulfuric acid, the degree of draft of two road drafting machine is 60%, and three bath temperatures are 85 DEG C；
I：Tow after being bathed through three delivers to step J by three road drafting machines, and the degree of draft of three road drafting machine is 12%；
J：The tow obtained to step I carries out desulfurization, bleaches and oil, wherein, the desulfurizing agent that desulfurization is used is by concentration
8g/L vulcanized sodium and concentration constitutes for 3g/L sodium carbonate, sets desulfurization temperature as 55 DEG C, desulfurization time is 3min, and bleaching makes
Bleaching agent is concentration 0.3g/L hydrogen peroxide, sets bleaching temperature as 50 DEG C, bleaching time is 1min；Oil the temperature used
The finish for 50 DEG C is spent, its addition is 8g/L, the pH value of tow is 7 after oiling；
K：To using drying machine drying through desulfurization, the tow bleached and obtained after oiling in step J, drying temperature is set as
105 DEG C, after drying, high-strength flatness viscose rayon product is obtained, product regain is controlled 12%.
From above-mentioned production process, this preparation process is not added with delustering agent, and the viscose rayon product of acquisition, which belongs to, light
Type viscose rayon, after testing, the viscose rayon meet the product performance of high-strength flatness viscose rayon.
The high-strength flatness viscose rayon that above-described embodiment 1~7 is obtained is detected that the desired value to acquisition is united
Meter, is shown in Table 1.
Table 1
The high-strength flatness viscose rayon that above-described embodiment 8~14 is obtained is detected that the desired value to acquisition is united
Meter, is shown in Table 2.
Table 2
The high-strength flatness viscose rayon that above-described embodiment 15~21 is obtained is detected that the desired value to acquisition is united
Meter, is shown in Table 3.
Table 3
The desired value for the high-strength flatness viscose rayon that above-described embodiment 1~21 is related to is removed to be counted after maximum and minimum value
Calculate average value, by calculate obtain average value respectively with Modal fibre, differential viscose rayon（CN102296373A contrast texts
Part 1, CN100359050C documents 2, CN102251301A documents 3）And the product index of common viscose fiber enters
Row compares, as shown in table 4.
Table 4
From table 4, it can be seen that the fibre strength of high-strength flatness viscose rayon of the present invention（See dry fracture strength and wet
Fracture strength data）Apparently higher than common viscose fiber and differential viscose rayon（Documents 2, documents 3）Data
Index, fibre strength is slightly below the data target of Modal fibre；Elongate fiber rate（Wet elongation at break and dry elongation at break
Data）Data target compared with common viscose fiber and Modal fibre is lower, with high-strength, flatness product performance, the opposing party
Face, from the point of view of radial water swelling degrees of data, the present invention has more preferable skin-friendly compared with Modal fibre again, therefore, it can substitute
Modal fibre has wider array of application field, certainly, in addition, and the present invention passes through advanced process meanses（That is raw material
Selection, auxiliary material control, yellow and improvement of spinning technique etc.）The viscose rayon prepared also has higher compared with Modal fibre
Cost performance, ton silk price it is low compared with Modal fibre 4000~5000 yuan/ton, therefore, also with good market value.
From table 4, it can be seen that the Denier range of high-strength flatness viscose rayon of the present invention is wider, Denier range exists
Between 0.88~1.11D, plain edition viscose rayon is applicable to.
In the above-described embodiments, the high-strength flatness that any embodiment chosen in embodiment 1~21 is prepared glues
Glue fiber product, such as embodiment 19, microscope sectional drawing is carried out to its fibre section, it is possible to find, its section remains with clearly anti-
Vestige is answered, its fibrocortex, the color of sandwich layer show shallow, deep difference respectively, and cortex is substantially partially shallow, and sandwich layer is partially deep,（It is interior
Layer+middle level）：" area " ratio of outer layer is 69：31, belong to sandwich layer：Cortex=（40~70）：（30~60）In the range of.
It is described above, be only presently preferred embodiments of the present invention, any formal limitation not done to the present invention, it is every according to
According to the present invention technical spirit above example is made any simple modification, equivalent variations, each fall within the present invention protection
Within the scope of.
Claims (1)
1. a kind of preparation method of superfine type viscose rayon, it is characterised in that：The preparation method bag of the superfine type viscose rayon
Include following steps：
A：Mass ratio will be used for 5：1 cotton pulp and jute pulp is mixed, and its degree of polymerization is impregnated in dress for 1100 pulp material
Have in the treating tank of alkali lye, 35 DEG C of dipping temperature, dip time 70min, ground by tubular type grinder after 30s, concentration, which is made, is
5% slurry congee, wherein, pulp material is made up of wood pulp, and alkali lye is 110~240g/L of concentration sodium hydroxide solution, the slurry of acquisition
The temperature of congee is 30 DEG C；
B：Congee will be starched made from step A and delivers to squeezer, 60 DEG C of pressing temperature of setting, squeezing multiple 2.5 deliver to powder after squeezing
Broken machine is crushed, and sets degree of grinding as 160g/L, is obtained alkali cellulose, is obtained after the alkali cellulose is delivered into kneading machine, processing
Obtain the slurry congee that concentration is 35%；
C：Reactor is delivered to by being starched made from step B after congee is mixed with alkali lye, pure oxygen is added in the reactor, is gathered after drop is poly-
Right is the alkali cellulose that the fine purity of 600, first is 98.5%, wherein, alkali lye selects concentration 180g/L sodium hydroxide solution, instead
The addition for answering pure oxygen in device is 8%, drops poly- reaction time control in 60min；
D：Alkali cellulose made from step C is delivered into xanthating machine, it is anti-that in xanthating machine with carbon disulfide yellow occurs for alkali cellulose
Should, wherein, the addition of carbon disulfide is 37% of the fine content of first in alkali cellulose made from step B, and the yellow reaction time should
Control is in 50min, and the cellulose sulfonate that the control of yellow reaction temperature is obtained after 30 DEG C, yellow reaction dissolves with solvent, molten
Solution preocess is that cellulose sulfonate is mixed with solvent, stirred and is ground, and solvent then uses concentration for 45 g/L hydroxides
Sodium solution and the sodium sulfite aqueous solution that concentration is 7 g/L, solution temperature is 15 DEG C, and dissolution time is 45min, is made after dissolving
Concentration is 10.0% cellulose sulfonate solution；
E：Cellulose sulfonate solution made from step D is obtained into spinning solution after filtering, deaeration, maturation；
F：The obtained spinning solutions of step E are delivered into spinning-drawing machine, silk is formed after a bath by the shower nozzle extruding spinning thread of spinning-drawing machine
Beam, the coagulating bath that a bath is used includes the sulphur of 90~100g/L sulfuric acid, 220~260g/L sodium sulphate and 8~12g/L
Sour zinc, a bath temperature is 40~50 DEG C, the acid bath drop of a bath is 4.5g/L；
G：Tow after being bathed through one is sent into two by one of drafting machine and bathed, and the coagulating bath that two bath is used includes 18~20g/L's
Sulfuric acid, the degree of draft of one of drafting machine is 50~80%, and two bath temperatures are 80~88 DEG C；
H：Tow after being bathed through two is bathed by two road drafting machine feedings three, and it is 1~2 that the coagulating bath that three bath is used, which includes pH value,
Sulfuric acid, the degree of draft of two road drafting machine is 40~58%, and three bath temperatures are 80~90 DEG C；
I：Tow after being bathed through three delivers to step J by three road drafting machines, and the degree of draft of three road drafting machine is 5%；
J：The tow obtained to step I carries out desulfurization, bleaches and oil, wherein, the desulfurizing agent that desulfurization is used is 8g/L by concentration
Vulcanized sodium and concentration constituted for 4g/L sodium carbonate, set desulfurization temperature as 55 DEG C, desulfurization time is 2min, bleaches and use
Bleaching agent is concentration 0.5g/L hydrogen peroxide, sets bleaching temperature as 55 DEG C, bleaching time is 2min；The temperature used that oils is
55 DEG C of finish, its addition is 9g/L, and the pH value of tow is 7 after oiling；
K：To using drying machine drying through desulfurization, the tow bleached and obtained after oiling in step J, drying temperature is set as 115
DEG C, after drying, the superfine type viscose rayon product of high-strength flatness is obtained, product regain is controlled 12%,
The superfine type viscose rayon product of the high-strength flatness is met：
0.91~1.11D of fiber number, does 3.43~3.6cN/dtex of fracture strength,
1.65~1.85cN/dtex of wet breaking strength,
0.55~0.65cN/dtex of intensity needed for 5% elongation is produced under wet condition,
Dry elongation at break 14.0~15.0%, wet elongation at break 18%,
Crystallinity 42%, radial water swelling capacity 23~24%,
Line density deviation ratio -1.5~1%, whiteness 83.2~83.35%,
Residual sulphur 7mg/100g, length variation rate 0.5~1%,
Overlength fiber rate 0~0.2%, over-length fibre 0mg/100g,
0.9~1.5mg/100g of fault, the dry ultimate strength coefficient of variation 18%.
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| EP3596133A4 (en) * | 2017-03-15 | 2021-01-27 | TreeToTextile AB | Regenerated cellulosic fibres spun from an aqueous alkaline spindope |
| CN107326460B (en) * | 2017-07-27 | 2019-11-15 | 阜宁澳洋科技有限责任公司 | Equipment for after-treatment used in a kind of preparation method and preparation method of flocking viscose rayon |
| CN107938010A (en) * | 2017-10-30 | 2018-04-20 | 宜宾丝丽雅股份有限公司 | High-strength fine-denier flame-retardant viscose fiber and production process thereof |
| CN107974722A (en) * | 2017-10-30 | 2018-05-01 | 宜宾丝丽雅股份有限公司 | Production process of high-strength fine-denier flame-retardant viscose fiber |
| CN107964693A (en) * | 2017-10-30 | 2018-04-27 | 宜宾丝丽雅股份有限公司 | Production process of high-strength flame-retardant viscose fiber |
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| CN101851802A (en) * | 2010-05-24 | 2010-10-06 | 杭州奥通科技有限公司 | Method for producing functional high wet modulus fiber by using hemp-containing pulp |
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