CN107541808A - A kind of method that vinegar nitrile filaments are prepared using wet spinning technology - Google Patents
A kind of method that vinegar nitrile filaments are prepared using wet spinning technology Download PDFInfo
- Publication number
- CN107541808A CN107541808A CN201610496034.3A CN201610496034A CN107541808A CN 107541808 A CN107541808 A CN 107541808A CN 201610496034 A CN201610496034 A CN 201610496034A CN 107541808 A CN107541808 A CN 107541808A
- Authority
- CN
- China
- Prior art keywords
- vinegar
- prepared
- stoste
- nitrile
- wet spinning
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention belongs to textile technology field, specifically, is related to a kind of method that vinegar nitrile filaments are prepared using wet spinning technology, comprises the following steps：(1) cellulose diacetate and organic solvent are mixed, dissolving, then through deaeration, be filtrated to get cellulose acetate stoste；(2) the acrylic fibers stoste after cellulose acetate stoste and deaeration, filtering is mixed to get spinning solution；(3) sprayed after spinning solution deaeration, filtering from spinneret, double diffusion is then carried out in coagulating bath, strand separates out shaping and obtains as-spun fibre；(4) as-spun fibre again by drawing-off, wash, oil, drying, winding, winder, classification, packaging process generation vinegar nitrile filaments.Present invention process is simple, is more suitable for industrial production, and gained long filament wet strength and regain significantly improve.
Description
Technical field
The invention belongs to textile technology field, specifically, is related to one kind and prepares vinegar nitrile filaments using wet spinning technology
Method.
Background technology
Vinegar nitrile fiber is Jilin Chemical Fiber Group Co., Ltd.'s independent research and registers brand positioning last word, be by
Jilin Jilin Fu Bo fiber research institute of subordinate Liang Jia subsidiaries of chemical fibre group and Jilin Qifeng Chemical Fibre Stock Co., Ltd. grind jointly
Send out and register brand positioning last word.Wherein vinegar nitrile chopped fiber has carried out patent by Jilin Qifeng Chemical Fibre Stock Co., Ltd.
Application.Vinegar nitrile fiber breaches the technical bottleneck of natural fiber and polyester fiber blending first, turns into a brand-new fabric
Kind, cause highest attention in the industry.Acetate silk and acrylic fiber long filament have been taken into account as the vinegar nitrile filaments in vinegar nitrile fiber
Advantage, while the deficiency of acetate silk and acrylic fiber long filament is compensate for, open another new chemical-fibres filaments kind.With vinegar
Fine long filament is compared, and its intensity is higher, and wearability is more preferable, and intensity can reach more than 1.8CN/dtex, compared with viscose filament yarn, is not had
There is serious exhaust environment pollution, there is good development prospect, compared with acrylic filaments, moisture regain is high, is not likely to produce electrostatic, significantly
The application field of acrylic filaments has been expanded,
Vinegar nitrile filaments be polyacrylonitrile and cellulose acetate with molecular level is combined and a kind of manufactured brand-new fiber, before being
The technological innovation not having.Vinegar nitrile filaments section is in approximate circle, is closer to cashmere fiber section by contrast, both retained
The characteristic advantages such as acrylic fiber and cellulose fibre are fluffy, soft, smooth, intensity is high, have again good dimensional stability,
Warmth retention property and antistatic behaviour, enable a wearer to feel more snugness.Vinegar nitrile filaments be mainly used in cold-proof underwear, sweater, shirt,
The fields such as bed necessaries.
The process that Application No. CN201510079823.2 Chinese patent application provides is complicated, and powdery is poly-
Blob of viscose occurs when being mixed with solvent NaSCN in acrylonitrile, influences stock solution quality, and then influences finished fiber quality, in addition,
Big blob of viscose can block pipeline in pipeline flowing, and small blob of viscose can block spinneret orifice.Because polymer substance is due to molecular weight
Greatly, intermolecular force is also big, and solvent molecule is not easy to penetrate between macromolecular and intermolecular active force is completely eliminated, high polymer
No dissolved gum block phenomenon just occurs.Prior art in order to prevent the generation of blob of viscose, the dissolving of high polymer be divided into swelling and
Two steps are dissolved, the low NaSCN of temperature is added and is swelled, now high-polymer molecular intermolecular forces are substantially reduced, and add temperature
High NaSCN is dissolved, and Application No. CN201510079823.2 Chinese patent application is not involved with.Stoste is spun
Property, have a strong impact on the mechanical property of finished fiber.Spinneret part is mounted in the important precision component at fibre spinning position, is to spin
The primary element of silk shaping, its quality directly influence the economic indicators such as labor productivity, strand quality and cost.
In view of this, it is special to propose the present invention.
The content of the invention
It is an object of the invention to provide a kind of method that vinegar nitrile filaments are prepared using wet spinning technology, present invention process
Simply, industrial production is more suitable for, gained long filament wet strength and regain significantly improve.
To achieve the above object, the present invention comprises the following steps：
(1) cellulose diacetate and organic solvent are mixed, dissolving, then through deaeration, be filtrated to get cellulose acetate stoste；
(2) the acrylic fibers stoste after cellulose acetate stoste and deaeration, filtering is mixed to get spinning solution；
(3) sprayed after spinning solution deaeration, filtering from spinneret, double diffusion is then carried out in coagulating bath, strand separates out
Shaping obtains as-spun fibre；
(4) as-spun fibre again by drawing-off, wash, oil, drying, winding, winder, classification, packaging process generation vinegar nitrile
Long filament.
Blob of viscose occurs when the polyacrylonitrile of powdery mixes with solvent NaSCN in existing patent application, influences stock solution quality,
And then finished fiber quality is influenceed, big blob of viscose can block pipeline in pipeline flowing, and small blob of viscose can block spinneret orifice.Except above-mentioned
It is insufficient outer, powdered polypropylene nitrile, cellulose acetate are dissolved in solvent together, because reunion and solid may occur for powder raw material
Between competitive relation be present, raw material is possible to be completely dissolved, and causes the wasting of resources.Lacked present invention effectively avoids above-mentioned
Point, cellulose diacetate is mixed with organic solvent, dissolved, then through deaeration, be filtrated to get cellulose acetate stoste after again with it is de-
Acrylic fibers stoste mixing after bubble, filtering, the two is all liquid, can be sufficiently mixed, and all passes through deaeration before the two mixing
Filter, evenly, spinning properties are more preferable for mixed spinning solution, and it is superior to obtain fiber index.
For the present invention using acrylonitrile, vinyl acetate as comonomer, dimethyl acetamide, dimethylformamide and dimethyl are sub-
The one of which of sulfone is solvent, and azodiisobutyronitrile is initiator, and acrylic fibers stoste, wherein propylene are obtained using homogeneous solution polymerization
The mass ratio of nitrile and vinyl acetate is 91~92%:8~9%, the proportioning of comonomer, solvent and initiator is 17~18%:
81~82%:1.0%, by experiment investigation, the acrylic fibers stoste that is obtained under above-mentioned condition is with cellulose acetate stoste arbitrarily to compare
Example mixing can obtain the good spinning solution of performance, and then obtain the superior fiber of index.
The degree of acetifying of cellulose diacetate described in step (1) is 2.1~2.8, and water content is 1~7%.
The organic solvent is one kind in dimethyl acetamide, dimethylformamide, dimethyl sulfoxide (DMSO).It is above-mentioned organic molten
Agent is known as good dissolubility energy to acetate fiber of the present invention.
The solid content of dissolving is 10~35%, and dissolution time is 0.5~200 hour.
The temperature of dissolving is 25~120 DEG C.
By experiment investigation, the cellulose acetate stoste obtained under above-mentioned condition has good spinnability, former with acrylic fibers
Liquid can obtain the good spinning solution of performance with arbitrary proportion mixing, and then obtain the superior fiber of index.
The temperature of spinning solution described in step (2) is 25~120 DEG C.Cellulose acetate stoste under above-mentioned condition is protected
Good spinnability is held, the spinning solution obtained after being mixed with acrylic fibers stoste also keeps good performance.
Cellulose acetate stoste is mixed with acrylic fibers stoste with arbitrary proportion.
Coagulator used in coagulating bath is dimethyl acetamide, dimethylformamide or dimethyl sulfoxide solvent in step (3)
The aqueous solution.
The concentration of coagulator used in coagulating bath is 5~70%, and temperature is 20~90 DEG C.
The drafting multiple of drafting process is between 1.0~15.0 in step (4).
By experiment investigation, the fiber index obtained under above-mentioned condition is superior.
Compared with prior art, present invention process is simple, is more suitable for industrial production, gained long filament wet strength and regain
Significantly improve.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below to the technical side in embodiment
Case is clearly and completely described, and following examples are used to illustrate the present invention, but are not limited to the scope of the present invention.
Embodiment 1
(1) it is 1% cellulose diacetate and solvent dimethylformamide mixing by water content, dissolves, wherein, dissolving contains
Gu amount be 10%, solution temperature be 25 DEG C, then through deaeration, be filtrated to get cellulose acetate stoste；
(2) by the acrylic fibers stoste after cellulose acetate stoste and deaeration, filtering according to 20:80 ratios are mixed to get spinning original
Liquid；
(3) spinning solution is sprayed after deaeration, filtering from spinneret, and double expand is carried out in dimethylformamide in water
Dissipate, wherein, coagulant concentration 10%, temperature is 50 DEG C, and strand separates out shaping and obtains as-spun fibre；
(4) as-spun fibre again by 1.0 times of drawing-offs, wash, oil, drying, winding, winder, classification, packaging process generation
Vinegar nitrile filaments.
Relevant parameter：Dry strength：2.4CN/dtex；Wet strength：1.9CN/dtex；Regain is 3%.
Embodiment 2
(1) it is 3% cellulose diacetate and dimethylacetamide solvent mixing by water content, dissolves, wherein, dissolving contains
Gu amount be 15%, solution temperature be 50 DEG C, then through deaeration, be filtrated to get cellulose acetate stoste；
(2) by the acrylic fibers stoste after cellulose acetate stoste and deaeration, filtering according to 50:50 ratios are mixed to get spinning original
Liquid；
(3) spinning solution is sprayed after deaeration, filtering from spinneret, and double expand is carried out in dimethylacetamide amine aqueous solution
Dissipate, wherein, coagulant concentration 5%, temperature is 20 DEG C, and strand separates out shaping and obtains as-spun fibre；
(4) as-spun fibre again by 5.0 times of drawing-offs, wash, oil, drying, winding, winder, classification, packaging process generation
Vinegar nitrile filaments.
Relevant parameter：Dry strength：2.2CN/dtex, wet strength：1.7CN/dtex：Regain is 4%.
Embodiment 3
(1) it is 5% cellulose diacetate and dimethyl sulfoxide solvent mixing by water content, dissolves, wherein, containing for dissolving is solid
Measure as 25%, solution temperature is 100 DEG C, then through deaeration, be filtrated to get cellulose acetate stoste；
(2) by the acrylic fibers stoste after cellulose acetate stoste and deaeration, filtering according to 70:30 ratios are mixed to get spinning original
Liquid；
(3) spinning solution is sprayed after deaeration, filtering from spinneret, and double diffusion is carried out in dimethyl sulphoxide aqueous solution,
Wherein, coagulant concentration 50%, temperature are 70 DEG C, and strand separates out shaping and obtains as-spun fibre；
(4) as-spun fibre again by 7.0 times of drawing-offs, wash, oil, drying, winding, winder, classification, packaging process generation
Vinegar nitrile filaments.
Relevant parameter：Dry strength：2.4CN/dtex；Wet strength：2.0CN/dtex；Regain：7%.
Embodiment 4
(1) it is 7% cellulose diacetate and dimethylacetamide solvent mixing by water content, dissolves, wherein, dissolving contains
Gu amount be 20%, solution temperature be 80 DEG C, then through deaeration, be filtrated to get cellulose acetate stoste；
(2) by the acrylic fibers stoste after cellulose acetate stoste and deaeration, filtering according to 85:15 ratios are mixed to get spinning original
Liquid；
(3) spinning solution is sprayed after deaeration, filtering from spinneret, and double expand is carried out in dimethylacetamide amine aqueous solution
Dissipate, wherein, coagulant concentration 50%, temperature is 50 DEG C, and strand separates out shaping and obtains as-spun fibre；
(4) as-spun fibre again by 10.0 times of drawing-offs, wash, oil, drying, winding, winder, classification, packaging process life
Into vinegar nitrile filaments.
Relevant parameter：Dry strength：2.5CN/dtex；Wet strength：2.1CN/dtex；Regain is 5%.
It is below embodiment 5~24, for operating procedure with embodiment 1, specific process parameter is shown in Table 1.
Table 1
| Embodiment | Cellulose water content (%) | The solid content (%) of dissolving | Solution temperature (DEG C) |
| 5 | 0.2 | 10 | 25 |
| 6 | 0.5 | 10 | 25 |
| 7 | 1 | 10 | 25 |
| 8 | 5 | 10 | 25 |
| 9 | 7 | 10 | 25 |
| 10 | 8 | 10 | 25 |
| 11 | 10 | 10 | 25 |
| 12 | 1 | 5 | 25 |
| 13 | 1 | 8 | 25 |
| 14 | 1 | 20 | 25 |
| 15 | 1 | 35 | 25 |
| 16 | 1 | 38 | 25 |
| 17 | 1 | 40 | 25 |
| 18 | 1 | 10 | 18 |
| 20 | 1 | 10 | 20 |
| 21 | 1 | 10 | 80 |
| 22 | 1 | 10 | 120 |
| 23 | 1 | 10 | 130 |
| 24 | 1 | 10 | 150 |
It is below embodiment 25~44, for operating procedure with embodiment 1, specific process parameter is shown in Table 2.
Table 2
The process that the Application No. CN201510079823.2 of comparative example 1 Chinese patent application provides prepares vinegar nitrile fibre
Dimension
1) production of polymer：Two kinds of 92wt% acrylonitrile, 8wt% vinyl acetates monomers are mixed, and after being mixed
Concentration be adjusted to 30~40wt%, in 58~62 DEG C, pH is carried out continuously aqueous suspension polymerization reaction under being 2.5~3.5；After reaction
Polymer terminated through chelatropic reaction, deviate from unreacted monomer with stripper, then remove salinity, water through water washed filter
Point, obtain powdered polypropylene nitrile through drying after granulating and forming；
2) powdered polypropylene nitrile, cellulose acetate and solvent dimethyl acetamide are pressed into powdered polypropylene nitrile and acetate fiber
Element (85wt%：15wt%) sum presses quality 20wt% with dimethyl acetamide：80wt% ratios are mixed, and 80 are heated to through heating
DEG C, polyacrylonitrile, cellulose acetate is dissolved completely in solvent dimethyl acetamide, then cool to 70 DEG C carry out filtering be made
Spinning solution；
3) spinning solution is spun through temperature-adjustment pressure-adjustment, filtering after at 0.7~0.9MPa pressure, 80~97 DEG C of temperature again
Silk, is 85wt% in powdered polypropylene nitrile and cellulose acetate ratio：15wt% carries out spinning, through coagulating bath (coagulating bath two
The aqueous solution of methylacetamide, its concentration are 30~55wt%, and temperature is 25~50 DEG C.) double diffusion shaping, through washing, drawing-off,
Oil, dry, crimp, its drafting multiple is 10 times, and by 200KPa sizing pressure shapings, vinegar nitrile fiber is made.
The preparation of test example 1, cellulose acetate stoste
1st, the selection of cellulose acetate water content
This experiment has investigated the vinegar using different moisture content in the case of other condition identicals (method is with embodiment 1)
The index of the final obtained fiber of the cellulose acetate stoste that acid cellulose obtains, the results are shown in Table 3.
Table 3
| Cellulose acetate water content (%) | Dry strength (CN/dtex) | Wet strength (CN/dtex) | Regain (%) |
| 0.2 | 1.5 | 1.0 | 1.9 |
| 0.5 | 1.8 | 1.2 | 2.2 |
| 1 | 2.2 | 1.8 | 3.2 |
| 5 | 2.4 | 2.1 | 3.3 |
| 7 | 2.3 | 2.0 | 3.1 |
| 8 | 1.9 | 1.3 | 2.5 |
| 10 | 1.7 | 1.2 | 2.4 |
As shown in Table 3, using the obtained acetate fiber of cellulose acetate that water content is less than 1% and water content is higher than 7%
Finally the dry and wet intensity of obtained fiber and regain reduce plain stoste, and to obtain the superior fiber of index, the present invention selects
Water content is 1~7% cellulose acetate.
2nd, the selection of the solid content of dissolving
In the case of other condition identicals (method is with embodiment 1), the acetic acid for having investigated different solid contents is fine for this experiment
The index of the final obtained fiber of plain stoste is tieed up, the results are shown in Table 4.
Table 4
| The solid content (%) of dissolving | Dry strength (CN/dtex) | Wet strength (CN/dtex) | Regain (%) |
| 5 | 1.6 | 1.1 | 1.8 |
| 8 | 1.7 | 1.3 | 2.2 |
| 10 | 2.2 | 1.8 | 3.2 |
| 20 | 2.3 | 2.0 | 3.4 |
| 35 | 2.2 | 1.9 | 3.3 |
| 38 | 1.8 | 1.4 | 2.1 |
| 40 | 1.5 | 1.0 | 2.0 |
As shown in Table 4, solid content is less than 10% and cellulose acetate stoste of the solid content higher than 35% is final obtained fine
The dry and wet intensity and regain of dimension are relatively low, and to obtain the superior fiber of index, the present invention is 10~35% from solid content
Cellulose acetate stoste.
3rd, the selection of solution temperature
This experiment has investigated the acetate fiber of different temperatures in the case of other condition identicals (method is with embodiment 1)
The index of the final obtained fiber of plain stoste, the results are shown in Table 5.
Table 5
As shown in Table 5, temperature is less than the final obtained fiber of the cellulose acetate stoste of 25 DEG C and temperature higher than 120 DEG C
Dry and wet intensity and regain are relatively low, and to obtain the superior fiber of index, the present invention is fine from the acetic acid that temperature is 25~120 DEG C
Tie up plain stoste.
In summary, the present invention is mixed with organic solvent, dissolved from the cellulose diacetate that water content is 1~7%
To cellulose acetate stoste, wherein the solid content dissolved is 10~35%, solution temperature is 25~120 DEG C, under above-mentioned condition
To cellulose acetate stoste there is good spinnability, the good spinning of performance can be obtained by being mixed with acrylic fibers stoste with arbitrary proportion
Silk stock solution, and then obtain the superior fiber of index.
The preparation of test example 2, acrylic fibers stoste
1st, the selection of the mass ratio of acrylonitrile and vinyl acetate
The spinning solution of the present invention is mixed by cellulose acetate stoste and acrylic fibers stoste, from prior art, vinegar
Fiber made from acid cellulose stoste has excellent dyeability, and therefore, the present invention is not added with during acrylic fibers stoste is prepared
Enter the Third monomer for being mainly used in improving dyeability.
This experiment has been investigated using different acrylonitrile and vinegar in the case of other condition identicals (method is with embodiment 1)
The index of the final obtained fiber of the acrylic fibers stoste of the mass ratio of sour ethene, the results are shown in Table 6.
Table 6
| Acrylonitrile (%) | Vinyl acetate (%) | Dry strength (CN/dtex) | Wet strength (CN/dtex) | Regain (%) |
| 90 | 10 | 1.9 | 1.3 | 2.1 |
| 91 | 9 | 2.3 | 2.0 | 3.3 |
| 92 | 8 | 2.5 | 2.1 | 3.4 |
| 93 | 7 | 1.8 | 1.2 | 2.0 |
| 94 | 6 | 1.6 | 1.1 | 1.8 |
As shown in Table 6, the mass ratio of acrylonitrile and vinyl acetate is 91~92%:When 8~9%, the acrylic fibers stoste of gained
Final obtained fibre property is good.
2nd, the selection of the proportioning of comonomer, solvent and initiator
This experiment in the case of other condition identicals (method is with embodiment 1), investigated using different copolymer monomer,
The index of the final obtained fiber of the acrylic fibers stoste of the proportioning of solvent and initiator, the results are shown in Table 7.
Table 7
| Comonomer (%) | Solvent (%) | Initiator (%) | Dry strength (CN/dtex) | Wet strength (CN/dtex) | Regain (%) |
| 15 | 84 | 1.0 | 1.5 | 1.1 | 1.6 |
| 16 | 83 | 1.0 | 1.7 | 1.2 | 1.8 |
| 17 | 82 | 1.0 | 2.3 | 1.9 | 3.0 |
| 18 | 81 | 1.0 | 2.4 | 2.0 | 3.2 |
| 19 | 80 | 1.0 | 1.6 | 1.0 | 1.9 |
As shown in Table 7, the proportioning of comonomer, solvent and initiator is 17~18%:81~82%:When 1.0%, gained
Acrylic fibers stoste finally obtained fibre property is good.
In summary, the present invention is using acrylonitrile, vinyl acetate as comonomer, dimethyl acetamide, dimethylformamide
One of which with dimethyl sulfoxide (DMSO) is solvent, and azodiisobutyronitrile is initiator, the acrylic fibers obtained using homogeneous solution polymerization
The mass ratio of stoste, wherein acrylonitrile and vinyl acetate is 91~92%:8~9%, comonomer, solvent and initiator are matched somebody with somebody
Than for 17~18%:81~82%:1.0%, the acrylic fibers stoste obtained under above-mentioned condition is with cellulose acetate stoste arbitrarily to compare
Example mixing can obtain the good spinning solution of performance, and then obtain the superior fiber of index.
The selection of the spinning technology parameter of test example 3
1st, the selection of coagulant concentration
This experiment has investigated the coagulator of various concentrations most in the case of other condition identicals (method is with embodiment 1)
The index of fiber made from end, the results are shown in Table 8.
Table 8
| Coagulant concentration (%) | Dry strength (CN/dtex) | Wet strength (CN/dtex) | Regain (%) |
| 1 | 1.7 | 1.2 | 1.7 |
| 3 | 1.9 | 1.3 | 2.0 |
| 5 | 2.3 | 1.9 | 3.1 |
| 10 | 2.5 | 2.1 | 3.2 |
| 50 | 2.6 | 2.3 | 3.1 |
| 70 | 2.5 | 2.2 | 3.0 |
| 80 | 1.8 | 1.2 | 2.2 |
| 100 | 1.6 | 1.1 | 1.9 |
As shown in Table 8, concentration less than 5% and concentration higher than 70% coagulator finally the dry and wet intensity of obtained fiber and
Regain is relatively low, and to obtain the superior fiber of index, the present invention is from the coagulator that concentration is 5~70%.
2nd, the selection of coagulator temperature
This experiment has investigated the coagulator of different temperatures most in the case of other condition identicals (method is with embodiment 1)
The index of fiber made from end, the results are shown in Table 9.
Table 9
| Coagulator temperature (DEG C) | Dry strength (CN/dtex) | Wet strength (CN/dtex) | Regain (%) |
| 10 | 1.6 | 1.0 | 1.8 |
| 15 | 1.8 | 1.2 | 2.1 |
| 20 | 2.3 | 1.9 | 3.1 |
| 50 | 2.4 | 2.1 | 3.2 |
| 90 | 2.3 | 2.0 | 3.1 |
| 100 | 1.9 | 1.4 | 2.3 |
| 120 | 1.7 | 1.3 | 2.0 |
As shown in Table 9, dry and wet intensity of the temperature less than the final obtained fiber of the coagulator of 20 DEG C and temperature higher than 90 DEG C
And regain is relatively low, to obtain the superior fiber of index, the present invention is from the coagulator that temperature is 20~90 DEG C.
3rd, the selection of drafting multiple
It is final to have investigated different drafting multiples in the case of other condition identicals (method is with embodiment 1) for this experiment
The index of obtained fiber, the results are shown in Table 10.
Table 10
| Drafting multiple | Dry strength (CN/dtex) | Wet strength (CN/dtex) | Regain (%) |
| 0.5 | 1.4 | 1.0 | 1.9 |
| 0.8 | 1.6 | 1.1 | 2.2 |
| 1 | 2.3 | 1.9 | 3.1 |
| 5 | 2.5 | 2.1 | 3.2 |
| 15 | 2.4 | 2.0 | 3.2 |
| 17 | 1.8 | 1.3 | 2.1 |
| 20 | 1.3 | 0.9 | 1.7 |
As shown in Table 10, dry and wet intensity and regain of the drafting multiple less than 1.0 and higher than 15.0 final obtained fibers
Relatively low, to obtain the superior fiber of index, the drafting multiple that the present invention selects is between 1.0~15.0.
In summary, the spinning process condition that the present invention selects is as follows：The concentration of coagulator is 5~70%, temperature 20
~90 DEG C, drafting multiple can obtain the superior fiber of index between 1.0~15.0, under above-mentioned condition.
Test example 3
The fiber index of vinegar nitrile fiber made from comparative example 1 of the present invention is detected, and the fiber index pair obtained with embodiment 4
Than the results are shown in Table 11.
Table 11
| Dry strength (CN/dtex) | Wet strength (CN/dtex) | Regain (%) | |
| Embodiment 4 | 2.5 | 2.1 | 5.0 |
| Comparative example 1 | 2.3 | 1.6 | 2.5 |
As shown in Table 11, the dry strength of vinegar nitrile filaments produced by the present invention is slightly above vinegar nitrile fiber made from comparative example 1, wet
Intensity and regain are then apparently higher than vinegar nitrile fiber made from comparative example 1.
Described above is only presently preferred embodiments of the present invention, not makees any formal limitation to the present invention, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any familiar technology people of the invention
Member without departing from the scope of the present invention, when the technology contents using above-mentioned prompting make it is a little change or be modified to
The equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, the technical spirit pair according to the present invention
Any simple modification, equivalent change and modification that above example is made, in the range of still falling within the present invention program.
Claims (10)
- A kind of 1. method that vinegar nitrile filaments are prepared using wet spinning technology, it is characterised in that comprise the following steps：(1) cellulose diacetate and organic solvent are mixed, dissolving, then through deaeration, be filtrated to get cellulose acetate stoste；(2) the acrylic fibers stoste after cellulose acetate stoste and deaeration, filtering is mixed to get spinning solution；(3) sprayed after spinning solution deaeration, filtering from spinneret, double diffusion is then carried out in coagulating bath, strand separates out shaping Obtain as-spun fibre；(4) as-spun fibre again by drawing-off, wash, oil, drying, winding, winder, classification, packaging process generation vinegar nitrile filaments.
- A kind of 2. method that vinegar nitrile filaments are prepared using wet spinning technology according to claim 1, it is characterised in that step Suddenly the degree of acetifying of cellulose diacetate described in (1) is 2.1~2.8, and water content is 1~7%.
- A kind of 3. method that vinegar nitrile filaments are prepared using wet spinning technology according to claim 1, it is characterised in that step Suddenly organic solvent described in (1) is one kind in dimethyl acetamide, dimethylformamide, dimethyl sulfoxide (DMSO).
- A kind of 4. method that vinegar nitrile filaments are prepared using wet spinning technology according to claim 1, it is characterised in that step Suddenly the solid content of dissolving is 10~35% in (1), and dissolution time is 0.5~200 hour.
- A kind of 5. method that vinegar nitrile filaments are prepared using wet spinning technology according to claim 1, it is characterised in that step Suddenly the temperature of dissolving is 25~120 DEG C in (1).
- A kind of 6. method that vinegar nitrile filaments are prepared using wet spinning technology according to claim 1, it is characterised in that step Suddenly cellulose acetate stoste is mixed with acrylic fibers stoste with arbitrary proportion in (2).
- A kind of 7. method that vinegar nitrile filaments are prepared using wet spinning technology according to claim 1, it is characterised in that step Suddenly the temperature of spinning solution is 25~120 DEG C in (2).
- A kind of 8. method that vinegar nitrile filaments are prepared using wet spinning technology according to claim 1, it is characterised in that step Suddenly coagulator used in coagulating bath is the aqueous solution of dimethyl acetamide, dimethylformamide or dimethyl sulfoxide solvent in (3).
- A kind of 9. method that vinegar nitrile filaments are prepared using wet spinning technology according to claim 1, it is characterised in that step Suddenly the concentration of coagulator used in coagulating bath is 5~70% in (3), and temperature is 20~90 DEG C.
- A kind of 10. method that vinegar nitrile filaments are prepared using wet spinning technology according to claim 1, it is characterised in that The drafting multiple of drafting process is between 1.0~15.0 in step (4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610496034.3A CN107541808B (en) | 2016-06-29 | 2016-06-29 | Method for preparing vinyl acetate filaments by adopting wet spinning process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610496034.3A CN107541808B (en) | 2016-06-29 | 2016-06-29 | Method for preparing vinyl acetate filaments by adopting wet spinning process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107541808A true CN107541808A (en) | 2018-01-05 |
| CN107541808B CN107541808B (en) | 2020-08-04 |
Family
ID=60965883
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610496034.3A Active CN107541808B (en) | 2016-06-29 | 2016-06-29 | Method for preparing vinyl acetate filaments by adopting wet spinning process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107541808B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110295437A (en) * | 2018-03-23 | 2019-10-01 | 上海水星家用纺织品股份有限公司 | A kind of home textile fabric using vinegar blueness fiber |
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105002592A (en) * | 2015-02-13 | 2015-10-28 | 吉林奇峰化纤股份有限公司 | Acetate fiber and preparation method thereof |
-
2016
- 2016-06-29 CN CN201610496034.3A patent/CN107541808B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105002592A (en) * | 2015-02-13 | 2015-10-28 | 吉林奇峰化纤股份有限公司 | Acetate fiber and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 祖立武: "《化学纤维成型工艺学》", 30 September 2014, 哈尔滨工业大学出版社 第1版 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110295437A (en) * | 2018-03-23 | 2019-10-01 | 上海水星家用纺织品股份有限公司 | A kind of home textile fabric using vinegar blueness fiber |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107541808B (en) | 2020-08-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107419367B (en) | A kind of antibacterial acrylic fibre and preparation method thereof | |
| CN109957856B (en) | Parallel composite fiber and preparation method thereof | |
| CN105002592B (en) | A kind of vinegar nitrile fiber and preparation method thereof | |
| CN106400166B (en) | A kind of three leaf special-shaped polyester fiber of porous superbright light and preparation method thereof | |
| CN110344131B (en) | Sericin modified regenerated cellulose fiber and preparation method thereof | |
| CN102517671B (en) | Method for preparing carbon fiber precursor by two-step process of aqueous suspension and solution polymerization | |
| CA1097864A (en) | Hygroscopic fibres and filaments of synthetic polymers | |
| CN104630923A (en) | Method for preparing carbon nano tube modified polyacrylonitrile fibers with solution in-situ polymerization technology | |
| CN101195933A (en) | Method for producing Lyocell fibre for tire cord | |
| CN106012076B (en) | A kind of wet spinning preparation method of acetate fiber | |
| CN107313128A (en) | A kind of PBT fiber fabrication process | |
| CN106283251A (en) | A kind of porous ptt fiber HOY silk and preparation method thereof | |
| CN107815741A (en) | A kind of meta-aramid filament preparation process | |
| CN109355730A (en) | A kind of preparation method with high-modulus high resilience polyurethane fiber | |
| CN107541808A (en) | A kind of method that vinegar nitrile filaments are prepared using wet spinning technology | |
| CN106283260A (en) | A kind of porous surpasses flexible polyester fiber FDY silk and preparation method thereof | |
| CN106400168A (en) | Porous super-soft cotton-like polyester fiber, and preparation method thereof | |
| CN106319678B (en) | Porous super soft imitative hair polyester fiber of one kind and preparation method thereof | |
| CN106283261A (en) | A kind of super soft super fine denier polyester fiber of porous and preparation method thereof | |
| CN106521680A (en) | Polyacrylonitrile-based flat fiber preparation method | |
| CN105064029A (en) | Ultra-bright polyester DTY fibers and preparation method thereof | |
| CN112680816B (en) | Polyamide 56 fiber and preparation method and application thereof | |
| CN106283258A (en) | A kind of porous PBT fiber DTY silk and preparation method thereof | |
| CN104088033B (en) | Preparation method for special-shaped lustrous fine-denier polyester low-elastic fiber | |
| CN106319677A (en) | Porous PTT (polytrimethylene terephthalate) fiber FDY (fully drawn yarn) and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |