CN110004704A - A kind of method of polyacrylonitrile fibre fire proofing pre-treatment - Google Patents
A kind of method of polyacrylonitrile fibre fire proofing pre-treatment Download PDFInfo
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- CN110004704A CN110004704A CN201910217471.0A CN201910217471A CN110004704A CN 110004704 A CN110004704 A CN 110004704A CN 201910217471 A CN201910217471 A CN 201910217471A CN 110004704 A CN110004704 A CN 110004704A
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- Prior art keywords
- polyacrylonitrile fibre
- fire proofing
- polyacrylonitrile
- treatment
- darkening process
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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
- D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/50—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with hydrogen peroxide or peroxides of metals; with persulfuric, permanganic, pernitric, percarbonic acids or their salts
-
- 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
- D06M11/58—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 nitrogen or compounds thereof, e.g. with nitrides
- D06M11/63—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 nitrogen or compounds thereof, e.g. with nitrides with hydroxylamine or hydrazine
-
- 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
- D06M13/10—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 oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/188—Monocarboxylic acids; Anhydrides, halides or salts thereof
-
- 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
-
- 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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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention belongs to polyacrylonitrile fibre fire proofing technical fields, and in particular to a kind of method of polyacrylonitrile fibre fire proofing pre-treatment, the following steps are included: (1) weighs, hydrazine hydrate, hydroxylamine chloride are soluble in water to be made modified solution to method；(2) polyacrylonitrile fibre is put into 30-60 DEG C of modified solution, to modifying polyacrylonitrile；(3) sodium acetate, ammonium acetate, potassium permanganate are weighed to be dissolved in acid solution, Darkening process liquid is made；(4) step (2) modified polyacrylonitrile fibre completed is put into impregnate in Darkening process liquid and carries out Darkening process, be then cleaned and dried to obtain the polyacrylonitrile fibre material through pre-treatment.The present invention can reduce the temperature of later period Darkening process by chemical modification, enhance flame retardant effect.
Description
Technical field
The invention belongs to polyacrylonitrile fibre fire proofing technical fields, and in particular to a kind of fire-retardant material of polyacrylonitrile fibre
Expect the method for pre-treatment.
Background technique
Polyacrylonitrile fibre is to be accounted for as polyacrylonitrile or acrylonitrile made from 85% or more copolymer, have it is soft,
Merrily and lightheartedly, bulk, easy dye, lovely luster, antibacterial, it is warming the advantages that, can pure spinning or natural fine according to the requirements of different purposes
It ties up blended, is widely used in the fields such as clothes, decoration.Conventional synthesis fiber is with polyester fiber, polypropylene fibre, polyvinyl alcohol
Based on several big kinds such as fiber, polyacrylonitrile fibre, Fypro, domestic technique level is generally suitable with foreign countries.In recent years
Come, domestic synthetic fiber product quality, technological innovation, structure optimization and in terms of achieve huge advance, but in height
The industrialization of high technical fibre material including the tencels such as performance fibers, biological fiber and differential, functionalization of new generation,
Engineering still has biggish gap with developed country with marketization aspect.Polyacrylonitrile fibre is used as and is only second to polyester and polyamide
The third-largest synthetic fibers kind, especially China possesses the maximum acrylic fibers consumption market in the whole world, has and greatly produces work
Skill optimization value and innovation and development space.
Patent ZL201710221401.3 is related to a kind of flame-resistant polyacrylonitrile fiber based on hydroxylamine hydrochloride chemical modification
Polyacrylonitrile fibre is sufficiently reacted preparation functional group containing oximido by preparation method with certain density hydroxylamine hydrochloride solution first
The modified acrylic fibre of oximate is carried out phosphatizing treatment by modification acrylonitrile fiber, and by treated, fiber wash is dried
Weighing obtains flame-resistant polyacrylonitrile fiber.Its disadvantage is exactly that technique is relatively complicated, needs to provide high temperature ring in preparation process
Border and processing time are long, and need to carry out catalytic action as catalyst by urea.
Summary of the invention
Invention broadly provides a kind of methods of polyacrylonitrile fibre fire proofing pre-treatment, can by chemical modification
The temperature of later period Darkening process is reduced, flame retardant effect is enhanced.Its technical solution is as follows:
A kind of method of polyacrylonitrile fibre fire proofing pre-treatment, comprising the following steps:
(1) weigh that hydrazine hydrate, hydroxylamine chloride are soluble in water to be made modified solution；
(2) polyacrylonitrile fibre is put into 30-60 DEG C of modified solution, to modifying polyacrylonitrile；
(3) sodium acetate, ammonium acetate, potassium permanganate are weighed to be dissolved in acid solution, Darkening process liquid is made；
(4) step (2) modified polyacrylonitrile fibre completed is put into impregnate in Darkening process liquid and carries out Darkening process, so
It is cleaned and dried to obtain the polyacrylonitrile fibre material through pre-treatment afterwards.
Preferably, the concentration of hydrazine hydrate is 0-5.9443g/L in step (1), and the concentration of hydroxylamine chloride is 0-3.3024g/
L。
Preferably, 0.5-2g polyacrylonitrile fibre is added in step (2) in every 100ml modified solution.
Preferably, sodium acetate 0-2g, ammonium acetate 0-1g, potassium permanganate 0- is added in step (3) in every 200ml acid solution
5g, the acid solution are the sulfuric acid solution of molar concentration 1-20%.
Preferably, the temperature that melanism is impregnated in step (4) is 60-80 DEG C, soaking time 2-4h.
Preferably, cleaning method is ultrasonic cleaning in step (4).
Using the above scheme, the invention has the following advantages that
The present invention carries out pre-treatment to polyacrylonitrile fibre fire proofing by the method for chemical modification, after effectively reducing
The temperature of phase Darkening process, treated before menstruation, and polyacrylonitrile fibre fire proofing flame retardant effect is excellent, stability is good, quality is equal
Even, easy processing, low cost, good colour.
Detailed description of the invention
Fig. 1, Fig. 2 are the SEM figure of the polyacrylonitrile fibre material handled under different times mirrors through embodiment 1.
Specific embodiment
Experimental method in following embodiment is conventional method unless otherwise required, related experiment reagent and material
Material is conventional biochemical reagent and material unless otherwise required.
Embodiment 1
The method of the present embodiment polyacrylonitrile fibre material pre-treatment are as follows:
(1) modified solution that total volume is 100mL is prepared, wherein hydrazine hydrate 3g/L, hydroxylamine chloride 3.3g/L, deionized water
68mL is placed in water-bath and is warming up to 50 DEG C, weighs 1.2g polyacrylonitrile fibre and is put into modified solution, carries out after modified 40min
Cleaning, drying；
(2) sulfuric acid solution of 200mL prepared 10% molar concentration is added in 250mL conical flask, with electronics day
It is flat to accurately weigh sodium acetate 1.6g, ammonium acetate 0.8g, potassium permanganate 4g and be put in conical flask, conical flask is put into ultrasonic 2min,
Dissolve each substance sufficiently；
(3) the Darkening process liquid that step (2) are prepared is warming up in water-bath 80 DEG C, then will be modified in step (1)
At polyacrylonitrile fibre be put into Darkening process liquid and impregnate 3h, it is cleaning, dry, then carry out combustion testing.Experimental result can
Know and burn the time up to 12s, illustrates that the polyacrylonitrile fibre flame retardant effect is good.
Fig. 1 is 20000 times of the polyacrylonitrile fibre surface SEM photograph that the present embodiment is prepared.It can be seen from SEM figure
The surface for examining out the polyacrylonitrile fibre prepared using 1 method of example forms one layer of fine and close reticular structure, reticular structure
The fire retardancy of polyacrylonitrile fibre can be enhanced in upper also part slight crack and block, the reticular structure of surface compact.
Fig. 2 is 5000 times of the polyacrylonitrile fibre surface SEM photograph that embodiment 1 prepares.It can be seen from SEM figure
The relatively small crackle in surface for the polyacrylonitrile fibre prepared using 1 method of example is examined out, and adheres to some blocks
The generation position of body, block is on slight crack, and block makes up negative effect brought by a part of crackle, to make the fibre
The flame retardant property of dimension does not decline with the generation of slight crack.
Embodiment 2
(1) prepare total volume be 100mL modified solution, wherein hydrazine hydrate 5.9443g/L, hydroxylamine chloride 0.6605g/L,
Deionized water 68mL is placed in water-bath and is warming up to 50 DEG C, weighs 1.2g polyacrylonitrile fibre and is put into modified solution, modified 40min
It cleaned, dried later；
(2) sulfuric acid solution of 200mL prepared 10% molar concentration is added in 250mL conical flask, with electronics day
It is flat to accurately weigh sodium acetate 1.6g, ammonium acetate 0.8g, potassium permanganate 4g and be put in conical flask, conical flask is put into ultrasonic 2min,
Dissolve each substance sufficiently；
(3) the Darkening process liquid that step (2) are prepared is warming up in water-bath 70 DEG C, then will be modified in step (1)
At polyacrylonitrile fibre be put into Darkening process liquid and impregnate 2.5h, it is cleaning, dry.
Embodiment 3
(1) prepare total volume be 100mL modified solution, wherein hydrazine hydrate 4.6234g/L, hydroxylamine chloride 1.3210g/L,
Deionized water 68mL is placed in water-bath and is warming up to 50 DEG C, weighs 1.2g polyacrylonitrile fibre and is put into modified solution, modified 40min
It cleaned, dried later；
(2) sulfuric acid solution of 200mL prepared 10% molar concentration is added in 250mL conical flask, with electronics day
It is flat to accurately weigh sodium acetate 1.6g, ammonium acetate 0.8g, potassium permanganate 4g and be put in conical flask, conical flask is put into ultrasonic 2min,
Dissolve each substance sufficiently；
(3) the Darkening process liquid that step (2) are prepared is warming up in water-bath 80 DEG C, then will be modified in step (1)
At polyacrylonitrile fibre be put into Darkening process liquid and impregnate 3h, it is cleaning, dry.
It will be apparent to those skilled in the art that can make various other according to the above description of the technical scheme and ideas
Corresponding change and deformation, and all these changes and deformation all should belong to the protection scope of the claims in the present invention
Within.
Claims (6)
1. a kind of method of polyacrylonitrile fibre fire proofing pre-treatment, it is characterised in that: the following steps are included:
(1) weigh that hydrazine hydrate, hydroxylamine chloride are soluble in water to be made modified solution；
(2) polyacrylonitrile fibre is put into 30-60 DEG C of modified solution, to modifying polyacrylonitrile；
(3) sodium acetate, ammonium acetate, potassium permanganate are weighed to be dissolved in acid solution, Darkening process liquid is made；
(4) step (2) modified polyacrylonitrile fibre completed is put into impregnate in Darkening process liquid and carries out Darkening process, then clearly
It washes and is dried to obtain the polyacrylonitrile fibre material through pre-treatment.
2. the method for polyacrylonitrile fibre fire proofing pre-treatment according to claim 1, it is characterised in that: step (1)
The concentration of middle hydrazine hydrate is 1-6g/L, and the concentration of hydroxylamine chloride is 0.5-4g/L.
3. the method for polyacrylonitrile fibre fire proofing pre-treatment according to claim 1, it is characterised in that: step (2)
In 0.5-2g polyacrylonitrile fibre is added in every 100ml modified solution.
4. the method for polyacrylonitrile fibre fire proofing pre-treatment according to claim 1, it is characterised in that: step (3)
In sodium acetate 0.5-2g, ammonium acetate 0.2-1g, potassium permanganate 0.5-5g, the acid solution are added in every 200ml acid solution
For the sulfuric acid solution of molar concentration 1-20%.
5. the method for polyacrylonitrile fibre fire proofing pre-treatment according to claim 1, it is characterised in that: step (4)
The temperature that middle melanism is impregnated is 60-80 DEG C, soaking time 2-4h.
6. the method for polyacrylonitrile fibre fire proofing pre-treatment according to claim 1, it is characterised in that: step (4)
Middle cleaning method is ultrasonic cleaning.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910217471.0A CN110004704A (en) | 2019-03-21 | 2019-03-21 | A kind of method of polyacrylonitrile fibre fire proofing pre-treatment |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910217471.0A CN110004704A (en) | 2019-03-21 | 2019-03-21 | A kind of method of polyacrylonitrile fibre fire proofing pre-treatment |
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| CN110004704A true CN110004704A (en) | 2019-07-12 |
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Citations (6)
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|---|---|---|---|---|
| CN101550616A (en) * | 2009-05-08 | 2009-10-07 | 北京化工大学 | Method of preparing high strength carbon fibre |
| CN101591857A (en) * | 2009-06-24 | 2009-12-02 | 山东理工大学 | Method with manufacturing pre-oxidized fibers for spinning by using large and small orlon filament bundles |
| CN101709517A (en) * | 2009-11-26 | 2010-05-19 | 中复神鹰碳纤维有限责任公司 | PAN-based carbon fiber precursor pre-oxidation pretreatment process |
| CN101811069A (en) * | 2010-04-15 | 2010-08-25 | 天津工业大学 | Double-modification polyacrylonitrile fiber metal complex catalyst and preparation method thereof |
| CN102732988A (en) * | 2012-06-21 | 2012-10-17 | 精源(南通)化纤制品有限公司 | High temperature resistant polyacrylonitrile artificial hair and its preparation method |
| CN106884228A (en) * | 2017-04-06 | 2017-06-23 | 天津工业大学 | A kind of preparation method of the flame-resistant polyacrylonitrile fiber based on hydroxylamine hydrochloride chemical modification |
-
2019
- 2019-03-21 CN CN201910217471.0A patent/CN110004704A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550616A (en) * | 2009-05-08 | 2009-10-07 | 北京化工大学 | Method of preparing high strength carbon fibre |
| CN101591857A (en) * | 2009-06-24 | 2009-12-02 | 山东理工大学 | Method with manufacturing pre-oxidized fibers for spinning by using large and small orlon filament bundles |
| CN101709517A (en) * | 2009-11-26 | 2010-05-19 | 中复神鹰碳纤维有限责任公司 | PAN-based carbon fiber precursor pre-oxidation pretreatment process |
| CN101811069A (en) * | 2010-04-15 | 2010-08-25 | 天津工业大学 | Double-modification polyacrylonitrile fiber metal complex catalyst and preparation method thereof |
| CN102732988A (en) * | 2012-06-21 | 2012-10-17 | 精源(南通)化纤制品有限公司 | High temperature resistant polyacrylonitrile artificial hair and its preparation method |
| CN106884228A (en) * | 2017-04-06 | 2017-06-23 | 天津工业大学 | A kind of preparation method of the flame-resistant polyacrylonitrile fiber based on hydroxylamine hydrochloride chemical modification |
Non-Patent Citations (1)
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|---|
| 王超: "腈纶的改性及其在预氧化过程纤维阻燃性能的关联性研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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