CN107653511A - A kind of preparation method of viscose staple fibre - Google Patents

A kind of preparation method of viscose staple fibre Download PDF

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Publication number
CN107653511A
CN107653511A CN201710961349.5A CN201710961349A CN107653511A CN 107653511 A CN107653511 A CN 107653511A CN 201710961349 A CN201710961349 A CN 201710961349A CN 107653511 A CN107653511 A CN 107653511A
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pulp
chitosan
staple fibre
mass ratio
viscose staple
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高俊
徐颜峰
陈龙
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/02Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/07Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/09Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/18Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances

Abstract

The invention discloses a kind of preparation method of viscose staple fibre, belong to textile material technical field.Pulp is mixed with soda bath, impregnated, filtering, obtains alkalization pulp;Pulp will be alkalized through squeezing, crushing, obtain crushing pulp, activation chitosan mixed liquor will be mixed with crushing pulp, and add nano silicon, sonic oscillation obtains chitosan pulp mixture, by chitosan pulp mixture through experienced, after yellow, obtains spinning solution;By spinning solution after spinning-drawing machine spinning, drawing-off in drafting machine is added, precursor is obtained, after precursor treatment fluid hybrid reaction, then ammonia is passed through into treatment fluid, continues to react, obtain processing precursor, after processing precursor is washed with deionized, dried, obtain viscose staple fibre.Viscose staple fibre prepared by the present invention has excellent mechanical performance, while the antistatic behaviour of viscose staple fibre and biocidal property are all improved.

Description

A kind of preparation method of viscose staple fibre
Technical field
The invention discloses a kind of preparation method of viscose staple fibre, belong to textile material technical field.
Background technology
Viscose staple fibre obtains as a kind of common and important chemical raw material in industrial production and daily life It is extensive to use, but its combination property such as antistatic property etc. has much room for improvement.
FRC has inorganic FRC, the major class of organic fire-resisting viscose rayon two.Organic fire-resisting viscose glue is fine For the inorganic fire-retarded viscose rayon of peacekeeping silicon nitrogen system because being influenceed by fire retardant price is high, its price is also expensive, make its application market by To considerable restraint.And the inorganic fire-retarded viscose rayon produced with silicates fire retardant, not only fire retardant is cheap, fire-retardant effect Fruit is good, also have low cigarette during burning, without poison gas, do not melt the good characteristics such as drippage, thus its application prospect is very good.It is but raw To ensure that its efficient flame retardant effect need to add a large amount of silicate fire retardants when producing silicate inorganic fire retardant viscose short filament, cause The dry fracture strength of finished fiber, wet breaking strength are relatively low, it is impossible to meet downstream textile mills spinning requirement, be only capable of producing non-woven Dry goods product, application field are very limited.
Secondly, one of bacteriostasis property evaluation viscose staple fibre combination property.At present, antibacterial chopped fiber preparation method mainly has Two kinds, when finishing method, second, fiber blend is modified method.Finishing method is to develop earliest and continue up textile so far Antibacterial processing method, this method is with the solution containing antiseptic or finished fiber and fabric are impregnated resin or coating processing, So as to assign fiber and antibacterial fabric activity, easy to operate and alternative antiseptic scope is wide, but finishing method obtains The anti-microbial property persistence of antibacterial fabric is poor, in general by the antibacterial fabric that afterfinish method is processed in washing time Afterwards, antibacterial functions almost without.Fiber blend is modified method compared with finishing method, due to the equal Uniform distributions of antiseptic in the fibre Therefore washing resistance performance is better than the fiber and fabric obtained through antibiotic finish, antibacterial efficacy is more longlasting.In addition, the process of final finishing at present The antiseptic of addition is mainly inorganic antiseptic and organic antiseptic.Wherein inorganic antiseptic mainly there is antibacterial to make Metal inorganic salt and antibacterial zeolite particles, inorganic antiseptic contain contents of many kinds of heavy metal ion, not only to the hand of textile after addition Sense and wearing comfortable have a great impact, and easily by being good for contact human skin and the influence human body that is absorbed by the body Health.
Therefore, viscose staple fibre antistatic property, fire resistance, bacteriostasis property and mechanical property are improved, turns into its popularization With applied to broader field urgent problem to be solved.
The content of the invention
The present invention solves the technical problem of:It is antibacterial for traditional viscose staple fibre antistatic property, fire resistance A kind of the problem of performance and bad mechanical property, there is provided preparation method of viscose staple fibre.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
(1)By chitosan and biogas slurry in mass ratio 1:7~1:10 mixing, ferment at constant temperature, concentrated by rotary evaporation, chitosan concentration must be activated Liquid;
(2)By silver nitrate and calcium nitrate in mass ratio 2:1~3:1 mixing, and add the nitric acid of 0.6~0.8 times of silver nitrate quality The water of 30~40 times of aluminium and silver nitrate quality, is stirred, obtains mixed liquor;
(3)By chitosan concentrate and mixed liquor in mass ratio 5:1~8:1 mixes, and after stirring reaction, must activate chitosan mixing Liquid;
(4)By pulp and sodium hydroxide solution in mass ratio 1:4~1:7 mixing, impregnate, and filtering, obtain alkalization pulp;
(5)By alkalization pulp through squeezing, crush, obtain crushing pulp, chitosan mixed liquor will be activated and crush pulp in mass ratio 2:3~2:5 mixing, and the nano silicon for crushing 0.08~0.10 times of pulp quality is added, sonic oscillation, obtain chitosan slurry Dregs of rice mixture, by chitosan pulp mixture through experienced, after yellow, obtain spinning solution;
(6)By spinning solution after spinning-drawing machine spinning, drawing-off in drafting machine is added, obtains precursor, by reducing agent and water in mass ratio 1:4~1:8 mixing, obtain treatment fluid, by precursor and treatment fluid in mass ratio 1:8~1:12 mixing, after ultrasonic immersing, then to processing Ammonia is passed through in liquid, continues to react, obtains processing precursor, by processing precursor washing, dries, obtains viscose staple fibre.
Step(2)Described silver nitrate, calcium nitrate and aluminum nitrate are that analysis is pure.
Step(3)The pulp is wood pulps, any one in bamboo pulp or Cotton Pulp.
Step(6)Described reducing agent is any one in zinc powder or vitamin C.
The beneficial effects of the invention are as follows:
(1)The present invention makes addition activate chitosan when preparing viscose staple fibre, and first, chitosan is after activated, active group Group's number increases, and can react and combine with the pulp small molecule after alkalization, so that the molecule between viscose staple fibre combines Power strengthens, and is improved the mechanical strength of product, and secondly, activation chitosan is living after being added in viscose staple fibre system Change chitosan molecule and can be adsorbed on viscose staple fibre molecular surface, and because chitosan has the ability of chelated metal ions, So that metal ion can be in viscose rayon adsorption, while disperseed well;
(2)The present invention adds silver nitrate in the chitosan mixed liquor that viscose staple fibre uses is prepared, and silver ion can be gathered by shell Sugar chelating, and then viscose staple fibre surface is evenly distributed on, moreover, after reducing agent is added, silver ion can be from chelating systems In be replaced out, equally distributed elemental silver is formed in the system of chitosan and viscose staple fibre, so that product is anti- Antistatic property and bacteriostasis property are improved;
(3)The present invention adds calcium nitrate and aluminum nitrate in the chitosan mixed liquor that viscose staple fibre uses is prepared, and Add nano silicon and ammonia in post-processing into viscose staple fibre system, the calcium in the calcium nitrate and aluminum nitrate of addition Ion and chlorion can be chelated by chitosan molecule, be evenly distributed on viscose staple fibre surface, after ammonia is passed through into system, The calcium ion and aluminium ion of chelating can gradually become hydroxide and be present in system, run into high-temperature condition meeting in use The raw oxide adsorbent that is dehydrated into viscose staple fibre surface, caused moisture can effective blocking oxygen, play fire retardation, and shape Into oxide can densification be covered in fiber surface, play heat-insulating flame-retardant effect, also, add nano-silica surface live Property it is higher, after being added in system, hydration reaction can occur with the hydroxide of formation, form hydrated product, so as in viscose glue Chopped fiber surface forms one layer of hydrated gel diaphragm with some strength, the mechanical performance of product is further increased By force.
Brief description of the drawings
The specific testing result of Fig. 1 viscose staple fibre fire resistances.
The specific testing result of Fig. 2 viscose staple fibre mechanical properties.
Embodiment
By chitosan and biogas slurry in mass ratio 1:7~1:10 are mixed in fermentation cauldron, in the condition that temperature is 32~38 DEG C Under, ferment at constant temperature 3~5 days, obtain chitosan zymotic fluid, by chitosan zymotic fluid move into Rotary Evaporators, in temperature be 75~85 DEG C, rotating speed is 150~180r/min, under conditions of pressure is 600~800Pa, 1~2h of concentrated by rotary evaporation, it is dense must to activate chitosan Contracting liquid;By silver nitrate and calcium nitrate in mass ratio 2:1~3:1 is mixed in beaker, and silver nitrate quality 0.6 is added into beaker ~0.8 times of aluminum nitrate and the water of 30~40 times of silver nitrate quality, beaker immigration digital display is tested the speed constant temperature blender with magnetic force, Yu Wen Spend for 50~60 DEG C, under conditions of rotating speed is 280~350r/min, constant temperature 45~55min of stirring reaction, obtain mixed liquor;By shell Glycan concentrate and mixed liquor in mass ratio 5:1~8:1 mixing, it is 45~60 DEG C in temperature, rotating speed is 280~320r/min's Under the conditions of be stirred, chitosan mixed liquor must be activated;Pulp and mass fraction are pressed into matter for 30~40% sodium hydroxide solution Measure ratio 1:4~1:7 mixing, under conditions of temperature is 25~32 DEG C, 80~100min is impregnated, filtering, obtains alkalization pulp;By alkali After being squeezed in slurrying dregs of rice squeezer, move into pulverizer and crush, obtain crushing pulp, by activation chitosan mixed liquor with crushing pulp In mass ratio 2:3~2:5 mixing, and the nano silicon for crushing 0.08~0.10 times of pulp quality is added, blank is obtained, by base Material moves into sonic oscillation instrument, under conditions of frequency is 50~60kHz, 25~50min of sonic oscillation, filtering, obtains chitosan slurry Dregs of rice mixture, chitosan pulp mixture is moved into experienced drum and carries out experienced operation, under conditions of temperature is 20~28 DEG C, After going out 30~60min of processing always, experienced mixture is obtained, experienced mixture is added in xanthating machine, and is added always into xanthating machine The carbon disulfide that 0.04~0.06 times of resulting mixture quality, under conditions of temperature is 25~32 DEG C, 60~70min of yellow, obtain Spinning solution;Spinning solution is moved into spinning-drawing machine and is woven into silk, and the silk being spun into moves into drawing-off in drafting machine, obtains precursor, By reducing agent and water in mass ratio 1:4~1:8 mixing, it is 50~60 DEG C in temperature, rotating speed is under conditions of 280~300r/min It is stirred, obtains treatment fluid, by precursor and treatment fluid in mass ratio 1:8~1:Sonic oscillation instrument is moved into after 12 mixing, in frequency For 50~60kHz bar enter under, after 45~60min of ultrasonic immersing, obtain dipping mixed liquor, and with 10~15mL/min speed to Ammonia is passed through in dipping mixed liquor, continues 50~70min of reaction, filters, obtains processing precursor, processing precursor is washed with deionized water After washing 3~5 times, drying box is moved into, under conditions of temperature is 80~120 DEG C, 20~35min is dried, obtains viscose staple fibre.Institute The silver nitrate stated, calcium nitrate and aluminum nitrate are that analysis is pure.The pulp is wood pulps, any one in bamboo pulp or Cotton Pulp Kind.Described reducing agent is any one in zinc powder or vitamin C.
Example 1
By chitosan and biogas slurry in mass ratio 1:10 are mixed in fermentation cauldron, under conditions of temperature is 38 DEG C, ferment at constant temperature 5 My god, chitosan zymotic fluid is obtained, chitosan zymotic fluid is moved into Rotary Evaporators, is 85 DEG C, rotating speed 180r/min in temperature, presses Under conditions of power is 800Pa, concentrated by rotary evaporation 2h, chitosan concentrate must be activated;By silver nitrate and calcium nitrate in mass ratio 3:1 is mixed Together in beaker, and the aluminum nitrate of 0.8 times of silver nitrate quality and the water of 40 times of silver nitrate quality are added into beaker, beaker is moved Enter digital display to test the speed constant temperature blender with magnetic force, in temperature be 60 DEG C, under conditions of rotating speed is 350r/min, constant temperature stirring reaction 55min, obtain mixed liquor;By chitosan concentrate and mixed liquor in mass ratio 8:1 mixing, in temperature be 60 DEG C, rotating speed 320r/ It is stirred under conditions of min, chitosan mixed liquor must be activated;Pulp is pressed with mass fraction for 40% sodium hydroxide solution Mass ratio 1:7 mixing, under conditions of temperature is 32 DEG C, 100min is impregnated, filtering, obtains alkalization pulp;Will alkalization pulp squeezing After being squeezed in machine, move into pulverizer and crush, obtain crushing pulp, by activation chitosan mixed liquor with crushing pulp in mass ratio 2: 5 mixing, and the nano silicon for crushing 0.10 times of pulp quality is added, blank is obtained, blank is moved into sonic oscillation instrument, Yu Pin Under conditions of rate is 60kHz, sonic oscillation 50min, filtering, chitosan pulp mixture is obtained, chitosan pulp mixture is moved Enter and experienced operation is carried out in experienced drum, under conditions of temperature is 28 DEG C, go out always after handling 60min, obtain experienced mixture, will be old Resulting mixture is added in xanthating machine, and the carbon disulfide of experienced 0.06 times of mixture quality is added into xanthating machine, is in temperature Under conditions of 32 DEG C, yellow 70min, spinning solution is obtained;Spinning solution is moved into spinning-drawing machine and is woven into silk, and the silk being spun into Drawing-off in drafting machine is moved into, precursor is obtained, by reducing agent and water in mass ratio 1:8 mixing, in temperature be 60 DEG C, rotating speed 300r/ It is stirred under conditions of min, obtains treatment fluid, by precursor and treatment fluid in mass ratio 1:Sonic oscillation instrument is moved into after 12 mixing, Under the bar that frequency is 60kHz enters, after ultrasonic immersing 60min, dipping mixed liquor is obtained, and it is mixed to dipping with 15mL/min speed Close in liquid and be passed through ammonia, continue to react 70min, filtering, obtain processing precursor, after processing precursor is washed with deionized into 5 times, move Enter drying box, under conditions of temperature is 120 DEG C, dries 35min, obtain viscose staple fibre.Described silver nitrate, calcium nitrate and nitre Sour aluminium is that analysis is pure.The pulp is wood pulps.Described reducing agent is zinc powder.
Example 2
By silver nitrate and calcium nitrate in mass ratio 3:1 is mixed in beaker, and the nitre of 0.8 times of silver nitrate quality is added into beaker The water of sour 40 times of aluminium and silver nitrate quality, beaker immigration digital display is tested the speed constant temperature blender with magnetic force, is 60 DEG C in temperature, rotating speed is Under conditions of 350r/min, constant temperature stirring reaction 55min, mixed liquor is obtained;Pulp is molten for 40% sodium hydroxide with mass fraction Liquid in mass ratio 1:7 mixing, under conditions of temperature is 32 DEG C, 100min is impregnated, filtering, obtains alkalization pulp;To be alkalized pulp After being squeezed in squeezer, move into pulverizer and crush, obtain crushing pulp, by nano silicon with crushing pulp in mass ratio 1: 10 mixing, obtain blank, and blank is moved into sonic oscillation instrument, under conditions of frequency is 60kHz, sonic oscillation 50min, and filtering, Chitosan pulp mixture, chitosan pulp mixture is moved into experienced drum and carry out experienced operation, in temperature be 28 DEG C Under the conditions of, go out always after handling 60min, obtain experienced mixture, experienced mixture is added in xanthating machine, and is added into xanthating machine The carbon disulfide of experienced 0.06 times of mixture quality, under conditions of temperature is 32 DEG C, yellow 70min, obtain spinning solution;It will spin Silk stock solution moves into spinning-drawing machine and is woven into silk, and the silk being spun into moves into drawing-off in drafting machine, obtains precursor, reducing agent and water are pressed Mass ratio 1:8 mixing, it is 60 DEG C in temperature, rotating speed is stirred under conditions of being 300r/min, obtains treatment fluid, by precursor and place Manage liquid in mass ratio 1:Sonic oscillation instrument is moved into after 12 mixing, under the bar that frequency is 60kHz enters, after ultrasonic immersing 60min, is obtained Mixed liquor is impregnated, and ammonia is passed through into dipping mixed liquor with 15mL/min speed, continues to react 70min, filtering, must handle Precursor, after processing precursor is washed with deionized into 5 times, drying box is moved into, under conditions of temperature is 120 DEG C, dried 35min, obtain viscose staple fibre.Described silver nitrate, calcium nitrate and aluminum nitrate are that analysis is pure.The pulp is wood pulps.Institute The reducing agent stated is zinc powder.
Example 3
By chitosan and biogas slurry in mass ratio 1:10 are mixed in fermentation cauldron, under conditions of temperature is 38 DEG C, ferment at constant temperature 5 My god, chitosan zymotic fluid is obtained, chitosan zymotic fluid is moved into Rotary Evaporators, is 85 DEG C, rotating speed 180r/min in temperature, presses Under conditions of power is 800Pa, concentrated by rotary evaporation 2h, chitosan concentrate must be activated;By aluminum nitrate and calcium nitrate in mass ratio 12:5 It is mixed in beaker, and the water of 50 times of aluminum nitrate quality is added into beaker, beaker immigration digital display is tested the speed temperature constant magnetic stirring Device, it is 60 DEG C in temperature, under conditions of rotating speed is 350r/min, constant temperature stirring reaction 55min, obtains mixed liquor;Chitosan is dense Contracting liquid and mixed liquor in mass ratio 8:1 mixing, it is 60 DEG C in temperature, rotating speed is stirred under conditions of being 320r/min, obtains work Change chitosan mixed liquor;By the sodium hydroxide solution in mass ratio 1 that pulp and mass fraction are 40%:7 mixing, in temperature be 32 Under conditions of DEG C, 100min is impregnated, filtering, obtains alkalization pulp;After being squeezed in alkalization pulp squeezer, powder in pulverizer is moved into It is broken, crushing pulp is obtained, by activation chitosan mixed liquor with crushing pulp in mass ratio 2:5 mixing, and add crushing pulp quality 0.10 times of nano silicon, obtains blank, and blank is moved into sonic oscillation instrument, and under conditions of frequency is 60kHz, ultrasound is shaken 50min is swung, filters, obtains chitosan pulp mixture, chitosan pulp mixture is moved into experienced drum and carries out experienced operation, in Under conditions of temperature is 28 DEG C, goes out always after handling 60min, obtain experienced mixture, experienced mixture is added in xanthating machine, and to The carbon disulfide of experienced 0.06 times of mixture quality is added in xanthating machine, under conditions of temperature is 32 DEG C, yellow 70min, is obtained Spinning solution;Spinning solution is moved into spinning-drawing machine and is woven into silk, and the silk being spun into moves into drawing-off in drafting machine, obtains precursor, By precursor and water in mass ratio 1:Sonic oscillation instrument is moved into after 12 mixing, under the bar that frequency is 60kHz enters, ultrasonic immersing After 60min, dipping mixed liquor is obtained, and ammonia is passed through into dipping mixed liquor with 15mL/min speed, continues to react 70min, Filtering, obtains processing precursor, after processing precursor is washed with deionized into 5 times, moves into drying box, in the condition that temperature is 120 DEG C Under, 35min is dried, obtains viscose staple fibre.Described calcium nitrate and aluminum nitrate is that analysis is pure.The pulp is wood pulps.
Example 4
By chitosan and biogas slurry in mass ratio 1:10 are mixed in fermentation cauldron, under conditions of temperature is 38 DEG C, ferment at constant temperature 5 My god, chitosan zymotic fluid is obtained, chitosan zymotic fluid is moved into Rotary Evaporators, is 85 DEG C, rotating speed 180r/min in temperature, presses Under conditions of power is 800Pa, concentrated by rotary evaporation 2h, chitosan concentrate must be activated;By silver nitrate and water in mass ratio 1:40 mixing In beaker, beaker immigration digital display is tested the speed constant temperature blender with magnetic force, is 60 DEG C in temperature, rotating speed is 350r/min condition Under, constant temperature stirring reaction 55min, obtain mixed liquor;By chitosan concentrate and mixed liquor in mass ratio 8:1 mixing, it is in temperature 60 DEG C, rotating speed is stirred under conditions of being 320r/min, must activate chitosan mixed liquor;It is 40% by pulp and mass fraction Sodium hydroxide solution in mass ratio 1:7 mixing, under conditions of temperature is 32 DEG C, 100min is impregnated, filtering, must alkalize slurry The dregs of rice;Will alkalization pulp squeezer in squeeze after, move into pulverizer in crush, obtain crushing pulp, will activation chitosan mixed liquor with Crush pulp in mass ratio 2:5 mixing, obtain blank, and blank is moved into sonic oscillation instrument, under conditions of frequency is 60kHz, surpass Sound oscillation 50min, filtering, obtains chitosan pulp mixture, and chitosan pulp mixture is moved into experienced drum and carries out experienced behaviour Make, under conditions of temperature is 28 DEG C, goes out always after handling 60min, obtain experienced mixture, experienced mixture is added into xanthating machine In, and the carbon disulfide of experienced 0.06 times of mixture quality is added into xanthating machine, and under conditions of temperature is 32 DEG C, yellow 70min, obtain spinning solution;Spinning solution is moved into spinning-drawing machine and is woven into silk, and the silk being spun into moves into drawing-off in drafting machine, Precursor is obtained, by reducing agent and water in mass ratio 1:8 mixing, it is 60 DEG C in temperature, rotating speed stirs mixed under conditions of being 300r/min Close, treatment fluid is obtained, by precursor and treatment fluid in mass ratio 1:Sonic oscillation instrument is moved into after 12 mixing, in the bar that frequency is 60kHz Under entering, after ultrasonic immersing 60min, dipping mixed liquor is obtained, filters, obtains processing precursor, processing precursor is washed with deionized 5 times Afterwards, drying box is moved into, under conditions of temperature is 120 DEG C, 35min is dried, obtains viscose staple fibre.Described silver nitrate is analysis It is pure.The pulp is wood pulps.Described reducing agent is zinc powder.
Comparative example:The viscose staple fibre of Nantong Fabritex S.r.l production.
The viscose staple fibre of the gained of example 1 to 4 and comparative example product are subjected to performance detection, specific detection method is as follows:
1. mechanical property:Dry fracture strength is carried out to test specimen according to GB/T14463 detection methods, wet breaking strength and dry fracture are stretched Long rate detection;
2. fire resistance:Test specimen limited oxygen index is detected according to FZ/T50016 detection methods;
3. bacteriostasis property:Biocidal property detection is carried out to test specimen according to GB/T14463 detection methods, and calculated respectively to golden yellow Portugal Grape coccus and Escherichia coli bacteriostasis rate;
4. antistatic property:Test specimen ratio resistance is detected according to standard GB/T12703, antistatic fibre can be divided into A, B, C Three-level, ratio resistance are less than 107Ω cm are A levels, and ratio resistance is more than or equal to 107Ω cm are less than 1010Ω cm are B levels, than electricity Resistance is more than or equal to 1010Ω cm are less than or equal to 1013Ω cm are C levels.Ratio resistance is smaller, then antistatic property is better.
The specific testing result of fire resistance is shown in brief description of the drawings Fig. 1.
The specific testing result of mechanical property is shown in brief description of the drawings Fig. 2.
The specific testing result of bacteriostasis property is as shown in table 1:
Table 1
The specific testing result of antistatic property is as shown in table 2:
Table 2
Detection project Example 1 Example 2 Example 3 Example 4 Comparative example
Ratio resistance(Ω·cm) 1.3×106 2.6×106 8.5×106 3.3×106 1.9×108
From Fig. 1, Fig. 2, Tables 1 and 2 testing result, viscose staple fibre prepared by technical solution of the present invention has excellent power The characteristics of learning performance and fire resistance, while its biocidal property and antistatic behaviour also obtain larger improvement, in textile material industry Development in have broad prospects.

Claims (4)

1. a kind of preparation method of viscose staple fibre, it is characterised in that specifically preparation process is:
(1)By chitosan and biogas slurry in mass ratio 1:7~1:10 mixing, ferment at constant temperature, concentrated by rotary evaporation, chitosan concentration must be activated Liquid;
(2)By silver nitrate and calcium nitrate in mass ratio 2:1~3:1 mixing, and add the nitric acid of 0.6~0.8 times of silver nitrate quality The water of 30~40 times of aluminium and silver nitrate quality, is stirred, obtains mixed liquor;
(3)By chitosan concentrate and mixed liquor in mass ratio 5:1~8:1 mixes, and after stirring reaction, must activate chitosan mixing Liquid;
(4)By pulp and sodium hydroxide solution in mass ratio 1:4~1:7 mixing, impregnate, and filtering, obtain alkalization pulp;
(5)By alkalization pulp through squeezing, crush, obtain crushing pulp, chitosan mixed liquor will be activated and crush pulp in mass ratio 2:3~2:5 mixing, and the nano silicon for crushing 0.08~0.10 times of pulp quality is added, sonic oscillation, obtain chitosan slurry Dregs of rice mixture, by chitosan pulp mixture through experienced, after yellow, obtain spinning solution;
(6)By spinning solution after spinning-drawing machine spinning, drawing-off in drafting machine is added, obtains precursor, by reducing agent and water in mass ratio 1:4~1:8 mixing, obtain treatment fluid, by precursor and treatment fluid in mass ratio 1:8~1:12 mixing, after ultrasonic immersing, then to processing Ammonia is passed through in liquid, continues to react, filters, obtains processing precursor, by processing precursor washing, dries, obtains viscose staple fibre.
A kind of 2. preparation method of viscose staple fibre according to claim 1, it is characterised in that:Step(2)Described nitre Sour silver, calcium nitrate and aluminum nitrate are that analysis is pure.
A kind of 3. preparation method of viscose staple fibre according to claim 1, it is characterised in that:Step(3)The pulp For wood pulps, any one in bamboo pulp or Cotton Pulp.
A kind of 4. preparation method of viscose staple fibre according to claim 1, it is characterised in that:Step(6)Described goes back Former agent is any one in zinc powder or vitamin C.
CN201710961349.5A 2017-10-17 2017-10-17 A kind of preparation method of viscose staple fibre Pending CN107653511A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102304783A (en) * 2011-07-07 2012-01-04 狄友波 Preparation method of antibacterial anti-flaming protein viscose fiber
CN103643332A (en) * 2013-12-04 2014-03-19 阜宁澳洋科技有限责任公司 Functional composite fiber and preparation method thereof
CN106496998A (en) * 2016-11-18 2017-03-15 郑州丽福爱生物技术有限公司 A kind of high performance polycarbonate composite and preparation method and application

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102304783A (en) * 2011-07-07 2012-01-04 狄友波 Preparation method of antibacterial anti-flaming protein viscose fiber
CN103643332A (en) * 2013-12-04 2014-03-19 阜宁澳洋科技有限责任公司 Functional composite fiber and preparation method thereof
CN106496998A (en) * 2016-11-18 2017-03-15 郑州丽福爱生物技术有限公司 A kind of high performance polycarbonate composite and preparation method and application

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