CN1986919A - Process of producing polyacrylic fiber dyeable with both cationic dye and acid dye - Google Patents
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Abstract
The process of producing polyacrylic fiber dyeable with both cationic dye and acid dye includes dissolving polyacrylonitrile resin A and polyacrylonitrile resin B in the weight ratio of 1 to (0.6-1.6) in solvent of dimethyl formamide, dimethyl acetamide or dimethyl sulfoxide to form raw spinning liquor with total solid content of 25-40 %; spinning the raw spinning liquor at 70-130 deg.c to form nascent fiber; and post-treatment of the nascent fiber to produce polyacrylic fiber product. The second monomer for resin A and resin B is methyl acrylate or vinyl acetate, the third monomer for resin A is sodium styryl sulfonate and accounts for 0.8-5.0 wt%; and that for resin B is one of N, N-dimethyl amido ethyl methyl acrylate nitrate, N-dimethyl amido ethyl methyl acrylate hydrochloride or N-dimethyl amido ethyl methyl acrylate sulfate and accounts for 3.3-12.5 wt%.
Description
Technical field
The present invention relates to a kind of method of making acrylic fiber, particularly organic solvent dry-spinning technology is made the method for acrylic fiber.
Background technology
Acrylic fiber has good bulkiness and warmth retention property, and is soft, and performance exactly likes wool, and very superior light resistance and radiation resistance are arranged.The application surface of acrylic fibers is very wide, take, field such as bedding and soft decoration all is desirable textile raw material.The spinning material of acrylic fibers is a polyacrylonitrile resin, simple polyacrylonitrile resin dyeability is very poor, so improve the second flexible comonomer except adding in the resin, also must add the 3rd comonomer that is used for dyeing, modifying, so that the seat that dyes that dyes on the dyestuff to be provided to polymer molecule.In the prior art, the 3rd monomer of plain polypropylene nitrile resin only is fit to cationic dyeing.Because the performance of acrylic fibers exactly likes wool, acrylic fibers and wool blended, the mixed fabric of knitting occupy very big ratio in the converted products behind acrylic fibers.But wool should adopt ACID DYES to dye, and therefore hair-nitrile blending, mixes the fabric of knitting and requires acrylic fibers and wool can carry out " with bath " to dye, and promptly requires the 3rd comonomer in the polyacrylonitrile resin can be fit to the dyeing of ACID DYES.The manufacturing technology of acid-dyeable acrylic fibers has been seen more report, opens clear 56-21842, spy as the Japan Patent spy and opens the content that clear 55-8604 and the clear 48-7888 of Te Kai have all related to this respect.Although still there is obvious defects in these existing acid-dyeable acrylic fibers, reactivity ratio is on the low side in the copolymerization system that is constituted as the 3rd monomer of dyeing, modifying and acrylonitrile and flexible modification second monomer commonly used, so that easily cause dyeing saturation value can't reach desirable numerical value, but realized the acid-dyeable of acrylic fiber after all.
But existing acrylic fiber only has the dye accessible performance of single kind, or cationic dye capable of dyeing or acid-dyeable, can't accomplish that two kinds of dyestuffs all can dye.This obviously gives in the production of product sales management, the weaving processing of road, back and dyeing and finishing process of acrylic fiber and has increased difficulty in the management.
Summary of the invention
Technical problem to be solved by this invention provides the manufacture method of the acrylic fibers that a kind of cation dyes and ACID DYES all can dye, and no matter the acrylic fiber that this method makes all has desirable dyeing saturation value to cation dyes or ACID DYES.
Below be the technical scheme that the present invention solves the problems of the technologies described above:
The manufacture method of the acrylic fibers that a kind of CATION, ACID DYES all can be dyed, this method comprises process:
1) polyacrylonitrile resin A and B are dissolved in solvent and make spinning solution, A or B are terpolymer, viscosity average molecular weigh is 4～70,000, both first monomers are that acrylonitrile, second monomer are methyl acrylate or vinylacetate, wherein the 3rd monomer of A is a Sodium styrene sulfonate, and the 3rd monomer of B is a kind of in methacrylic acid N, silomate base ethyl ester nitrate, methacrylic acid N, silomate base carbethoxy hydrochloride or methacrylic acid N, the silomate base ethyl ester sulfate.In the total amount of three kinds of comonomers, second content of monomer of A or B is 5.5～16.5wt%, and the 3rd content of monomer of A is 0.8～5.0wt%, and the 3rd content of monomer of B is 3.3～12.5wt%.The weight ratio of A and B is A: B=1 in the spinning solution: (0.6～1.6), total solid content are 25～40%, and solvent is a kind of in dimethyl formamide, dimethylacetylamide or the dimethyl sulfoxide (DMSO);
2) spinning solution spray silk, spinning temperature is 70～130 ℃, and the shower nozzle degree of draft is 35～50%, and tow is an as-spun fibre through 300～500 ℃ high temperature inert gas heating back solvent evaporates solidification forming;
3) as-spun fibre is made the acrylic fiber product through last handling process.
The 3rd monomer of above-mentioned B is preferably methacrylic acid N, silomate base ethyl ester nitrate or methacrylic acid N, silomate base carbethoxy hydrochloride, and the 3rd content of monomer of B is preferably 6.0～10.0wt%;
Total solid content is preferably 30～32wt% in the spinning solution, and solvent is dimethyl formamide preferably;
A and B are preferably the powdery polymer that obtains by aqueous polymerization.
Above-mentioned inert gas is generally nitrogen.
Above-mentioned as-spun fibre the last handling process of process comprise washing, drawing-off, oil, curl and oven dry etc.
Key of the present invention is that the polyacrylonitrile resin raw material that is used for spinning has comprised two kinds of polyacrylonitrile copolymers, and wherein A is a cationic dye capable of dyeing polyacrylonitrile resin conventional in the prior art, and B then is a kind of polyacrylonitrile resin of acid-dyeable.This makes that the fiber of making still is that ACID DYES all has good stainability to cation dyes.Be understood that after comprising these two kinds of copolymers of A and B in the spinning material simultaneously, for a certain dyestuff (cation dyes or ACID DYES), what combine with dye molecule in the fiber dyes seat with corresponding minimizing in proportion.Therefore no matter be A or B, should be with the wherein corresponding raising of the 3rd content of monomer of dyeing, modifying, could guarantee like this in the fiber at a certain dye molecule to dye a content constant.By prior art as can be known, these known cationic dye capable of dyeing the 3rd monomers have very high reactivity ratio in the copolymerization system that constitutes with second monomer by acrylonitrile and flexible modification, so the raising of the 3rd content of monomer is not difficult in the copolymer.Rate is too low can't to guarantee that the 3rd monomer can be brought up to enough content in the copolymer because of gathering unexpectedly but as using existing those acid-dyeable the 3rd monomers of reporting.And the 3rd monomer that the acrylic resin B of the selected acid-dyeable of the present invention adopts has higher reactivity ratio in above-described copolymerization system, this has just guaranteed that the 3rd monomer can be brought up to enough content in resin under general polymerizing condition, thereby finally makes the acrylic fiber that has comprised A, B two kinds of copolymers in the spinning material that ACID DYES is had desirable dyeing saturation value equally.
It is that the process for suspension polymerization of medium is made that A and B preferably adopt water, and the resin that obtains like this is pulverous, and this will help, and both are mixed fully when the preparation spinning solution.
In the present invention, the last handling process of as-spun fibre is not distinct with existing conventional organic solvent dry-spinning technology, generally includes washing, drawing-off, oils, curls and oven dry etc.
As-spun fibre after the shaping is washed earlier, carries out preliminary draft simultaneously, and washing temperature is 40～90 ℃, and tow heats drawing-off then, and total drafting multiple is generally 1.2～8.5.
Tow after the drawing-off enters oil groove and oils, to eliminate fiber electrostatic.Tow is cooled off after oiling, and the processing of curling is then curled and can be adopted hot water heating or Steam Heating, 100～130 ℃ of heating-up temperatures.Requirement according to back processing is cut to different length again, is the acrylic staple fibre product after the fiber drying of cut-out.
Compared with prior art, the invention has the advantages that the acrylic fiber that makes all has desirable dye-uptake to cation dyes and ACID DYES, dyeing saturation value is all very high, and fibrous physical property index and conventional acrylic fibers do not have any difference.This gives in the production of product sales management, the weaving processing of road, back and dyeing and finishing process of acrylic fiber and has brought very big convenience in the management.
Below will the invention will be further described by specific embodiment.With respect to prior art, the present invention is that mainly the 3rd monomer changes to some extent in the spinning material polyacrylonitrile resin, because the amount of the 3rd monomer is less at the polyacrylonitrile resin proportion, obviously such variation can't bring tangible influence to its spinning properties.So the spinning of technical solution of the present invention and last handling process are identical with general organic solvent dry-spinning technology, are also known by those of ordinary skill in the art, so in an embodiment the process conditions of spinning and post processing are exceeded for example.
In addition, also same as the prior art as the A in the spinning material polyacrylonitrile resin, included by technical solution of the present invention, but the monomer ratio of the A that does not enumerate among the embodiment can be predicted its effect for those of ordinary skill in the art.Because dyeing and finishing add man-hour CATION or acid two kinds of dyestuffs can not use simultaneously, A is known to the dyeability of cation dyes, so embodiment does not too much enumerate the monomer ratio of A yet.
The specific embodiment
In an embodiment:
Fiber cationic dye dye-uptake (dye-uptake I) assay method:
Adopt cation dyes (peacock green, maximum absorption wavelength are 618nm), bath raio is 1: 100, PH=4～5 (regulating with acetic acid and sodium acetate).Dyeing is that initial temperature is 70 ℃, and programming rate is 1 ℃/min, to 100 ℃ of constant temperature 1 hour, and cool to room temperature then, washing.Measure the dyeing absorbance and the absorbance of raffinate afterwards that dyes of stoste before respectively with spectrophotometer, and obtain dye-uptake according to the dye-uptake formula.
Fiber ACID DYES dye-uptake (dye-uptake II) assay method:
Adopt that ACID DYES vapour crust Tectlion is red, maximum absorption wavelength is that 510nm, bath raio are 1: 100, PH=2～4 (acetic acid adjusting).30 ℃ of dyeing initial temperatures, 1.0 ℃/min of programming rate to 100 ℃ of constant temperature dyeings 1 hour, naturally cools to room temperature then, washing.Measure the dyeing absorbance and the absorbance of raffinate afterwards that dyes of stoste before respectively with spectrophotometer, and obtain dye-uptake according to the dye-uptake formula.
The dye-uptake formula:
Dye-uptake=[(A1-A2)/A1] * 100
A1: the absorbance of dye liquor before the dyeing
A2: the absorbance of raffinate after the dyeing
[embodiment 1～3]
Polyacrylonitrile copolymer A, B are dissolved in the dimethyl formamide in required ratio, make the spinning solution that total solid content is 30wt%.Spinning solution filters the back by spinneret component spray silk, and spinning temperature is 110 ℃, and the shower nozzle degree of draft is controlled to be 35%.The silk of ejection enters spinning shaft with the heating of 350～420 ℃ high temperature nitrogen, and the solidification forming in the nitrogen of heat of the solvent evaporates in thread is an as-spun fibre.The as-spun fibre tow is washed and the preliminary draft machine, and washing temperature is 80 ℃.Tow heats drawing-off with hot bath subsequently, and the total draft multiple is 6 times.Tow oils then, and through the tow chilled air cools that oils, temperature drops to about 70 ℃.Enter crimping machine after tow heats by the decatize case and curl, decatize oven temperature, degree is 120 ℃, and curling temperature is 82 ℃.Being cut to staple fibre after the tow cooling then, is the cotton acrylic fiber that 130 ℃ hot air dries makes 1.00dtex with temperature again.
First monomer of A, B is an acrylonitrile in the spinning material polyacrylonitrile resin, and second, third monomer and the content in copolymer molecule thereof see Table 1 (copolymer A) and table 2 (copolymer B), and the viscosity average molecular weigh of A and B all is 6.2 ten thousand, and the weight ratio of A and B sees Table 3.
The dyeability index of fiber sees Table 3, and the physical index of fiber sees Table 4.
[embodiment 4～6]
Polyacrylonitrile copolymer A, B are dissolved in the dimethyl formamide in required ratio, make the spinning solution that total solid content is 32wt%.Spinning solution filters the back by spinneret component spray silk, and spinning temperature is 110 ℃, and the shower nozzle degree of draft is controlled to be 40%.The silk of ejection enters spinning shaft with the heating of 350～420 ℃ high temperature nitrogen, and the solidification forming in the nitrogen of heat of the solvent evaporates in thread is an as-spun fibre.The as-spun fibre tow is washed and the preliminary draft machine, and washing temperature is 80 ℃.Tow heats drawing-off with hot bath subsequently, and the total draft multiple is 5.6 times.Tow oils then, and through the tow chilled air cools that oils, temperature drops to about 70 ℃.Enter crimping machine after tow heats by the decatize case and curl, decatize oven temperature, degree is 120 ℃, and curling temperature is 82 ℃.Being cut to staple fibre after the tow cooling then, is the cotton acrylic fiber that 130 ℃ hot air dries makes 1.67dtex with temperature again.
First monomer of A, B is an acrylonitrile in the spinning material polyacrylonitrile resin, and second, third monomer and the content in copolymer molecule thereof see Table 1 (copolymer A) and table 2 (copolymer B), and the viscosity average molecular weigh of A and B all is 6.2 ten thousand, and the weight ratio of A and B sees Table 3.
The dyeability index of fiber sees Table 3, and the physical index of fiber sees Table 4.
[embodiment 7～9]
Polyacrylonitrile copolymer A, B are dissolved in the dimethyl formamide in required ratio, make the spinning solution that total solid content is 31wt%.Spinning solution filters the back by spinneret component spray silk, and spinning temperature is 110 ℃, and the shower nozzle degree of draft is controlled to be 37%.The silk of ejection enters spinning shaft with the heating of 350～420 ℃ high temperature nitrogen, and the solidification forming in the nitrogen of heat of the solvent evaporates in thread is an as-spun fibre.The as-spun fibre tow is washed and the preliminary draft machine, and washing temperature is 80 ℃.Tow heats drawing-off with hot bath subsequently, and the total draft multiple is 4.2 times.Tow oils then, and through the tow chilled air cools that oils, temperature drops to about 70 ℃.Enter crimping machine after tow heats by the decatize case and curl, decatize oven temperature, degree is 122 ℃, and curling temperature is 85 ℃.Being cut to staple fibre after the tow cooling then, is the wool type acrylic fiber that 132 ℃ hot air dries makes 6.67dtex with temperature again.
First monomer of A, B is an acrylonitrile in the spinning material polyacrylonitrile resin, and second, third monomer and the content in copolymer molecule thereof see Table 1 (copolymer A) and table 2 (copolymer B), and the viscosity average molecular weigh of A and B all is 6.2 ten thousand, and the weight ratio of A and B sees Table 3.
The dyeability index of fiber sees Table 3, and the physical index of fiber sees Table 4.
Table 1
| Second monomer | Second content of monomer (wt%) | The 3rd monomer | The 3rd content of monomer (wt%) | |
| Embodiment 1 | Vinylacetate | 12 | Sodium styrene sulfonate | 0.82 |
| Embodiment 2 | Vinylacetate | 12 | Sodium styrene sulfonate | 1.25 |
| Embodiment 3 | Vinylacetate | 16.5 | Sodium styrene sulfonate | 1.36 |
| Embodiment 4 | Methyl acrylate | 8.4 | Sodium styrene sulfonate | 1.47 |
| Embodiment 5 | Methyl acrylate | 8.4 | Sodium styrene sulfonate | 5.0 |
| Embodiment 6 | Methyl acrylate | 8.4 | Sodium styrene sulfonate | 2.64 |
| Embodiment 7 | Methyl acrylate | 5.5 | Sodium styrene sulfonate | 0.84 |
| Embodiment 8 | Methyl acrylate | 5.5 | Sodium styrene sulfonate | 2.25 |
| Embodiment 9 | Methyl acrylate | 8 | Sodium styrene sulfonate | 4.96 |
Table 2
| Second monomer | Second content of monomer (wt%) | The 3rd monomer | The 3rd content of monomer (wt%) | |
| Embodiment 1 | Vinylacetate | 11.8 | Methacrylic acid N, silomate base ethyl ester sulfate | 3.4 |
| Embodiment 2 | Vinylacetate | 16.5 | Methacrylic acid N, silomate base ethyl ester sulfate | 4.5 |
| Embodiment 3 | Vinylacetate | 11.8 | Methacrylic acid N, silomate base ethyl ester sulfate | 8.8 |
| Embodiment 4 | Methyl acrylate | 8.5 | Methacrylic acid N, silomate base carbethoxy hydrochloride | 5.3 |
| Embodiment 5 | Methyl acrylate | 5.5 | Methacrylic acid N, silomate base carbethoxy hydrochloride | 10.0 |
| Embodiment 6 | Methyl acrylate | 8.5 | Methacrylic acid N, silomate base carbethoxy hydrochloride | 11.6 |
| Embodiment 7 | Vinylacetate | 16.5 | Methacrylic acid N, silomate base ethyl ester nitrate | 6.0 |
| Embodiment 8 | Vinylacetate | 11.5 | Methacrylic acid N, silomate base ethyl ester nitrate | 10.0 |
| Embodiment 9 | Vinylacetate | 11.5 | Methacrylic acid N, silomate base ethyl ester nitrate | 12.5 |
Table 3.
| A/B (weight ratio) | Dye-uptake I (%) | Dye-uptake II (%) | |
| Embodiment 1 | 1/0.65 | 88.5 | 85.1 |
| Embodiment 2 | 1/0.83 | 89.6 | 87.6 |
| Embodiment 3 | 1/1.09 | 89.0 | 89.7 |
| Embodiment 4 | 1/0.85 | 90.3 | 91.3 |
| Embodiment 5 | 1/1.06 | 96.9 | 95.4 |
| Embodiment 6 | 1/1.38 | 92.2 | 97.6 |
| Embodiment 7 | 1/0.72 | 88.4 | 91.8 |
| Embodiment 8 | 1/1.01 | 92.6 | 94.7 |
| Embodiment 9 | 1/1.60 | 95.7 | 98.5 |
Table 4.
| Fracture strength (CN/dtex) | Extension at break (%) | Fault (mg/100g) | Crimpness (individual/10cm) | |
| Embodiment 1 | 2.8 | 44 | 12 | 40 |
| Embodiment 2 | 2.8 | 45 | 15 | 39 |
| Embodiment 3 | 2.9 | 38 | 10 | 42 |
| Embodiment 4 | 2.8 | 43 | 10 | 41 |
| Embodiment 5 | 2.6 | 45 | 8 | 41 |
| Embodiment 6 | 2.8 | 43 | 9 | 43 |
| Embodiment 7 | 2.1 | 41 | 13 | 30 |
| Embodiment 8 | 2.0 | 46 | 15 | 33 |
| Embodiment 9 | 2.2 | 43 | 11 | 32 |
Claims (8)
1, the manufacture method of a kind of CATION, the ACID DYES acrylic fibers that all can dye, this method comprises process:
1) polyacrylonitrile resin A and B are dissolved in solvent and make spinning solution, A or B are terpolymer, viscosity average molecular weigh is 4～70,000, both first monomers are acrylonitrile, second monomer is methyl acrylate or vinylacetate, wherein the 3rd monomer of A is a Sodium styrene sulfonate, the 3rd monomer of B is methacrylic acid N, silomate base ethyl ester nitrate, methacrylic acid N, silomate base carbethoxy hydrochloride or methacrylic acid N, a kind of in the silomate base ethyl ester sulfate, total amount in three kinds of comonomers, second content of monomer of A or B is 5.5～16.5wt%, the 3rd content of monomer of A is 0.8～5.0wt%, the 3rd content of monomer of B is 3.3～12.5wt%, the weight ratio of A and B is A: B=1 in the spinning solution: (0.6～1.6), total solid content is 25～40%, solvent is a dimethyl formamide, dimethyl, a kind of in acetamide or the dimethyl sulfoxide (DMSO);
2) spinning solution spray silk, spinning temperature is 70～130 ℃, and the shower nozzle degree of draft is 35～50%, and tow is an as-spun fibre through 300～500 ℃ high temperature inert gas heating back solvent evaporates solidification forming;
3) as-spun fibre is made the acrylic fiber product through last handling process.
2, the manufacture method of acrylic fibers according to claim 1, the 3rd monomer that it is characterized in that described B are methacrylic acid N, silomate base ethyl ester nitrate or methacrylic acid N, silomate base carbethoxy hydrochloride.
3, the manufacture method of acrylic fibers according to claim 1, the 3rd content of monomer that it is characterized in that described B is 6.0～10.0wt%.
4, the manufacture method of acrylic fibers according to claim 1 is characterized in that total solid content is 30～32wt% in the described spinning solution.
5, the manufacture method of acrylic fibers according to claim 1 is characterized in that described solvent is a dimethyl formamide.
6, the manufacture method of acrylic fibers according to claim 1 is characterized in that described A and the B powdery polymer for obtaining by aqueous polymerization.
7, the manufacture method of acrylic fibers according to claim 1 is characterized in that described inert gas is a nitrogen.
8, the manufacture method of acrylic fibers according to claim 1, it is characterized in that described as-spun fibre the last handling process of process comprise washing, drawing-off, oil, curl and oven dry.
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| CN102121173A (en) * | 2011-02-22 | 2011-07-13 | 天津工业大学 | Method for preparing sound-absorbing and heat-insulating materials formed by superfine fiber nonwovens |
| CN102352537A (en) * | 2011-08-16 | 2012-02-15 | 黑龙江大学 | Coagulation-bath-free spinning method of polyacrylonitrile-based carbon fiber protofilament |
| CN105273125A (en) * | 2014-06-06 | 2016-01-27 | 中国石油化工股份有限公司 | Polyacrylonitrile dry powder suitable for dry acrylic fiber spinning, and preparation method thereof |
| CN111041631A (en) * | 2019-12-25 | 2020-04-21 | 山东恒泰纺织有限公司 | Acid-base cotton-sandwiched cashmere-like acrylic yarn and spinning process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS5436701B2 (en) * | 1972-10-03 | 1979-11-10 | ||
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| CN102071542A (en) * | 2011-02-22 | 2011-05-25 | 天津工业大学 | Method for preparing polymeric nano-micro fiber non-woven fabric |
| CN102121173A (en) * | 2011-02-22 | 2011-07-13 | 天津工业大学 | Method for preparing sound-absorbing and heat-insulating materials formed by superfine fiber nonwovens |
| CN102121173B (en) * | 2011-02-22 | 2012-05-30 | 天津工业大学 | Method for preparing sound-absorbing and heat-insulating materials formed by superfine fiber nonwovens |
| CN102071542B (en) * | 2011-02-22 | 2012-08-29 | 天津工业大学 | Method for preparing polymeric nano-micro fiber non-woven fabric |
| CN102352537A (en) * | 2011-08-16 | 2012-02-15 | 黑龙江大学 | Coagulation-bath-free spinning method of polyacrylonitrile-based carbon fiber protofilament |
| CN102352537B (en) * | 2011-08-16 | 2013-08-07 | 黑龙江大学 | Coagulation-bath-free spinning method of polyacrylonitrile-based carbon fiber protofilament |
| CN105273125A (en) * | 2014-06-06 | 2016-01-27 | 中国石油化工股份有限公司 | Polyacrylonitrile dry powder suitable for dry acrylic fiber spinning, and preparation method thereof |
| CN111041631A (en) * | 2019-12-25 | 2020-04-21 | 山东恒泰纺织有限公司 | Acid-base cotton-sandwiched cashmere-like acrylic yarn and spinning process thereof |
| CN115522384A (en) * | 2022-09-20 | 2022-12-27 | 阜南华翔羊毛衫有限公司 | Rapid vintage treatment method for artificial woolen sweater |
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