CN110158176A - A kind of preparation method of flame retardant viscose fiber - Google Patents
A kind of preparation method of flame retardant viscose fiber Download PDFInfo
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- CN110158176A CN110158176A CN201910462277.9A CN201910462277A CN110158176A CN 110158176 A CN110158176 A CN 110158176A CN 201910462277 A CN201910462277 A CN 201910462277A CN 110158176 A CN110158176 A CN 110158176A
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- flame retardant
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
- D01D5/0046—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion the fibre formed by coagulation, i.e. wet electro-spinning
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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
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
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Abstract
The present invention relates to a kind of preparation methods of flame retardant viscose fiber, belong to viscose rayon technical field.The present invention forms clad on viscose rayon surface and improves the wet strength and flame retardant property of viscose rayon under the premise of not changing fiber fine structure by wool protein solution modified flame-retardant viscose rayon, wool protein particle；Protein is high-molecular compound made of a variety of different a-amino acids are combined with each other, existing-NH in protein molecule2There is-COOH again, therefore protein can be reacted with acid but also be reacted with alkali, after spun filament enters coagulating bath, the hydroxyl on surface is oxidized to aldehyde radical and part carboxyl, these reactive groups can react with the amino in protein molecular, to which protein molecular is grafted on fiber surface, the flame retardant viscose fiber of preparation has natural gloss and soft feel, there is preferable moisture absorption, wet transmitting performance, fabulous warmth retention property.
Description
Technical field
The present invention relates to a kind of preparation methods of flame retardant viscose fiber, belong to viscose rayon technical field.
Background technique
Viscose rayon is to use the cellulose after alkalizing and carbon disulfide as reactant, under certain conditions through over-churning
Processing, is re-dissolved in the lye of certain mass score, obtains cellulose sulfonate solution, then the solution of preparation is passed through curing
Etc. spinning is carried out after processes and regeneration is made.
Great amount of hydroxy group existing for viscose rayon surface, for it is chemically and physically modified prepare various derivatives and
Blend provides condition, and viscose rayon is widely used in garment material, carbon fiber, exhaust-gas treatment, heat-resisting material, composite wood
The fields such as material.By various modifications and post-processing, the viscose rayon with different physical and chemical properties can be obtained, therefore except general
Outside logical viscose rayon, differentiation viscose rayon such as high-modulus viscose rayon, special property viscose rayon and high intensity also can be obtained
Glue clear and bright fiber etc..Although certain performances of viscose rayon are not so good as synthetic fibers, due to the distinctive physics of viscose rayon and chemistry
Structure makes owned good moisture permeability, excellent stainability energy, and can be dropped quickly by microorganism decomposition
Solution, not will cause environmental pollution, these performances make viscose rayon become the important fibre of one kind that can not be synthesized fiber substitution
Dimension.But since viscose rayon is mainly made of carbon, hydrogen and oxygen element, carbon and protium are easy to happen chemical reaction, and by
Oxidation, and not flame-retardant composition as this kind of such as halogen in its chemical component, this makes common viscose rayon in air
In be very easy to and oxygen react, there is violent burning, cause its anti-flammability very poor, it is certain special to cannot be directly used to
Purposes, this is very restricted the application of viscose rayon in some aspects, while viscose rayon product being made to have one
Fixed security risk.
It is flame-retardant modified, mainly by the way that flame retardance element is introduced or be mixed into base matter, so that material body be made to have
There is flame retardant effect: modification by copolymerization, blending fire retardant are modified and post-processing is modified etc. is divided into according to the difference of processing mode.
In order to fire preventing, safety of life and property is ensured, produce the textile with good flame-retardance energy and compel
In the eyebrows and eyelashes.Therefore, using the textile with good flame-retardance energy, for ensureing that safety of life and property is significant.
Summary of the invention
The technical problems to be solved by the invention: for the problem that existing viscose rayon anti-flammability is poor, one kind is provided
The preparation method of flame retardant viscose fiber.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water are mixed
It closes, carries out magnetic agitation processing to get thick solution, filter up to filtrate；
(2) fire retardant, deionized water, viscose glue stoste are taken, fire retardant and deionized water are mixed, 5~10min of ultrasonic disperse, i.e.,
Dispersion liquid is obtained, viscose glue stoste is added in dispersion liquid, is stirred to get blended liquid, is in deaeration temperature by blended liquid
40~60min of standing and defoaming is at 10~30 DEG C to get spinning solution；
(3) spinning solution is subjected to electrostatic spinning processing and green body is placed in coagulating bath using coagulating bath as reception source to get green body
Middle immersion treatment successively pass through to get spun filament, by spun filament multistage drafting, cutting, washing, alkali cleaning, oil, dry to get
Flame retardant viscose fiber.
Wool described in step (1), 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and
Mass ratio between deionized water is 1: 3: 15: 10: 15.
By wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite described in step (1)
It is mixed with deionized water, carries out magnetic agitation processing step are as follows: by wool, 2.2g/L sodium hydroxide solution, 15g/L dodecyl
Sodium sulphate, sodium hydrogensulfite and deionized water mixing are 70~80 DEG C in temperature, and mixing speed is 300~400r/min, sealing
Under the conditions of 3~4h of magnetic agitation.
The preparation step of fire retardant described in step (2) are as follows: in mass ratio 2: 3 mix thiocarbonyl group phosphamide and sodium metasilicate
Uniformly to get fire retardant.
Fire retardant described in step (2), deionized water, the ratio between viscose glue stoste are respectively as follows: according to parts by weight, point
Also known as take 1~10 part of fire retardant, 50~60 parts of deionized waters, 30~40 parts of viscose glue stostes.
Viscose glue stoste is added described in step (2) in dispersion liquid, is stirred step are as follows: be added in dispersion liquid
Viscose glue stoste, low whipping speed are 200~400r/min, stir 1~2h at room temperature.
Described in step (2) by blended liquid carry out deaeration processing step are as follows: by blended liquid deaeration temperature be 10~30 DEG C
40~60min of lower standing and defoaming.
Spinning solution is subjected to electrostatic spinning processing step described in step (3) are as follows: spinning solution is subjected to electrostatic spinning, spinning
60~70kV of voltage, 10~20r/min of generator revolving speed, 180~200mm of spinning distance, 1~5m/min of receiver revolving speed.
The preparation step of coagulating bath described in step (3) are as follows: filtrate, mass fraction are by mass ratio 10: 8: 23: 2: 40
70% sulfuric acid solution, sodium sulphate, zinc sulfate and deionized water are uniformly mixed to get coagulating bath.
Green body is placed in immersion treatment step in coagulating bath described in step (3) are as follows: green body is placed in coagulating bath, in temperature
Degree is that 1~2h is impregnated at 50~60 DEG C.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention is formed by wool protein solution modified flame-retardant viscose rayon, wool protein particle on viscose rayon surface
Clad improves the wet strength and flame retardant property of viscose rayon under the premise of not changing fiber fine structure；Protein
It is high-molecular compound made of a variety of different a-amino acids are combined with each other, existing-NH in protein molecule2, and have-
COOH, therefore protein can be reacted with acid but also be reacted with alkali, after spun filament enters coagulating bath, the hydroxyl on surface is oxidized to
Aldehyde radical and part carboxyl, these reactive groups can react with the amino in protein molecular, so that protein molecular is grafted
There is natural gloss and soft feel in the flame retardant viscose fiber of fiber surface, preparation, there is preferable moisture absorption, wet transmitting performance, pole
Good warmth retention property；What it is in viscose rayon surface grafting is the biggish keratin of molecular weight, they are easy to form one in fiber surface
Complete clad, and for keratin, molecular weight is bigger, and the plasticization capacity of the structure of their graft crosslinkings is stronger,
To reduce since grafting amount increases the enhancing of material fragility, the intensity of fiber is preferable；
(2) two kinds of fire retardants of thiocarbonyl group phosphamide and sodium metasilicate are blended to use by the present invention, and sodium metasilicate valence is low, nontoxic, reserves are big,
Without dense smoke when burning, residue can natural decomposition, and decomposable process no pollution to the environment, phosphorus-nitrogen collaboration in thiocarbonyl group phosphamide
Effect, flame retarding efficiency is high, and nontoxic；Sodium metasilicate is the composite solution of a variety of polysilicate compositions, and sodium metasilicate has stronger glue
Performance is tied, surface tension is smaller, and adhesion strength is strong, can soak many objects well, and sodium metasilicate is hydrolyzed into aqueous solution
Silicic acid, or and CO2Haptoreaction generates silicic acid, and can be polymerized to poly silicic acid certainly, and further dehydrating condensation is at "-Si-O-
Si- ", so as to form inoranic membrane, the inoranic membrane of generation forms the glassy interlayer of melting on viscose rayon surface, can prevent wood
The heated imflammable gas come that decomposites of material escapes and prevents the oxygen in atmosphere to enter timber, and has good heat-insulated work
With to reach good flame-retardant effect；
(3) present invention is made using composite flame-retardant agent and viscose glue dope blending as spinning solution by electrostatic spinning and coagulating bath
Flame retardant viscose fiber, coagulating bath make cellulose regenerated, and during silicic acid polymerization, zinc ion is in cellulose macromolecule and poly- former silicon
Acid molecule forms cross-linked crane span structure, and cross-linked structure, fire-retardant effective component are formed between poly- orthosilicic acid flame-retardant composition and cellulose
Completely retained, reduces and be lost, guarantee the high flame resistance of sample.
Specific embodiment
In mass ratio 1: 3: 15: 10: 15 by wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, Asia
Sodium bisulfate and deionized water mixing are 70~80 DEG C in temperature, and mixing speed is 300~400r/min, magnetic under air-proof condition
Power stirs 3~4h to get thick solution, filters up to filtrate；In mass ratio 10: 8: 23: 2: 40 by filtrate, mass fraction 70%
Sulfuric acid solution, sodium sulphate, zinc sulfate and deionized water are uniformly mixed to get coagulating bath；In mass ratio 2: 3 by thiocarbonyl group phosphamide
It is uniformly mixed with sodium metasilicate to get fire retardant；According to parts by weight, 1~10 part of fire retardant, 50~60 parts of deionizations are weighed respectively
Water, 30~40 parts of viscose glue stostes, fire retardant and deionized water are mixed, and 5~10min of ultrasonic disperse is dispersing to get dispersion liquid
Viscose glue stoste is added in liquid, low whipping speed is 200~400r/min, stirs 1~2h at room temperature to get blended liquid, will be blended
40~60min of standing and defoaming is at liquid is 10~30 DEG C in deaeration temperature to get spinning solution；Spinning solution is subjected to electrostatic spinning, is spun
60~70kV of filament voltage, 10~20r/min of generator revolving speed, 180~200mm of spinning distance, receiver 1~5m/min of revolving speed,
Using coagulating bath as reception source to get green body, green body is placed in coagulating bath, impregnates 1~2h at being 50~60 DEG C in temperature, i.e.,
Spun filament is obtained, spun filament is successively passed through to multistage drafting, cutting, washing, alkali cleaning, oils, dry to get flame retardant viscose fiber.
Example 1
Wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water are mixed, into
The processing of row magnetic agitation is filtered to get thick solution up to filtrate；Take fire retardant, deionized water, viscose glue stoste, by fire retardant and
Viscose glue stoste is added in dispersion liquid to get dispersion liquid in deionized water mixing, ultrasonic disperse 5min, be stirred to get
Blended liquid, standing and defoaming 40min is at being 10 DEG C in deaeration temperature by blended liquid to get spinning solution；Spinning solution is subjected to Static Spinning
Silk processing, using coagulating bath as reception source to get green body, green body is placed in immersion treatment in coagulating bath, will be first to get spun filament
Raw silk successively passes through multistage drafting, cutting, washing, alkali cleaning, oils, dries to get flame retardant viscose fiber.Wool, 2.2g/L hydrogen
Mass ratio between sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water is 1: 3: 15: 10:
15.Wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water are mixed, into
Row magnetic agitation processing step are as follows: by wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite
It is mixed with deionized water, is 70 DEG C, mixing speed 300r/min in temperature, magnetic agitation 3h under air-proof condition.Fire retardant
Preparation step are as follows: in mass ratio 2: 3 are uniformly mixed thiocarbonyl group phosphamide and sodium metasilicate to get fire retardant.Fire retardant, deionization
Ratio between water, viscose glue stoste is respectively as follows: according to parts by weight, weighs 1 part of fire retardant, 50 parts of deionized waters, 30 parts respectively
Viscose glue stoste.Viscose glue stoste is added in dispersion liquid, is stirred step are as follows: viscose glue stoste is added in dispersion liquid,
Mixing speed is 200r/min, stirs 1h at room temperature.Blended liquid is subjected to deaeration processing step are as follows: by blended liquid in deaeration temperature
It is standing and defoaming 40min at 10 DEG C.Spinning solution is subjected to electrostatic spinning processing step are as follows: spinning solution is subjected to electrostatic spinning, is spun
Filament voltage 60kV, generator revolving speed 10r/min, spinning distance 180mm, receiver revolving speed 1m/min.The preparation step of coagulating bath
Are as follows: in mass ratio 10: 8: 23: 2: 40 mix filtrate, mass fraction for 70% sulfuric acid solution, sodium sulphate, zinc sulfate and deionized water
It closes uniformly to get coagulating bath.Green body is placed in immersion treatment step in coagulating bath are as follows: green body is placed in coagulating bath, in temperature
It is to impregnate 1h at 50 DEG C.
Example 2
Wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water are mixed, into
The processing of row magnetic agitation is filtered to get thick solution up to filtrate；Take fire retardant, deionized water, viscose glue stoste, by fire retardant and
Viscose glue stoste is added in dispersion liquid to get dispersion liquid in deionized water mixing, ultrasonic disperse 6min, be stirred to get
Blended liquid, standing and defoaming 45min is at being 15 DEG C in deaeration temperature by blended liquid to get spinning solution；Spinning solution is subjected to Static Spinning
Silk processing, using coagulating bath as reception source to get green body, green body is placed in immersion treatment in coagulating bath, will be first to get spun filament
Raw silk successively passes through multistage drafting, cutting, washing, alkali cleaning, oils, dries to get flame retardant viscose fiber.Wool, 2.2g/L hydrogen
Mass ratio between sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water is 1: 3: 15: 10:
15.Wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water are mixed, into
Row magnetic agitation processing step are as follows: by wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite
It is mixed with deionized water, is 72 DEG C, mixing speed 320r/min in temperature, magnetic agitation 3h under air-proof condition.Fire retardant
Preparation step are as follows: in mass ratio 2: 3 are uniformly mixed thiocarbonyl group phosphamide and sodium metasilicate to get fire retardant.Fire retardant, deionization
Ratio between water, viscose glue stoste is respectively as follows: according to parts by weight, weighs 3 parts of fire retardants, 53 parts of deionized waters, 33 parts respectively
Viscose glue stoste.Viscose glue stoste is added in dispersion liquid, is stirred step are as follows: viscose glue stoste is added in dispersion liquid,
Mixing speed is 250r/min, stirs 1h at room temperature.Blended liquid is subjected to deaeration processing step are as follows: by blended liquid in deaeration temperature
It is standing and defoaming 45min at 15 DEG C.Spinning solution is subjected to electrostatic spinning processing step are as follows: spinning solution is subjected to electrostatic spinning, is spun
Filament voltage 63kV, generator revolving speed 13r/min, spinning distance 185mm, receiver revolving speed 2m/min.The preparation step of coagulating bath
Are as follows: in mass ratio 10: 8: 23: 2: 40 mix filtrate, mass fraction for 70% sulfuric acid solution, sodium sulphate, zinc sulfate and deionized water
It closes uniformly to get coagulating bath.Green body is placed in immersion treatment step in coagulating bath are as follows: green body is placed in coagulating bath, in temperature
It is to impregnate 1h at 53 DEG C.
Example 3
Wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water are mixed, into
The processing of row magnetic agitation is filtered to get thick solution up to filtrate；Take fire retardant, deionized water, viscose glue stoste, by fire retardant and
Viscose glue stoste is added in dispersion liquid to get dispersion liquid in deionized water mixing, ultrasonic disperse 8min, be stirred to get
Blended liquid, standing and defoaming 50min is at being 20 DEG C in deaeration temperature by blended liquid to get spinning solution；Spinning solution is subjected to Static Spinning
Silk processing, using coagulating bath as reception source to get green body, green body is placed in immersion treatment in coagulating bath, will be first to get spun filament
Raw silk successively passes through multistage drafting, cutting, washing, alkali cleaning, oils, dries to get flame retardant viscose fiber.Wool, 2.2g/L hydrogen
Mass ratio between sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water is 1: 3: 15: 10:
15.Wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water are mixed, into
Row magnetic agitation processing step are as follows: by wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite
It is mixed with deionized water, is 76 DEG C, mixing speed 360r/min in temperature, magnetic agitation 3h under air-proof condition.Fire retardant
Preparation step are as follows: in mass ratio 2: 3 are uniformly mixed thiocarbonyl group phosphamide and sodium metasilicate to get fire retardant.Fire retardant, deionization
Ratio between water, viscose glue stoste is respectively as follows: according to parts by weight, weighs 6 parts of fire retardants, 56 parts of deionized waters, 36 parts respectively
Viscose glue stoste.Viscose glue stoste is added in dispersion liquid, is stirred step are as follows: viscose glue stoste is added in dispersion liquid,
Mixing speed is 300r/min, stirs 1h at room temperature.Blended liquid is subjected to deaeration processing step are as follows: by blended liquid in deaeration temperature
It is standing and defoaming 50min at 20 DEG C.Spinning solution is subjected to electrostatic spinning processing step are as follows: spinning solution is subjected to electrostatic spinning, is spun
Filament voltage 66kV, generator revolving speed 16r/min, spinning distance 190mm, receiver revolving speed 3m/min.The preparation step of coagulating bath
Are as follows: in mass ratio 10: 8: 23: 2: 40 mix filtrate, mass fraction for 70% sulfuric acid solution, sodium sulphate, zinc sulfate and deionized water
It closes uniformly to get coagulating bath.Green body is placed in immersion treatment step in coagulating bath are as follows: green body is placed in coagulating bath, in temperature
It is to impregnate 1h at 56 DEG C.
Example 4
Wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water are mixed, into
The processing of row magnetic agitation is filtered to get thick solution up to filtrate；Take fire retardant, deionized water, viscose glue stoste, by fire retardant and
Viscose glue stoste is added in dispersion liquid to get dispersion liquid in deionized water mixing, ultrasonic disperse 8min, be stirred to get
Blended liquid, standing and defoaming 55min is at being 25 DEG C in deaeration temperature by blended liquid to get spinning solution；Spinning solution is subjected to Static Spinning
Silk processing, using coagulating bath as reception source to get green body, green body is placed in immersion treatment in coagulating bath, will be first to get spun filament
Raw silk successively passes through multistage drafting, cutting, washing, alkali cleaning, oils, dries to get flame retardant viscose fiber.Wool, 2.2g/L hydrogen
Mass ratio between sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water is 1: 3: 15: 10:
15.Wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water are mixed, into
Row magnetic agitation processing step are as follows: by wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite
It is mixed with deionized water, is 79 DEG C, mixing speed 390r/min in temperature, magnetic agitation 4h under air-proof condition.Fire retardant
Preparation step are as follows: in mass ratio 2: 3 are uniformly mixed thiocarbonyl group phosphamide and sodium metasilicate to get fire retardant.Fire retardant, deionization
Ratio between water, viscose glue stoste is respectively as follows: according to parts by weight, weighs 8 parts of fire retardants, 58 parts of deionized waters, 39 parts respectively
Viscose glue stoste.Viscose glue stoste is added in dispersion liquid, is stirred step are as follows: viscose glue stoste is added in dispersion liquid,
Mixing speed is 350r/min, stirs 2h at room temperature.Blended liquid is subjected to deaeration processing step are as follows: by blended liquid in deaeration temperature
It is standing and defoaming 55min at 25 DEG C.Spinning solution is subjected to electrostatic spinning processing step are as follows: spinning solution is subjected to electrostatic spinning, is spun
Filament voltage 69kV, generator revolving speed 19r/min, spinning distance 195mm, receiver revolving speed 3m/min.The preparation step of coagulating bath
Are as follows: in mass ratio 10: 8: 23: 2: 40 mix filtrate, mass fraction for 70% sulfuric acid solution, sodium sulphate, zinc sulfate and deionized water
It closes uniformly to get coagulating bath.Green body is placed in immersion treatment step in coagulating bath are as follows: green body is placed in coagulating bath, in temperature
It is to impregnate 2h at 58 DEG C.
Example 5
Wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water are mixed, into
The processing of row magnetic agitation is filtered to get thick solution up to filtrate；Take fire retardant, deionized water, viscose glue stoste, by fire retardant and
Viscose glue stoste is added in dispersion liquid, is stirred, i.e., to get dispersion liquid by deionized water mixing, ultrasonic disperse 10min
Blended liquid is obtained, standing and defoaming 60min is at being 30 DEG C in deaeration temperature by blended liquid to get spinning solution；Spinning solution is subjected to electrostatic
Spinning processing, using coagulating bath as reception source to get green body, green body is placed in immersion treatment in coagulating bath, will to get spun filament
Spun filament successively passes through multistage drafting, cutting, washing, alkali cleaning, oils, dries to get flame retardant viscose fiber.Wool, 2.2g/L
Mass ratio between sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water is 1: 3: 15: 10:
15.Wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water are mixed, into
Row magnetic agitation processing step are as follows: by wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite
It is mixed with deionized water, is 80 DEG C, mixing speed 400r/min in temperature, magnetic agitation 4h under air-proof condition.Fire retardant
Preparation step are as follows: in mass ratio 2: 3 are uniformly mixed thiocarbonyl group phosphamide and sodium metasilicate to get fire retardant.Fire retardant, deionization
Ratio between water, viscose glue stoste is respectively as follows: according to parts by weight, weighs 10 parts of fire retardants, 60 parts of deionized waters, 40 parts respectively
Viscose glue stoste.Viscose glue stoste is added in dispersion liquid, is stirred step are as follows: viscose glue stoste is added in dispersion liquid,
Mixing speed is 400r/min, stirs 2h at room temperature.Blended liquid is subjected to deaeration processing step are as follows: by blended liquid in deaeration temperature
It is standing and defoaming 60min at 30 DEG C.Spinning solution is subjected to electrostatic spinning processing step are as follows: spinning solution is subjected to electrostatic spinning, is spun
Filament voltage 70kV, generator revolving speed 20r/min, spinning distance 200mm, receiver revolving speed 5m/min.The preparation step of coagulating bath
Are as follows: in mass ratio 10: 8: 23: 2: 40 mix filtrate, mass fraction for 70% sulfuric acid solution, sodium sulphate, zinc sulfate and deionized water
It closes uniformly to get coagulating bath.Green body is placed in immersion treatment step in coagulating bath are as follows: green body is placed in coagulating bath, in temperature
It is to impregnate 2h at 60 DEG C.
Reference examples: the flame retardant viscose fiber of Dongguan company production.
The flame retardant viscose fiber that example and reference examples are prepared is detected, specific detection is as follows:
Limit oxygen index: F101D- limit oxygen index instrument is utilized, " textile combustion performance test: oxygen refers to by GB/T5454-1997
Number methods " limit oxygen index of sample after test is dry；
Mechanical property: the sample after drying is placed in SP-408A constant temperature humidity chamber, at 20 DEG C of temperature, relative humidity
Damping is for 24 hours in 65% environment.Mechanical property survey is carried out to the sample after damping using INSTRON5590 universal testing machine
Examination.
Specific test result such as table 1.
1 performance characterization contrast table of table
| Detection project | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Reference examples |
| Limit oxygen index/% | 32.8 | 31.6 | 33.5 | 33.6 | 32.9 | 18.3 |
| Elongation at break/% | 15 | 16 | 13 | 11 | 12 | 25 |
As shown in Table 1, flame retardant viscose fiber prepared by the present invention has good flame retardant property and mechanical property.
Claims (10)
1. a kind of preparation method of flame retardant viscose fiber, it is characterised in that specific preparation step are as follows:
(1) wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water are mixed
It closes, carries out magnetic agitation processing to get thick solution, filter up to filtrate；
(2) fire retardant, deionized water, viscose glue stoste are taken, fire retardant and deionized water are mixed, 5~10min of ultrasonic disperse, i.e.,
Dispersion liquid is obtained, viscose glue stoste is added in dispersion liquid, is stirred to get blended liquid, is in deaeration temperature by blended liquid
40~60min of standing and defoaming is at 10~30 DEG C to get spinning solution；
(3) spinning solution is subjected to electrostatic spinning processing and green body is placed in coagulating bath using coagulating bath as reception source to get green body
Middle immersion treatment successively pass through to get spun filament, by spun filament multistage drafting, cutting, washing, alkali cleaning, oil, dry to get
Flame retardant viscose fiber.
2. a kind of preparation method of flame retardant viscose fiber according to claim 1, it is characterised in that: described in step (1)
Mass ratio between wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water
It is 1: 3: 15: 10: 15.
3. a kind of preparation method of flame retardant viscose fiber according to claim 1, it is characterised in that: described in step (1)
Wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and deionized water are mixed, magnetic is carried out
Power stir process step are as follows: by wool, 2.2g/L sodium hydroxide solution, 15g/L lauryl sodium sulfate, sodium hydrogensulfite and go
Ionized water mixing is 70~80 DEG C in temperature, and mixing speed is 300~400r/min, 3~4h of magnetic agitation under air-proof condition.
4. a kind of preparation method of flame retardant viscose fiber according to claim 1, it is characterised in that: described in step (2)
The preparation step of fire retardant are as follows: in mass ratio 2: 3 are uniformly mixed thiocarbonyl group phosphamide and sodium metasilicate to get fire retardant.
5. a kind of preparation method of flame retardant viscose fiber according to claim 1, it is characterised in that: described in step (2)
Fire retardant, deionized water, the ratio between viscose glue stoste are respectively as follows: according to parts by weight, weigh respectively 1~10 part of fire retardant,
50~60 parts of deionized waters, 30~40 parts of viscose glue stostes.
6. a kind of preparation method of flame retardant viscose fiber according to claim 1, it is characterised in that: described in step (2)
Viscose glue stoste is added in dispersion liquid, is stirred step are as follows: viscose glue stoste is added in dispersion liquid, low whipping speed is
200~400r/min stirs 1~2h at room temperature.
7. a kind of preparation method of flame retardant viscose fiber according to claim 1, it is characterised in that: described in step (2)
Blended liquid is subjected to deaeration processing step are as follows: 40~60min of standing and defoaming at being 10~30 DEG C in deaeration temperature by blended liquid.
8. a kind of preparation method of flame retardant viscose fiber according to claim 1, it is characterised in that: described in step (3)
Spinning solution is subjected to electrostatic spinning processing step are as follows: spinning solution is subjected to electrostatic spinning, 60~70kV of spinning voltage, generator turn
10~20r/min of speed, 180~200mm of spinning distance, 1~5m/min of receiver revolving speed.
9. a kind of preparation method of flame retardant viscose fiber according to claim 1, it is characterised in that: described in step (3)
The preparation step of coagulating bath are as follows: in mass ratio 10: 8: 23: 2: 40 by filtrate, mass fraction be 70% sulfuric acid solution, sodium sulphate, sulphur
Sour zinc and deionized water are uniformly mixed to get coagulating bath.
10. a kind of preparation method of flame retardant viscose fiber according to claim 1, it is characterised in that: described in step (3)
Green body is placed in immersion treatment step in coagulating bath are as follows: green body is placed in coagulating bath, temperature be 50~60 DEG C at impregnate 1~
2h。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112918042A (en) * | 2020-06-24 | 2021-06-08 | 刘家浩 | Washable flame-retardant non-woven fabric |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1098149A (en) * | 1994-02-03 | 1995-02-01 | 赵玉山 | Flame-retarding fibre of cellulose polysilicate and production method thereof |
| CN101161878A (en) * | 2006-10-14 | 2008-04-16 | 山东海龙股份有限公司 | Flame-proof fusion-resistant viscose fiber and production method thereof |
| CN102304783A (en) * | 2011-07-07 | 2012-01-04 | 狄友波 | Preparation method of antibacterial anti-flaming protein viscose fiber |
| CN102383211A (en) * | 2011-08-30 | 2012-03-21 | 成都丽雅纤维股份有限公司 | Production technology of environmentally friendly composite flame-retardant viscose |
| CN102844477A (en) * | 2009-12-28 | 2012-12-26 | 连津格股份公司 | Functionalized molded cellulose body and method for producing the same |
| CN103668521A (en) * | 2013-12-12 | 2014-03-26 | 青岛大学 | Preparation method of water-insoluble magnesium silicate flame-retardant viscose fibers |
| CN104752658A (en) * | 2013-12-27 | 2015-07-01 | 中国科学院青岛生物能源与过程研究所 | Flame-retardant cellulose diaphragm of lithium battery prepared through electrostatic spinning |
| CN106120019A (en) * | 2016-07-19 | 2016-11-16 | 仇颖超 | A kind of moisture absorption, good permeability fire-retardant composite viscose fiber preparation method |
| CN107475794A (en) * | 2017-08-18 | 2017-12-15 | 山东银鹰化纤有限公司 | A kind of fire-retardant koplon of silicon nitrogen system and preparation method thereof |
-
2019
- 2019-05-30 CN CN201910462277.9A patent/CN110158176A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1098149A (en) * | 1994-02-03 | 1995-02-01 | 赵玉山 | Flame-retarding fibre of cellulose polysilicate and production method thereof |
| CN101161878A (en) * | 2006-10-14 | 2008-04-16 | 山东海龙股份有限公司 | Flame-proof fusion-resistant viscose fiber and production method thereof |
| CN102844477A (en) * | 2009-12-28 | 2012-12-26 | 连津格股份公司 | Functionalized molded cellulose body and method for producing the same |
| CN102304783A (en) * | 2011-07-07 | 2012-01-04 | 狄友波 | Preparation method of antibacterial anti-flaming protein viscose fiber |
| CN102383211A (en) * | 2011-08-30 | 2012-03-21 | 成都丽雅纤维股份有限公司 | Production technology of environmentally friendly composite flame-retardant viscose |
| CN103668521A (en) * | 2013-12-12 | 2014-03-26 | 青岛大学 | Preparation method of water-insoluble magnesium silicate flame-retardant viscose fibers |
| CN104752658A (en) * | 2013-12-27 | 2015-07-01 | 中国科学院青岛生物能源与过程研究所 | Flame-retardant cellulose diaphragm of lithium battery prepared through electrostatic spinning |
| CN106120019A (en) * | 2016-07-19 | 2016-11-16 | 仇颖超 | A kind of moisture absorption, good permeability fire-retardant composite viscose fiber preparation method |
| CN107475794A (en) * | 2017-08-18 | 2017-12-15 | 山东银鹰化纤有限公司 | A kind of fire-retardant koplon of silicon nitrogen system and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 全凤玉等: "无机阻燃粘胶纤维制备及结构性能研究", 《青岛大学学报(工程技术版)》 * |
| 赖小旭等: "阻燃粘胶纤维的研究进展及应用", 《成都纺织高等专科学校学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112918042A (en) * | 2020-06-24 | 2021-06-08 | 刘家浩 | Washable flame-retardant non-woven fabric |
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