CN112962160A - Solvent method for preparing vinylon - Google Patents
Solvent method for preparing vinylon Download PDFInfo
- Publication number
- CN112962160A CN112962160A CN202110326034.XA CN202110326034A CN112962160A CN 112962160 A CN112962160 A CN 112962160A CN 202110326034 A CN202110326034 A CN 202110326034A CN 112962160 A CN112962160 A CN 112962160A
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- CN
- China
- Prior art keywords
- solvent
- polyvinyl acetal
- vinylon
- electron beam
- filaments
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- 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.)
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Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/14—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of unsaturated alcohols, e.g. polyvinyl alcohol, or of their acetals or ketals
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
- D01F11/06—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/34—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds comprising unsaturated alcohols, acetals or ketals as the major constituent
Abstract
The invention discloses a method for preparing vinylon by a solvent method, which comprises the following steps: a. dissolving polyvinyl acetal in a solvent to obtain a liquid polyvinyl acetal solution; b. carrying out a spinning process on the polyvinyl acetal solution, and crosslinking and shaping filaments obtained by spinning under the irradiation of electron beams; c. spraying an anti-sticking agent on the surface of the fibril obtained after the electron beam irradiation; d. the filaments are subjected to post-treatment such as drawing and heat treatment to form vinylon fibers. Through the mode, the polyvinyl acetal is dissolved into liquid and then is sprayed, electron beam irradiation is adopted for crosslinking and shaping, the anti-sticking agent is sprayed, salt bath solidification is not needed, an acetal crosslinking procedure is not needed, and procedures such as stretching, heat treatment and the like are directly carried out.
Description
Technical Field
The invention relates to the technical field of fiber manufacturing, in particular to a method for preparing vinylon by a solvent method.
Background
Vinylon is a trade name of polyvinyl acetal fiber, also called vinylon, has properties close to cotton, is called as synthetic cotton, is a variety with the highest hygroscopicity in the existing synthetic fibers, and is widely concerned both in industry and outside because of excellent properties such as high strength, good hygroscopicity and the like in various fibers, and the vinylon fiber is a synthetic fiber prepared by wet spinning of an aqueous solution of polyvinyl alcohol (PVA) and then condensation of aldehyde.
Chinese patent CN101392412A discloses high strength vinylon and its preparation method, chinese patent CN103388190A discloses antibacterial degradable vinylon and its preparation method, chinese patent CN106884212A discloses preparation method of flame retardant vinylon fiber, chinese patent CN1804156A discloses preparation method of vinylon fiber filament bundle, chinese patent CN10153856A discloses preparation method of vinylon grafted soluble starch or polyhydroxy oligomer such as beta-cyclodextrin, chinese patent CN102797072A discloses preparation method of vinylon fiber by polyvinyl alcohol grafted soybean protein fiber, US patents U4612157, US4698194, US5110678, US4440711, US4851168 and the like disclose preparation method of vinylon, the preparation method of the above-mentioned most vinylon uses polyvinyl alcohol PVA as raw material to spray, then carries out coagulation forming in salt bath, then carries out processes of secondary acetal stretching, heat treatment, cross-linking treatment and the like, salt bath refers to saturated salt solution of sodium sulfate or sodium chloride, after the fiber is subjected to salt bath, a large amount of salt on the surface of the fiber needs to be cleaned, inorganic salts of sodium sulfate and sodium chloride are pollutants which are difficult to remove in sewage treatment, the inorganic salts cannot be removed by a filter screen, cannot be removed by an anaerobic and aerobic microbial method, and cannot be removed by precipitation, although the inorganic salts can be removed by methods such as a molecular sieve, ion resin exchange, triple-effect evaporation and the like, the removal cost is too high, and the investment cost and the operation production cost are greatly increased.
In addition, polyvinyl alcohol with 99% alcoholysis degree is usually dissolved in water (above 75 ℃), so continuous high-temperature heating is needed when the polyvinyl alcohol is used as a raw material, polyvinyl acetal PVB is insoluble in water but soluble in solvents such as formic acid, acetic acid and phenols, the relative density is 1.22-1.23, and the polyvinyl alcohol PVB has the advantages of high transparency, heat resistance, wear resistance, flexibility, good dielectricity and the like.
Based on the defects and shortcomings, the prior art needs to be improved, and a solvent method for preparing vinylon is designed.
Disclosure of Invention
The invention mainly solves the technical problem of providing a solvent method for preparing vinylon, which comprises the steps of dissolving polyvinyl acetal into liquid state, spraying yarns, irradiating, crosslinking and shaping by adopting electron beams, spraying an anti-sticking agent, not carrying out salt bath solidification, not carrying out an acetal crosslinking process, and directly carrying out processes such as stretching, heat treatment and the like.
In order to solve the technical problems, the invention adopts a technical scheme that: the method for preparing the vinylon by the solvent method comprises the following steps:
a. dissolving polyvinyl acetal in a solvent to obtain a liquid polyvinyl acetal solution;
b. carrying out a spinning process on the polyvinyl acetal solution, and crosslinking and shaping filaments obtained by spinning under the irradiation of electron beams;
c. and spraying an anti-sticking agent on the surface of the fibril obtained after the electron beam irradiation.
d. The filaments are subjected to post-treatment such as drawing and heat treatment to form vinylon fibers.
Preferably, the viscosity of the polyvinyl acetal in step a is controlled to be below 60mpa.s, preferably below 40 mpa.s.
Preferably, the solvent in step a includes, but is not limited to, methanol, ethanol, propanol, n-pentanol, benzyl alcohol, butanol, diacetone alcohol, propylene glycol ethyl ether/methyl ether/propyl ether, acetone, methyl ethyl ketone, cyclohexanone, dichloromethane, chloroform, acetates, acetic acid, etc., and the solvent is preferably ethanol or acetates.
Preferably, the solid concentration of the polyvinyl acetal solution in step a is controlled to 20% or less.
Preferably, in the spinning process in the step b, the polyvinyl acetal solution is vertically sprayed from top to bottom through a spray head, and the electron beam rays pass through the filaments sprayed from the spray head in the horizontal direction, so that the filaments are cross-linked and shaped.
Preferably, the dose of the electron beam irradiation in the step b is 1.0kGy to 120 kGy.
Preferably, the step c of spraying the anti-sticking agent on the surface of the fiber is to spray the anti-sticking agent into a mist form through a nozzle arranged at the lower end of the electron beam, so that the anti-sticking agent is uniformly sprayed on the surface of the fiber, and the adhesion of fibrils is prevented.
Preferably, the anti-sticking agent in step c is one or more selected from glycerol, ethylene glycol, propylene glycol, polyglycerol, sorbitol, butylene glycol, tween, span, sorbitol stearate, stearic acid, liquid wax and silicone oil.
Preferably, a solvent recovery system device is set in the processes of electron beam irradiation, stretching, heat treatment and the like in the step c, and the solvent condensation process is recycled.
Compared with the prior art, the invention has the beneficial effects that:
(1) the polyvinyl acetal solution is dissolved without a heating process, so that the consumption of heat energy is reduced;
(2) polyvinyl acetal is directly used as a raw material, so that the subsequent process of carrying out acetal crosslinking on the fiber is reduced;
(3) the electron beam irradiation crosslinking polyvinyl acetal solution is selected, so that the polyvinyl acetal solution is directly subjected to irradiation crosslinking and shaping by spinning, the breaking strength of vinylon is increased, the glass transition temperature of the vinylon is increased, and the subsequent acetal procedure is reduced.
(4) The electron beam irradiation crosslinking is adopted, so that the process of solidifying the fiber by using salt bath can be omitted, and the environmental pollution of salt chemicals is reduced.
Detailed Description
The following detailed description of the preferred embodiments of the invention is provided to enable those skilled in the art to more readily understand the advantages and features of the invention, and to clearly and unequivocally define the scope of the invention.
The embodiment of the invention comprises the following steps:
a solvent method for preparing vinylon comprises the following steps:
a. dissolving polyvinyl acetal in a solvent to obtain a liquid polyvinyl acetal solution;
b. carrying out a spinning process on the polyvinyl acetal solution, and crosslinking and shaping filaments obtained by spinning under the irradiation of electron beams;
c. spraying an anti-sticking agent on the surface of the fibril obtained after the electron beam irradiation;
d. the filaments are subjected to post-treatment such as drawing and heat treatment to form vinylon fibers.
The viscosity of the polyvinyl acetal in the step a is controlled below 60mPa.s, and the product with the viscosity below 40mPa.s is preferred.
The solvent in step a includes, but is not limited to, methanol, ethanol, propanol, n-pentanol, benzyl alcohol, butanol, diacetone alcohol, propylene glycol ethyl ether/methyl ether/propyl ether, acetone, methyl ethyl ketone, cyclohexanone, dichloromethane, chloroform, acetates, acetic acid, etc., and the solvent is preferably ethanol or acetates.
The solid concentration of the polyvinyl acetal solution in the step a is controlled to be below 20%.
And in the spinning process in the step b, the polyvinyl acetal solution is vertically sprayed out from top to bottom through a spray head, and the electron beam rays pass through the filaments sprayed out from the spray head in the horizontal direction, so that the filaments are cross-linked and shaped.
The irradiation dose of the electron beam in the step b is 1.0 kGy-120 kGy.
And c, spraying the anti-sticking agent on the surface of the fiber in the step c, namely spraying the anti-sticking agent into a mist shape by a nozzle arranged at the lower end of the electron beam ray, so that the anti-sticking agent is uniformly sprayed on the surface of the fiber, and the fibril is prevented from being stuck.
In the step c, the anti-sticking agent is one or more of glycerol, ethylene glycol, propylene glycol, polyglycerol, sorbitol, butanediol, tween, span, sorbitol stearate, stearic acid, liquid wax and silicone oil.
And c, setting a solvent recovery system device in the procedures of electron beam irradiation, stretching, heat treatment and the like in the step c, and recycling the solvent condensation process.
Example 1
A solvent method for preparing vinylon comprises the following steps:
a. dissolving polyvinyl acetal into ethanol to obtain 15% polyvinyl acetal solution for later use;
b. spraying the polyvinyl acetal solution in the step a into filaments through a spray head, and irradiating the filaments by electron beams with the dosage of 18kGy to crosslink and shape the filaments;
c. after electron beam irradiation, spraying glycerin on the surface of the fibril for anti-sticking treatment;
d. the filaments are processed into vinylon fibers by post-processing such as drawing, heat treatment and the like.
Example 2
A solvent method for preparing vinylon comprises the following steps:
a. dissolving polyvinyl acetal into ethyl acetate to obtain 18% polyvinyl acetal solution for later use;
b. spraying the polyvinyl acetal solution in the step a into filaments through a spray head, and irradiating the filaments by electron beams with the dose of 25kGy to crosslink and shape the filaments;
c. after electron beam irradiation, spraying glycerin on the surface of the fibril for anti-sticking treatment;
d. the fibril is processed into vinylon fiber after drawing, heat treatment and the like.
The invention relates to a solvent method for preparing vinylon, which comprises the steps of dissolving polyvinyl acetal into liquid state, spinning, irradiating, crosslinking and shaping by adopting electron beams, spraying an anti-sticking agent, directly performing procedures such as stretching, heat treatment and the like without performing salt bath solidification and acetal crosslinking.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (9)
1. A method for preparing vinylon by a solvent method is characterized by comprising the following steps: the method for preparing vinylon by the solvent method comprises the following steps:
a. dissolving polyvinyl acetal in a solvent to obtain a liquid polyvinyl acetal solution;
b. carrying out a spinning process on the polyvinyl acetal solution, and crosslinking and shaping filaments obtained by spinning under the irradiation of electron beams;
c. spraying an anti-sticking agent on the surface of the fibril obtained after the electron beam irradiation;
d. the filaments are subjected to post-treatment such as drawing and heat treatment to form vinylon fibers.
2. The solvent process of claim 1, wherein: the viscosity of the polyvinyl acetal in the step a is controlled below 60mPa.s, and the product with the viscosity below 40mPa.s is preferred.
3. The solvent process of claim 1, wherein: the solvent in step a includes, but is not limited to, methanol, ethanol, propanol, n-pentanol, benzyl alcohol, butanol, diacetone alcohol, propylene glycol ethyl ether/methyl ether/propyl ether, acetone, methyl ethyl ketone, cyclohexanone, dichloromethane, chloroform, acetates, acetic acid, etc., and the solvent is preferably ethanol or acetates.
4. The solvent process of claim 1, wherein: the solid concentration of the polyvinyl acetal solution in the step a is controlled to be below 20%.
5. The solvent process of claim 1, wherein: and in the spinning process in the step b, the polyvinyl acetal solution is vertically sprayed out from top to bottom through a spray head, and the electron beam rays pass through the filaments sprayed out from the spray head in the horizontal direction, so that the filaments are cross-linked and shaped.
6. The solvent process of claim 1, wherein: the irradiation dose of the electron beam in the step b is 1.0 kGy-120 kGy.
7. The solvent process of claim 1, wherein: and c, spraying the anti-sticking agent on the surface of the fiber in the step c, namely spraying the anti-sticking agent into a mist shape by a nozzle arranged at the lower end of the electron beam ray, so that the anti-sticking agent is uniformly sprayed on the surface of the fiber, and the fibril is prevented from being stuck.
8. The solvent process of claim 1, wherein: in the step c, the anti-sticking agent is one or more of glycerol, ethylene glycol, propylene glycol, polyglycerol, sorbitol, butanediol, tween, span, sorbitol stearate, stearic acid, liquid wax and silicone oil.
9. The solvent process of claim 1, wherein: and c, setting a solvent recovery system device in the procedures of electron beam irradiation, stretching, heat treatment and the like in the step c, and recycling the solvent condensation process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110326034.XA CN112962160A (en) | 2021-03-26 | 2021-03-26 | Solvent method for preparing vinylon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110326034.XA CN112962160A (en) | 2021-03-26 | 2021-03-26 | Solvent method for preparing vinylon |
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| CN112962160A true CN112962160A (en) | 2021-06-15 |
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| CN202110326034.XA Pending CN112962160A (en) | 2021-03-26 | 2021-03-26 | Solvent method for preparing vinylon |
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