CN109183174A - A kind of flame-retardant conductive fiber and preparation method thereof - Google Patents
A kind of flame-retardant conductive fiber and preparation method thereof Download PDFInfo
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- CN109183174A CN109183174A CN201810759860.1A CN201810759860A CN109183174A CN 109183174 A CN109183174 A CN 109183174A CN 201810759860 A CN201810759860 A CN 201810759860A CN 109183174 A CN109183174 A CN 109183174A
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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
- D01F6/44—Monocomponent 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
- D01F6/54—Monocomponent 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 polymers of unsaturated nitriles
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/42—Nitriles
- C08F120/44—Acrylonitrile
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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
- 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
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static 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
- 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
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- Polymers & Plastics (AREA)
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of flame-retardant conductive fibers, it is composed of the following raw materials by weight: ammonium polyphosphate, antimony oxide, carbon nanotube that ammonium polyphosphate 2-4, acrylonitrile 110-130, dibenzoyl peroxide 3-4, oleic acid diethyl amide 1-2, fire-retardant amide solution 200-240, calcium stearate 1-2, the silane coupling agent kh550 0.7-1 present invention are added can act as good flame retardant property, it can be improved the safety in utilization of fiber, and carbon nanotube then has good conductive stability, to improve the comprehensive performance of finished product.
Description
Technical field
The invention belongs to fiber arts, and in particular to a kind of flame-retardant conductive fiber and preparation method thereof.
Background technique
Conductive fiber is a kind of new fiber species occurred the 1960s, this fiber has good electric conductivity
And durability, especially still there is good durable antistatic under the low humidity, therefore have very in the fields such as industrial, civilian
Big purposes；However, improving the fire line of conductive fiber now with the continuous enhancing of people's awareness of safety, enhancing uses peace
Full performance is the emphasis studied at present.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of flame-retardant conductive fiber and its preparations
Method.
To achieve the above object, the invention adopts the following technical scheme:
A kind of flame-retardant conductive fiber, it is composed of the following raw materials by weight:
Ammonium polyphosphate 2-4, acrylonitrile 110-130, dibenzoyl peroxide 3-4, oleic acid diethyl amide 1-2, fire-retardant acyl
Amine aqueous solution 200-240, calcium stearate 1-2, silane coupling agent kh550 0.7-1.
The fire-retardant amide solution is made of following weight parts:
Antimony oxide 2-7, dimethylformamide 100-130, carbon nanotube 24-30, acrylamide 10-15, persulfuric acid
Ammonium 0.2-0.4, stearic acid 1-2, pentaerythrite 3-4.
The preparation method of the fire-retardant amide solution, comprising the following steps:
(1) carbon nanotube is taken, in sulfuric acid solution that be added to 20-30 times of its weight, 96-98%, ultrasonic 10-14 is small
When, precipitating is washed, is mixed with stearic acid by filtering, is sent into baking oven, and 1-2 hours dry at 70-80 DEG C, discharging cooling obtains
It is acidified carbon nanotube；
(2) ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly；
(3) antimony oxide, acrylamide mixing are taken, is added in the deionized water of 10-15 times of mixture weight, stirs
Uniformly, it is sent in reaction kettle, is passed through nitrogen, pentaerythrite is added, adjusting temperature of reaction kettle is 65-70 DEG C, and above-mentioned mistake is added
Ammonium sulfate solution, insulated and stirred 4-5 hours, discharging cooling obtained polymer solution；
(4) acidification carbon nanotube is taken, is added in above-mentioned polymer solution, stirs evenly, increasing temperature is 90-95 DEG C,
It insulated and stirred 2-3 hours, filters, filter cake is washed, air drying obtains composite carbon nanometer tube；
(5) above-mentioned composite carbon nanometer tube is taken, is added to dimethylformamide, ultrasonic 1-2 hours to get the fire-retardant amide
Solution.
A kind of preparation method of flame-retardant conductive fiber, comprising the following steps:
(1) calcium stearate is taken, is added in the dehydrated alcohol of 4-10 times of its weight, dibenzoyl peroxide, stirring is added
Uniformly, alcoholic solution is obtained；
(2) ammonium polyphosphate is taken, is added in the deionized water of 13-20 times of its weight, stirs evenly；
(3) acrylonitrile, silane coupling agent kh550 mixing are taken, is added in 10-14 times of deionized water of mixture weight, stirs
It mixes uniformly, is sent in reaction kettle, is passed through nitrogen, above-mentioned alcoholic solution is added, adjusting temperature of reaction kettle is 65-70 DEG C, is added poly-
Ammonium phosphate solution, insulated and stirred 4-5 hours, discharging cooling obtained polypropylene solution；
(4) oleic acid diethyl amide is taken, is added in above-mentioned polypropylene solution, 1-2 hours ultrasonic, filtering will precipitate water
It washes, air drying obtains modified polyacrylonitrile；
(5) above-mentioned modified polyacrylonitrile is taken, is added in fire-retardant amide solution, stirs evenly, spinning is to get described fire-retardant
Conductive fiber.
Advantages of the present invention:
In fire-retardant amide solution of the invention, carbon nanotube acidification is handled first, then using acrylamide as monomer, is led to
It crosses polymerization and intercalation modifying is carried out to carbon nanotube, be blended later with pentaerythrite, high temperature esterification, improve the surface of carbon nanotube
Activity, so as to improve its dispersibility between dimethylformamide；
Ammonium polyphosphate that the present invention is added, antimony oxide, carbon nanotube can act as good flame retardant property, can
The safety in utilization of fiber is improved, and carbon nanotube then has good conductive stability, to improve the comprehensive of finished product
Energy.
Specific embodiment
Embodiment 1
A kind of flame-retardant conductive fiber, it is composed of the following raw materials by weight:
Ammonium polyphosphate 4, acrylonitrile 130, dibenzoyl peroxide 4, oleic acid diethyl amide 2, fire-retardant amide solution 240,
Calcium stearate 2, silane coupling agent kh550 1.
The fire-retardant amide solution is made of following weight parts:
Antimony oxide 7, dimethylformamide 130, carbon nanotube 30, acrylamide 15, ammonium persulfate 0.4, stearic acid
2, pentaerythrite 4.
The preparation method of the fire-retardant amide solution, comprising the following steps:
(1) carbon nanotube is taken, is added in 30 times of its weight, 98% sulfuric acid solution, ultrasound 14 hours filters, will
Precipitating washing, mixes with stearic acid, is sent into baking oven, 2 hours dry at 80 DEG C, and discharging cooling obtains acidification carbon nanotube；
(2) ammonium persulfate is taken, is added in the deionized water of 30 times of its weight, stirs evenly；
(3) antimony oxide, acrylamide mixing are taken, is added in 15 times of mixture weight of deionized water, stirring is equal
It is even, it is sent in reaction kettle, is passed through nitrogen, pentaerythrite is added, adjusting temperature of reaction kettle is 70 DEG C, and above-mentioned ammonium persulfate is added
Aqueous solution, insulated and stirred 5 hours, discharging cooling obtained polymer solution；
(4) acidification carbon nanotube is taken, is added in above-mentioned polymer solution, stirs evenly, increasing temperature is 95 DEG C, heat preservation
Stirring 3 hours is filtered, filter cake is washed, air drying obtains composite carbon nanometer tube；
(5) above-mentioned composite carbon nanometer tube is taken, dimethylformamide is added to, ultrasound 2 hours molten to get the fire-retardant amide
Liquid.
A kind of preparation method of flame-retardant conductive fiber, comprising the following steps:
(1) calcium stearate is taken, is added in the dehydrated alcohol of 10 times of its weight, dibenzoyl peroxide is added, stirring is equal
It is even, obtain alcoholic solution；
(2) ammonium polyphosphate is taken, is added in the deionized water of 20 times of its weight, stirs evenly；
(3) acrylonitrile, silane coupling agent kh550 mixing are taken, is added in 14 times of deionized waters of mixture weight, stirring is equal
It is even, it is sent in reaction kettle, is passed through nitrogen, above-mentioned alcoholic solution is added, adjust 70 DEG C of temperature of reaction kettle, it is water-soluble that ammonium polyphosphate is added
Liquid, insulated and stirred 5 hours, discharging cooling obtained polypropylene solution；
(4) oleic acid diethyl amide is taken, is added in above-mentioned polypropylene solution, precipitating is washed in ultrasound 2 hours, filtering,
Air drying obtains modified polyacrylonitrile；
(5) above-mentioned modified polyacrylonitrile is taken, is added in fire-retardant amide solution, stirs evenly, spinning is to get described fire-retardant
Conductive fiber.
Embodiment 2
A kind of flame-retardant conductive fiber, it is composed of the following raw materials by weight:
Ammonium polyphosphate 2, acrylonitrile 110, dibenzoyl peroxide 3, oleic acid diethyl amide 1, fire-retardant amide solution 200,
Calcium stearate 1, silane coupling agent kh550 0.7.
The fire-retardant amide solution is made of following weight parts:
Antimony oxide 2, dimethylformamide 100, carbon nanotube 24, acrylamide 10, ammonium persulfate 0.2, stearic acid
1, pentaerythrite 3.
The preparation method of the fire-retardant amide solution, comprising the following steps:
(1) carbon nanotube is taken, is added in 20 times of its weight, 96% sulfuric acid solution, ultrasound 10 hours filters, will
Precipitating washing, mixes with stearic acid, is sent into baking oven, 1 hour dry at 70 DEG C, and discharging cooling obtains acidification carbon nanotube；
(2) ammonium persulfate is taken, is added in the deionized water of 20 times of its weight, stirs evenly；
(3) antimony oxide, acrylamide mixing are taken, is added in 10 times of mixture weight of deionized water, stirring is equal
It is even, it is sent in reaction kettle, is passed through nitrogen, pentaerythrite is added, adjusting temperature of reaction kettle is 65 DEG C, and above-mentioned ammonium persulfate is added
Aqueous solution, insulated and stirred 4 hours, discharging cooling obtained polymer solution；
(4) acidification carbon nanotube is taken, is added in above-mentioned polymer solution, stirs evenly, increasing temperature is 90 DEG C, heat preservation
Stirring 2 hours is filtered, filter cake is washed, air drying obtains composite carbon nanometer tube；
(5) above-mentioned composite carbon nanometer tube is taken, dimethylformamide is added to, ultrasound 1 hour molten to get the fire-retardant amide
Liquid.
A kind of preparation method of flame-retardant conductive fiber, comprising the following steps:
(1) calcium stearate is taken, is added in the dehydrated alcohol of 4 times of its weight, dibenzoyl peroxide is added, stirring is equal
It is even, obtain alcoholic solution；
(2) ammonium polyphosphate is taken, is added in the deionized water of 13 times of its weight, stirs evenly；
(3) acrylonitrile, silane coupling agent kh550 mixing are taken, is added in 10 times of deionized waters of mixture weight, stirring is equal
It is even, it is sent in reaction kettle, is passed through nitrogen, above-mentioned alcoholic solution is added, adjusting temperature of reaction kettle is 65 DEG C, and ammonium polyphosphate water is added
Solution, insulated and stirred 4 hours, discharging cooling obtained polypropylene solution；
(4) oleic acid diethyl amide is taken, is added in above-mentioned polypropylene solution, precipitating is washed in ultrasound 1 hour, filtering,
Air drying obtains modified polyacrylonitrile；
(5) above-mentioned modified polyacrylonitrile is taken, is added in fire-retardant amide solution, stirs evenly, spinning is to get described fire-retardant
Conductive fiber.
The conductivity range of antibacterial conductive fiber of the invention is 3.0-4.0S/m, fiber strength 3.0-3.9cn/
Dtex, oxygen index (OI) 29-31, UL-94 are V-1 rank.
Claims (4)
1. a kind of flame-retardant conductive fiber, which is characterized in that it is composed of the following raw materials by weight:
Ammonium polyphosphate 2-4, acrylonitrile 110-130, dibenzoyl peroxide 3-4, oleic acid diethyl amide 1-2, fire-retardant amide are molten
Liquid 200-240, calcium stearate 1-2, silane coupling agent kh550 0.7-1.
2. a kind of flame-retardant conductive fiber according to claim 1, which is characterized in that the fire-retardant amide solution is under
State the composition of parts by weight:
Antimony oxide 2-7, dimethylformamide 100-130, carbon nanotube 24-30, acrylamide 10-15, ammonium persulfate
0.2-0.4, stearic acid 1-2, pentaerythrite 3-4.
3. a kind of flame-retardant conductive fiber according to claim 2, which is characterized in that the preparation of the fire-retardant amide solution
Method, comprising the following steps:
(1) carbon nanotube is taken, 10-14 hours ultrasonic in sulfuric acid solution that be added to 20-30 times of its weight, 96-98%, mistake
Precipitating is washed, is mixed with stearic acid by filter, is sent into baking oven, 1-2 hours dry at 70-80 DEG C, and discharging cooling must be acidified
Carbon nanotube；
(2) ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly；
(3) antimony oxide, acrylamide mixing are taken, is added in the deionized water of 10-15 times of mixture weight, stirring is equal
It is even, it is sent in reaction kettle, is passed through nitrogen, pentaerythrite is added, adjusting temperature of reaction kettle is 65-70 DEG C, and above-mentioned over cure is added
Sour aqueous ammonium, insulated and stirred 4-5 hours, discharging cooling obtained polymer solution；
(4) acidification carbon nanotube is taken, is added in above-mentioned polymer solution, stirs evenly, increasing temperature is 90-95 DEG C, heat preservation
Stirring 2-3 hours is filtered, filter cake is washed, air drying obtains composite carbon nanometer tube；
(5) above-mentioned composite carbon nanometer tube is taken, dimethylformamide is added to, ultrasonic 1-2 hours molten to get the fire-retardant amide
Liquid.
4. a kind of preparation method of flame-retardant conductive fiber as described in claim 1, which comprises the following steps:
(1) calcium stearate is taken, is added in the dehydrated alcohol of 4-10 times of its weight, dibenzoyl peroxide is added, stirs evenly,
Obtain alcoholic solution；
(2) ammonium polyphosphate is taken, is added in the deionized water of 13-20 times of its weight, stirs evenly；
(3) acrylonitrile, silane coupling agent kh550 mixing are taken, is added in 10-14 times of deionized water of mixture weight, stirring is equal
It is even, it is sent in reaction kettle, is passed through nitrogen, above-mentioned alcoholic solution is added, adjusting temperature of reaction kettle is 65-70 DEG C, and polyphosphoric acid is added
Aqueous ammonium, insulated and stirred 4-5 hours, discharging cooling obtained polypropylene solution；
(4) oleic acid diethyl amide is taken, is added in above-mentioned polypropylene solution, 1-2 hours ultrasonic, filtering washes precipitating, often
Temperature is dry, obtains modified polyacrylonitrile；
(5) above-mentioned modified polyacrylonitrile is taken, is added in fire-retardant amide solution, stirs evenly, spinning is to get the flame-retardant conductive
Fiber.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810759860.1A CN109183174A (en) | 2018-07-11 | 2018-07-11 | A kind of flame-retardant conductive fiber and preparation method thereof |
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| CN201810759860.1A CN109183174A (en) | 2018-07-11 | 2018-07-11 | A kind of flame-retardant conductive fiber and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1455034A (en) * | 2002-04-29 | 2003-11-12 | 中国石油化工股份有限公司 | Fire resistant acrylonitrile copolymer fiber and manufacturing method thereof |
| CN104710564A (en) * | 2015-03-26 | 2015-06-17 | 天津工业大学 | Method for preparing flame-retardant acrylonitrile copolymer |
-
2018
- 2018-07-11 CN CN201810759860.1A patent/CN109183174A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1455034A (en) * | 2002-04-29 | 2003-11-12 | 中国石油化工股份有限公司 | Fire resistant acrylonitrile copolymer fiber and manufacturing method thereof |
| CN104710564A (en) * | 2015-03-26 | 2015-06-17 | 天津工业大学 | Method for preparing flame-retardant acrylonitrile copolymer |
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Application publication date: 20190111 |