CN109537099A - A kind of multicomponent polymeric blending fire retardant precursor and preparation method thereof - Google Patents
A kind of multicomponent polymeric blending fire retardant precursor and preparation method thereof Download PDFInfo
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- CN109537099A CN109537099A CN201811471898.5A CN201811471898A CN109537099A CN 109537099 A CN109537099 A CN 109537099A CN 201811471898 A CN201811471898 A CN 201811471898A CN 109537099 A CN109537099 A CN 109537099A
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- fire retardant
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- 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
-
- 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
- D01F1/10—Other agents for modifying properties
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/08—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyacrylonitrile as constituent
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Multicomponent Fibers (AREA)
- Artificial Filaments (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention provides a kind of multicomponent polymeric blending fire retardant precursor and preparation method thereof, its primary raw material and content are as follows: vinyl chloride-vinyl acetate is copolymerized 10~20 parts by weight of paste resin, 7~15 parts by weight of acrylonitrile-methylacrylate copolymer resins, 70~79 parts by weight of solvent, 1~4 parts by weight of solubilizer；By following preparation step: using physical solution blending method, be mixed to form spinning solution；Spinning solution is extruded from spinneret orifice；Spinneret solidification forming, is made spun filament；Stretch: control draw ratio stretches spun filament；Washing；It oils；Compacting by drying；Thermal finalization；Silk is received in curling；High, the good-extensibility by multicomponent polymeric blending fire retardant precursor intensity produced by the present invention, flame retardant property is high, suitable for fire retardant man-made fur, flame-retardant textile etc..
Description
Technical field
The present invention relates to a kind of fire-retardant precursor and preparation method thereof, especially a kind of multicomponent polymericIt is blendedFire-retardant precursor
And preparation method thereof.
Background technique
At abroad, many industries and field have quite stringent flame-retardancy requirements to fabric, fabric lining etc., such as public field
Interior trim, carpet, curtain, wall cloth of institute, hotel etc. etc., it is necessary to meet corresponding legal fire-protection standard；The nightwear of baby,
The fireproof garment of the special trades such as fireman must also use fire proofing.And at home, professional standard, the decree regulation of this respect
Not yet sound, with the development of national economy and the continuous improvement of living standards of the people, people gradually recognize fiber fire prevention, resistance
The importance of combustion, therefore, the exploitation of fire resistance fibre have very big realistic meaning and market value.
Acrylic fiber is widely used in clothing, imitative wool fabric etc. as a kind of common fibrous material.Currently,
The fire-retardant method for mostly using addition fire retardant of acrylic fibers is solved.It is raw using addition fire retardant (halogen, phosphorus system substance etc.)
The acrylic fiber of production, flameproof effect is poor, and fire retardant is easy to be lost in the process of processing and using, make the fire resistance property of fiber by
Gradually reduce；Meanwhile most of fire retardant used at present can generate very big pollution to environment, be unfavorable for sustainable development；And
And additive be added can the mechanical performance indexs such as tensile strength, elongation at break rate to acrylic fiber generate adverse effect.
Solve the problems, such as that a kind of fire-retardant desirable route of acrylic fibers is acrylic fibers resin of the synthesis with flame retardant effect itself.Both at home and abroad
Study more, and the non-additive flame retardant acrylic fibers resin for having industrialized production is vinylidene chloride-acrylonitrile compolymer resin, but
It is after introducing acrylonitrile polymerization as flame-retardant monomer using vinylidene chloride, obtained copolymer spinning, feel is partially hard, fine
Dimension is not so good as common acrylic fiber in terms of flexibility, is not suitable for doing artificial fur, and the feel of acrylic fiber, appearance are similar to sheep
Hair.The disadvantage is that: easily burn, wear no resistance, intensity bottom, elasticity it is bad, the acrylonitrile-vinyl chloride of also useful emulsion method synthesis is total to
The fire resistance fibre that polymers is spun into, the polymer made from this method need the sodium chloride solution demulsification with saturation, polymerize after demulsification
Object need to be washed with a large amount of deionized waters, can generate a large amount of washes.
Vinyl chloride-vinyl acetate is copolymerized paste resin, is widely used in automobile chassis shock resistance coating, plastisol, foaming
Product etc., the both at home and abroad not application in the preparation technical field of artificial fur.
Summary of the invention
The present invention provides a kind of multicomponent polymeric blending fire retardant precursor preparation methods.
Realize the multicomponent polymeric blending fire retardant precursor preparation method of one of the object of the invention, primary raw material and content
It is as follows:
Vinyl chloride-vinyl acetate is copolymerized paste resin 10~16
Acrylonitrile-methylacrylate copolymer resins 7~15
Dimethyl acetamide 70~79
Unit is parts by weight；
According to the above ratio, using wet spinning technology, including following preparation step:
A. physical solution blending method is used, spinning solution is mixed to form, dissolved polymer solution is filtered, is prevented not
Molten object, insoluble matter influence finishing operations；
B. spinning solution is extruded from spinneret orifice, the eyelet aperture arranged on spinning head is 0.05~0.12mm, spinneret orifice
Select dumbbell shape or hollow type；
C. coagulating bath is done using acid, alkali, salt, organic solvent etc., spun filament is made in spinneret solidification forming；
D. stretch: control draw ratio stretches spun filament；
E. it washes；
F. it oils；
G. compacting by drying；
H. thermal finalization；
I. silk is received in curling.
Spinneret orifice selects dumbbell shape or hollow type in the step of preparation process b, and the draw ratio of spinneret orifice is in 1:12, emulation
Degree is more preferable, and gloss is more nearly true hair.
The vinyl chloride-vinyl acetate copolymerization paste resin is copolymerized by vinyl chloride and vinyl acetate, the acetic acid second
Alkene accounts for total weight ratio: 5%~10%.
The acrylonitrile-methylacrylate copolymer resins are formed by acrylonitrile and methyl acrylate copoly, the acrylic acid
Methyl esters accounts for total weight ratio: 5%~10%.
The acrylonitrile-methylacrylate copolymer resins can also use the spinning of acrylonitrile-methylacrylate copolymer resins
Made of acrylic fiber replace, in preparation process of the present invention, need to add basic solvent and do coagulating bath, acrylic fiber has resistance to
Alkalinity facilitates the formation of coagulating bath.
The solvent selects dimethyl acetamide or dimethylformamide.
Primary raw material further includes 1~4 parts by weight of solubilizer.
The solubilizer selects polycaprolactone, reduces the interface abilities between each component, increases the dispersion between each component
Compatibility.
Multicomponent polymeric blending fire retardant precursor of the invention and preparation method thereof has the beneficial effect that:
1, in multicomponent polymeric blending fire retardant precursor preparation method of the invention, compared to the propylene synthesized with emulsion method
The fire resistance fibre that nitrile-vinyl chloride copolymer is spun into does not need the sodium chloride solution demulsification with saturation, will not generate a large amount of washing
Waste water.
2, in multicomponent polymeric blending fire retardant precursor preparation method of the invention, acrylonitrile-methylacrylate copolymerization tree
Rouge can also the replacement of the acrylic fiber made of acrylonitrile-methylacrylate copolymer resins spinning.In preparation process of the present invention
In, it needs to add basic solvent and does coagulating bath, acrylic fiber has alkali resistance, facilitates the formation of coagulating bath, shortens the time, mentions
High processing efficiency.
3, in multicomponent polymeric blending fire retardant precursor preparation method of the invention, solubilizer is added, oneself is especially gathered
Lactones will can sufficiently disperse mutually to mix between each polymer as solubilizer, by the polymer glass temperature control after blending
System is in a lesser range.
4, multicomponent polymeric blending fire retardant precursor of the invention has intensity height, good-extensibility, flame retardant property height.
Specific embodiment
Embodiment 1
Multicomponent polymeric blending fire retardant precursor of the invention, including vinyl chloride-vinyl acetate are copolymerized 10 weight of paste resin
Amount part, 13 parts by weight of acrylonitrile-methylacrylate copolymer resins, 1 parts by weight of polycaprolactone, 76 parts by weight of dimethyl acetamide,
55 DEG C of dispersion temperature of dissolution, obtained precursor is through detecting, breaking strength 2.80CN/dt, elongation at break 59.1%, limit oxygen index
28。
Embodiment 2
Multicomponent polymeric blending fire retardant precursor of the invention, including vinyl chloride-vinyl acetate are copolymerized 10 weight of paste resin
Amount part, 15 parts by weight of acrylonitrile-methylacrylate copolymer resins, 1 parts by weight of polycaprolactone, 74 parts by weight of dimethyl acetamide,
60 DEG C of dispersion temperature of dissolution, obtained precursor is through detecting, breaking strength 2.65CN/dt, elongation at break 53%, limit oxygen index
28。
Embodiment 3
Multicomponent polymeric blending fire retardant precursor of the invention, including vinyl chloride-vinyl acetate are copolymerized 11 weight of paste resin
Amount part, 11 parts by weight of acrylonitrile-methylacrylate copolymer resins, 2 parts by weight of polycaprolactone, 76 parts by weight of dimethyl acetamide,
55 DEG C of dispersion temperature of dissolution, obtained precursor is through detecting, breaking strength 3.51CN/dt, elongation at break 55%, limit oxygen index
32。
Embodiment 4
Multicomponent polymeric blending fire retardant precursor of the invention, including vinyl chloride-vinyl acetate are copolymerized 11 weight of paste resin
Amount part, 11 parts by weight of acrylonitrile-methylacrylate copolymer resins, 2 parts by weight of polycaprolactone, 76 parts by weight of dimethyl acetamide,
55 DEG C of dispersion temperature of dissolution, obtained precursor is through detecting, breaking strength 2.74CN/dt, elongation at break 50.1%, limit oxygen index
32。
Embodiment 5
Multicomponent polymeric blending fire retardant precursor of the invention, including vinyl chloride-vinyl acetate are copolymerized 12 weight of paste resin
Amount part, 12 parts by weight of acrylonitrile-methylacrylate copolymer resins, 2 parts by weight of polycaprolactone, 74 parts by weight of dimethyl acetamide,
60 DEG C of dispersion temperature of dissolution, obtained precursor is through detecting, breaking strength 2.76CN/dt, elongation at break 52%, limit oxygen index
32。
Embodiment 6
Multicomponent polymeric blending fire retardant precursor of the invention, including vinyl chloride-vinyl acetate are copolymerized 12 weight of paste resin
Amount part, 15 parts by weight of acrylonitrile-methylacrylate copolymer resins, 1 parts by weight of polycaprolactone, 72 parts by weight of dimethyl acetamide,
65 DEG C of dispersion temperature of dissolution, obtained precursor is through detecting, breaking strength 3.16CN/dt, elongation at break 60.8%, limit oxygen index
28。
Embodiment 7
Multicomponent polymeric blending fire retardant precursor of the invention, including vinyl chloride-vinyl acetate are copolymerized 13 weight of paste resin
Amount part, 7 parts by weight of acrylonitrile-methylacrylate copolymer resins, 4 parts by weight of polycaprolactone, 79 parts by weight of dimethyl acetamide are molten
55 DEG C of dispersion temperature of solution, obtained precursor is through detecting, breaking strength 2.63CN/dt, elongation at break 47.3%, limit oxygen index
34。
Embodiment 8
Multicomponent polymeric blending fire retardant precursor of the invention, including vinyl chloride-vinyl acetate are copolymerized 13 weight of paste resin
Amount part, 10 parts by weight of acrylonitrile-methylacrylate copolymer resins, 3 parts by weight of polycaprolactone, 74 parts by weight of dimethyl acetamide,
60 DEG C of dispersion temperature of dissolution, obtained precursor is through detecting, breaking strength 2.68CN/dt, elongation at break 50.5%, limit oxygen index
33。
Embodiment 9
Multicomponent polymeric blending fire retardant precursor of the invention, including vinyl chloride-vinyl acetate are copolymerized 13 weight of paste resin
Amount part, 13 parts by weight of acrylonitrile-methylacrylate copolymer resins, 2 parts by weight of polycaprolactone, 72 parts by weight of dimethyl acetamide,
65 DEG C of dispersion temperature of dissolution, obtained precursor is through detecting, breaking strength 3.02CN/dt, elongation at break 58.5%, limit oxygen index
28。
Embodiment 10
Multicomponent polymeric blending fire retardant precursor of the invention, including vinyl chloride-vinyl acetate are copolymerized 15 weight of paste resin
Amount part, 7 parts by weight of acrylonitrile-methylacrylate copolymer resins, 4 parts by weight of polycaprolactone, 74 parts by weight of dimethyl acetamide are molten
60 DEG C of dispersion temperature of solution, obtained precursor is through detecting, breaking strength 2.56CN/dt, elongation at break 45.5%, limit oxygen index
34。
Embodiment 11
Multicomponent polymeric blending fire retardant precursor of the invention, including vinyl chloride-vinyl acetate are copolymerized 15 weight of paste resin
Amount part, 10 parts by weight of acrylonitrile-methylacrylate copolymer resins, 3 parts by weight of polycaprolactone, 72 parts by weight of dimethyl acetamide,
65 DEG C of dispersion temperature of dissolution, obtained precursor is through detecting, breaking strength 2.91CN/dt, elongation at break 53%, limit oxygen index
33。
Embodiment 12
Multicomponent polymeric blending fire retardant precursor of the invention, including vinyl chloride-vinyl acetate are copolymerized 16 weight of paste resin
Amount part, 8 parts by weight of acrylonitrile-methylacrylate copolymer resins, 4 parts by weight of polycaprolactone, 72 parts by weight of dimethyl acetamide are molten
65 DEG C of dispersion temperature of solution, obtained precursor is through detecting, breaking strength 2.61CN/dt, elongation at break 46%, limit oxygen index 34.
Through overtesting, the multicomponent polymeric blending fire retardant precursor performance parameter of above-mentioned 12 embodiments is as follows:
It can be seen that the breaking strength of multicomponent polymeric blending fire retardant precursor of the invention has reached 2.6~3.01CN/
Dt, elongation at break rate have reached 45.5~60.8%, and limit oxygen index (flame retardant property) has reached 28~34；
And acrylic fibers 2.1~2.4CN/dt of breaking strength, the elongation at break rate 40-45% of common wet process spinning, it does not hinder
Combustion, easily burning (being detailed in Chemical Industry Press " high molecular material handbook " P891)；
To sum up, breaking strength of the invention, elongation at break rate, limit oxygen index (flame retardant property) experimental index be much
Greater than the acrylic fibers of the common wet process spinning of the prior art.
The present invention has intensity height, good-extensibility, flame retardant property height.
The above-described embodiments are merely illustrative of preferred embodiments of the present invention, not to model of the invention
It encloses and is defined, without departing from the spirit of the design of the present invention, this field ordinary engineering and technical personnel is to the technology of the present invention side
The various changes and improvements that case is made, should fall within the scope of protection determined by the claims of the present invention.
Claims (9)
1. a kind of preparation method of multicomponent polymeric blending fire retardant precursor, primary raw material and content are as follows:
Vinyl chloride-vinyl acetate is copolymerized paste resin 10~20
Acrylonitrile-methylacrylate copolymer resins 7~15
Solvent 70~79
Unit is parts by weight；
According to the above ratio, using wet spinning technology, by following preparation step:
A. physical solution blending method is used, spinning solution is mixed to form；
B. spinning solution is extruded from spinneret orifice；
C. spun filament is made in spinneret solidification forming；
D. stretch: control draw ratio stretches spun filament；
E. it washes；
F. it oils；
G. compacting by drying；
H. thermal finalization；
I. silk is received in curling.
2. the preparation method of multicomponent polymeric blending fire retardant precursor according to claim 1, it is characterised in that: the chlorine
Ethene-vinyl acetate copolymerization paste resin is copolymerized by vinyl chloride and vinyl acetate, and the vinyl acetate accounts for total weight ratio:
5%~10%.
3. the preparation method of multicomponent polymeric blending fire retardant precursor according to claim 1, it is characterised in that: described third
Alkene nitrile-methyl acrylate copoly resin is formed by acrylonitrile and methyl acrylate copoly, and the methyl acrylate accounts for total weight ratio:
5%~10%.
4. the preparation method of any multicomponent polymeric blending fire retardant precursor according to claim 1, it is characterised in that: institute
It states solvent and selects dimethyl acetamide or dimethylformamide.
5. the preparation method of any multicomponent polymeric blending fire retardant precursor according to claim 1, it is characterised in that: main
Wanting raw material further includes 1~4 parts by weight of solubilizer.
6. the preparation method of multicomponent polymeric blending fire retardant precursor according to claim 5, it is characterised in that: the increasing
Solvent selects polycaprolactone.
7. the preparation method of multicomponent polymeric blending fire retardant precursor according to claim 1, it is characterised in that: described third
Alkene nitrile-methyl acrylate copoly resin can also the acrylic fiber made of acrylonitrile-methylacrylate copolymer resins spinning
Instead of.
8. the preparation method of multicomponent polymeric blending fire retardant precursor according to claim 1, it is characterised in that: it is main
Raw material and content are as follows:
Vinyl chloride-vinyl acetate is copolymerized paste resin 11~12
Acrylonitrile-methylacrylate copolymer resins 11~12
Solvent 70~79
Unit is parts by weight.
9. a kind of multicomponent polymeric blending fire retardant precursor, it is characterised in that: pass through multiple groups a method as claimed in any one of claims 1-8
The preparation method of polymer blending fire retardant precursor is divided to be made.
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| CN201811471898.5A CN109537099A (en) | 2018-12-04 | 2018-12-04 | A kind of multicomponent polymeric blending fire retardant precursor and preparation method thereof |
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| US5306437A (en) * | 1991-11-30 | 1994-04-26 | Hoechst Aktiengesellschaft | Copolymers and their use as lubricants and release agents for processing thermoplastics |
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| CN101113211A (en) * | 2007-07-17 | 2008-01-30 | 中国石油化工股份有限公司 | Combustion inhibitor and preparing method and flame-proof acrylic fibre using the same |
| CN102352537A (en) * | 2011-08-16 | 2012-02-15 | 黑龙江大学 | Coagulation-bath-free spinning method of polyacrylonitrile-based carbon fiber protofilament |
| CN102560747A (en) * | 2011-12-11 | 2012-07-11 | 武汉纺织大学 | Preparation method of durable low-smoke halogen-free flame-retardant polyacrylonitrile fiber |
| CN102677191A (en) * | 2011-10-31 | 2012-09-19 | 中原工学院 | Preparation method of hair protein fiber spinning solution |
| CN103124812A (en) * | 2010-10-06 | 2013-05-29 | 株式会社钟化 | Fiber for artificial hair, and hair accessory formed from same |
| CN108330563A (en) * | 2017-12-08 | 2018-07-27 | 吉林奇峰化纤股份有限公司 | A kind of acrylic fiber and preparation method thereof |
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2018
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Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5306437A (en) * | 1991-11-30 | 1994-04-26 | Hoechst Aktiengesellschaft | Copolymers and their use as lubricants and release agents for processing thermoplastics |
| CN1911974A (en) * | 2006-06-26 | 2007-02-14 | 余天石 | Synthesis method of acrylonitrile and chloroethylene copolymer |
| CN101113211A (en) * | 2007-07-17 | 2008-01-30 | 中国石油化工股份有限公司 | Combustion inhibitor and preparing method and flame-proof acrylic fibre using the same |
| CN103124812A (en) * | 2010-10-06 | 2013-05-29 | 株式会社钟化 | Fiber for artificial hair, and hair accessory formed from same |
| CN102352537A (en) * | 2011-08-16 | 2012-02-15 | 黑龙江大学 | Coagulation-bath-free spinning method of polyacrylonitrile-based carbon fiber protofilament |
| CN102677191A (en) * | 2011-10-31 | 2012-09-19 | 中原工学院 | Preparation method of hair protein fiber spinning solution |
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| CN108330563A (en) * | 2017-12-08 | 2018-07-27 | 吉林奇峰化纤股份有限公司 | A kind of acrylic fiber and preparation method thereof |
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