CN113913957A - Processing method for online adding flame-retardant anti-dripping polyester fiber in melt direct spinning - Google Patents
Processing method for online adding flame-retardant anti-dripping polyester fiber in melt direct spinning Download PDFInfo
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- CN113913957A CN113913957A CN202111141980.3A CN202111141980A CN113913957A CN 113913957 A CN113913957 A CN 113913957A CN 202111141980 A CN202111141980 A CN 202111141980A CN 113913957 A CN113913957 A CN 113913957A
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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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
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention relates to the field of polyester fibers, in particular to a processing method for adding flame-retardant anti-dripping polyester fibers on line in melt direct spinning, which comprises the following steps: the method comprises the following steps: preparing a flame-retardant anti-dripping agent; step two: a first esterification reaction; step three: performing second esterification reaction; step four: performing polycondensation reaction; step five: the preparation of the flame-retardant anti-dripping polyester fiber is characterized in that the flame-retardant anti-dripping agent formed by mixing decabromodiphenylethane, a phosphorus flame retardant and zinc borate in a proper proportion is added into the polyester fiber, so that the flame retardant performance of the polyester fiber is effectively improved, the overall performance of the polyester fiber is greatly improved, the polyester fiber can be better applied to various fields, and in addition, the flame retardant formed by mixing decabromodiphenylethane, the phosphorus flame retardant and zinc borate is used as an environment-friendly and nontoxic novel flame retardant, so that the flame-retardant anti-dripping polyester fiber is good in thermal stability and good in compatibility with polyester.
Description
Technical Field
The invention relates to the field of polyester fibers, in particular to a processing method for adding flame-retardant anti-dripping polyester fibers on line in melt direct spinning.
Background
Polyester fibers have the characteristics of high strength, good elasticity, crease resistance, ironing resistance, corrosion resistance and the like, and are widely applied to the fields of clothing, articles for daily use, industrial articles and the like, but the polyester fibers have low limiting oxygen index, belong to flammable materials, have serious dripping phenomenon during combustion, can ignite surrounding articles to cause secondary combustion and harm to human bodies, bring potential safety hazards to people's life, life and property, greatly limit the application range of the polyester fibers, improve the flame retardance of the polyester fibers, and ensure the excellent characteristics of the polyester fibers to the greatest extent, so that the problem which needs to be solved is solved urgently.
Disclosure of Invention
The invention aims to provide a melt direct spinning on-line added flame-retardant anti-dripping polyester fiber and a processing method thereof, so as to solve the problems in the process.
In order to achieve the purpose, the invention provides the following technical scheme: a processing method for adding flame-retardant anti-dripping polyester fiber on line by melt direct spinning comprises the following steps,
a melt direct spinning on-line added flame-retardant anti-dripping polyester fiber and a processing method thereof comprise the following steps:
the method comprises the following steps: preparation of flame-retardant anti-dripping agent: adding decabromodiphenylethane, a phosphorus flame retardant and zinc borate into a certain amount of methanol solution according to a certain proportion, reacting for a period of time under a certain condition by using methanol metal salt as a catalyst, and filtering, cleaning and drying after the reaction is finished to obtain a flame-retardant anti-dripping agent;
step two: a first esterification reaction: pulping and mixing ethylene glycol and terephthalic acid, adding the flame-retardant anti-dropping agent obtained in the step one into a mixed solution of the ethylene glycol and the terephthalic acid according to a certain proportion, and then fully mixing the ethylene glycol and the terephthalic acid for esterification reaction;
step three: second esterification reaction: continuously supplementing ethylene glycol into the solution of the first esterification reaction obtained in the step two to perform a second esterification reaction;
step four: and (3) polycondensation reaction: adding the flame-retardant anti-dripping agent obtained in the step one into a product of the second esterification reaction according to a certain proportion for polycondensation reaction, and obtaining flame-retardant anti-dripping polyester through polycondensation reaction;
step five: preparing flame-retardant anti-dripping polyester fibers: and (2) uniformly and fully mixing the flame-retardant anti-dripping polyester obtained in the fourth step with the flame-retardant anti-dripping agent obtained in the first step, drying at high temperature, performing melt extrusion through a double-screw extruder, enabling the melt to enter a spinning box body, spraying out the melt through a spinneret orifice, entering a spinning channel, performing air cooling, bundling, oiling, drafting, thermoforming and winding to obtain the flame-retardant anti-dripping polyester fiber.
Preferably, the phosphorus-based flame retardant in the first step is one or more of [ (6-oxo-6H-dibenzo [ c, e ] [1,2] oxaphosphorin-6-yl) methyl ] succinic acid (DDP), 10- (2, 5-dihydroxyphenyl) -10-hydro-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), and bis (p-carboxyphenyl) phenylphosphine oxide (BCPPO).
Preferably, in the first step, the methanol solution contains 0.01-5% of decabromodiphenylethane by mass and 0.02-4% of zinc borate by mass.
Preferably, the pressure of the first esterification reaction in the second step is 0.03-0.6 MPa, and the reaction temperature is 210-240 ℃.
Preferably, the addition amount of the flame-retardant anti-dropping agent for the second esterification reaction in the third step is 0.1-10% of the mass content of the ethylene glycol, the pressure of the second esterification reaction is 0.2-0.6 Mpa, and the reaction temperature is 250-280 ℃.
Preferably, the polycondensation reaction in the fourth step is carried out at 280-290 ℃ under vacuum condition.
Preferably, the drying temperature of the preparation of the flame-retardant anti-dripping polyester fiber in the step five is between 100 ℃ and 180 ℃ and the water content of the preparation is lower than 100 ppm.
Compared with the prior art, the invention has the beneficial effects that: the flame-retardant anti-dripping agent formed by mixing the decabromodiphenylethane, the phosphorus flame retardant and the zinc borate in a proper proportion effectively improves the flame retardant property of the polyester fiber when being added into the polyester fiber, so that the overall performance of the polyester fiber is greatly improved, the polyester fiber can be better applied to various fields, and in addition, the flame retardant formed by mixing the decabromodiphenylethane, the phosphorus flame retardant and the zinc borate is used as a novel flame retardant which is environment-friendly and nontoxic, has good thermal stability and good compatibility with the polyester.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
A processing method for adding flame-retardant anti-dripping polyester fibers on line in melt direct spinning comprises the following steps:
preparation of flame-retardant anti-dripping agent:
adding decabromodiphenylethane, zinc borate and a phosphorus flame retardant into a certain amount of methanol solution according to a certain proportion, reacting for a period of time under a certain condition by using methanol metal salt as a catalyst, and filtering, cleaning and drying after the reaction is finished to obtain the flame-retardant anti-dripping agent.
Wherein: the phosphorus flame retardant is [ (6-oxo-6H-dibenzo [ c, e ] [1,2] oxaphosphorin-6-yl) methyl ] succinic acid (DDP); the mass ratio of the decabromodiphenylethane to the phosphorus flame retardant to the zinc borate is 1:3: 1; the content of decabromodiphenylethane in the methanol solution is 5 percent, and the content of zinc borate is 4 percent; the reaction condition is that the reaction temperature is 60 ℃, and the reaction time is 12 hours; the drying condition of (2) is drying at 90 ℃ for 10 h.
Esterification reaction:
carrying out first esterification reaction, pulping and mixing ethylene glycol and terephthalic acid according to the mol ratio of 1.05:1.01, adding a flame-retardant anti-dropping agent into the pulp according to a certain proportion, pulping to obtain mixed pulp, and then carrying out first esterification reaction on the mixed pulp, wherein the pressure of the first esterification reaction is 0.03MPa, and the reaction temperature is 210 ℃; and when the water yield of the first esterification reaction reaches 92% of the theoretical water yield, finishing the first esterification reaction.
Performing a second esterification reaction, namely performing the second esterification reaction on the material obtained by the first esterification reaction after supplementing ethylene glycol, wherein the reaction pressure is 0.2Mpa, and the reaction temperature is 250 ℃; and (3) terminating the second esterification reaction until the esterification water yield reaches more than 99% of the theoretical water yield, and finishing the second esterification reaction.
And (3) polycondensation reaction: adding the flame-retardant anti-dripping agent obtained in the step one to a product of a second esterification reaction according to a certain proportion for a polycondensation reaction, and preparing flame-retardant anti-dripping polyester through the polycondensation reaction, wherein the temperature of the polycondensation reaction is kept at 280 ℃; the polycondensation reaction lasted 2 h.
Preparing flame-retardant anti-dripping polyester fibers:
and (2) uniformly and fully mixing the flame-retardant anti-dripping polyester obtained in the fourth step with the flame-retardant anti-dripping agent obtained in the first step, drying at a high temperature, performing melt extrusion through a double-screw extruder, enabling the melt to enter a spinning box body, spraying out the melt through a spinneret hole, enabling the melt to enter a spinning channel, performing air cooling, bundling, oiling, drafting, heat setting and winding to obtain the flame-retardant anti-dripping polyester fiber, wherein the drying temperature is 100 ℃.
Example two
A processing method for adding flame-retardant anti-dripping polyester fibers on line in melt direct spinning comprises the following steps:
preparation of flame-retardant anti-dripping agent:
adding decabromodiphenylethane, zinc borate and a phosphorus flame retardant into a certain amount of methanol solution according to a certain proportion, reacting for a period of time under a certain condition by using methanol metal salt as a catalyst, and filtering, cleaning and drying after the reaction is finished to obtain the flame-retardant anti-dripping agent.
Wherein: the phosphorus flame retardant is 10- (2, 5-dihydroxyphenyl) -10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB); the mass ratio of the decabromodiphenylethane to the phosphorus flame retardant to the zinc borate is 1.5:3.5: 2; the content of decabromodiphenylethane in the methanol solution is 4 percent, and the content of zinc borate is 3 percent; the reaction condition is that the reaction temperature is 70 ℃, and the reaction time is 20 hours; the drying condition of (2) is drying at 120 ℃ for 15 h.
Esterification reaction:
carrying out first esterification reaction, pulping and mixing ethylene glycol and terephthalic acid according to the mol ratio of 1.2:1.07, adding a flame-retardant anti-dropping agent into the pulp according to a certain proportion, pulping to obtain mixed pulp, and then carrying out first esterification reaction on the mixed pulp, wherein the pressure of the first esterification reaction is 0.1MPa, and the reaction temperature is 220 ℃; when the water yield of the first esterification reaction reaches 94% of the theoretical water yield, the first esterification reaction is completed.
Performing a second esterification reaction, namely performing the second esterification reaction on the material obtained by the first esterification reaction after supplementing ethylene glycol, wherein the reaction pressure is 0.3Mpa, and the reaction temperature is 260 ℃; and (3) terminating the second esterification reaction until the esterification water yield reaches more than 99% of the theoretical water yield, and finishing the second esterification reaction.
And (3) polycondensation reaction: adding the flame-retardant anti-dripping agent obtained in the step one to a product of a second esterification reaction according to a certain proportion for a polycondensation reaction, and preparing flame-retardant anti-dripping polyester through the polycondensation reaction, wherein the temperature of the polycondensation reaction is kept at 282 ℃; the polycondensation reaction was continued for 3 h.
Preparing flame-retardant anti-dripping polyester fibers:
and (2) uniformly and fully mixing the flame-retardant anti-dripping polyester obtained in the fourth step with the flame-retardant anti-dripping agent obtained in the first step, drying at high temperature, melt-extruding by a double-screw extruder, feeding the melt into a spinning manifold, spraying the melt by a spinneret orifice, feeding the melt into a spinning channel, cooling by air, bundling, oiling, drafting, heat setting and winding to obtain the flame-retardant anti-dripping polyester fiber, wherein the drying temperature is 120 ℃.
Example three:
a processing method for adding flame-retardant anti-dripping polyester fibers on line in melt direct spinning comprises the following steps:
preparation of flame-retardant anti-dripping agent:
adding decabromodiphenylethane, zinc borate and a phosphorus flame retardant into a certain amount of methanol solution according to a certain proportion, reacting for a period of time under a certain condition by using methanol metal salt as a catalyst, and filtering, cleaning and drying after the reaction is finished to obtain the flame-retardant anti-dripping agent.
Wherein: the phosphorus flame retardant is bis (p-carboxyphenyl) phenyl phosphine oxide (BCPPO); the mass ratio of the decabromodiphenylethane to the phosphorus flame retardant to the zinc borate is 1.6:3.6: 2.1; the content of decabromodiphenylethane in the methanol solution is 3.5 percent, and the content of zinc borate is 2.5 percent; the reaction condition is that the reaction temperature is 80 ℃ and the reaction time is 25 h; the drying condition of (2) is drying at 140 ℃ for 20 h.
Esterification reaction:
carrying out first esterification reaction, pulping and mixing ethylene glycol and terephthalic acid according to the mol ratio of 1.3:1.1, adding a flame-retardant anti-dropping agent into the pulp according to a certain proportion, pulping to obtain mixed pulp, and then carrying out first esterification reaction on the mixed pulp, wherein the pressure of the first esterification reaction is 0.2MPa, and the reaction temperature is 230 ℃; and when the water yield of the first esterification reaction reaches 95 percent of the theoretical water yield, finishing the first esterification reaction.
Performing a second esterification reaction, namely performing the second esterification reaction on the material obtained by the first esterification reaction after supplementing ethylene glycol, wherein the reaction pressure is 0.4Mpa, and the reaction temperature is 270 ℃; and (3) terminating the second esterification reaction until the esterification water yield reaches more than 99% of the theoretical water yield, and finishing the second esterification reaction.
And (3) polycondensation reaction: adding the flame-retardant anti-dripping agent obtained in the step one to a product of the second esterification reaction according to a certain proportion for polycondensation reaction, and preparing flame-retardant anti-dripping polyester through the polycondensation reaction, wherein the temperature of the polycondensation reaction is kept at 285 ℃; the polycondensation reaction was continued for 4 h.
Preparing flame-retardant anti-dripping polyester fibers:
and (2) uniformly and fully mixing the flame-retardant anti-dripping polyester obtained in the fourth step with the flame-retardant anti-dripping agent obtained in the first step, drying at high temperature, performing melt extrusion through a double-screw extruder, enabling the melt to enter a spinning box body, spraying out the melt through a spinneret hole, enabling the melt to enter a spinning channel, performing air cooling, bundling, oiling, drafting, heat setting and winding to obtain the flame-retardant anti-dripping polyester fiber, wherein the drying temperature is 140 ℃.
Example four:
a processing method for adding flame-retardant anti-dripping polyester fibers on line in melt direct spinning comprises the following steps:
preparation of flame-retardant anti-dripping agent:
adding decabromodiphenylethane, zinc borate and a phosphorus flame retardant into a certain amount of methanol solution according to a certain proportion, reacting for a period of time under a certain condition by using methanol metal salt as a catalyst, and filtering, cleaning and drying after the reaction is finished to obtain the flame-retardant anti-dripping agent.
Wherein: the phosphorus flame retardant is bis (p-carboxyphenyl) phenyl phosphine oxide (BCPPO); the mass ratio of the decabromodiphenylethane to the phosphorus flame retardant to the zinc borate is 1.7:3.8: 2.4; the content of decabromodiphenylethane in the methanol solution is 2 percent, and the content of zinc borate is 2 percent; the reaction conditions are that the reaction temperature is 100 ℃ and the reaction time is 30 h; the drying condition of (2) is drying at 150 ℃ for 30 h.
Esterification reaction:
carrying out first esterification reaction, pulping and mixing ethylene glycol and terephthalic acid according to the mol ratio of 1.4:1.3, adding a flame-retardant anti-dropping agent into the pulp according to a certain proportion, pulping to obtain mixed pulp, and then carrying out first esterification reaction on the mixed pulp, wherein the pressure of the first esterification reaction is 0.5MPa, and the reaction temperature is 240 ℃; and when the water yield of the first esterification reaction reaches 96% of the theoretical water yield, finishing the first esterification reaction.
Performing a second esterification reaction, namely performing the second esterification reaction on the material obtained by the first esterification reaction after supplementing ethylene glycol, wherein the reaction pressure is 0.6Mpa, and the reaction temperature is 280 ℃; and (3) terminating the second esterification reaction until the esterification water yield reaches more than 99% of the theoretical water yield, and finishing the second esterification reaction.
And (3) polycondensation reaction: adding the flame-retardant anti-dripping agent obtained in the step one to a product of the second esterification reaction according to a certain proportion for polycondensation reaction, and preparing flame-retardant anti-dripping polyester through the polycondensation reaction, wherein the temperature of the polycondensation reaction is kept at 290 ℃; the polycondensation reaction lasted 6 h.
Preparing flame-retardant anti-dripping polyester fibers:
and (2) uniformly and fully mixing the flame-retardant anti-dripping polyester obtained in the fourth step with the flame-retardant anti-dripping agent obtained in the first step, drying at high temperature, performing melt extrusion through a double-screw extruder, enabling the melt to enter a spinning box body, spraying out the melt through a spinneret hole, enabling the melt to enter a spinning channel, performing air cooling, bundling, oiling, drafting, heat setting and winding to obtain the flame-retardant anti-dripping polyester fiber, wherein the drying temperature is 140 ℃.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A processing method for adding flame-retardant anti-dripping polyester fibers on line in melt direct spinning comprises the following steps:
the method comprises the following steps: preparation of flame-retardant anti-dripping agent: adding decabromodiphenylethane, a phosphorus flame retardant and zinc borate into a certain amount of methanol solution according to a certain proportion, reacting for a period of time under a certain condition by using methanol metal salt as a catalyst, and filtering, cleaning and drying after the reaction is finished to obtain a flame-retardant anti-dripping agent;
step two: a first esterification reaction: pulping and mixing ethylene glycol and terephthalic acid, adding the flame-retardant anti-dropping agent obtained in the step one into a mixed solution of the ethylene glycol and the terephthalic acid according to a certain proportion, and then fully mixing the ethylene glycol and the terephthalic acid for esterification reaction;
step three: second esterification reaction: continuously supplementing ethylene glycol into the solution of the first esterification reaction obtained in the step two to perform a second esterification reaction;
step four: and (3) polycondensation reaction: adding the flame-retardant anti-dripping agent obtained in the step one into a product of the second esterification reaction according to a certain proportion for polycondensation reaction, and obtaining flame-retardant anti-dripping polyester through polycondensation reaction;
step five: preparing flame-retardant anti-dripping polyester fibers: and (2) uniformly and fully mixing the flame-retardant anti-dripping polyester obtained in the fourth step with the flame-retardant anti-dripping agent obtained in the first step, drying at high temperature, performing melt extrusion through a double-screw extruder, enabling the melt to enter a spinning box body, spraying out the melt through a spinneret orifice, entering a spinning channel, performing air cooling, bundling, oiling, drafting, thermoforming and winding to obtain the flame-retardant anti-dripping polyester fiber.
2. The processing method of the melt direct spinning online added flame-retardant anti-dripping polyester fiber according to claim 1, characterized in that: the phosphorus flame retardant in the first step is one or more of [ (6-oxo-6H-dibenzo [ c, e ] [1,2] oxaphosphorin-6-yl) methyl ] succinic acid (DDP), 10- (2, 5-dihydroxyphenyl) -10-hydro-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB) and bis (p-carboxyphenyl) phenylphosphine oxide (BCPPO).
3. The processing method of the melt direct spinning online added flame-retardant anti-dripping polyester fiber according to claim 1, characterized in that: in the first step, the methanol solution contains 0.01-5% of decabromodiphenylethane and 0.02-4% of zinc borate.
4. The processing method of the melt direct spinning online added flame-retardant anti-dripping polyester fiber according to claim 1, characterized in that: in the second step, the pressure of the first esterification reaction is 0.03-0.6 MPa, and the reaction temperature is 210-240 ℃.
5. The processing method of the melt direct spinning online added flame-retardant anti-dripping polyester fiber according to claim 1, characterized in that: in the third step, the addition amount of the flame-retardant anti-dropping agent for the second esterification reaction is 0.1-10% of the mass content of the ethylene glycol, the pressure of the second esterification reaction is 0.2-0.6 Mpa, and the reaction temperature is 250-280 ℃.
6. The processing method of the melt direct spinning online added flame-retardant anti-dripping polyester fiber according to claim 1, characterized in that: and the polycondensation reaction in the fourth step is carried out at 280-290 ℃ under a vacuum condition.
7. The processing method of the melt direct spinning online added flame-retardant anti-dripping polyester fiber according to claim 1, characterized in that: and the drying temperature of the preparation of the flame-retardant anti-dripping polyester fiber in the step five is between 100 ℃ and 180 ℃ and the water content of the prepared flame-retardant anti-dripping polyester fiber is lower than 100 ppm.
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| CN202111141980.3A CN113913957A (en) | 2021-09-28 | 2021-09-28 | Processing method for online adding flame-retardant anti-dripping polyester fiber in melt direct spinning |
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