CN105220256A - Be applicable to spinning solution and the preparation method of dry acrylic spinning - Google Patents
Be applicable to spinning solution and the preparation method of dry acrylic spinning Download PDFInfo
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- CN105220256A CN105220256A CN201410250071.7A CN201410250071A CN105220256A CN 105220256 A CN105220256 A CN 105220256A CN 201410250071 A CN201410250071 A CN 201410250071A CN 105220256 A CN105220256 A CN 105220256A
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Abstract
The present invention relates to a kind of stoste being suitable for polyacrylonitrile spinning, in particular to a kind of spinning solution being applicable to dry acrylic spinning, be made up of polyacrylonitrile dry powder and solvent, wherein polyacrylonitrile dry powder is that comonomer is made through polymerisation by acrylonitrile, methyl acrylate, Sodium styrene sulfonate and 2-acrylamide-2-methylpro panesulfonic acid.The present invention is by selecting suitable comonomer and parts by weight thereof, obtain the polyacrylonitrile dry powder that a kind of porosity, molecular weight and molecular weight distribution are suitable, again by selecting suitable solvent and content, control mixing temperature and solution temperature, by the spinning solution that the polypropylene dry composition obtained becomes rotary viscosity within the scope of 45000 ~ 65000mpa.s, the spinning solution viscoplasticity prepared is moderate, moisture is few, this spinning solution is conducive to the even running of spinning, reduce spinning plate amount, increase and spin figure place.The present invention also provides its preparation method, rational technology.
Description
Technical field
The present invention relates to a kind of stoste and the preparation method that are suitable for polyacrylonitrile spinning, particularly a kind of spinning solution and preparation method being applicable to dry acrylic spinning.
Background technology
Polyacrylonitrile spinning technique is divided into dry method and wet spinning technology, dry spinning is that polyacrylonitrile is dissolved into spinning solution, desolvation is carried out by hot nitrogen after again spinning solution being transported to spinning shaft, dry spinning is compared with wet spinning, forming process relaxes, fibrous inner structure is even, make the physical and mechanical properties of dry-spinning fiber and dyeability better, spinning cross-sectional strength is good.Dry spinning speed is higher in addition, spinning head hole count is less, solvent recovery simple, and spinning line is simple, and floor space is little; Dry-spinning fiber distinctive dog bone-shaped structure makes its characteristic close to natural wool, makes that fabric elasticity is good, lightweight, manufactured goods have the features such as warming, comfortable, gloss is graceful; But dry spinning easily occurs as the following problem that document " dry acrylic fiber stock solution quality is on the impact of spinning properties " is mentioned in the preparation process of carrying out spinning solution: (1) spinning solution viscoplasticity is poor, when causing spinning solution tapping, flow velocity is fast, and adapter No way out swells phenomenon; (2) the moisture increased air bubble that can make when exceeding standard in spinning solution in spinning solution, causes the problem such as doubling, fracture of wire easily occurs when spinning and cannot spinning smoothly; (3) color and luster of spinning solution is poor etc., and problem causes product final mass to be affected.Because these problems can cause spinning not smooth, the quality of final products is impacted, also can cause the problems such as the production intensity increasing of workman during production simultaneously, and by controlling monomer ratio during adjustment polymerization, control the parameters such as the molecular weight of polymer, the preparing process of adjustment stoste can solve viscoplasticity difference and the moisture problem exceeded standard of stoste, produced problem when therefore this patent solves acrylic spinning mainly through these means.
Chinese patent 102747451A refer to the preparation being suitable for carbon fiber spinning primary fluid, excessive and the stoste of the dope viscosity existed in main technical solution easily produces the problem of gel, but the polymerization single polymerization monomer that this patent is selected only has two kinds of monomers, be respectively acrylonitrile and itaconic acid, adopt simultaneously for DMF do solvent one-step method polymerization.
Patent JPH02169711 discloses a kind of dry-spinning flat acrylic fiber and preparation method thereof, acrylonitrile content >=85% of resin, and solvent is dimethyl formamide, the mass concentration 32% ~ 40% of resin in mixture.Contrast patent JPS6426710 discloses the method for a kind of dry spinning production cross section modified acrylic fibres, and acrylonitrile content >=94% of resin, solvent is dimethyl formamide, the mass concentration 24% ~ 29% of resin in mixture.But the molecular weight of not mentioned polymer, moisture, the rotary viscosity and stoste preparing process etc. of spinning solution have the parameter of material impact to spinning.
In prior art during dry spinning because the problems such as spinning solution viscoplasticity is poor, bubble is many, shade deviation easily cause fluctuation and product quality to be affected.
Summary of the invention
For the deficiencies in the prior art, the object of this invention is to provide a kind of spinning solution being applicable to dry acrylic spinning, the spinning solution viscoplasticity prepared is moderate, moisture is few, and this spinning solution is conducive to the even running of spinning, reduce spinning plate amount, increase and spin figure place; The present invention also provides its preparation method, rational technology.
The spinning solution being applicable to dry acrylic spinning of the present invention, be made up of polyacrylonitrile dry powder and solvent, wherein polyacrylonitrile dry powder is that comonomer is made through polymerisation by acrylonitrile, methyl acrylate, Sodium styrene sulfonate and 2-acrylamide-2-methylpro panesulfonic acid.
Wherein: the mass ratio of comonomer is acrylonitrile: methyl acrylate: Sodium styrene sulfonate: 2-acrylamide-2-methylpro panesulfonic acid is 92:4-7:1-4:0.1-2.The present invention have employed four kinds of monomer polymerizations when polyacrylonitrile is polymerized, the 4th monomer selects 2-acrylamide-2-methylpro panesulfonic acid, can increase the flexibility of polymer segment, be beneficial to polymer dissolving in a solvent.
Solvent is the one in dimethyl formamide or dimethylacetylamide, preferred dimethyl formamide.
The quality of polyacrylonitrile dry powder accounts for 25% ~ 35% of the mixture of polyacrylonitrile dry powder and solvent, preferably 28 ~ 32wt%.
The preparation method being applicable to the spinning solution of dry acrylic spinning of the present invention, comprises the following steps:
(1) comonomer acrylonitrile, methyl acrylate, Sodium styrene sulfonate and 2-acrylamide-2-methylpro panesulfonic acid are added in polymeric kettle, then add initator, regulate pH to 2.5-3.5, carry out polymerisation;
(2) add EDTA cessation reaction after polymerisation, polymerisation gained material after filtration, washing, obtain polyacrylonitrile resin after drying, then through being ground into smalls, obtain polyacrylonitrile dry powder;
(3) polyacrylonitrile dry powder is mixed with solvent in mark's mixer, dissolve, in course of dissolution, pass into inert gas, obtain the spinning solution being applicable to dry acrylic spinning.
Wherein: the polymerisation in step (1) is aqueous suspension polymerization.The present invention have employed four kinds of monomer polymerizations when acrylonitrile polymerization, the 4th monomer selects 2-acrylamide-2-methylpro panesulfonic acid, can increase the flexibility of polymer segment.
In step (1), initator is potassium peroxydisulfate, sodium hydrogensulfite and iron ammonium sulfate.The ratio that potassium peroxydisulfate, sodium hydrogensulfite and iron ammonium sulfate account for monomer mass is respectively 0.2%, 0.01% and 0.01%.Add in system after three kinds of initator desalted waters dissolve.
PH to 2.5-3.5 is regulated to regulate pH to 2.5-3.5 with sulfur dioxide in step (1).
Polymeric reaction temperature 59.5-60.5 DEG C in step (1).
The quality adding EDTA in step (2) accounts for 0.1% of monomer mass.Step is ground into smalls in (2), to the particle diameter not requirement of smalls.
Dry in step (2) is 0.1%-0.3% for being dried to water content.
In step (2), the weight average molecular weight of polyacrylonitrile resin is 80,000-12 ten thousand, molecular weight distribution is 2.80-3.20, molecular weight preferably 90,000-11 ten thousand, the preferred 2.9-3.0 of molecular weight distribution, select this kind of polyacrylonitrile can make the moderate spinning solution of rotary viscosity, be beneficial to the stable operation of spinning.
In step (2), the porosity of=58.0% of polyacrylonitrile dry powder, is conducive to polyacrylonitrile dissolving in a solvent, is beneficial to the inside that solvent enters polyacrylonitrile dry powder fast, accelerates polymer dissolution, can prepare qualified spinning solution.
Polyacrylonitrile dry powder mixes in mark's mixer with solvent in (3) by step, and before mixing, the temperature of solvent is 70 ~ 95 DEG C, preferably 60 ~ 80 DEG C; The temperature maintaining mixture after mixing is 50 ~ 70 DEG C and dissolves, and dissolution time is 6 ~ 10h.Be selected in this temperature and time to dissolve, rate of dissolution is suitable, can not destroy the performance of polymer, less energy consumption.
The rotary viscosity of the spinning solution that the present invention prepares is 45000 ~ 65000mpa.s, preferably 50000 ~ 60000mpa.s.
In sum, the present invention has the following advantages:
(1) the polyacrylonitrile dry powder moisture content prepared of the present invention is low, molecular chain conformation is moderate, the interior porosity of the granularity of dry powder and particle is good, the spinning solution viscoplasticity prepared is better, bubble is few, bright, and spinning process smoothly and obtain good, the bibulous spinning of dyeability.
(2) the present invention is by selecting suitable comonomer and parts by weight thereof, obtain the polyacrylonitrile dry powder that a kind of porosity, molecular weight and molecular weight distribution are suitable, again by selecting suitable solvent and content, control mixing temperature and solution temperature, by the spinning solution that the polypropylene dry composition obtained becomes rotary viscosity within the scope of 45000 ~ 65000mpa.s, the spinning solution viscoplasticity prepared is moderate, moisture is few, this spinning solution is conducive to the even running of spinning, reduce spinning plate amount, increase and spin figure place.
(3) the present invention also provides its preparation method, rational technology.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
(1) acrylonitrile=92 by weight, methyl acrylate=6.7, Sodium styrene sulfonate=1.2, the ratio of 2-acrylamide-2-methylpro panesulfonic acid=0.1, comonomer acrylonitrile, methyl acrylate, Sodium styrene sulfonate and 2-acrylamide-2-methylpro panesulfonic acid are added in polymeric kettle, the initiator potassium persulfate of reaction aequum, sodium hydrogensulfite, iron ammonium sulfate and desalted water, sulfur dioxide are joined in polymeric kettle together simultaneously, control polymerization temperature 60 DEG C, the pH value 3.0 of polymerization reaction system, carries out aqueous deposited polymerization reaction;
(2) EDTA cessation reaction is added after polymerisation, polymerization gained material after filtration, wash, be dried to the dry polymer that water content is 0.3%, the weight average molecular weight of the polymer obtained is 8.5 ten thousand, molecular weight distribution is 2.95, porosity is 65%, then obtains polyacrylonitrile dry powder after being ground into smalls.
(3) by dimethyl formamide mixed at high speed in mark's mixer of above-mentioned polyacrylonitrile resin and 80 DEG C, the content of mixture is 25wt%, the temperature maintaining mixture after mixing is 60 DEG C and dissolves, dissolution time is 7h, the emptying deoxygenation of inert gas is passed in course of dissolution, the rotary viscosity having dissolved rear spinning solution is 45000mp.s, and the water content in spinning solution is 0.2%.
Embodiment 2
According to spinning solution prepared by the method for embodiment 1, difference is that the parts by weight of its each comonomer are: acrylonitrile=92, methyl acrylate=6.4, Sodium styrene sulfonate=1.2,2-acrylamide-2-methylpro panesulfonic acid=0.4.
Embodiment 3
According to spinning solution prepared by the method for embodiment 1, difference is that the parts by weight of its each comonomer are: acrylonitrile=92, methyl acrylate=4.0, Sodium styrene sulfonate=4.0,2-acrylamide-2-methylpro panesulfonic acid=2.0, in step (2), the weight average molecular weight of polymer is 80,000, and molecular weight distribution is 3.2.
Embodiment 4
According to spinning solution prepared by the method for embodiment 1, difference is that the parts by weight of its each comonomer are: acrylonitrile=92, methyl acrylate=6.5, Sodium styrene sulfonate=2.0,2-acrylamide-2-methylpro panesulfonic acid=0.5, in step (2), the porosity of polymer is 70%.
Embodiment 5
According to spinning solution prepared by the method for embodiment 1, difference is that the solvent that in step (3), dissolving polyacrylonitrile is selected is dimethylacetylamide.
Embodiment 6
According to spinning solution prepared by the method for embodiment 1, when difference is to mix with polyacrylonitrile in step (3), the temperature of dimethyl formamide is 95 DEG C.
Embodiment 7
According to spinning solution prepared by the method for embodiment 1, difference is that the content of mixture in step (3) is 32wt%.
Embodiment 8
According to spinning solution prepared by the method for embodiment 1, difference is that the temperature of maintenance mixture after mixing in step (3) is 55 DEG C and dissolves, and dissolution time is 8h.
Embodiment 9
According to spinning solution prepared by the method for embodiment 1, difference is that the parts by weight of its each comonomer are: acrylonitrile=92, methyl acrylate=5.0, Sodium styrene sulfonate=3.0,2-acrylamide-2-methylpro panesulfonic acid=1.0, the rotary viscosity having dissolved rear spinning solution in step (3) is 60000mpa.s.
Embodiment 10
According to spinning solution prepared by the method for embodiment 1, difference is to be dried to the dry polymer that water content is 0.25% in step (2), and in step (3), the water content dissolved in rear spinning solution is 0.15%.
Comparative example 1
Comonomer for the preparation of polyacrylonitrile resin is acrylonitrile, methyl acrylate and Sodium styrene sulfonate, the parts by weight of each comonomer are: acrylonitrile=92, methyl acrylate=7, Sodium styrene sulfonate=1, the weight average molecular weight of polymer is 70,000, porosity is 40%, dissolves when solution temperature is 50 DEG C, and after dissolving, the rotary viscosity of spinning solution is 35000mpa.s.
Comparative example 2
Comonomer for the preparation of polyacrylonitrile resin is acrylonitrile, methyl acrylate and Sodium styrene sulfonate, the parts by weight of each comonomer are: acrylonitrile=92, methyl acrylate=6.9, Sodium styrene sulfonate=1.1, the weight average molecular weight of polymer is 80,000 4, and porosity is 45%, dissolve when solution temperature is 80 DEG C, after dissolving, the rotary viscosity of spinning solution is 43000mpa.s, and do not control the moisture of spinning solution, moisture is 0.6%.
The performance test results of the product that embodiment 1-10 and comparative example 1-2 prepares is in table 1.
The spinning Comparative result of table 1 embodiment and comparative example
| Viscoplasticity | Bubble situation | Color and luster | With plate amount/block | |
| Embodiment 1 | Good | Seldom | Bright, yellowish | 15 |
| Embodiment 2 | Good | Seldom | Bright, yellowish | 12 |
| Embodiment 3 | Good | Seldom | Bright, yellowish | 14 |
| Embodiment 4 | Good | Seldom | Bright, yellowish | 12 |
| Embodiment 5 | Good | Seldom | Bright, yellowish | 20 |
| Embodiment 6 | Good | Seldom | Bright, yellowish | 18 |
| Embodiment 7 | Good | Seldom | Bright, yellowish | 21 |
| Embodiment 8 | Good | Seldom | Bright, yellowish | 22 |
| Embodiment 9 | Good | Seldom | Bright, yellowish | 14 |
| Embodiment 10 | Good | Seldom | Bright, yellowish | 17 |
| Comparative example 1 | Poor | Less | Unclarity | 40 |
| Comparative example 2 | Better | More | Unclarity | 45 |
Claims (10)
1. one kind is applicable to the spinning solution of dry acrylic spinning, it is characterized in that: be made up of polyacrylonitrile dry powder and solvent, wherein polyacrylonitrile dry powder is that comonomer is made through polymerisation by acrylonitrile, methyl acrylate, Sodium styrene sulfonate and 2-acrylamide-2-methylpro panesulfonic acid.
2. the spinning solution being applicable to dry acrylic spinning according to claim 1, is characterized in that: the mass ratio of comonomer is acrylonitrile: methyl acrylate: Sodium styrene sulfonate: 2-acrylamide-2-methylpro panesulfonic acid is 92:4-7:1-4:0.1-2.
3. the spinning solution being applicable to dry acrylic spinning according to claim 1, is characterized in that: solvent is the one in dimethyl formamide or dimethylacetylamide.
4. the spinning solution being applicable to dry acrylic spinning according to claim 1, is characterized in that: the quality of polyacrylonitrile dry powder accounts for 25% ~ 35% of the mixture of polyacrylonitrile dry powder and solvent.
5. the arbitrary described preparation method being applicable to the spinning solution of dry acrylic spinning of claim 1-4, is characterized in that: comprise the following steps:
(1) comonomer acrylonitrile, methyl acrylate, Sodium styrene sulfonate and 2-acrylamide-2-methylpro panesulfonic acid are added in polymeric kettle, then add initator, regulate pH to 2.5-3.5, carry out polymerisation;
(2) add EDTA cessation reaction after polymerisation, polymerisation gained material after filtration, washing, obtain polyacrylonitrile resin after drying, then through being ground into smalls, obtain polyacrylonitrile dry powder;
(3) polyacrylonitrile dry powder is mixed with solvent in mark's mixer, dissolve, in course of dissolution, pass into inert gas, obtain the spinning solution being applicable to dry acrylic spinning.
6. the preparation method being applicable to the spinning solution of dry acrylic spinning according to claim 5, is characterized in that: in step (1), initator is potassium peroxydisulfate, sodium hydrogensulfite and iron ammonium sulfate; PH to 2.5-3.5 is regulated to regulate pH to 2.5-3.5 with sulfur dioxide.
7. the preparation method being applicable to the spinning solution of dry acrylic spinning according to claim 5, is characterized in that: dry in step (2) is 0.1%-0.3% for being dried to water content.
8. the preparation method being applicable to the spinning solution of dry acrylic spinning according to claim 5, is characterized in that: in step (2), the weight average molecular weight of polyacrylonitrile resin is 80,000-12 ten thousand, and molecular weight distribution is 2.80-3.20.
9. the preparation method being applicable to the spinning solution of dry acrylic spinning according to claim 5, is characterized in that: the porosity of=58.0% of polyacrylonitrile dry powder in step (2).
10. the preparation method being applicable to the spinning solution of dry acrylic spinning according to claim 5, is characterized in that: polyacrylonitrile dry powder mixes in mark's mixer with solvent in (3) by step, and before mixing, the temperature of solvent is 70 ~ 95 DEG C; The temperature maintaining mixture after mixing is 50 ~ 70 DEG C and dissolves, and dissolution time is 6 ~ 10h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110724217A (en) * | 2018-07-16 | 2020-01-24 | 中国石油化工股份有限公司 | Process for preparing low molecular weight polyacrylonitrile homopolymer |
| CN113584607A (en) * | 2020-04-30 | 2021-11-02 | 中国石油化工股份有限公司 | Acrylic fiber spinning solution and preparation method and application thereof |
| CN113832564A (en) * | 2020-06-24 | 2021-12-24 | 中国石油化工股份有限公司 | Method for manufacturing environment-friendly dry acrylic fiber |
| CN114164503A (en) * | 2020-09-11 | 2022-03-11 | 中国石油化工股份有限公司 | Dry acrylic fiber spinning method and stock solution preparation method |
| CN116043349A (en) * | 2022-12-24 | 2023-05-02 | 烟台泰和兴材料科技股份有限公司 | Preparation method of polyacrylonitrile fiber and pulp for sealing and friction materials |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110724217A (en) * | 2018-07-16 | 2020-01-24 | 中国石油化工股份有限公司 | Process for preparing low molecular weight polyacrylonitrile homopolymer |
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| CN113584607A (en) * | 2020-04-30 | 2021-11-02 | 中国石油化工股份有限公司 | Acrylic fiber spinning solution and preparation method and application thereof |
| CN113832564A (en) * | 2020-06-24 | 2021-12-24 | 中国石油化工股份有限公司 | Method for manufacturing environment-friendly dry acrylic fiber |
| CN113832564B (en) * | 2020-06-24 | 2023-10-20 | 中国石油化工股份有限公司 | Method for manufacturing environment-friendly dry acrylic fiber |
| CN114164503A (en) * | 2020-09-11 | 2022-03-11 | 中国石油化工股份有限公司 | Dry acrylic fiber spinning method and stock solution preparation method |
| CN114164503B (en) * | 2020-09-11 | 2022-12-27 | 中国石油化工股份有限公司 | Dry acrylic fiber spinning method and stock solution preparation method |
| CN116043349A (en) * | 2022-12-24 | 2023-05-02 | 烟台泰和兴材料科技股份有限公司 | Preparation method of polyacrylonitrile fiber and pulp for sealing and friction materials |
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Application publication date: 20160106 |