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CN108179492A - A kind of preparation method of estersil cladded type flame-retardant polypropylene long filament - Google Patents

A kind of preparation method of estersil cladded type flame-retardant polypropylene long filament Download PDF

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Publication number
CN108179492A
CN108179492A CN201711277918.0A CN201711277918A CN108179492A CN 108179492 A CN108179492 A CN 108179492A CN 201711277918 A CN201711277918 A CN 201711277918A CN 108179492 A CN108179492 A CN 108179492A
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weight
parts
estersil
added
taken
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金昱轩
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/46Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/07Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention discloses a kind of preparation methods of estersil cladded type flame-retardant polypropylene long filament, zinc borate, Ludox, the talcum powder of the material addition of the present invention can play good fire retardant performance, wherein esterification cladding material can form stable charcoal ball in burning, the effect of good gas phase barrier is played, achievees the effect that further to reduce the intensity of a fire.

Description

A kind of preparation method of estersil cladded type flame-retardant polypropylene long filament
Technical field
The invention belongs to polypropylene filament yarn fields, and in particular to a kind of preparation method of estersil cladded type flame-retardant polypropylene long filament.
Background technology
Polypropylene filament yarn is to make that raw material is aggregated, fiber made from melt spinning as propylene.Polypropylene fibre in nineteen fifty-seven formally Industrialized production is the up-and-coming youngster in synthetic fibers.Since polypropylene fibre has simple production process, product is inexpensive, and intensity is high, phase The advantages that light to density, so polypropylene fibre develops quickly.Polypropylene fibre has been the fourth-largest kind of synthetic fibers at present, is general chemical Most light fiber in fiber.The kind of polypropylene fibre have long filament (including not deformed long filament and varicosity modified continuous filament), staple fiber, bristlelike monofilament, Film-fibre, doughnut, profiled filament, various composite fibres and bonded fabric etc..It is mainly used for making carpet (including ground Blanket base fabric and matte), bunting, furniture stuff, various ropes, band, fishing net, asphalt felt, building reinforcing material, packaging material and Industrial cloth, such as filter cloth, bagging.In addition in terms of clothing using also increasingly extensively, can with multiple fiber is blended that difference is made Shirt, coat, sweat shirt, socks etc. can be made after knitting is processed in the blended fabric of type.By polypropylene fibre doughnut system Into wadding quilt, light, warming, elasticity is good.Fiber obtained.Polypropylene fibre formally starts industrialized production in nineteen fifty-seven, is synthesis Up-and-coming youngster in fiber.Due to the advantages that polypropylene fibre has simple production process, and product is inexpensive, and intensity is high, and relative density is light, institute Develop quickly with polypropylene fibre.Polypropylene fibre has been the fourth-largest kind of synthetic fibers at present, is fiber most light in general chemical fiber;
However polypropylene is mainly made of elements such as carbon, hydrogen, material poor fire itself, is easily dropped under the action of heat Solution generates imflammable gas, easily burning, and so as to which fire occur, great harm is brought to the safety of life and property of people, because This often adds multiple additives wherein when polypropylene fibre is prepared, including inorganic additive and organic additive, wherein Inorganic additive is easily reduced the mechanical property of finished product long filament due to the poor compatibility with polymeric matrix, and organic filament master If containing halogen and phosphorous fire retardant, the fire retardant particularly containing chlorine, bromine is even more to be widely used, but it is special in burning It does not release the hydrogen halide of irritation and radiativity easily, there is very strong harm to human body;
It is therefore an object of the present invention to provide a kind of anti-flammability preferable polypropylene filament yarn, it is made also to have very in burning Good Safety and Environmental Protection, while the problem of improve poor compatibility of the inorganic fire-retarded additive of tradition in polypropylene matrix, effectively Raising finished product mechanical property.
Invention content
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of estersil cladded type flame-retardant polypropylene is long The preparation method of silk.
To achieve the above object, the present invention uses following technical scheme:
A kind of preparation method of estersil cladded type flame-retardant polypropylene long filament, includes the following steps:
(1) lauryl mercaptan of 2-3 parts by weight is taken, is added in the absolute ethyl alcohol of 10-12 times of its weight, stirring is equal It is even, the ricinoleic acid calcium of 0.6-1 parts by weight is added in, insulated and stirred 4-5 minutes at 60-65 DEG C, obtains compound alcoholic solution;
(2) presoma of 36-40 parts by weight is taken, is added in above-mentioned compound alcoholic solution, adds in the diformazan of 1-2 parts by weight Amine, it is 10-15 minutes ultrasonic, obtain amination alcohol dispersion liquid;
(3) hydration zinc borate of 4-5 parts by weight is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly, Above-mentioned amination alcohol dispersion liquid is added in, raising temperature is 50-60 DEG C, adds in the Dodecydimethylammonium bronides of 0.7-1 parts by weight, Insulated and stirred 10-20 minutes, reduction temperature are room temperature, and the ammonium hydroxide of dropwise addition 5-6 parts by weight, a concentration of 10-13% is added dropwise After be stirred to react 3-4 hours, obtain Sol-gel Coated solution;
(4) talcum powder of 4-5 parts by weight is taken, is added in the deionized water of 17-20 times of its weight, adds in 10-14 weight The orthosilicic acid of part, stirs evenly, obtains silicate solution;
(5) above-mentioned Sol-gel Coated solution, silicate solution mixing are taken, stirs evenly, is sent in reaction kettle, adjust reaction kettle Temperature is 90-95 DEG C, and the catalyst solution of 2-3 parts by weight is added dropwise, is added dropwise latter insulated and stirred 3-4 hours, discharges, obtains estersil Sol-gel Coated solution;
(6) glyceryl tristearate of 0.3-0.5 parts by weight is taken, is added in above-mentioned estersil Sol-gel Coated solution, is stirred Uniformly, estersil Sol-gel Coated lotion is obtained;
(7) isotactic polypropylene of 110-120 parts by weight is taken, is added to 6-9 times of its weight, 70-75% ethanol solution In, the gamma-aminopropyl-triethoxy-silane of 3-4 parts by weight is added in, it is 10-29 minutes ultrasonic, obtain silane polypropylene dispersion liquid;
(8) above-mentioned estersil Sol-gel Coated lotion, the mixing of silane polypropylene dispersion liquid are taken, is sent to 65-70 DEG C of thermostatted water In bath, insulated and stirred 16-20 hours discharges, and precipitation is washed in filtering, and it is 0.1- to be dried at 46-50 DEG C of vacuum to water content 0.2%, it is cooled to room temperature, obtains estersil Sol-gel Coated modified polypropene;
(9) above-mentioned estersil Sol-gel Coated modified polypropene is taken, is sent in screw extruder, melting extrusion, extrusion temperature It is 270-300 DEG C, melt is subjected to spinning, by receives silk processing to get the estersil cladded type flame-retardant polypropylene long filament.
The presoma is ethyl orthosilicate.
The preparation method of the catalyst solution is:
The p-methyl benzenesulfonic acid of 1-2 parts by weight is taken, is added in the deionized water of 24-30 times of its weight, stirs evenly, i.e., .
Advantages of the present invention:
The present invention is disperseed in alcoholic solution, is handled using dimethylamine, obtained first using ethyl orthosilicate as presoma in advance Amination dispersion liquid, then using hydration zinc borate as raw material, Dodecydimethylammonium bronides are dispersant, by ethyl orthosilicate water Solution by hydrolysis by sol deposition to boric acid zinc surface, obtains amination Sol-gel Coated solution, then mixes it with orthosilicic acid, Esterification is carried out under catalyst action, obtains esters of silicon acis cladding Sol-gel Coated solution, then disperse by glyceryl tristearate, Dispersion esterification lotion is obtained, isotactic polypropylene is handled using amino silicane coupling agent later, obtains amino silane polypropylene dispersion liquid, Finally by itself and dispersion esterification emulsion blending dispersion, esterification lotion the having in polypropylene containing inorganic coating filler is realized It imitates compatible, effectively raises the mechanical property of finished product polypropylene fibre, zinc borate that material of the invention adds in, Ludox, talcum powder Good fire retardant performance can be played, wherein esterification cladding material can form stable charcoal ball in burning, is played very The effect of good gas phase barrier, achievees the effect that further to reduce the intensity of a fire.
Specific embodiment
Embodiment 1
A kind of preparation method of estersil cladded type flame-retardant polypropylene long filament, includes the following steps:
(1) lauryl mercaptan of 3 parts by weight is taken, is added in the absolute ethyl alcohol of 12 times of its weight, stirs evenly, is added in The ricinoleic acid calcium of 1 parts by weight, insulated and stirred 5 minutes at 65 DEG C, obtains compound alcoholic solution;
(2) presoma of 40 parts by weight is taken, is added in above-mentioned compound alcoholic solution, adds in the dimethylamine of 2 parts by weight, ultrasound 15 minutes, obtain amination alcohol dispersion liquid;
(3) hydration zinc borate of 5 parts by weight is taken, is added in the deionized water of 30 times of its weight, stirs evenly, in addition Amination alcohol dispersion liquid is stated, raising temperature is 60 DEG C, adds in the Dodecydimethylammonium bronides of 1 parts by weight, and insulated and stirred 20 is divided Clock, reduction temperature are room temperature, and 6 parts by weight, a concentration of 13% ammonium hydroxide is added dropwise, is stirred to react 4 hours, obtains molten after being added dropwise Glue cladding solution;
(4) talcum powder of 5 parts by weight is taken, is added in the deionized water of 20 times of its weight, adds in the former silicon of 14 parts by weight Acid stirs evenly, and obtains silicate solution;
(5) above-mentioned Sol-gel Coated solution, silicate solution mixing are taken, stirs evenly, is sent in reaction kettle, adjust reaction kettle Temperature is 95 DEG C, and the catalyst solution of 3 parts by weight is added dropwise, rear insulated and stirred is added dropwise 4 hours, discharges, obtains estersil colloidal sol packet Cover solution;
(6) glyceryl tristearate of 0.5 parts by weight is taken, is added in above-mentioned estersil Sol-gel Coated solution, stirs evenly, Obtain estersil Sol-gel Coated lotion;
(7) isotactic polypropylene of 120 parts by weight is taken, is added in 9 times of its weight, 75% ethanol solution, adds in 4 weights The gamma-aminopropyl-triethoxy-silane of part is measured, ultrasound 29 minutes obtains silane polypropylene dispersion liquid;
(8) above-mentioned estersil Sol-gel Coated lotion, the mixing of silane polypropylene dispersion liquid are taken, is sent to 70 DEG C of water bath with thermostatic control In, insulated and stirred 20 hours discharges, and precipitation is washed in filtering, and it is 0.2% to be dried at 50 DEG C of vacuum to water content, is cooled to often Temperature obtains estersil Sol-gel Coated modified polypropene;
(9) above-mentioned estersil Sol-gel Coated modified polypropene is taken, is sent in screw extruder, melting extrusion, extrusion temperature It is 300 DEG C, melt is subjected to spinning, by receives silk processing to get the estersil cladded type flame-retardant polypropylene long filament.
The presoma is ethyl orthosilicate.
The preparation method of the catalyst solution is:
Take the p-methyl benzenesulfonic acid of 2 parts by weight, be added in the deionized water of 30 times of its weight, stir evenly to get.
Embodiment 2
A kind of preparation method of estersil cladded type flame-retardant polypropylene long filament, includes the following steps:
(1) lauryl mercaptan of 2 parts by weight is taken, is added in the absolute ethyl alcohol of 10 times of its weight, stirs evenly, is added in The ricinoleic acid calcium of 0.6 parts by weight, insulated and stirred 4 minutes at 60 DEG C, obtains compound alcoholic solution;
(2) presoma of 36 parts by weight is taken, is added in above-mentioned compound alcoholic solution, adds in the dimethylamine of 1 parts by weight, ultrasound 10 minutes, obtain amination alcohol dispersion liquid;
(3) hydration zinc borate of 4 parts by weight is taken, is added in the deionized water of 20 times of its weight, stirs evenly, in addition Amination alcohol dispersion liquid is stated, raising temperature is 50 DEG C, adds in the Dodecydimethylammonium bronides of 0.7 parts by weight, insulated and stirred 10 Minute, reduction temperature is room temperature, and 5 parts by weight, a concentration of 10% ammonium hydroxide is added dropwise, is stirred to react 3 hours, obtains after being added dropwise Sol-gel Coated solution;
(4) talcum powder of 4 parts by weight is taken, is added in the deionized water of 17 times of its weight, adds in the former silicon of 10 parts by weight Acid stirs evenly, and obtains silicate solution;
(5) above-mentioned Sol-gel Coated solution, silicate solution mixing are taken, stirs evenly, is sent in reaction kettle, adjust reaction kettle Temperature is 90 DEG C, and the catalyst solution of 2 parts by weight is added dropwise, rear insulated and stirred is added dropwise 3 hours, discharges, obtains estersil colloidal sol packet Cover solution;
(6) glyceryl tristearate of 0.3 parts by weight is taken, is added in above-mentioned estersil Sol-gel Coated solution, stirs evenly, Obtain estersil Sol-gel Coated lotion;
(7) isotactic polypropylene of 110 parts by weight is taken, is added in 6 times of its weight, 70% ethanol solution, adds in 3 weights The gamma-aminopropyl-triethoxy-silane of part is measured, ultrasound 10 minutes obtains silane polypropylene dispersion liquid;
(8) above-mentioned estersil Sol-gel Coated lotion, the mixing of silane polypropylene dispersion liquid are taken, is sent to 65 DEG C of water bath with thermostatic control In, insulated and stirred 16 hours discharges, and precipitation is washed in filtering, and it is 0.1% to be dried at 46 DEG C of vacuum to water content, is cooled to often Temperature obtains estersil Sol-gel Coated modified polypropene;
(9) above-mentioned estersil Sol-gel Coated modified polypropene is taken, is sent in screw extruder, melting extrusion, extrusion temperature It is 270 DEG C, melt is subjected to spinning, by receives silk processing to get the estersil cladded type flame-retardant polypropylene long filament.
The presoma is ethyl orthosilicate.
The preparation method of the catalyst solution is:
Take the p-methyl benzenesulfonic acid of 1 parts by weight, be added in the deionized water of 24 times of its weight, stir evenly to get.
Performance test:
The estersil cladded type flame-retardant polypropylene long filament of embodiment 1:
Intensity is 9.9g/d, and elongation at break 13.9%, oxygen index (OI) 32, UL-94 are V-1 ranks;
The estersil cladded type flame-retardant polypropylene long filament of embodiment 2:
Intensity is 10.3g/d, and elongation at break 14.5%, oxygen index (OI) 33, UL-94 are V-1 ranks;
Commercially available polypropylene filament yarn:
Intensity is 4-5g/d, and elongation at break 10-12%, oxygen index (OI) 20-25, UL-94 are V-2 ranks;
As can be seen that the estersil cladded type flame-retardant polypropylene long filament of the present invention has better mechanical property and fire-retardant fireproof Property.

Claims (3)

1. a kind of preparation method of estersil cladded type flame-retardant polypropylene long filament, which is characterized in that include the following steps:
(1) lauryl mercaptan of 2-3 parts by weight is taken, is added in the absolute ethyl alcohol of 10-12 times of its weight, stirs evenly, add Enter the ricinoleic acid calcium of 0.6-1 parts by weight, insulated and stirred 4-5 minutes at 60-65 DEG C, obtain compound alcoholic solution;
(2) presoma of 36-40 parts by weight is taken, is added in above-mentioned compound alcoholic solution, adds in the dimethylamine of 1-2 parts by weight, is surpassed Sound 10-15 minutes obtains amination alcohol dispersion liquid;
(3) hydration zinc borate of 4-5 parts by weight is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly, is added in Above-mentioned amination alcohol dispersion liquid, raising temperature are 50-60 DEG C, add in the Dodecydimethylammonium bronides of 0.7-1 parts by weight, heat preservation Stirring 10-20 minutes, reduction temperature are room temperature, and the ammonium hydroxide of dropwise addition 5-6 parts by weight, a concentration of 10-13% stirs after being added dropwise Reaction 3-4 hours is mixed, obtains Sol-gel Coated solution;
(4) talcum powder of 4-5 parts by weight is taken, is added in the deionized water of 17-20 times of its weight, adds in 10-14 parts by weight Orthosilicic acid stirs evenly, and obtains silicate solution;
(5) above-mentioned Sol-gel Coated solution, silicate solution mixing are taken, stirs evenly, is sent in reaction kettle, adjust temperature of reaction kettle It is 90-95 DEG C, the catalyst solution of 2-3 parts by weight is added dropwise, is added dropwise latter insulated and stirred 3-4 hours, discharges, obtain estersil colloidal sol Cladding solution;
(6) glyceryl tristearate of 0.3-0.5 parts by weight is taken, is added in above-mentioned estersil Sol-gel Coated solution, stirs evenly, Obtain estersil Sol-gel Coated lotion;
(7) isotactic polypropylene of 110-120 parts by weight is taken, in ethanol solution that be added to 6-9 times of its weight, 70-75%, is added Enter the gamma-aminopropyl-triethoxy-silane of 3-4 parts by weight, it is 10-29 minutes ultrasonic, obtain silane polypropylene dispersion liquid;
(8) above-mentioned estersil Sol-gel Coated lotion, the mixing of silane polypropylene dispersion liquid are taken, is sent in 65-70 DEG C of water bath with thermostatic control, Insulated and stirred 16-20 hours discharges, and precipitation is washed in filtering, and it is 0.1-0.2% to be dried at 46-50 DEG C of vacuum to water content, It is cooled to room temperature, obtains estersil Sol-gel Coated modified polypropene;
(9) above-mentioned estersil Sol-gel Coated modified polypropene is taken, is sent in screw extruder, melting extrusion, extrusion temperature is 270-300 DEG C, melt is subjected to spinning, by receiving silk processing to get the estersil cladded type flame-retardant polypropylene long filament.
2. the preparation method of a kind of estersil cladded type flame-retardant polypropylene long filament according to claim 1, which is characterized in that described Presoma be ethyl orthosilicate.
3. the preparation method of a kind of estersil cladded type flame-retardant polypropylene long filament according to claim 1, which is characterized in that described The preparation method of catalyst solution be:
Take the p-methyl benzenesulfonic acid of 1-2 parts by weight, be added in the deionized water of 24-30 times of its weight, stir evenly to get.
CN201711277918.0A 2017-12-06 2017-12-06 A kind of preparation method of estersil cladded type flame-retardant polypropylene long filament Pending CN108179492A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1554568A (en) * 2003-12-19 2004-12-15 华东师范大学 Silica gel-coated multi-metal oxygen-containing cluster nanoparticle material and preparation method thereof
CN1922275A (en) * 2004-02-18 2007-02-28 财团法人川村理化学研究所 Organic and inorganic composite nanofiber, organic and inorganic composite structure and methods for producing the same
CN101318644A (en) * 2008-07-01 2008-12-10 上海大学 A Novel Method for Coating Carbon Nanotubes with Silica
CN103044061A (en) * 2011-10-11 2013-04-17 旭化成化学株式会社 Formed body, coated body, manufacturing method of formed body and heat insulation method
CN103130231A (en) * 2011-11-25 2013-06-05 航天特种材料及工艺技术研究所 Silica aerogel material and preparation method thereof
CN103290511A (en) * 2013-05-24 2013-09-11 宁波三邦超细纤维有限公司 Breathable terylene-polypropylene composite superfine fiber and production method thereof
US20150056471A1 (en) * 2012-02-16 2015-02-26 Cornell University Ordered porous nanofibers, methods, and applications

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1554568A (en) * 2003-12-19 2004-12-15 华东师范大学 Silica gel-coated multi-metal oxygen-containing cluster nanoparticle material and preparation method thereof
CN1922275A (en) * 2004-02-18 2007-02-28 财团法人川村理化学研究所 Organic and inorganic composite nanofiber, organic and inorganic composite structure and methods for producing the same
CN101318644A (en) * 2008-07-01 2008-12-10 上海大学 A Novel Method for Coating Carbon Nanotubes with Silica
CN103044061A (en) * 2011-10-11 2013-04-17 旭化成化学株式会社 Formed body, coated body, manufacturing method of formed body and heat insulation method
CN103130231A (en) * 2011-11-25 2013-06-05 航天特种材料及工艺技术研究所 Silica aerogel material and preparation method thereof
US20150056471A1 (en) * 2012-02-16 2015-02-26 Cornell University Ordered porous nanofibers, methods, and applications
CN103290511A (en) * 2013-05-24 2013-09-11 宁波三邦超细纤维有限公司 Breathable terylene-polypropylene composite superfine fiber and production method thereof

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Application publication date: 20180619