CN105887482B - A kind of preparation method of the fire-retardant polyacrylonitrile fire resistance fibre containing high vertical structure polyacrylonitrile - Google Patents
A kind of preparation method of the fire-retardant polyacrylonitrile fire resistance fibre containing high vertical structure polyacrylonitrile Download PDFInfo
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- CN105887482B CN105887482B CN201610294975.9A CN201610294975A CN105887482B CN 105887482 B CN105887482 B CN 105887482B CN 201610294975 A CN201610294975 A CN 201610294975A CN 105887482 B CN105887482 B CN 105887482B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/402—Amides imides, sulfamic acids
- D06M13/432—Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/68—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/70—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
- D06M15/256—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons containing fluorine
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
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- Chemical & Material Sciences (AREA)
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- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The present invention relates to a kind of preparation methods of polyacrylonitrile-based flame-retardant fiber, it is the polyacrylonitrile fibre of 30~50wt% at a temperature of 60~80 DEG C by high vertical structure polyacrylonitrile content, it immerses in the mixed solution of modifying agent and hypophosphorous acid, carry out 2~5h of chemical modification, apply the drawing-off of+13~+20% elongation in modifying process to fiber simultaneously, modified polyacrylonitrile acrylic fiber is impregnated to be dried in air medium, obtain modified polyacrylonitrile acrylic fiber, modified polyacrylonitrile acrylic fiber is pre-oxidized again, obtain polyacrylonitrile-based flame-retardant fiber, the modifying agent is 1- (4- fluorophenyl) biguanide hydrochloride, the ethylene glycol solution of lignosulfonates and poly- ethylene fluoride, the tensile strength of obtained polyacrylonitrile-based flame-retardant fiber is high, and good flame retardation effect, its tensile strength is up to 3 GPa, limited oxygen index is 50 or more.
Description
Technical field
The present invention relates to a kind of preparation methods of polyacrylonitrile-based flame-retardant fiber, are prepared with polyacrylonitrile acrylic fibers precursor fire-retardant
Fiber.
Background technique
Naturally occurring or synthetic fiber, since its different flammability of its chemical structure are also different, ignite when by burning degree, combustion
The features such as speed, breath combustion property are burnt, fiber can be qualitatively divided into fire resistance fibre and non-flame resistant fiber two major classes.It is wide in the world at present
The general combustibility that fiber and its products are characterized using limited oxygen index LOI (Limit Oxygen Index).Limited oxygen index LOI value
Bigger, the concentration of requisite oxygen is higher when material combustion, i.e. more difficult to burn.In usual air the volume fraction of oxygen close to 20 so
Fiber can also classify by LOI value, and LOI value is known as flammable fiber, 20~30 referred to as fire resistance fibre lower than 20.
Polyacrylonitrile-based flame-retardant fiber is former generally by extraordinary polyacrylonitrile used in carbon fiber preparation is specialized at present
Silk is washed, prepared by segmentation two steps of pre-oxidation, since the group of the main copolymer of extraordinary polyacrylonitrile fibril becomes third
Alkene nitrile and itaconic acid, need special process to prepare, and preparation cost is high.To reduce cost, the general industry of lower price is selected to use
Polyacrylonitrile acrylic fiber prepares fire resistance fibre, and the general industry is acrylonitrile, acrylic acid with acrylic fiber main component
Methyl esters and sodium styrene sulfonate, it is highly exothermic during being pre-oxidized although the more extraordinary precursor of its cost is low, it makes
It is molten simultaneously at fiber, it is hardened, phenomena such as mechanical property reduces.Limit oxygen currently with the fire resistance fibre of common acrylic fiber preparation refers to
Number (LOI) can only achieve 25-30, and mechanical property is only capable of reaching 0.20GPa or less.And it is former for carbon fiber Wesy special type polyacrylonitrile acrylic fibers
The fire resistance fibre of silk preparation, limited oxygen index and mechanical property can respectively reach 30 and 0.2GPa or more.There is document using CuCl pairs
Carbon fiber Wesy polyacrylonitrile special fibre is handled (Guangdong chemical fibre, 1999, the 12nd phase), reduces fiber and oxidation occurs instead
The initial temperature answered improves the exothermicity of fiber.But this method is since modifying agent is for the oxidation process of industrial acrylic fibers
Apparent facilitation cannot be played, so modified effect is not obvious, and the complex process equipment, is unfavorable for industrial metaplasia
It produces.
103451913 A of CN discloses a kind of preparation method of polypropylene-base fire resistance fibre, using the vertical structure polyacrylonitrile of height
The polyacrylonitrile fibre that content is 30wt~50wt% is raw material, by fiber at a temperature of 45~110 DEG C, in ZnCl2With acid
It impregnates, carries out chemical modification 1~10 minute in mixed aqueous solution modifying agent, 0~+10% is applied to fiber simultaneously in modifying process
The drawing-off of elongation impregnates modified polyacrylonitrile acrylic fiber in air medium at 80~140 DEG C, carries out 1~10
The drying process of minute obtains modified polyacrylonitrile acrylic fiber, then modified polyacrylonitrile acrylic fiber is pre-oxidized, and obtains
To polyacrylonitrile-based flame-retardant fiber.The polyacrylonitrile-based flame-retardant fiber being prepared, at low cost, tensile strength reaches 0.2GPa
More than, limited oxygen index reaches 40 or more.But the tensile strength and flame retardant property are still relatively poor, are not able to satisfy practical application
In demand.
Summary of the invention
For the above-mentioned problems in the prior art, the purpose of the present invention is to provide one kind have high tensile and
The preparation method of the polypropylene-base fire resistance fibre of flame retardant property.
In order to achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of polypropylene-base fire resistance fibre is poly- the third of 30~50wt% with high vertical structure polyacrylonitrile content
Alkene nitrile fiber is that raw material impregnates in the mixed solution of modifying agent and hypophosphorous acid by the fiber at a temperature of 60~80 DEG C, is carried out
2~5h of chemical modification applies the drawing-off of+13~+20% elongation, dipping modified poly- third in modifying process to fiber simultaneously
Alkene nitrile acrylic fiber at 80~140 DEG C, carries out drying process in 1~10 minute in air medium, obtains modified polypropene
Nitrile acrylic fiber, then modified polyacrylonitrile acrylic fiber is pre-oxidized, obtain polyacrylonitrile-based flame-retardant fiber.
Modifying agent of the present invention is the second of 1- (4- fluorophenyl) biguanide hydrochloride, lignosulfonates and poly- ethylene fluoride
Glycol solution.
Below as the optimal technical scheme of the method for the invention, but not as limitation of the present invention.
Preferably, the content of each component is in the modifying agent
In this optimal technical scheme, the content of 1- (4- fluorophenyl) biguanide hydrochloride is 30~45 weight in the modifying agent
Part, it may be, for example, 30 parts by weight, 35 parts by weight, 38 parts by weight, 40 parts by weight or 45 parts by weight etc..
In this optimal technical scheme, the content of lignosulfonates is 10~15 parts by weight in the modifying agent, such as can
For 10 parts by weight, 12 parts by weight, 13 parts by weight, 14 parts by weight or 15 parts by weight etc..
In this optimal technical scheme, the content of poly- ethylene fluoride is 5~8 parts by weight in the modifying agent, may be, for example, 5 weights
Measure part, 6 parts by weight, 6.5 parts by weight, 7 parts by weight or 8 parts by weight etc..
In this optimal technical scheme, the content of ethylene glycol is 75~100 parts by weight in the modifying agent, may be, for example, 75 weights
Measure part, 80 parts by weight, 82 parts by weight, 85 parts by weight, 90 parts by weight or 100 parts by weight etc..
As further optimal technical scheme, the content of each component is in the modifying agent
Further, the content of each component is in the modifying agent
Preferably, the mass ratio of the modifying agent and hypophosphorous acid is (3~5): 1, it may be, for example, 3:1,3.5:1,4:1 or 5:
1 etc..
In method of the invention, before general industry polyacrylonitrile fiber by modification of acrylics, preferably first by fiber 50~98
Water-washing pre-treatment is carried out in DEG C water bath with thermostatic control, is removed fiber surface and is remained finish.
In method of the invention, the preoxidation process is conventional process, by modified fiber 190~
It is pre-oxidized at 280 DEG C, pre-oxidation atmosphere is air.Apply the drawing-off of 0~+20% elongation altogether.Preoxidation time is 60
~120 minutes.
In method of the invention, the polyacrylonitrile acrylic fiber is using dry method, wet process or wet-dry change copolymerization spinning
Made of general industry acrylic fiber.Wherein in mass of fibers monofilament hole count be 1~320k, filament number be 0.5~
3.0dex, acrylonitrile monemer mass content is not less than 90% in polyacrylonitrile acrylic fiber, can also contain 10% mass content
One or more copolymers below, such as acrylic acid, methacrylic acid, methyl methacrylate, methyl acrylate, hydroxyalkyl third
Alkene nitrile, hydroxyalkyl acrylic acid and its esters, the present invention are applicable.The invention is also applied for 1~320k, filament number 0.5
The carbon fiber special fiber of~3.0dex, and the method for modifying has a degree of change for the hot property of special fibre
It is kind.
Compared with the prior art, the invention has the following advantages:
The present invention uses unique formula of modifier, and mixes with suitable hypophosphorous acid, to polyacrylonitrile fibre raw material into
Row chemical modification cooperates suitable process and parameter, and the tensile strength for the polyacrylonitrile-based flame-retardant fiber being prepared is high,
And good flame retardation effect, tensile strength is up to 3GPa, and limited oxygen index is 50 or more.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.
Embodiment 1
Using high vertical structure polyacrylonitrile content for 35wt% polyacrylonitrile copolymer fibre as raw material, monofilament hole count is
12000 12K, fiber copolymer composition is: acrylonitrile monemer 90wt%, vinylacetate 8wt%, methyl-propane sulfonic acid sodium
Fiber is immersed in the mixed solution of modifying agent and hypophosphorous acid (mass ratio of modifying agent and hypophosphorous acid is 3:1), solution by 2wt%
Temperature 60 C, modification time 5h.By modified polyacrylonitrile fibre in air medium at 80 DEG C, carry out 5 minutes
It is dried.Fiber is pre-oxidized at 200~280 DEG C, and pre-oxidation atmosphere is air, is divided four sections and is heated up.Apply altogether
9% drawing-off.Polyacrylonitrile-based flame-retardant fiber is made.
The content of each component is in modifying agent in the present embodiment
Performance detection, tensile strength 2.5GPa, limit are carried out to the polyacrylonitrile-based flame-retardant fiber that the present embodiment obtains
Oxygen index (OI) is 52.
Embodiment 2
Acrylic fiber used is the same as embodiment 1.Fiber is immersed in the mixed solution of modifying agent and hypophosphorous acid (modifying agent and time
The mass ratio of phosphoric acid is 5:1), 80 DEG C of solution temperature, modification time 2h.By modified polyacrylonitrile fibre in air dielectric
In at 80 DEG C, carry out drying process in 5 minutes.Fiber obtained carries out pre- oxygen under the pre-oxidizing conditions in such as example 1
Change, polyacrylonitrile-based flame-retardant fiber is made.
The content of each component is in modifying agent in the present embodiment
Performance detection, tensile strength 2.3GPa, limit are carried out to the polyacrylonitrile-based flame-retardant fiber that the present embodiment obtains
Oxygen index (OI) is 54.
Embodiment 3
Acrylic fiber used is the same as embodiment 1.Fiber is immersed in the mixed solution of modifying agent and hypophosphorous acid, solution temperature 70
DEG C, modification time 3.5h.By modified polyacrylonitrile fibre in air medium at 80 DEG C, drying in 5 minutes is carried out
Processing.Fiber obtained is pre-oxidized under the pre-oxidizing conditions in such as example 1, and polyacrylonitrile-based flame-retardant fiber is made.
The content of each component is in modifying agent in the present embodiment
Performance detection, tensile strength 3.0GPa, limit are carried out to the polyacrylonitrile-based flame-retardant fiber that the present embodiment obtains
Oxygen index (OI) is 60.
Comparative example 1
In addition to the mixed solution for replacing modifying agent and hypophosphorous acid with deionized water, other preparation methods and condition and embodiment
1 is identical.
The pan based fibers of this comparative example are detected, tensile strength 0.1GPa, limited oxygen index is 30.
Comparative example 2
In addition to the mixed solution for writing on one's behalf modifying agent and hypophosphorous acid with hypophosphorous acid, other preparation methods and condition and embodiment 1
It is identical.
The pan based fibers of this comparative example are detected, tensile strength 1.0GPa, limited oxygen index is 35.
Comparative example 3
In addition to the mixed solution for using modifying agent to replace modifying agent and hypophosphorous acid, the types of other each components, content and
Preparation method and condition are same as Example 1.
The pan based fibers of this comparative example are detected, tensile strength 1.3GPa, limited oxygen index is 49.
The Applicant declares that the present invention is explained by the above embodiments method detailed of the invention, but the present invention not office
Be limited to above-mentioned method detailed, that is, do not mean that the invention must rely on the above detailed methods to implement.Technical field
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, selection of concrete mode etc., all of which fall within the scope of protection and disclosure of the present invention.
Claims (9)
1. a kind of preparation method of polyacrylonitrile-based flame-retardant fiber, which is characterized in that with the vertical structure polyacrylonitrile content of height be 30~
The polyacrylonitrile fibre of 50wt% is raw material, molten in the mixing of modifying agent and hypophosphorous acid by the fiber at a temperature of 60~80 DEG C
It is impregnated in liquid, carries out 2~5h of chemical modification, apply the drawing-off of+13~+20% elongation, leaching in modifying process to fiber simultaneously
The modified polyacrylonitrile acrylic fiber of stain at 80~140 DEG C, carries out drying process in 1~10 minute in air medium,
Modified polyacrylonitrile acrylic fiber is obtained, then modified polyacrylonitrile acrylic fiber is pre-oxidized, obtains polyacrylonitrile-radical resistance
Fiber is fired,
Wherein, the modifying agent is the second two of 1- (4- fluorophenyl) biguanide hydrochloride, lignosulfonates and poly- ethylene fluoride
Alcoholic solution.
2. preparation method according to claim 1, which is characterized in that the content of each component in the modifying agent are as follows:
3. preparation method according to claim 1, which is characterized in that the content of each component in the modifying agent are as follows:
4. preparation method according to claim 1, which is characterized in that the content of each component in the modifying agent are as follows:
5. preparation method according to claim 1, which is characterized in that the mass ratio of the modifying agent and hypophosphorous acid be (3~
5):1。
6. preparation method according to claim 1, which is characterized in that the polyacrylonitrile acrylic fiber passes through in 50-
Pretreatment 0.5-3 minutes is carried out in 98 DEG C of waters bath with thermostatic control.
7. preparation method according to claim 1, which is characterized in that the preoxidation process is by modified poly- third
Alkene nitrile acrylic fiber is pre-oxidized at 190~280 DEG C, and pre-oxidation atmosphere is air, applies 0~+20% elongation altogether
Drawing-off, preoxidation time are 60~120 minutes.
8. preparation method according to claim 1, which is characterized in that the polyacrylonitrile acrylic fiber is using dry
Method, wet process or wet-dry change spin, and acrylonitrile monemer mass content is not less than 90% in precursor.
9. preparation method according to claim 1, which is characterized in that the polyacrylonitrile acrylic fiber wherein a branch of fibre
Monofilament hole count is 1~320k in tieing up, and filament number is 0.5~3.0dex.
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| CN201610294975.9A CN105887482B (en) | 2016-05-05 | 2016-05-05 | A kind of preparation method of the fire-retardant polyacrylonitrile fire resistance fibre containing high vertical structure polyacrylonitrile |
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| CN201610294975.9A CN105887482B (en) | 2016-05-05 | 2016-05-05 | A kind of preparation method of the fire-retardant polyacrylonitrile fire resistance fibre containing high vertical structure polyacrylonitrile |
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| CN107460738B (en) * | 2017-08-25 | 2019-12-17 | 中国科学院宁波材料技术与工程研究所 | Preparation method of polyacrylonitrile oxidized fiber felt |
| CN109930383A (en) * | 2019-03-21 | 2019-06-25 | 江苏理工学院 | A kind of method of polyacrylonitrile fibre material oxidation |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1777715A (en) * | 2003-02-21 | 2006-05-24 | 罗地安尼尔公司 | Fire-resistant threads, fibres, filaments and textile articles |
| CN101845749A (en) * | 2010-05-05 | 2010-09-29 | 山东理工大学 | Method for producing inflaming retarding modified nitrilon |
| CN101851857A (en) * | 2010-05-05 | 2010-10-06 | 山东理工大学 | Flame retarding modification preparation method of acrylic yarn, acrylic knitting yarn or acrylic woolen yarn |
| CN103451913A (en) * | 2013-08-15 | 2013-12-18 | 苏州龙杰特种纤维股份有限公司 | Preparation method of flame-retardant polyacrylonitrile flame-retardant fiber containing high-stereotacticity polyacrylonitrile |
| CN104532576A (en) * | 2014-12-23 | 2015-04-22 | 李哲 | Processing technology for high-temperature-resistant fabric |
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- 2016-05-05 CN CN201610294975.9A patent/CN105887482B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1777715A (en) * | 2003-02-21 | 2006-05-24 | 罗地安尼尔公司 | Fire-resistant threads, fibres, filaments and textile articles |
| CN101845749A (en) * | 2010-05-05 | 2010-09-29 | 山东理工大学 | Method for producing inflaming retarding modified nitrilon |
| CN101851857A (en) * | 2010-05-05 | 2010-10-06 | 山东理工大学 | Flame retarding modification preparation method of acrylic yarn, acrylic knitting yarn or acrylic woolen yarn |
| CN103451913A (en) * | 2013-08-15 | 2013-12-18 | 苏州龙杰特种纤维股份有限公司 | Preparation method of flame-retardant polyacrylonitrile flame-retardant fiber containing high-stereotacticity polyacrylonitrile |
| CN104532576A (en) * | 2014-12-23 | 2015-04-22 | 李哲 | Processing technology for high-temperature-resistant fabric |
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