CN107022808A - A kind of comfortableness fire resistance fibre and preparation method thereof - Google Patents
A kind of comfortableness fire resistance fibre and preparation method thereof Download PDFInfo
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- CN107022808A CN107022808A CN201710241935.2A CN201710241935A CN107022808A CN 107022808 A CN107022808 A CN 107022808A CN 201710241935 A CN201710241935 A CN 201710241935A CN 107022808 A CN107022808 A CN 107022808A
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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
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
-
- 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
-
- 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
- D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
-
- 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
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
Abstract
The present invention relates to a kind of comfortableness fire resistance fibre and preparation method thereof, it is dissolved in after being blended in proportion with Inherent Flame Retardant Polymers using cellulose or acrylonitrile copolymer in solvent and spinning solution is made, by the ratio of viscosities for controlling blend, using high power jet stretch, the blended fiber that fiber sheath is rich in Inherent Flame Retardant Polymers is obtained.The limited oxygen index of blended fiber is 27~32%, from fiery self-extinguishing time≤5s, and equilibrium moisture regain is 8~15%, and fracture strength is that the content of Inherent Flame Retardant Polymers in 2.6~5.5cN/dtex, blended fiber is 5~18wt%.The present invention can effectively adjust two phase morphologies in blended fiber, the fire resistance of blended fiber is improved, the content of inherent fire-retardant fiber is reduced, it is simple with technique, with low cost the features such as, there is important meaning to developing low-cost, environment-friendly comfortable fire resistance fibre.
Description
Technical field
The invention belongs to fire resistance fibre field, it is related to a kind of comfortableness fire resistance fibre and preparation method thereof.
Background technology
Most of textile used in everyday all has inflammability, indoor decorative fabric, bedding, sofa, electric blanket
Deng the source for being all once fire, thus developed country extremely payes attention to the exploitation of flame retardant textiles.China is to Fire-proof Finishing Agents for Textile technology
Research also pay attention to increasingly.The anti-flammability for improving textile fabric at this stage is mainly added fire retardant to matrix fiber or changed
Learn and be modified, but there are many deficiencies in this method, the mechanical performance of such as fiber declines, and fire retardant is easily migrated, toxicant
It is volatile etc..
Emphasis with people to environmental protection, inherent fire-retardant fiber starts to exhibit one's skill to the full in flame retardant textiles field.This
Matter fire resistance fibre refers to due to itself special chemical constitution, even if making them without chemical assistant or carrying out chemical modification still
With good anti-flammability.Common inherent fire-retardant fiber mainly has aramid fiber 1313, PSA fiber, polyimide fiber, polyphenylene sulfide
Ether fiber etc..This fiber has fire retardancy persistently, environment-friendly, the advantages of being migrated in the absence of fire retardant, but these are fine
Dimension all has that hygroscopicity is poor to some extent, modulus height, spinning performance is poor, dyeing is difficult, therefore usually
Carry out blending spinning to improve the suction of inherent fire-retardant fiber with inherent fire-retardant fiber from cellulose fibre or polyacrylonitrile fibre
Moist, spinning property, dyeability etc..
Patent CN105350132A discloses the blending method of a kind of organic silazane fire retardant viscose short filament and aramid fiber 1313,
Organic silazane fire retardant viscose short filament is made by cellulose and silicon nitrogen combustion inhibitor, and clothing fabric made from the blending method, which has, to be worn
Comfortable, good flame resistance, safety and environmental protection, it is wear-resisting the advantages of, but its technique is complex, and it is big that it adds inherent flame retardant molecular weight,
Cost is higher.
Patent CN104213335A provides a kind of heat-resistance and flame-retardant fiber non-woven cloth and its manufacture method, high temperature resistant resistance
Combustion fiber non-woven is to be composited by preoxidized polyacrylonitrile chopped fiber and different flame-retardant yarns through stitched technique, can be passed through
Following steps are obtained：Shredding, mixing, combing, lapping, loop bonding reinforcing, cutting edge.The invention using loop bonding reinforcement technique come
The unmanageable defect of pre-oxidised acrylic fibre fabric is overcome, obtained product has outstanding fire-retardant, the property such as heat-resisting
Can, but its complex process, inherent fire-retardant fiber content height is added, cost is higher.
Patent CN101724964A provides a kind of high-temperature resistant flame-retarding textile, the fabric woven by heat-resistant fireproof yarn and
Into yarn is formed by pre-oxidized fibers, high-tenacity fire resistance fibre, common fire resistance fibre blending, this method solve pre-oxidation
Fiber is difficult spinning, low intensity, the defect of single black, and obtained product is heat-resist, and comfortableness is good, and intensity is high, but still deposits
In complex process, the shortcoming that inherent fire-retardant fiber content is high, cost is high.
Patent ZL201410186603.5 discloses a kind of preparation method of fire resistance fibre, and this method is using cellulose or poly-
Acrylonitrile is mixed in proportion with Inherent Flame Retardant Polymers, and high-temperature digestion spinning is prepared from, and this method technique is simple, the resistance of preparation
Fire flame-retardant fiber performance good, but when Inherent Flame Retardant Polymers addition content is less than 20%, the limited oxygen index (LOI) of fiber is low
In 27%, anti-flammability declines.
In summary, a kind of simple technique, few addition inherent fire-retardant fiber, good flame retardation effect, comfortableness are currently developed good
And the fire resistance fibre of low cost is the urgent demand in market.
The content of the invention
The purpose of the present invention is to overcome the problems such as prior art processes are complicated, inherent fire-retardant fiber addition is big, cost is high,
There is provided the good and inexpensive fire resistance fibre of a kind of technique simple, few addition inherent fire-retardant fiber, good flame retardation effect, comfortableness and its
Preparation method.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：
A kind of comfortableness fire resistance fibre, comfortableness fire resistance fibre is by cellulose or acrylonitrile copolymer and inherent flame retardant high score
Sub- co-blended spinning is made, and the Inherent Flame Retardant Polymers are mainly distributed on fiber sheath.
It is used as preferred technical scheme：
A kind of comfortableness fire resistance fibre as described above, the thickness of the fiber sheath accounts for the 1/5~1/3 of fiber radius,
Content >=60wt% of Inherent Flame Retardant Polymers in the fiber sheath, the concentration of the Inherent Flame Retardant Polymers is in fiber sheath
Cross section on distribution gradient, be gradually reduced by the lateral most inner side of the outermost of fiber sheath, this mainly due to cellulose or
Viscosity differences of the acrylonitrile copolymer with Inherent Flame Retardant Polymers in a solvent are larger, the sheet of low viscosity during extrusion molding
Matter flame-retardant high-molecular is more distributed in caused by fiber sheath.
The content of Inherent Flame Retardant Polymers is 5 in a kind of comfortableness fire resistance fibre as described above, comfortableness fire resistance fibre
~18wt%, the limited oxygen index of comfortableness fire resistance fibre is 27~32%, and from fiery self-extinguishing time≤5s, equilibrium moisture regain is 8
~15%, equilibrium moisture regain is higher, illustrates that the moisture pick-up properties of fire resistance fibre prepared by the present invention is excellent, with the excellent of comfortableness
Point, fracture strength is 2.6~5.5cN/dtex.
A kind of comfortableness fire resistance fibre as described above, the degree of polymerization of the cellulose is 200~1600, the acrylonitrile
The viscosity average molecular weigh of copolymer is 2 × 104~1.2 × 105, the content of acrylonitrile monemer is more than when preparing acrylonitrile copolymer
90wt%.
A kind of comfortableness fire resistance fibre as described above, the Inherent Flame Retardant Polymers are phenyl-diformyl isophthalic two between gathering
Amine, aromatic polysulfonamide or polybenzimidazoles containing sulfuryl, under solvent permissive condition, it is also contemplated that adding two or more simultaneously
Inherent Flame Retardant Polymers are planted, meanwhile, other Inherent Flame Retardant Polymers are also applied for the present invention, poly
1.5~2.5dL/g of logarithmic viscosity number, 0.7~1.5dL/g of logarithmic viscosity number of aromatic polysulfonamide, polyphenyl containing sulfuryl is simultaneously
1.0~3.0dL/g of logarithmic viscosity number of imidazoles.
A kind of comfortableness fire resistance fibre as described above, the aromatic polysulfonamide is poly- (4,4'- diphenyl sulphone (DPS) paraphenylene terephthalamides
Amine), poly- (3,3'- diphenyl sulphone (DPS)s terephthalamide), poly- (4,4'- diphenyl sulphone (DPS)s isophtalamide), poly- (between 3,3'- diphenyl sulphone (DPS)s
Benzenedicarboxamide) or any two or more construction units are constituted in above-mentioned homopolymer fragrant sulfonamide copolymer；It is described to contain sulfone
Base polybenzimidazoles is the homopolymer being made up of a kind of constitutional repeating unit, and the structural formula of the construction unit is as follows：
Present invention also offers a kind of preparation method of comfortableness fire resistance fibre, by cellulose or acrylonitrile copolymer and this
It is dissolved in after the mixing of matter flame-retardant high-molecular and homogeneous spinning solution is obtained in solvent, the fire-retardant fibre of comfortableness is made through spinning in spinning solution
The ratio of dimension, the wherein viscosity of cellulose or acrylonitrile copolymer in a solvent and the viscosity of Inherent Flame Retardant Polymers in a solvent
For 20~800, the jet stretch multiple in spinning process is 6~15.Under super drawing effect, spinning solution is in extrusion
The trend gradually increased by center to face, the inherent flame retardant of low viscosity are presented along fibre section for suffered shearing-tensile stress
Macromolecule more moves to the ratio 20~800 of each component viscosity in fiber surface high stress areas, the present invention and drawn with shower nozzle
Stretch the mutual cooperation of multiple 6~15, it is ensured that the viscosity of Inherent Flame Retardant Polymers is relatively low, and can be provided in drawing process enough
Drive force Inherent Flame Retardant Polymers migrated to fiber sheath.
It is used as preferred technical scheme：
Cellulose or acrylonitrile copolymer and Inherent Flame Retardant Polymers in preparation method as described above, the spinning solution
Mass ratio is 82~95:18~5, the cellulose or acrylonitrile copolymer are with Inherent Flame Retardant Polymers sum in spinning solution
Concentration is 5~30wt%.
Preparation method as described above, the solvent is the aqueous solution of 4- methyhnorpholine-N-oxides 50%, N, N- dimethyl
Formamide, DMAC N,N' dimethyl acetamide, dimethyl sulfoxide (DMSO), 1- butyl -3- methylimidazole villaumites, 1- pi-allyl -3- methylimidazoles
In villaumite, 1- butyl -3- N-Methylimidazoleacetics salt, 1- butyl -3- methylimidazoles bromide or 1- ethyl-3-methylimidazole formates
More than one.
Preparation method as described above, the solvent also contains inorganic salts, and inorganic salts can play a part of hydrotropy, described
Inorganic salts are content≤8wt% of inorganic salts in calcium chloride or lithium chloride, solvent.
Beneficial effect：
(1) comfortableness fire resistance fibre fire resistance of the invention is good, fire-retardant durable and comfortableness is good, and meeting environmental protection will
Ask.
(2) preparation method that the present invention is provided can effectively adjust two phase morphologies in blended fiber, improve blended fiber
Fire resistance, reduces the content of inherent fire-retardant fiber.
(3) preparation method that the present invention is provided has technique simple, the features such as with low cost, to developing low-cost, environment
Friendly comfortable fire resistance fibre has important meaning.
Embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, art technology
Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Fixed scope.
Embodiment 1
A kind of comfortableness fire resistance fibre and preparation method thereof, with logarithmic viscosity number be by the cellulose that the degree of polymerization is 200
1.5dL/g poly is 82 according to mass ratio:18 ratio mixing, in 4- methyl morpholines-N- oxidations
Stir, dissolved at 90 DEG C in the aqueous solution of thing 50%, obtain the spinning solution that polymer total solid content is 5%, wherein cellulose with it is poly-
The viscosity ratio of mpd-i in a solvent is 50, is extruded after spinning solution is pressurized, passes through 15 DEG C of air section
After coagulating bath (distilled water, 25 DEG C), through the first roller drawing-off, wherein jet stretch multiple is 6 times, then respectively enters 60 DEG C of water
Drawing-off bath, 90 DEG C of washing drawing-off bath, dried in 100 DEG C, thermal finalization, obtain a kind of comfortableness fire resistance fibre.
Test result shows：The filament number of comfortableness fire resistance fibre is 3.0dtex, and fracture strength is 2.6cN/dtex,
Equilibrium moisture regain is 15%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath, top layer in fiber obtained by the present embodiment
Thickness is the 1/4 of fiber radius, and Inherent Flame Retardant Polymers content is 60wt% in top layer.Surveyed using JF-3 types oxygen index measurer
Fixed, according to GB/T5454, the LOI values for measuring the present embodiment obtained flame-retardant fiber are 29.20%, are 2s, tool from fiery self-extinguishing time
There is good anti-flammability.
Comparative example 1
A kind of comfortableness fire resistance fibre and preparation method thereof, with logarithmic viscosity number be by the cellulose that the degree of polymerization is 200
1.5dL/g poly is 82 according to mass ratio:18 ratio mixing, in 4- methyl morpholines-N- oxidations
Stir, be swelled at 90 DEG C in the aqueous solution of thing 50%, vacuum dehydration obtains the spinning that polymer total solid content is 5% to being completely dissolved
Silk liquid.Deaeration, conveying, filtering, cool to 70 DEG C at 80 DEG C, apply 0.4MPa pressure, by 20mm air section and solidifying
Gu bathing after (water, 25 DEG C), the draw ratio in coagulating bath is 2 times, and into the drawing-off bath of 60 DEG C of water, 2 times of drawing-off enters back into boiling water and led
Bath is stretched, then 1.2 times of drawing-off is washed, dried, thermal finalization, obtain fiber.
Test result shows：The filament number of the fiber is 2.8dtex, and fracture strength is 3.0cN/dtex, the fibre of formation
The phase size of dimension element is 20nm.Determined using JF-3 types oxygen index measurer, according to GB/T5454, measure the LOI values of fiber
For 22.00%, light be more than 10s from the fiery fall time in atmosphere.By being contrasted with embodiment 1, raw material is identical and anti-
In the case of answering addition identical, using fire resistance fibre performance made from the inventive method more preferably, inherent flame retardant high score of the present invention
When son addition content is less than 20%, the limited oxygen index (LOI) of fiber is still very high, is only 2s from fiery self-extinguishing time, and contrasts
When Inherent Flame Retardant Polymers addition content is less than 20% in example, the limited oxygen index (LOI) of fiber is only 22.00%, from fire certainly
Put out time up to 7s, it can be seen that the present invention significantly reduces Inherent Flame Retardant Polymers addition content, solves control methods warp
The problem of Ji property is bad.
Embodiment 2
A kind of comfortableness fire resistance fibre and preparation method thereof, with logarithmic viscosity number be by the cellulose that the degree of polymerization is 900
2.0dL/g poly is 85 according to mass ratio:15 ratio mixing, in 1- butyl -3- methylimidazoles
Stir, dissolved at 85 DEG C in villaumite, obtain the spinning solution that polymer total solid content is 10%, wherein cellulose and poly- isophthalic diformazan
The viscosity ratio of acyl m-phenylene diamine (MPD) in a solvent is 110, is extruded after spinning solution is pressurized, air section and coagulating bath by 15 DEG C
After (distilled water, 25 DEG C), through the first roller drawing-off, wherein jet stretch multiple is 8 times, then respectively enters the drawing-off of 60 DEG C of water
Bath, 90 DEG C of washing drawing-off bath, dry, thermal finalization in 100 DEG C, obtain a kind of comfortableness fire resistance fibre.
Test result shows：The filament number of comfortableness fire resistance fibre is 3.0dtex, and fracture strength is 3.0cN/dtex,
Equilibrium moisture regain is 14%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath, top layer in fiber obtained by the present embodiment
Thickness is the 1/4 of fiber radius, and Inherent Flame Retardant Polymers content is 65wt% in top layer.Surveyed using JF-3 types oxygen index measurer
Fixed, according to GB/T5454, the LOI values for measuring the present embodiment obtained flame-retardant fiber are 28.90%, are 3s, tool from fiery self-extinguishing time
There is good anti-flammability.
Comparative example 2
A kind of comfortableness fire resistance fibre and preparation method thereof, with logarithmic viscosity number be by the cellulose that the degree of polymerization is 900
2.0dL/g poly is 85 according to mass ratio:15 ratio mixing, in 1- butyl -3- methylimidazoles
Stir, be swelled at 85 DEG C in villaumite, vacuum dehydration obtains the spinning solution that polymer total solid content is 10% to being completely dissolved.
Deaeration at 80 DEG C, conveying, filtering, cool to 70 DEG C, apply 0.4MPa pressure, by 20mm air section and coagulating bath (water,
25 DEG C) after, the draw ratio in coagulating bath is 2 times, and into the drawing-off bath of 60 DEG C of water, 2 times of drawing-off enters back into boiling water drawing-off bath, led
1.2 times are stretched, then washes, dry, thermal finalization, obtain fiber.
Test result shows：The filament number of the fiber is 2.8dtex, and fracture strength is 3.0cN/dtex, the fibre of formation
The phase size of dimension element is 20nm.Determined using JF-3 types oxygen index measurer, according to GB/T5454, measure the LOI values of fiber
For 24.00%, it is 8s to light in atmosphere from the fiery fall time.By being contrasted with embodiment 2, raw material is identical and reaction adds
In the case of dosage identical, using fire resistance fibre performance made from the inventive method more preferably, Inherent Flame Retardant Polymers of the present invention add
Plus content, when being less than 20%, the limited oxygen index (LOI) of fiber is still very high, is only 3s from fiery self-extinguishing time, and in comparative example
When Inherent Flame Retardant Polymers addition content is less than 20%, the limited oxygen index (LOI) of fiber is only 24.00%, when extinguishing from fire
Between up to 6s, it can be seen that the present invention significantly reduce Inherent Flame Retardant Polymers addition content, solve control methods economy
Bad the problem of.
Embodiment 3
A kind of comfortableness fire resistance fibre and preparation method thereof, with logarithmic viscosity number be by the cellulose that the degree of polymerization is 1600
2.5dL/g poly is 88 according to mass ratio:12 ratio mixing, in 1- butyl -3- methylimidazoles
Stir, dissolved at 80 DEG C in bromide, obtain the spinning solution that polymer total solid content is 15%, wherein cellulose and poly- isophthalic diformazan
The viscosity ratio of acyl m-phenylene diamine (MPD) in a solvent is 230, is extruded after spinning solution is pressurized, air section and coagulating bath by 15 DEG C
After (distilled water, 25 DEG C), through the first roller drawing-off, wherein jet stretch multiple is 15 times, then respectively enters the drawing-off of 60 DEG C of water
Bath, 90 DEG C of washing drawing-off bath, dry, thermal finalization in 100 DEG C, obtain a kind of comfortableness fire resistance fibre.
Test result shows：The filament number of the fiber is 2.8dtex, and fracture strength is 4.8cN/dtex, balance moisture regain
Rate is 12%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fibre
It is 70wt% to tie up Inherent Flame Retardant Polymers content in the 1/4 of radius, top layer.Determined using JF-3 types oxygen index measurer, foundation
GB/T5454, the LOI values for measuring fiber are 29.50%, and it is 4s to light in atmosphere from the fiery fall time, and anti-flammability is preferable.
Embodiment 4
A kind of comfortableness fire resistance fibre and preparation method thereof, by viscosity average molecular weigh for 30000 polyacrylonitrile homopolymer with
Poly- (the 4,4'- diphenyl sulphone (DPS)s terephthalamide) that logarithmic viscosity number is 1.0dL/g is 90 according to mass ratio:10 ratio is mixed
Close, stirred in DMA, dissolved at 90 DEG C, obtain the spinning solution that polymer total solid content is 30%, wherein
Polyacrylonitrile is 100 with the viscosity ratio of poly- (4,4'- diphenyl sulphone (DPS) terephthalamide) in a solvent, is squeezed after spinning solution is pressurized
Go out, after 15 DEG C of air sections and coagulating bath (distilled water, 25 DEG C), through the first roller drawing-off, wherein jet stretch multiple is 8
Times, drawing-off bath, 90 DEG C of the washing drawing-off bath of 60 DEG C of water are then respectively enterd, is dried in 100 DEG C, thermal finalization, obtains a kind of
Comfortableness fire resistance fibre.
Test result shows：The filament number of the fiber is 3.4dtex, and fracture strength is 3.2cN/dtex, balance moisture regain
Rate is 8%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fiber
Inherent Flame Retardant Polymers content is 62wt% in the 1/4 of radius, top layer.Determined using JF-3 types oxygen index measurer, according to GB/
T5454, the LOI values for measuring fiber are 30.0%, and it is 4s to light in atmosphere from the fiery fall time, there is good anti-flammability.
Embodiment 5
A kind of comfortableness fire resistance fibre and preparation method thereof, by viscosity average molecular weigh for 50000 polyacrylonitrile copolymer (the
One monomer is acrylonitrile, and mass fraction 90%, second comonomer is methyl acrylate, and mass fraction 8%, Third monomer is clothing health
Acid, mass fraction be 2%) with logarithmic viscosity number for 1.5dL/g poly- (3,3'- diphenyl sulphone (DPS) terephthalamide) according to quality
Than for 82:18 ratio mixing, stirs in dimethyl sulfoxide (DMSO), is dissolved at 65 DEG C, and it is 12% to obtain polymer total solid content
Spinning solution, wherein polyacrylonitrile are 190, spinning with the viscosity ratio of poly- (3,3'- diphenyl sulphone (DPS) terephthalamide) in a solvent
Extruded after liquid is pressurized, after 15 DEG C of air sections and coagulating bath (distilled water, 25 DEG C), through the first roller drawing-off, wherein shower nozzle
Draw ratio is 10 times, then respectively enters drawing-off bath, 90 DEG C of the washing drawing-off bath of 60 DEG C of water, is dried in 100 DEG C, heat is fixed
Type, obtains a kind of comfortableness fire resistance fibre.
Test result shows：The filament number of the fiber is 3.0dtex, and fracture strength is 3.4cN/dtex, balance moisture regain
Rate is 9%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fiber
Inherent Flame Retardant Polymers content is 68wt% in the 1/4 of radius, top layer.Determined using JF-3 types oxygen index measurer, according to GB/
T5454, the LOI values for measuring fiber are 32.0%, and it is 3s to light in atmosphere from the fiery fall time, there is good anti-flammability.
Embodiment 6
A kind of comfortableness fire resistance fibre and preparation method thereof, by viscosity average molecular weigh for 50000 polyacrylonitrile copolymer (the
One monomer is acrylonitrile, and mass fraction 91%, second comonomer is methyl acrylate, mass fraction 9%) be with logarithmic viscosity number
2.0dL/g poly is 92 according to mass ratio:8 ratio mixing, in DMF
Stirring, dissolves at 70 DEG C, obtains the spinning solution that polymer total solid content is 26%, wherein polyacrylonitrile and it is poly- between phenyl-diformyl
The viscosity ratio of phenylenediamine in a solvent is 230, is extruded after spinning solution is pressurized, (is steamed by 15 DEG C of air sections and coagulating bath
Distilled water, 25 DEG C) after, through the first roller drawing-off, wherein jet stretch multiple is 11 times, then respectively enter 60 DEG C of water drawing-off bath,
90 DEG C of washing drawing-off bath, dries, thermal finalization in 100 DEG C, obtains a kind of comfortableness fire resistance fibre.
Test result shows：The filament number of the fiber is 3.3dtex, and fracture strength is 3.5cN/dtex, balance moisture regain
Rate is 10%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fibre
It is 69wt% to tie up Inherent Flame Retardant Polymers content in the 1/5 of radius, top layer.Determined using JF-3 types oxygen index measurer, foundation
GB/T5454, the LOI values for measuring fiber are 27.8%, and it is 4s to light in atmosphere from the fiery fall time, there is preferable anti-flammability.
Embodiment 7
A kind of comfortableness fire resistance fibre and preparation method thereof, by viscosity average molecular weigh for 80000 polyacrylonitrile copolymer (the
One monomer is acrylonitrile, and mass fraction 92%, second comonomer is methyl methacrylate, and mass fraction 6%, Third monomer is third
Alkene sodium sulfonate, mass fraction be 2%) with logarithmic viscosity number for 2.2dL/g poly according to quality
Than for 95:5 ratio mixing, in lithium chloride/DMA solvent, (lithium chloride accounts for lithium chloride/N, N- dimethyl second
The mass fraction of acid amides stirs to be 8%) middle, is dissolved at 70 DEG C, obtains the spinning solution that polymer total solid content is 18%, wherein gathering
Acrylonitrile is 300 with the viscosity ratio of poly in a solvent, is extruded after spinning solution is pressurized, passes through 15
DEG C air section and coagulating bath (distilled water, 25 DEG C) after, through the first roller drawing-off, wherein jet stretch multiple is 9 times, is then distinguished
Drawing-off bath, 90 DEG C of washing drawing-off bath into 60 DEG C of water, dry, thermal finalization in 100 DEG C, obtain a kind of fire-retardant fibre of comfortableness
Dimension.
Test result shows：The filament number of the fiber is 3.6dtex, and fracture strength is 3.8cN/dtex, balance moisture regain
Rate is 10%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fibre
It is 72wt% to tie up Inherent Flame Retardant Polymers content in the 1/5 of radius, top layer.Determined using JF-3 types oxygen index measurer, foundation
GB/T5454, the LOI values for measuring fiber are 29.7%, and it is 3s to light in atmosphere from the fiery fall time, there is good anti-flammability.
Embodiment 8
A kind of comfortableness fire resistance fibre and preparation method thereof, with logarithmic viscosity number be by the cellulose that the degree of polymerization is 1200
0.7dL/g poly- (4,4'- diphenyl sulphone (DPS)s isophtalamide) is 95 according to mass ratio:5 ratio mixing, in 1- butyl -3- first
Stir, dissolved at 95 DEG C in base imidazoles villaumite, obtain the spinning solution that polymer total solid content is 16%, wherein cellulose with it is poly-
The viscosity ratio of (4,4'- diphenyl sulphone (DPS) isophtalamide) in a solvent is 800, is extruded after spinning solution is pressurized, passes through 15 DEG C
Air section and coagulating bath (distilled water, 25 DEG C) after, through the first roller drawing-off, wherein jet stretch multiple is 14 times, is then distinguished
Drawing-off bath, 90 DEG C of washing drawing-off bath into 60 DEG C of water, dry, thermal finalization in 100 DEG C, obtain a kind of fire-retardant fibre of comfortableness
Dimension.
Test result shows：The filament number of the fiber is 3.3dtex, and fracture strength is 4.2cN/dtex, balance moisture regain
Rate is 12%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fibre
It is 90wt% to tie up Inherent Flame Retardant Polymers content in the 1/5 of radius, top layer.Determined using JF-3 types oxygen index measurer, foundation
GB/T5454, the LOI values for measuring fiber are 27.0%, and it is 5s to light in atmosphere from the fiery fall time, there is good anti-flammability.
Embodiment 9
A kind of comfortableness fire resistance fibre and preparation method thereof, with logarithmic viscosity number be by the cellulose that the degree of polymerization is 1600
1.5dL/g poly- (3,3'- diphenyl sulphone (DPS)s isophtalamide) is 92 according to mass ratio:8 ratio mixing, in 1- ethyl -3- first
Stir, dissolved at 80 DEG C in base imidazole formic acid salt, obtain the spinning solution that polymer total solid content is 13%, wherein cellulose with it is poly-
The viscosity ratio of (3,3'- diphenyl sulphone (DPS) isophtalamide) in a solvent is 800, is extruded after spinning solution is pressurized, passes through 15 DEG C
Air section and coagulating bath (distilled water, 25 DEG C) after, through the first roller drawing-off, wherein jet stretch multiple is 15 times, is then distinguished
Drawing-off bath, 90 DEG C of washing drawing-off bath into 60 DEG C of water, dry, thermal finalization in 100 DEG C, obtain a kind of fire-retardant fibre of comfortableness
Dimension.
Test result shows：The filament number of the fiber is 3.7dtex, and fracture strength is 5.5cN/dtex, balance moisture regain
Rate is 15%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fibre
It is 88wt% to tie up Inherent Flame Retardant Polymers content in the 1/4 of radius, top layer.Determined using JF-3 types oxygen index measurer, foundation
GB/T5454, the LOI values for measuring fiber are 27.3%, and it is 5s to light in atmosphere from the fiery fall time, there is preferable anti-flammability.
Embodiment 10
A kind of comfortableness fire resistance fibre and preparation method thereof, with logarithmic viscosity number be by the cellulose that the degree of polymerization is 1000
1.0dL/g by 4,4' diaminodiphenyl sulfone, 3,3'- diaminodiphenylsulfones and paraphthaloyl chloride with 3:1:4 copolymerization ratio group
Into fragrant sulfonamide copolymer according to mass ratio be 90:10 ratio mixing, is stirred in 1- butyl -3- N-Methylimidazoleacetic salt
Mix, dissolved at 80 DEG C, obtain the spinning solution that polymer total solid content is 8%, wherein cellulose and fragrant sulfonamide copolymer is viscous
It is 640 to spend ratio, is extruded after spinning solution is pressurized, after 15 DEG C of air sections and coagulating bath (distilled water, 25 DEG C), through first
Roller drawing-off, wherein jet stretch multiple are 12 times, then respectively enter drawing-off bath, 90 DEG C of the washing drawing-off bath of 60 DEG C of water,
Dried in 100 DEG C, thermal finalization, obtain a kind of comfortableness fire resistance fibre.
Test result shows：The filament number of the fiber is 3.0dtex, and fracture strength is 3.4cN/dtex, balance moisture regain
Rate is 12%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fibre
It is 85wt% to tie up Inherent Flame Retardant Polymers content in the 1/4 of radius, top layer.Determined using JF-3 types oxygen index measurer, foundation
GB/T5454, the LOI values for measuring fiber are 27.8%, and it is 4s to light in atmosphere from the fiery fall time, there is preferable anti-flammability.
Embodiment 11
A kind of comfortableness fire resistance fibre and preparation method thereof, by viscosity average molecular weigh for 80000 polyacrylonitrile homopolymer with
Logarithmic viscosity number for 1.1dL/g by 4,4' diaminodiphenyl sulfone, 3,3'- diaminodiphenylsulfones and paraphthaloyl chloride with
1:1:The fragrant sulfonamide copolymer of 2 copolymerization ratio composition is 85 according to mass ratio:15 ratio mixing, in dimethyl sulfoxide (DMSO)/N,
(volume ratio of dimethyl sulfoxide (DMSO) and DMAC N,N' dimethyl acetamide is 1 to N- dimethylacetamide solvents:1) stirred in, it is molten at 65 DEG C
Solution, obtains the spinning solution that polymer total solid content is 20%, and the viscosity ratio of wherein polyacrylonitrile and fragrant sulfonamide copolymer is
550, extruded after spinning solution is pressurized, after 15 DEG C of air sections and coagulating bath (distilled water, 25 DEG C), through the first roller drawing-off,
Wherein jet stretch multiple is 10 times, drawing-off bath, 90 DEG C of the washing drawing-off bath of 60 DEG C of water is then respectively enterd, in 100 DEG C
Dry, thermal finalization, obtain a kind of comfortableness fire resistance fibre.
Test result shows：The filament number of the fiber is 3.4dtex, and fracture strength is 3.5cN/dtex, balance moisture regain
Rate is 10%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fibre
It is 87wt% to tie up Inherent Flame Retardant Polymers content in the 1/3 of radius, top layer.Determined using JF-3 types oxygen index measurer, foundation
GB/T5454, the LOI values for measuring fiber are 29.8%, and it is 3s to light in atmosphere from the fiery fall time, there is preferable anti-flammability.
Embodiment 12
A kind of comfortableness fire resistance fibre and preparation method thereof, by viscosity average molecular weigh for 90000 polyacrylonitrile copolymer (the
One monomer is acrylonitrile, and mass fraction 95%, second comonomer is methyl acrylate, mass fraction 5%) be with logarithmic viscosity number
1.3dL/g by 4,4' diaminodiphenyl sulfone, 3,3'- diaminodiphenylsulfones and m-phthaloyl chloride with 2:1:3 copolymerization ratio group
Into fragrant sulfonamide copolymer according to mass ratio be 88:12 ratio mixing, in lithium chloride/DMA solvent
Stirred in (mass fraction that lithium chloride accounts for lithium chloride/DMA is 7%), dissolved at 70 DEG C, obtain polymer
Total solid content is 20% spinning solution, and the viscosity ratio of wherein polyacrylonitrile and fragrant sulfonamide copolymer is 520, and spinning solution is through adding
Extruded after pressure, after 15 DEG C of air sections and coagulating bath (distilled water, 25 DEG C), through the first roller drawing-off, wherein jet stretch times
Number is 13 times, then respectively enters drawing-off bath, 90 DEG C of the washing drawing-off bath of 60 DEG C of water, is dried in 100 DEG C, thermal finalization is obtained
Obtain a kind of comfortableness fire resistance fibre.
Test result shows：The filament number of the fiber is 3.1dtex, and fracture strength is 3.6cN/dtex, balance moisture regain
Rate is 8%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fiber
Inherent Flame Retardant Polymers content is 81wt% in the 1/4 of radius, top layer.Determined using JF-3 types oxygen index measurer, according to GB/
T5454, the LOI values for measuring fiber are 29.9%, and it is 3s to light in atmosphere from the fiery fall time, there is good anti-flammability.
Embodiment 13
A kind of comfortableness fire resistance fibre and preparation method thereof, with logarithmic viscosity number be by the cellulose that the degree of polymerization is 400
1.0dL/g polybenzimidazoles containing sulfuryl is 82 according to mass ratio:18 ratio mixing, in 1- pi-allyl -3- methylimidazole chlorine
Stir, dissolved at 90 DEG C in salt, obtain the spinning solution that polymer total solid content is 15%, wherein cellulose and polyphenyl containing sulfuryl simultaneously
The ratio of viscosities of imidazoles in a solvent is 560, is extruded after spinning solution is pressurized, by 15 DEG C of air sections and coagulating bath (distilled water,
25 DEG C) after, through the first roller drawing-off, wherein jet stretch multiple is 13 times, then respectively enter 60 DEG C of water drawing-off bath, 90 DEG C
Drawing-off bath is washed, is dried in 100 DEG C, thermal finalization, a kind of comfortableness fire resistance fibre, the structure of the polybenzimidazoles containing sulfuryl is obtained
Unit is as follows：
Test result shows：The filament number of the fiber is 3.6dtex, and fracture strength is 3.5cN/dtex, balance moisture regain
Rate is 11%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fibre
It is 79wt% to tie up Inherent Flame Retardant Polymers content in the 1/4 of radius, top layer.Determined using JF-3 types oxygen index measurer, foundation
GB/T5454, the LOI values for measuring fiber are 29.8%, and it is 3s to light in atmosphere from the fiery fall time, there is good anti-flammability.
Embodiment 14
A kind of comfortableness fire resistance fibre and preparation method thereof, with logarithmic viscosity number be by the cellulose that the degree of polymerization is 1200
3.0dL/g polybenzimidazoles containing sulfuryl is 92 according to mass ratio:8 ratio mixing, in 1- butyl -3- methylimidazole bromides
Stir, dissolved at 80 DEG C, obtain the spinning solution that polymer total solid content is 18%, wherein cellulose and polybenzimidazoles containing sulfuryl
Ratio of viscosities in a solvent is 760, is extruded after spinning solution is pressurized, passes through 15 DEG C of air sections and coagulating bath (distilled water, 25
DEG C) after, through the first roller drawing-off, wherein jet stretch multiple is 15 times.Then the drawing-off bath of 60 DEG C of water, 90 DEG C of water are respectively enterd
Drawing-off bath is washed, is dried in 100 DEG C, thermal finalization, a kind of comfortableness fire resistance fibre, the structure list of the polybenzimidazoles containing sulfuryl is obtained
Member is as follows：
Test result shows：The filament number of the fiber is 3.5dtex, and fracture strength is 3.8cN/dtex, balance moisture regain
Rate is 14%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fibre
It is 86wt% to tie up Inherent Flame Retardant Polymers content in the 1/4 of radius, top layer.Determined using JF-3 types oxygen index measurer, foundation
GB/T5454, the LOI values for measuring fiber are 27.6%, and it is 4s to light in atmosphere from the fiery fall time, there is preferable anti-flammability.
Embodiment 15
A kind of comfortableness fire resistance fibre and preparation method thereof, by the polyacrylonitrile copolymer that viscosity average molecular weigh is 100000
(the first monomer is acrylonitrile, and mass fraction 96%, second comonomer is methyl acrylate, and mass fraction 3%, Third monomer is first
Base propylene benzene sulfonic acid sodium salt, mass fraction be 1%) with logarithmic viscosity number for 2.8dL/g polybenzimidazoles containing sulfuryl according to matter
Amount is than being 85:15 ratio mixing, stirs in dimethyl sulfoxide (DMSO), is dissolved at 65 DEG C, and it is 25% to obtain polymer total solid content
Spinning solution, wherein polyacrylonitrile and the ratio of viscosities of polybenzimidazoles containing sulfuryl in a solvent is 340, is squeezed after spinning solution is pressurized
Go out, after 15 DEG C of air sections and coagulating bath (distilled water, 25 DEG C), through the first roller drawing-off, wherein jet stretch multiple is 8
Times.Then drawing-off bath, 90 DEG C of the washing drawing-off bath of 60 DEG C of water are respectively enterd, is dried in 100 DEG C, thermal finalization, obtains a kind of
Comfortableness fire resistance fibre, the construction unit of the polybenzimidazoles containing sulfuryl is as follows：
Test result shows：The filament number of the fiber is 3.8dtex, and fracture strength is 4.6cN/dtex, balance moisture regain
Rate is 10%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fibre
It is 71wt% to tie up Inherent Flame Retardant Polymers content in the 1/3 of radius, top layer.Determined using JF-3 types oxygen index measurer, foundation
GB/T5454, the LOI values for measuring fiber are 29.6%, and it is 3s to light in atmosphere from the fiery fall time, there is good anti-flammability.
Embodiment 16
A kind of comfortableness fire resistance fibre and preparation method thereof, by viscosity average molecular weigh for 20000 polyacrylonitrile copolymer (the
One monomer is acrylonitrile, and mass fraction 90%, second comonomer is vinyl acetate, and mass fraction 7%, Third monomer is itaconic acid,
The polybenzimidazoles containing sulfuryl that 3%) it is 2.5dL/g with logarithmic viscosity number that mass fraction is is 82 according to mass ratio:18 ratio
Example mixing, is stirred in DMA, is dissolved at 60 DEG C, obtains the spinning solution that polymer total solid content is 8%, its
Middle polyacrylonitrile is 20 with the ratio of viscosities of polybenzimidazoles containing sulfuryl in a solvent, is extruded after spinning solution is pressurized, passes through 15 DEG C
Air section and coagulating bath (distilled water, 25 DEG C) after, through the first roller drawing-off, wherein jet stretch multiple is 6 times, is then entered respectively
Enter drawing-off bath, 90 DEG C of the washing drawing-off bath of 60 DEG C of water, dried in 100 DEG C, thermal finalization, obtain a kind of fire-retardant fibre of comfortableness
Dimension, the construction unit of the polybenzimidazoles containing sulfuryl is as follows：
Test result shows：The filament number of the fiber is 3.5dtex, and fracture strength is 3.1cN/dtex, balance moisture regain
Rate is 9%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fiber
Inherent Flame Retardant Polymers content is 60wt% in the 1/3 of radius, top layer.Determined using JF-3 types oxygen index measurer, according to GB/
T5454, the LOI values for measuring fiber are 28.8%, and it is 3s to light in atmosphere from the fiery fall time, there is good anti-flammability.
Embodiment 17
A kind of comfortableness fire resistance fibre and preparation method thereof, by viscosity average molecular weigh for 50000 polyacrylonitrile copolymer (the
One monomer is acrylonitrile, and mass fraction 92%, second comonomer is methyl acrylate, and mass fraction 5%, Third monomer is methyl-prop
Alkene sodium sulfonate, the polybenzimidazoles containing sulfuryl that 3%) it is 2.3dL/g with logarithmic viscosity number that mass fraction is is according to mass ratio
95:5 ratio mixing, in calcium chloride/DMF solvent, (calcium chloride accounts for calcium chloride/DMF
Mass fraction to stir in 8%), dissolved at 65 DEG C, obtain the spinning solution that polymer total solid content is 12%, wherein polypropylene
Nitrile is 410 with the ratio of viscosities of polybenzimidazoles containing sulfuryl in a solvent, is extruded after spinning solution is pressurized, passes through 15 DEG C of air section
After coagulating bath (distilled water, 25 DEG C), through the first roller drawing-off, wherein jet stretch multiple is 8 times, then respectively enters 60 DEG C of water
Drawing-off bath, 90 DEG C of washing drawing-off bath, dried in 100 DEG C, thermal finalization, a kind of comfortableness fire resistance fibre obtained, containing sulfuryl
The construction unit of polybenzimidazoles is as follows：
Test result shows：The filament number of the fiber is 3.5dtex, and fracture strength is 3.2cN/dtex, balance moisture regain
Rate is 9%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fiber
Inherent Flame Retardant Polymers content is 88wt% in the 1/5 of radius, top layer.Determined using JF-3 types oxygen index measurer, according to GB/
T5454, the LOI values for measuring fiber are 27.5%, and it is 4s to light in atmosphere from the fiery fall time, there is preferable anti-flammability.
Embodiment 18
A kind of comfortableness fire resistance fibre and preparation method thereof, by viscosity average molecular weigh for 70000 polyacrylonitrile homopolymer with
The poly that logarithmic viscosity number is 2.0dL/g is 87 according to mass ratio:13 ratio mixing, in chlorination
Stirred in calcium/N,N-dimethylformamide solvent (mass fraction that calcium chloride accounts for calcium chloride/N,N-dimethylformamide is 6%)
Mix, dissolved at 55 DEG C, obtain the spinning solution that polymer total solid content is 10%, polyacrylonitrile and poly
Ratio of viscosities in a solvent is 120.Extruded after spinning solution is pressurized, pass through 15 DEG C of air sections and coagulating bath (distilled water, 25
DEG C) after, through the first roller drawing-off, wherein jet stretch multiple is 8 times, then respectively enters the drawing-off bath of 60 DEG C of water, 90 DEG C of water
Drawing-off bath is washed, is dried in 100 DEG C, thermal finalization, a kind of comfortableness fire resistance fibre is obtained.
Test result shows：The filament number of the fiber is 3.2dtex, and fracture strength is 3.1cN/dtex, balance moisture regain
Rate is 10%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fibre
It is 68wt% to tie up Inherent Flame Retardant Polymers content in the 1/4 of radius, top layer.Determined using JF-3 types oxygen index measurer, foundation
GB/T5454, the LOI values for measuring fiber are 28.7%, and it is 3s to light in atmosphere from the fiery fall time, there is good anti-flammability.
Embodiment 19
A kind of comfortableness fire resistance fibre and preparation method thereof, with logarithmic viscosity number be by the cellulose that the degree of polymerization is 500
2.0dL/g polybenzimidazoles containing sulfuryl is 90 according to mass ratio:10 ratio mixing, in 1- pi-allyl -3- methylimidazole chlorine
Stir, dissolved at 80 DEG C in salt, obtain the spinning solution that polymer total solid content is 20%, wherein cellulose and the miaow of benzo containing sulfuryl
The ratio of viscosities of azoles in a solvent is 240, is extruded after spinning solution is pressurized, passes through 15 DEG C of air sections and coagulating bath (distilled water, 25
DEG C) after, through the first roller drawing-off, wherein jet stretch multiple is 12 times, then respectively enters the drawing-off bath of 60 DEG C of water, 90 DEG C of water
Drawing-off bath is washed, is dried in 100 DEG C, thermal finalization, a kind of comfortableness fire resistance fibre, the structure list of the polybenzimidazoles containing sulfuryl is obtained
Member is as follows：
Test result shows：The filament number of the fiber is 3.1dtex, and fracture strength is 4.0cN/dtex, balance moisture regain
Rate is 11%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fibre
It is 69wt% to tie up Inherent Flame Retardant Polymers content in the 1/4 of radius, top layer.Determined using JF-3 types oxygen index measurer, foundation
GB/T5454, the LOI values for measuring fiber are 29.5%, and it is 3s to light in atmosphere from the fiery fall time, there is good anti-flammability.
Embodiment 20
A kind of comfortableness fire resistance fibre and preparation method thereof, by the polyacrylonitrile copolymer that viscosity average molecular weigh is 120000
(the first monomer is acrylonitrile, and mass fraction 95%, second comonomer is methyl methacrylate, mass fraction 4%, Third monomer
For itaconic acid, 1%) it is 1.3dL/g with logarithmic viscosity number by 4,4'- diaminodiphenylsulfones, 3,3'- diaminos that mass fraction is
Base diphenyl sulphone (DPS), paraphthaloyl chloride and m-phthaloyl chloride are with 1:1:1:1 copolymerization ratio composition fragrant sulfonamide copolymer according to
Mass ratio is 88:12 ratio mixing, in 1- butyl -3- N-Methylimidazoleacetics salt/1- pi-allyl -3- methylimidazole villaumite solvents
(1- butyl -3- N-Methylimidazoleacetics salt is 1 with 1- pi-allyl -3- methylimidazole villaumites volume ratio:2) stirred in, it is molten at 85 DEG C
Solution, obtains the spinning solution that polymer total solid content is 30%, wherein polyacrylonitrile and fragrant sulfonamide copolymer in a solvent viscous
Degree is extruded, after 15 DEG C of air sections and coagulating bath (distilled water, 25 DEG C), through the first roller than being 140 after spinning solution is pressurized
Drawing-off, wherein jet stretch multiple are 10 times, drawing-off bath, 90 DEG C of the washing drawing-off bath of 60 DEG C of water are then respectively enterd, 100
Dried in DEG C, thermal finalization, obtain a kind of comfortableness fire resistance fibre.
Test result shows：The filament number of the fiber is 3.7dtex, and fracture strength is 5.1cN/dtex, balance moisture regain
Rate is 10%.Inherent Flame Retardant Polymers are mainly distributed on fiber sheath in fiber obtained by the present embodiment, and skin depth is fibre
It is 67wt% to tie up Inherent Flame Retardant Polymers content in the 1/4 of radius, top layer.Determined using JF-3 types oxygen index measurer, foundation
GB/T5454, the LOI values for measuring fiber are 30.3%, and it is 3s to light in atmosphere from the fiery fall time, there is good anti-flammability.
Claims (10)
1. a kind of comfortableness fire resistance fibre, it is characterized in that：It is blended by cellulose or acrylonitrile copolymer with Inherent Flame Retardant Polymers
Spinning is made, and the Inherent Flame Retardant Polymers are distributed in fiber sheath.
2. a kind of comfortableness fire resistance fibre according to claim 1, it is characterised in that the thickness of the fiber sheath accounts for fibre
Tie up content >=60wt% of Inherent Flame Retardant Polymers in the 1/5~1/3 of radius, the fiber sheath, the inherent flame retardant high score
The concentration of son distribution gradient on the cross section of fiber sheath, is gradually reduced by the lateral most inner side of the outermost of fiber sheath.
3. a kind of comfortableness fire resistance fibre according to claim 1, it is characterised in that essence resistance in comfortableness fire resistance fibre
Fire high molecular content for 5~18wt%, the limited oxygen index of comfortableness fire resistance fibre is 27~32%, from fiery self-extinguishing time≤
5s, equilibrium moisture regain is 8~15%, and fracture strength is 2.6~5.5cN/dtex.
4. a kind of comfortableness fire resistance fibre according to claim 1, it is characterised in that the degree of polymerization of the cellulose is
200~1600, the viscosity average molecular weigh of the acrylonitrile copolymer is 2 × 104~1.2 × 105, third when preparing acrylonitrile copolymer
The content of alkene nitrile monomer is more than 90wt%.
5. a kind of comfortableness fire resistance fibre according to claim 1, it is characterised in that the Inherent Flame Retardant Polymers are poly-
Mpd-i, aromatic polysulfonamide or polybenzimidazoles containing sulfuryl, the ratio of poly are dense right
Number viscosity 1.5~2.5dL/g, 0.7~1.5dL/g of logarithmic viscosity number of aromatic polysulfonamide, the ratio of the polybenzimidazoles containing sulfuryl
Dense 1.0~3.0dL/g of log viscosities.
6. a kind of comfortableness fire resistance fibre according to claim 5, it is characterised in that the aromatic polysulfonamide for it is poly- (4,
4'- diphenyl sulphone (DPS)s terephthalamide), poly- (3,3'- diphenyl sulphone (DPS)s terephthalamide), poly- (phenyl-diformyl between 4,4'- diphenyl sulphone (DPS)s
Amine), poly- (3,3'- diphenyl sulphone (DPS)s isophtalamide) or any two or more construction units are constituted in above-mentioned homopolymer fragrant sulfone
Amide copolymer；The polybenzimidazoles containing sulfuryl is the homopolymer being made up of a kind of constitutional repeating unit, the construction unit
Structural formula is as follows：
7. a kind of preparation method of comfortableness fire resistance fibre as described in any one of claim 1~6, it is characterized in that：By fiber
Element or acrylonitrile copolymer are dissolved in after being mixed with Inherent Flame Retardant Polymers and homogeneous spinning solution are obtained in solvent, and spinning solution is through spinning
The obtained comfortableness fire resistance fibre of silk, the wherein viscosity of cellulose or acrylonitrile copolymer in a solvent exist with Inherent Flame Retardant Polymers
The ratio of viscosity in solvent is that the jet stretch multiple in 20~800, spinning process is 6~15.
8. preparation method according to claim 7, it is characterised in that cellulose or acrylonitrile copolymer in the spinning solution
Mass ratio with Inherent Flame Retardant Polymers is 82~95:18~5, the cellulose or acrylonitrile copolymer and inherent flame retardant high score
Concentration of the sub- sum in spinning solution is 5~30wt%.
9. preparation method according to claim 7, it is characterised in that the solvent is 4- methyhnorpholine-N-oxides
50% aqueous solution, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, dimethyl sulfoxide (DMSO), 1- butyl -3- methylimidazole chlorine
Salt, 1- pi-allyl -3- methylimidazole villaumites, 1- butyl -3- N-Methylimidazoleacetics salt, 1- butyl -3- methylimidazoles bromide or 1-
One or more of ethyl-3-methylimidazole formates.
10. preparation method according to claim 9, it is characterised in that the solvent also contains inorganic salts, the inorganic salts
For calcium chloride or lithium chloride, content≤8wt% of inorganic salts in solvent.
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| CN108641102A (en) * | 2018-06-20 | 2018-10-12 | 北京林业大学 | A kind of highly effective cellulose dicyandiamide solution and application thereof |
| CN110541208A (en) * | 2019-09-29 | 2019-12-06 | 东华大学 | preparation method of polyisophthaloyl metaphenylene diamine/polyacrylonitrile blended fiber |
| CN115323524A (en) * | 2022-09-06 | 2022-11-11 | 青岛大学 | Degradable moisture-absorbing temperature-regulating composite functional filament and preparation method thereof |
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| CN104018243A (en) * | 2014-05-05 | 2014-09-03 | 东华大学 | Flame retardant fiber and preparation method thereof |
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| CN104018243A (en) * | 2014-05-05 | 2014-09-03 | 东华大学 | Flame retardant fiber and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108641102A (en) * | 2018-06-20 | 2018-10-12 | 北京林业大学 | A kind of highly effective cellulose dicyandiamide solution and application thereof |
| CN108641102B (en) * | 2018-06-20 | 2020-12-08 | 北京林业大学 | High-efficiency cellulose solvent system and application thereof |
| CN110541208A (en) * | 2019-09-29 | 2019-12-06 | 东华大学 | preparation method of polyisophthaloyl metaphenylene diamine/polyacrylonitrile blended fiber |
| CN110541208B (en) * | 2019-09-29 | 2022-01-18 | 东华大学 | Preparation method of polyisophthaloyl metaphenylene diamine/polyacrylonitrile blended fiber |
| CN115323524A (en) * | 2022-09-06 | 2022-11-11 | 青岛大学 | Degradable moisture-absorbing temperature-regulating composite functional filament and preparation method thereof |
| CN115323524B (en) * | 2022-09-06 | 2023-10-20 | 青岛大学 | Degradable moisture-absorbing temperature-regulating composite functional filament and preparation method thereof |
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