CN106283224B - A kind of wet process has greatly the preparation method of light acrylic fibers - Google Patents
A kind of wet process has greatly the preparation method of light acrylic fibers Download PDFInfo
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Abstract
A kind of wet process has greatly the preparation method of light acrylic fiber, include the following steps: the preparation of (1) polymer: two kinds of acrylonitrile, vinyl acetate monomers are mixed, aqueous suspension polymerization reaction is carried out, processing obtains polyacrylonitrile powdery polymer after reaction；(2) preparation of spinning solution: the powdery polymer of step (1) is dissolved in dimethyl acetamide, by spinning solution is obtained by filtration；(3) retarder is added in spinning solution, 0.7~0.9MPa pressure, 80~97 DEG C at a temperature of carry out spinning, solidification bath in coagulation forming；(4) molding tow passes through washing, drawing-off, oils, dries, crimps and be formed, and is had light acrylic fiber greatly.Fiber surface groove and inner void are reduced by improving stoste and spinning moulding and aftertreatment technology condition, the gloss and translucency of fiber is improved, meets the market demand.Production method simple possible, technique are easy to control.
Description
Technical field
The invention belongs to field of textiles, in particulaing relate to a kind of wet process has greatly light acrylic fiber and preparation method thereof.
Background technique
There is light acrylic fiber to refer to that acrylic fiber is differential nitrile with a kind of gloss that more conventional lustrous fibre is brighter greatly
One important species of synthetic fibre, is widely used in woollen blanket especially artificial fur industry, but domestic technique is short of, so always
It is unable to satisfy the market demand, the overwhelming majority has greatly light acrylic fiber by import.
Therefore, exploitation has light acrylic fiber promise well greatly, while it is increasing to quality of life also to meet people
Demand, social benefit is obvious, has sizable growth potential.But since wet spinning acrylic fibers operational characteristic determines fiber table
There is groove in face and fibrous inside has hole, influences the gloss of fiber and the translucency of fiber, how can be reduced groove and hole
Hole is the key that solve fiber gloss and translucency.
A kind of preparation of dry spinning bright polyacrylic fibre is disclosed in Chinese patent application CN200510062744.3
Method in washing, drafting process, improves washing temperature, controls in 96- by improving original spinning moulding aftertreatment technology
100 DEG C, drafting multiple control is reduced at 2.65-4.5 times, draft speed is controlled in 230-360m/min, while being improved washing, being led
The drying temperature and steam flow for stretching rear drying process not only ensure that strand had enough Extensional periods, but also avoid point
The damage of subchain improves fiber finish and densification degree to reduce the roughness and degree of injury of fiber surface.
There is the method for light acrylic fiber to widen production greatly, for example wet process preparation there are light acrylic fibers greatly, and the present invention is specifically proposed.
Summary of the invention
The purpose of an aspect of of the present present invention is, the preparation method that a kind of wet process has greatly light acrylic fiber is provided, by changing
Kind stoste and spinning moulding and aftertreatment technology condition reduce fiber surface groove and inner void, improve the gloss of fiber with
Translucency meets the market demand.Production method simple possible, technique are easy to control.
To achieve the purpose of the present invention, it adopts the following technical scheme that
A kind of wet process has greatly the preparation method of light acrylic fiber, includes the following steps:
(1) preparation of polymer: two kinds of acrylonitrile, vinyl acetate monomers are mixed, carry out aqueous suspension polymerization reaction, instead
It should terminate post-processing and obtain polyacrylonitrile powdery polymer；
(2) preparation of spinning solution: the powdery polymer of step (1) is dissolved in dimethyl acetamide, solution passed through
Retarder is added after filter, obtains spinning solution；
Or retarder mixing is first added in solvent dimethyl acetamide and is obtained in the powdery polymer that step (1) is added
To spinning solution；
(3) spinning solution that step (2) obtains 0.7~0.9MPa pressure, 80~97 DEG C at a temperature of carry out spinning,
Solidify coagulation forming in bath；
(4) molding tow passes through washing, drawing-off, oils, dries, crimps and be formed, and is had light acrylic fiber greatly.
There is the further details of introduction of preparation method of light acrylic fiber greatly to a kind of wet process of the invention below.
A kind of wet process has greatly the preparation method of light acrylic fiber, includes the following steps:
(1) preparation of polymer: two kinds of acrylonitrile, vinyl acetate monomers are mixed, carry out aqueous suspension polymerization reaction, instead
It should terminate post-processing and obtain polyacrylonitrile powdery polymer；
(2) preparation of spinning solution: the powdery polymer of step (1) is dissolved in dimethyl acetamide, solution passed through
Retarder is added after filter, obtains spinning solution；
Or retarder mixing is first added in solvent dimethyl acetamide, the powdery polymer of step (1) is added, is obtained
To spinning solution；
(3) spinning solution that step (2) obtains 0.7~0.9MPa pressure, 80~97 DEG C at a temperature of carry out spinning,
Solidify coagulation forming in bath；
(4) molding tow passes through washing, drawing-off, oils, dries, crimps and be formed, and is had light acrylic fiber greatly.
Further, in step (1), the weight percent of starting monomer acrylonitrile and vinyl acetate is respectively 92~
94wt%, 6~8wt%.
Further, in step (1), the mixed total concentration of two monomers is 30~40wt%.
Further, in step (1), polymeric reaction condition are as follows: 58~62 DEG C of temperature, pH is 2.5~3.5.
Polymerization reaction in step (1), polymer reach field of textiles routine needs can reaction was completed.In this hair
In bright, the polymer after polymerization reaction is terminated through chelatropic reaction, deviates from unreacted monomer with stripper, then through washing filtering
Machine removes salinity, moisture, the powdery polymer obtained after granulating and forming through drying.
Preferably, step (1) of the present invention is that reaction was completed by 0.147-0.157 in the intrinsic viscosity of polymeric reaction product.
Suitable catalyst or stabilizer etc. can be added as needed in the polymerization reaction of step (1), be all ability
What field technique personnel can need to select according to reaction.
In step (2), at 80~90 DEG C of temperature, polymer is dissolved completely in dimethyl acetamide, is filtered
Spinning solution obtained.
Further, in step (2), the concentration of the spinning solution of preparation is 23~28wt%, be preferably 24.8~
25.5wt%.
Further, in step (3), the additional amount of the retarder is 0.5~2wt% of polyacrylonitrile weight,
Preferably 1.0~1.5wt%.
Further, retarder can be directly appended to be uniformly mixed in spinning solution；Retarder first can also be dissolved in two
Retarder solution is obtained in methylacetamide, then in being added to spinning solution；Preferably, retarder is first dissolved in dimethyl
Retarder solution is obtained in acetamide, is then then added in spinning solution.
Term " retarder " in the present invention refers to, in fibre solidification forming process, slows down the coagulation forming speed of fiber
Degree.
Further, the retarder includes but is not limited to water, boric acid, Boratex, zinc sulfate, phosphoric acid, phosphatic one kind
Or two or more mixtures, be preferably Boratex, zinc sulfate, water, phosphatic one or two or more kinds mixture, more
Preferably one or more kinds of mixtures of Boratex, zinc sulfate, water.
Further, the coagulating bath is dimethylacetamide amine aqueous solution, and mass percent concentration is 25~50wt%；
Preferably, mass percent concentration is 30~48wt%.
Further, 25~40 DEG C of the temperature of the coagulating bath, preferably, the temperature of coagulating bath are 25~35 DEG C.
By the way that retarder is added in spinning solution, when forming double diffusion, a part of water is used to dissolve out retarder fiber
Or slow down the solution of coagulating bath and the speed of spinning solution progress double diffusion to slow down fiberizing.
Further, during the drawing-off of step (4), drafting multiple is 4~10 times；Its preferred drafting multiple 6~9
Times.
It further, include pressure shaping of being formed by 200~330KPa in the sizing of step (4).
The washing, the processes such as oil, dry, crimping are carried out using the common method of the prior art.
It is produced by the present invention to there is light acrylic fiber and routine to there is light acrylic fiber facade and surface to compare greatly: from above data
It sees there is the densification degree of light acrylic fiber to have light acrylic fiber better than conventional greatly with picture, and has light acrylic fiber and often greatly
Rule have light acrylic fiber specific surface groove shallowly and few, and inner void is bright small, such as sees attached drawing 2,4.
The present invention has substantive distinguishing features outstanding and marked improvement and good effect compared with prior art:
(1) control of the invention by technique, production have light acrylic fiber good luster greatly, and translucency is strong.
(2) present invention process simple possible is easy to control, and is produced using the existing apparatus tissue such as existing spinning, to downstream
The continuity of process production will not have any impact.
Detailed description of the invention
Fig. 1 routinely has light acrylic fiber facade
Fig. 2 it is of the invention have a light acrylic fiber facade greatly
Fig. 3 routinely has light acrylic fiber surface
Fig. 4 it is of the invention have a light acrylic fiber surface greatly
Specific embodiment
There is the preparation method of light acrylic fiber to be described in further detail greatly of the invention below, does not limit of the invention
Protection scope, protection scope are defined with claims.Certain disclosed details propose each disclosed embodiment
For comprehensive understanding.However, those skilled in the relevant art know, one or more of these concrete details are not used, and are used
The situation of other materials etc. can also realize embodiment.
Embodiment 1
(1) preparation of polymer: two kinds of 94wt% acrylonitrile, 6wt% vinyl acetate monomers are mixed, and after being mixed
Concentration be adjusted to 35wt%, in 58~62 DEG C, pH is 2.5 to be carried out continuously aqueous suspension polymerization reaction；In the characteristic of reaction system
It when glutinous number reaches 0.152, is terminated through chelatropic reaction, deviates from unreacted monomer with stripper, then removed through water washed filter
Salinity, moisture, through drying obtained polyacrylonitrile powdery polymer after granulating and forming；
(2) preparation of spinning solution: by polyacrylonitrile powdery polymer through 80~90 DEG C of heating heating, keep polymer complete
It is dissolved in dimethyl acetamide, adds water, obtain spinning solution, wherein the concentration of spinning solution adds in 25wt%, water
Enter the 0.5wt% that amount is polyacrylonitrile weight；
(3) spinning solution that step (2) obtains again after pressure regulation, filtering at a temperature of 0.9MPa pressure, 80~97 DEG C,
Spinning is carried out in coagulating bath, wherein coagulating bath is dimethylacetamide amine aqueous solution, concentration 30wt%, temperature for 25~
40℃；It through washing, drawing-off, oils, dry, crimp, drafting multiple is 7 times, is formed pressure shaping by 260KPa, is made big
There is light acrylic fiber.
Embodiment 2
Embodiment preparation has greatly the technical process and technological parameter reference implementation example 1 of light acrylic fiber, unlike,
Retarder is Boratex, and the additional amount of Boratex is the 1.0wt% of polyacrylonitrile weight.
Embodiment 3
Embodiment preparation has greatly the technical process and technological parameter reference implementation example 1 of light acrylic fiber, unlike,
Retarder is zinc sulfate, and the additional amount of zinc sulfate is the 1.5wt% of polyacrylonitrile weight.
Embodiment 4
Embodiment preparation has greatly the technical process and technological parameter reference implementation example 1 of light acrylic fiber, unlike,
Retarder is zinc sulfate and water, the 2wt% of zinc sulfate and water added up into amount for polyacrylonitrile weight.
Embodiment 5
(1) preparation of polymer: two kinds of 92wt% acrylonitrile, 8wt% vinyl acetate monomers are mixed, and after being mixed
Concentration be adjusted to 30wt%, in 58~62 DEG C, pH is carried out continuously aqueous suspension polymerization reaction under being 3.5；In the spy of reaction system
Property glutinous number when reaching 0.152, terminated through chelatropic reaction, deviate from unreacted monomer with stripper, then removed through water washed filter
Remove salinity, moisture, the powdery polymer obtained after granulating and forming through drying；
(2) preparation of spinning solution:
By polyacrylonitrile powdery polymer through 80~90 DEG C of heating heating, polymer is made to be dissolved completely in dimethyl acetamide
In, water is added, spinning solution is obtained, wherein the concentration of spinning solution is polyacrylonitrile weight in 28wt%, the additional amount of water
1.0wt%；
(3) spinning solution again after pressure regulation, filtering at a temperature of 0.7MPa pressure, 80~97 DEG C, in coagulating bath into
Row spinning, wherein coagulating bath is dimethylacetamide amine aqueous solution, and concentration 25wt%, temperature is 25~40 DEG C；Washed,
Drawing-off oils, dries, crimping, and drafting multiple is 9 times, and by 220KPa sizing pressure shaping, being made greatly has light acrylic fibers fine
Dimension.
Embodiment 6
(1) preparation of polymer: two kinds of 93wt% acrylonitrile, 7wt% vinyl acetate monomers are mixed, and after being mixed
Concentration be adjusted to 40wt%, in 58~62 DEG C, pH is carried out continuously aqueous suspension polymerization reaction under being 3.0, in the spy of reaction system
Property glutinous number when reaching 0.152, terminated through chelatropic reaction, deviate from unreacted monomer with stripper, then removed through water washed filter
Remove salinity, moisture, the powdery polymer obtained after granulating and forming through drying；
(2) preparation of spinning solution: Boratex is dissolved with solvent dimethyl acetamide, makes Boratex and solvent shape
At homogeneous solution, powdery polymer is added, through 80~90 DEG C of heating heating, polymer is made to be dissolved completely in dimethyl acetamide
In, it is filtered spinning solution obtained, wherein the concentration of spinning solution is polypropylene in 23wt%, the additional amount of Boratex
The 1.5wt% of nitrile weight；
(3) spinning solution again after pressure regulation, filtering at a temperature of 0.8MPa pressure, 80~97 DEG C, in coagulating bath into
Row spinning, wherein coagulating bath is dimethylacetamide amine aqueous solution, and concentration 40wt%, temperature is 25~40 DEG C；Washed,
Drawing-off oils, dries, crimping, and drafting multiple is 7 times, and by 330KPa sizing pressure shaping, being made greatly has light acrylic fibers fine
Dimension.
Embodiment 7
Embodiment preparation has greatly the technical process and technological parameter reference implementation example 6 of light acrylic fiber, unlike,
Retarder is water, and the additional amount of water is the 1.5wt% of polyacrylonitrile weight.
Embodiment 8
Embodiment preparation has greatly the technical process and technological parameter reference implementation example 6 of light acrylic fiber, unlike,
Retarder is boric acid and water, and total additional amount of boric acid and water is the 1.0wt% of polyacrylonitrile weight.
Experimental example 1
The key technical indexes comparison that big lustrous fibre and conventional acrylic fiber is made to the embodiment of the present invention 1 see the table below:
| Specification (dtex) | Kind (has light) | Fiber number (dtex) | Intensity (CN/dtex) | It extends (%) |
| 2.78 | There is light acrylic fiber greatly | 2.8 | 2.81 | 34 |
| 2.78 | Routine has light acrylic fiber | 2.72 | 2.79 | 41 |
| 3.33 | There is light acrylic fiber greatly | 3.44 | 2.84 | 38 |
| 3.33 | Routine has light acrylic fiber | 3.33 | 2.62 | 44 |
Claims (11)
1. a kind of wet process has greatly the preparation method of light acrylic fiber, include the following steps:
(1) preparation of polymer: two kinds of acrylonitrile, vinyl acetate monomers are mixed, and carry out aqueous suspension polymerization reaction, reaction knot
Beam post-processes to obtain polyacrylonitrile powdery polymer；
(2) under conditions of 80~90 DEG C of temperature, the powdery polymer of step (1) preparation of spinning solution: is dissolved in dimethyl
In acetamide, retarder is added after filtering in solution, obtains spinning solution；
Or retarder mixing is first added in solvent dimethyl acetamide, step is added under conditions of 80~90 DEG C of temperature
(1) powdery polymer, obtains spinning solution,
Wherein, the retarder includes one or more mixtures of water, Boratex, zinc sulfate, phosphate, described
Retarder additional amount be polyacrylonitrile weight 1~1.5wt%,
The concentration of spinning solution is 23~28wt%；
(3) spinning solution that step (2) obtains 0.7~0.9MPa pressure, 80~97 DEG C at a temperature of carry out spinning, solidifying
Coagulation forming in bath；The coagulating bath be dimethylacetamide amine aqueous solution, mass percent concentration be 25~
50wt%, 25~40 DEG C of the temperature of the coagulating bath；
(4) molding tow passes through washing, drawing-off, oils, dries, crimps and be formed, and is had light acrylic fiber greatly.
2. preparation method according to claim 1, which is characterized in that in step (3), the additional amount of the retarder
For 0.5~2wt% of polyacrylonitrile weight.
3. preparation method according to claim 1, which is characterized in that in step (1), starting monomer acrylonitrile and acetic acid
The weight percent of ethylene is respectively 92~94wt%, 6~8wt%；The mixed total concentration of two monomers is 30~40wt%.
4. preparation method according to claim 1-3, which is characterized in that in step (1), polymeric reaction condition
Are as follows: 58~62 DEG C of temperature, pH is 2.5~3.5.
5. preparation method according to claim 1-3, which is characterized in that during the drawing-off of step (4),
Drafting multiple is 4~10 times；
It include pressure shaping of being formed by 200~330KPa in the sizing of step (4).
6. preparation method according to claim 1, which is characterized in that the retarder includes Boratex, zinc sulfate, water
One or more kinds of mixtures.
7. preparation method according to claim 1, which is characterized in that the mass percent of dimethylacetamide amine aqueous solution is dense
Degree is 30~50wt%.
8. preparation method according to claim 1, which is characterized in that the mass percent of dimethylacetamide amine aqueous solution is dense
Degree is 30~48wt%.
9. preparation method according to claim 1, which is characterized in that the temperature of the coagulating bath is 25~30 DEG C.
10. preparation method according to claim 1, which is characterized in that in step (2), the concentration of spinning solution is
24.8~25.5wt%.
11. preparation method according to claim 5, which is characterized in that 6~8 times of drafting multiple.
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| CN107419351A (en) * | 2017-07-27 | 2017-12-01 | 合肥远科服装设计有限公司 | A kind of preparation technology of acrylic fiber |
| CN108330563B (en) * | 2017-12-08 | 2020-11-03 | 吉林奇峰化纤股份有限公司 | Acrylic fiber and preparation method thereof |
| CN110468460B (en) * | 2018-05-11 | 2022-02-18 | 河北艾科瑞纤维有限公司 | Preparation method of recycled acrylic fiber and recycled acrylic fiber product |
| CN112251824B (en) * | 2020-09-21 | 2023-03-28 | 吉林富博纤维研究院有限公司 | Preparation process of polyacrylonitrile fiber and polyacrylonitrile fiber |
| CN112410898A (en) * | 2020-11-26 | 2021-02-26 | 常熟市正太纺织有限公司 | Fur-like fiber fabric with softness and high glossiness and preparation method thereof |
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| CN100362149C (en) * | 2004-09-23 | 2008-01-16 | 中国石化上海石油化工股份有限公司 | Wet spinning method for polyacryl-nitrile fibre |
| CN100535210C (en) * | 2007-07-31 | 2009-09-02 | 浙江杭州湾腈纶有限公司 | Method for preparing acrylic fibre used for building |
| CN101445967B (en) * | 2008-12-12 | 2010-11-10 | 浙江杭州湾腈纶有限公司 | Preparation method of flat acrylic fiber |
| JP2012224955A (en) * | 2011-04-19 | 2012-11-15 | Teijin Techno Products Ltd | Method for producing para-type whole aromatic polyamide fiber and fiber obtained by the method |
| JP5608627B2 (en) * | 2011-11-25 | 2014-10-15 | 株式会社Ｎｔｔドコモ | Transmitting apparatus, receiving apparatus and method |
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| CN102260919A (en) * | 2011-06-29 | 2011-11-30 | 中国科学院宁波材料技术与工程研究所 | Method for homogenizing, solidifying and forming polyacrylonitrile precursor |
| CN103498208A (en) * | 2013-09-26 | 2014-01-08 | 吉林奇峰化纤股份有限公司 | Thermal storage fiber and preparation method thereof |
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