CN106283224A - A kind of wet method has greatly the preparation method of light acrylon - Google Patents
A kind of wet method has greatly the preparation method of light acrylon Download PDFInfo
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Abstract
A kind of wet method has greatly the preparation method of light acrylic fiber, comprise the steps: the preparation of (1) polymer: by acrylonitrile, two kinds of monomer mixing of vinyl acetate, carrying out aqueous suspension polymerization reaction, reaction terminates post processing and obtains polyacrylonitrile powdery polymer；(2) preparation of spinning solution: the powdery polymer of step (1) is dissolved in dimethyl acetylamide, is filtrated to get spinning solution；(3) in spinning solution, add retarder, carry out spinning at 0.7～0.9MPa pressure, at a temperature of 80～97 DEG C, coagulation forming in coagulating bath aqueous solution；(4) tow of molding passes through washing, drawing-off, oils, dries, crimps and shape, and is had greatly light acrylic fiber.Reduce fiber surface groove and inner void by improving stock solution and spinning moulding and aftertreatment technology condition, improve gloss and the light transmission of fiber, meet the market demand.Production method simple possible, technique is easily controlled.
Description
Technical field
The invention belongs to field of textiles, in particulaing relate to a kind of wet method has greatly light acrylic fiber and preparation method thereof.
Background technology
Acrylic fiber has the gloss that a kind of more conventional lustrous fibre is brighter to have greatly light acrylic fiber to refer to, is differential
One important kind of acrylon, is widely used in woollen blanket especially artificial fur industry, but domestic technique shortcoming,
So cannot meet the market demand always, the overwhelming majority has greatly light acrylic fiber to rely on import.
Therefore, exploitation has greatly light acrylic fiber promise well, also meets people simultaneously and day by day improves quality of life
Demand, social benefit is obvious, has sizable growth potential.But due to wet spinning acrylic fibers operational characteristic certainly
Determine fiber surface and had groove and fibrous inside has hole, affect the gloss of fiber and the light transmission of fiber, as
What can reduce groove with hole is to solve fiber gloss and the key of light transmission.
The system of a kind of dry spinning bright polyacrylic fibre is disclosed in Chinese patent application CN200510062744.3
Preparation Method, by improving original spinning moulding aftertreatment technology, in washing, drafting process, improves washing temperature,
Controlling at 96-100 DEG C, reduce drafting multiple and control at 2.65-4.5 times, draft speed controls
230-360m/min, improves baking temperature and the steam flow of drying process after washing, drawing-off simultaneously, both ensure that
Strand has enough Extensional periods, avoids again causing the damage of strand, thus decreases the coarse of fiber surface
Degree and degree of injury, improve fiber finish and densification degree.
In order to widen the method having greatly light acrylic fiber that produces, such as wet method preparation has greatly light acrylon, spy to propose this
Bright.
Summary of the invention
The purpose of an aspect of of the present present invention is, it is provided that a kind of wet method has greatly the preparation method of light acrylic fiber, passes through
Improve stock solution and spinning moulding and aftertreatment technology condition to reduce fiber surface groove and inner void, improve fiber
Gloss and light transmission, meet the market demand.Production method simple possible, technique is easily controlled.
For realizing the purpose of the present invention, adopt the following technical scheme that
A kind of wet method has greatly the preparation method of light acrylic fiber, comprises the steps:
(1) preparation of polymer: by acrylonitrile, two kinds of monomer mixing of vinyl acetate, carry out aqueous suspension polymerization reaction,
Reaction terminates post processing and obtains polyacrylonitrile powdery polymer；
(2) preparation of spinning solution: be dissolved in dimethyl acetylamide by the powdery polymer of step (1), solution passes through
Add retarder after filtration, obtain spinning solution；
Or in solvent dimethyl acetylamide, first add retarder mixing, add the powdery polymer of step (1),
To spinning solution；
(3) spinning solution that step (2) obtains carries out spinning at 0.7～0.9MPa pressure, at a temperature of 80～97 DEG C,
Coagulation forming in coagulating bath aqueous solution；
(4) tow of molding passes through washing, drawing-off, oils, dries, crimps and shape, and is had greatly light acrylon fine
Dimension.
A kind of wet method to the present invention has greatly the further details of introduction of preparation method of light acrylic fiber below.
A kind of wet method has greatly the preparation method of light acrylic fiber, comprises the steps:
(1) preparation of polymer: by acrylonitrile, two kinds of monomer mixing of vinyl acetate, carry out aqueous suspension polymerization reaction,
Reaction terminates post processing and obtains polyacrylonitrile powdery polymer；
(2) preparation of spinning solution: be dissolved in dimethyl acetylamide by the powdery polymer of step (1), solution passes through
Add retarder after filtration, obtain spinning solution；
Or in solvent dimethyl acetylamide, first add retarder mixing, add the powdery polymer of step (1),
To spinning solution；
(3) spinning solution that step (2) obtains carries out spinning at 0.7～0.9MPa pressure, at a temperature of 80～97 DEG C,
Coagulation forming in coagulating bath aqueous solution；
(4) tow of molding passes through washing, drawing-off, oils, dries, crimps and shape, and is had greatly light acrylon fine
Dimension.
Further, in step (1), the percentage by weight of starting monomer acrylonitrile and vinyl acetate is respectively 92～94wt%,
6～8wt%.
Further, in step (1), the two mixed total concentrations of monomer are 30～40wt%.
Further, in step (1), polymeric reaction condition is: temperature 58～62 DEG C, and pH is 2.5～3.5.
Polyreaction in step (1), reaches the conventional needs of field of textiles at polymer and can terminate reaction.At this
In bright, the polymer after polyreaction terminates through chelatropic reaction, deviates from unreacted monomer with stripper, then through washing
Filter removes salinity, moisture, the powdery polymer obtained through drying after granulating and forming.
Preferably, step of the present invention (1) is that 0.147-0.157 terminates reaction at the intrinsic viscosity of polymeric reaction product.
In the polyreaction of step (1), appropriate catalyst or stabilizer etc. can be added as required, be all this area
Technical staff can need selection according to reaction.
In step (2), when temperature 80～90 DEG C, polymer is dissolved completely in dimethyl acetylamide, filters
The spinning solution prepared.
Further, in step (2), the concentration of the spinning solution of preparation is 23～28wt%, its be preferably 24.8～
25.5wt%.
Further, in step (3), the addition of described retarder is the 0.5～2wt% of polyacrylonitrile weight, its
It is preferably 1.0～1.5wt%.
Further, retarder can be directly appended to mix homogeneously in spinning solution；First retarder can also be dissolved in diformazan
Yl acetamide obtains retarder solution, then in adding spinning solution to；Preferably, first retarder is dissolved in diformazan
Yl acetamide obtains retarder solution, 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, described retarder include but not limited to water, boric acid, sodium borate, zinc sulfate, phosphoric acid, phosphatic one
Kind or two or more mixture, it is preferably sodium borate, zinc sulfate, water, one or two or more kinds mixed phosphatic
Compound, more preferably one or more mixture of sodium borate, zinc sulfate, water.
Further, described coagulating bath is dimethylacetamide amine aqueous solution, and its mass percent concentration is 25～50wt%；
Being preferably, its mass percent concentration is 30～48wt%.
Further, the temperature 25 of described coagulating bath～40 DEG C, it is preferred, and the temperature of coagulating bath is 25～35 DEG C.
By in spinning solution add retarder, fiber when molding double diffusion, a part of water be used for dissolution retarder or
Person slows down the solution of coagulating bath and carries out double diffused speed with spinning solution thus slow down fiberizing.
Further, during the drawing-off of step (4), drafting multiple is 4～10 times；Its preferred drafting multiple 6～9
Times.
Further, the sizing in step (4) includes by 200～330KPa sizing pressure shapings.
Described washing, oil, dry, method that the process such as curling uses prior art conventional is carried out.
What the present invention prepared have greatly, and light acrylic fiber has light acrylic fiber facade to contrast with surface with routine: from data above and
Picture is seen, has greatly the densification degree of light acrylic fiber to be better than routine and has light acrylic fiber, and has greatly light acrylic fiber
Having light acrylic fiber specific surface groove shallow with routine and few, inner void is bright little, as seen accompanying drawing 2,4.
The present invention compared with prior art has prominent substantive distinguishing features and marked improvement and a good effect:
(1) present invention control by technique, production have greatly light acrylic fiber good luster, light transmission is strong.
(2) present invention process simple possible, is easily controlled, and utilizes the existing apparatus tissues such as existing spinning to produce,
The seriality producing lower procedure does not results in any impact.
Accompanying drawing explanation
Fig. 1 routine has light acrylic fiber facade
Fig. 2 present invention has greatly light acrylic fiber facade
Fig. 3 routine has light acrylic fiber surface
Fig. 4 present invention has greatly light acrylic fiber surface
Detailed description of the invention
Below the preparation method having greatly light acrylic fiber of the present invention is described in further detail, does not limit the present invention's
Protection domain, its protection domain defines with claims.Detail disclosed in some is to embodiment disclosed in each
There is provided and understand comprehensively.But, those skilled in the relevant art know, do not use these concrete details one or more,
And use the situation of other material etc. also can realize embodiment.
Embodiment 1
(1) preparation of polymer: by 94wt% acrylonitrile, the two kinds of monomer mixing of 6wt% vinyl acetate, and will
Its mixed concentration is adjusted to 35wt%, in 58～62 DEG C, pH be 2.5 be carried out continuously aqueous suspension polymerization reaction；
When the intrinsic viscosity of reaction system reaches 0.152, terminate through chelatropic reaction, unreacted with stripper abjection
Monomer, then removes salinity, moisture through water washed filter, the polyacrylonitrile powder obtained through drying after granulating and forming
Shaped polymer；
(2) preparation of spinning solution: by polyacrylonitrile powdery polymer through the heating 80～90 DEG C that heats up, make to gather
Compound is dissolved completely in dimethyl acetylamide, adds water, obtains spinning solution, wherein, and spinning solution
Concentration is at 25wt%, and the addition of water is the 0.5wt% of polyacrylonitrile weight；
(3) spinning solution that step (2) obtains again through pressure regulation, filter after in 0.9MPa pressure, 80～97
Carrying out spinning at a temperature of DEG C, in coagulating bath, wherein, coagulating bath is dimethylacetamide amine aqueous solution, and it is dense
Degree is 30wt%, and temperature is 25～40 DEG C；Through washing, drawing-off, oil, dry, crimp, its drafting multiple
It is 7 times, by 260KPa sizing pressure shaping, prepares and have greatly light acrylic fiber.
Embodiment 2
The preparation of this embodiment has greatly technical process and the technological parameter reference example 1 of light acrylic fiber, different
Being that retarder is sodium borate, the addition of sodium borate is the 1.0wt% of polyacrylonitrile weight.
Embodiment 3
The preparation of this embodiment has greatly technical process and the technological parameter reference example 1 of light acrylic fiber, different
Being that retarder is zinc sulfate, the addition of zinc sulfate is the 1.5wt% of polyacrylonitrile weight.
Embodiment 4
The preparation of this embodiment has greatly technical process and the technological parameter reference example 1 of light acrylic fiber, different
It is that retarder is that the totalling of zinc sulfate and water, zinc sulfate and water enters the 2wt% that amount is polyacrylonitrile weight.
Embodiment 5
(1) preparation of polymer: by 92wt% acrylonitrile, the two kinds of monomer mixing of 8wt% vinyl acetate, and by it
Mixed concentration is adjusted to 30wt%, and in 58～62 DEG C, pH is to be carried out continuously aqueous suspension polymerization reaction for 3.5 times；
When the intrinsic viscosity of reaction system reaches 0.152, terminate through chelatropic reaction, unreacted with stripper abjection
Monomer, then removes salinity, moisture through water washed filter, the powdery polymer obtained through drying after granulating and forming；
(2) preparation of spinning solution:
By polyacrylonitrile powdery polymer through the heating 80～90 DEG C that heats up, polymer is made to be dissolved completely in dimethyl second
In amide, adding water, obtain spinning solution, wherein, the concentration of spinning solution is in 28wt%, the addition of water
Amount is the 1.0wt% of polyacrylonitrile weight；
(3) spinning solution again through pressure regulation, filter after in 0.7MPa pressure, at a temperature of 80～97 DEG C,
Carrying out spinning in coagulating bath, wherein, coagulating bath is dimethylacetamide amine aqueous solution, and its concentration is 25wt%, temperature
Degree is 25～40 DEG C；Through washing, drawing-off, oiling, dry, crimp, its drafting multiple is 9 times, passes through
220KPa shapes pressure shaping, prepares and has greatly light acrylic fiber.
Embodiment 6
(1) preparation of polymer: by 93wt% acrylonitrile, the two kinds of monomer mixing of 7wt% vinyl acetate, and by it
Mixed concentration is adjusted to 40wt%, and in 58～62 DEG C, pH is to be carried out continuously aqueous suspension polymerization reaction for 3.0 times,
When the intrinsic viscosity of reaction system reaches 0.152, terminate through chelatropic reaction, unreacted with stripper abjection
Monomer, then removes salinity, moisture through water washed filter, the powdery polymer obtained through drying after granulating and forming；
(2) preparation of spinning solution: sodium borate solvent dimethyl acetylamide is dissolved, makes sodium borate
Form homogeneous solution with solvent, add powdery polymer, through the heating 80～90 DEG C that heats up, make polymer complete
Being dissolved in dimethyl acetylamide, carry out filtering the spinning solution prepared, wherein, the concentration of spinning solution exists
23wt%, the addition of sodium borate is the 1.5wt% of polyacrylonitrile weight；
(3) spinning solution again through pressure regulation, filter after in 0.8MPa pressure, at a temperature of 80～97 DEG C,
Carrying out spinning in coagulating bath, wherein, coagulating bath is dimethylacetamide amine aqueous solution, and its concentration is 40wt%, temperature
Degree is 25～40 DEG C；Through washing, drawing-off, oiling, dry, crimp, its drafting multiple is 7 times, passes through
330KPa shapes pressure shaping, prepares and has greatly light acrylic fiber.
Embodiment 7
The preparation of this embodiment has greatly technical process and the technological parameter reference example 6 of light acrylic fiber, different
Being that retarder is water, the addition of water is the 1.5wt% of polyacrylonitrile weight.
Embodiment 8
The preparation of this embodiment has greatly technical process and the technological parameter reference example 6 of light acrylic fiber, different
It is that retarder is the 1.0wt% that total addition is polyacrylonitrile weight of boric acid and water, boric acid and water.
Experimental example 1
The key technical indexes contrast that the embodiment of the present invention 1 prepares big lustrous fibre and conventional acrylic fiber see table:
| Specification (dtex) | Kind (has light) | Fiber number (dtex) | Intensity (CN/dtex) | Elongation (%) |
| 2.78 | There is greatly light acrylic fiber | 2.8 | 2.81 | 34 |
| 2.78 | Routine has light acrylic fiber | 2.72 | 2.79 | 41 |
| 3.33 | There is greatly light acrylic fiber | 3.44 | 2.84 | 38 |
| 3.33 | Routine has light acrylic fiber | 3.33 | 2.62 | 44 |
Claims (10)
1. wet method has greatly a preparation method for light acrylic fiber, comprises the steps:
(1) preparation of polymer: by acrylonitrile, two kinds of monomer mixing of vinyl acetate, carry out aqueous suspension polymerization reaction,
Reaction terminates post processing and obtains polyacrylonitrile powdery polymer；
(2) preparation of spinning solution: be dissolved in dimethyl acetylamide by the powdery polymer of step (1), solution passes through
Add retarder after filtration, obtain spinning solution；
Or in solvent dimethyl acetylamide, first add retarder mixing, add the powdery polymer of step (1),
To spinning solution；
(3) spinning solution that step (2) obtains carries out spinning at 0.7～0.9MPa pressure, at a temperature of 80～97 DEG C,
Coagulation forming in coagulating bath aqueous solution；
(4) tow of molding passes through washing, drawing-off, oils, dries, crimps and shape, and is had greatly light acrylon fine
Dimension.
Preparation method the most according to claim 1, it is characterised in that in step (3), described retarder
Addition is polyacrylonitrile weight 0.5～2wt%, it is preferably 1～1.5wt%.
Preparation method the most according to claim 1 and 2, it is characterised in that described retarder include water, boric acid,
One or more mixture in sodium borate, zinc sulfate, phosphoric acid, phosphate；It is preferably sodium borate, zinc sulfate,
One or more mixture in water, phosphate；More preferably sodium borate, zinc sulfate, water one or both with
On mixture.
Preparation method the most according to claim 1 and 2, in step (2), when temperature 80～90 DEG C, poly-
Compound is dissolved completely in dimethyl acetylamide, obtains spinning solution.
5. according to the preparation method described in any one of claim 1-4, it is characterised in that described coagulating bath is dimethyl
Acetamide aqueous solution, its mass percent concentration is 25～50wt%；Being preferably, its mass percent concentration is 30～50
Wt%, more preferably 30～48wt%.
Preparation method the most according to claim 5, it is characterised in that the temperature 25 of described coagulating bath～40 DEG C,
It is preferred, and the temperature of coagulating bath is 25～30 DEG C.
7. according to the preparation method described in any one of claim 1-6, it is characterised in that in step (1), raw material
The percentage by weight of monomers acrylonitrile and vinyl acetate is respectively 92～94wt%, 6～8wt%；Two monomers are mixed always
Concentration is 30～40wt%.
8., according to the preparation method described in any one of claim 1-6, it is characterised in that in step (1), polymerization is anti-
The condition is answered to be: temperature 58～62 DEG C, pH is 2.5～3.5.
9. according to the preparation method described in any one of claim 1-6, it is characterised in that in step (2), spinning
The concentration of stock solution is 23～28wt%, and it is preferably 24.8～25.5wt%.
10. according to the preparation method described in any one of claim 1-9, it is characterised in that in the drawing-off of step (4)
During, drafting multiple is 4～10 times；Its preferred drafting multiple 6～8 times；
Sizing in step (4) includes by 200～330KPa sizing pressure shapings.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN108330563A (en) * | 2017-12-08 | 2018-07-27 | 吉林奇峰化纤股份有限公司 | A kind of acrylic fiber and preparation method thereof |
| CN110468460A (en) * | 2018-05-11 | 2019-11-19 | 河北艾科瑞纤维有限公司 | A kind of preparation method and regeneration acrylic fibers product of regeneration acrylic fibers |
| CN112251824A (en) * | 2020-09-21 | 2021-01-22 | 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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| 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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| CN106283224B (en) | 2019-08-20 |
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