CN110184666A - Spinning head used in the manufacturing method and manufacturing process of flame retardant cellulose fiber - Google Patents
Spinning head used in the manufacturing method and manufacturing process of flame retardant cellulose fiber Download PDFInfo
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- CN110184666A CN110184666A CN201910540261.5A CN201910540261A CN110184666A CN 110184666 A CN110184666 A CN 110184666A CN 201910540261 A CN201910540261 A CN 201910540261A CN 110184666 A CN110184666 A CN 110184666A
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- sulfate crystal
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- calcium sulfate
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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
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/06—Washing or drying
-
- 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
- D01D4/00—Spinnerette packs; Cleaning thereof
- D01D4/02—Spinnerettes
-
- 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
- D01D5/06—Wet spinning methods
-
- 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
- D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
-
- 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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/02—Chemical after-treatment of artificial filaments or the like during manufacture of 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
- 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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- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The present invention provides spinning heads used in the manufacturing method of flame retardant cellulose fiber and manufacturing process, belong to the field of production of viscose rayon, the following steps are included: calcium sulfate crystal whiskers and magnesium sulfate crystal whisker microcapsules processing method are obtained microcapsule-type fire retardant by (1)；(2) microcapsule flame retardant is added in atoleine, obtains mixed liquor A, the mass ratio that the gross mass of calcium sulfate crystal whiskers and magnesium sulfate crystal whisker accounts for atoleine is 16%-24%；(3) mixed liquor A is added in viscose glue syringe pump, is uniformly mixed in static mixer later, obtains mixed liquid B, calcium sulfate crystal whiskers and magnesium sulfate crystal whisker gross mass account for the 1%-15% of first fibre mass ratio in viscose glue；(4) spinning head, spinning coagulation forming in the acid bath in acid bath groove is added in mixed liquid B metering pump；(5) strand after coagulation forming is by first wash, desulfurization, second wash, soft treatment, obtained by drying.Product has the features such as excellent anti-flammability, superhigh intensity, and manufacturing method is simple.
Description
Method field
The present invention relates to the field of production of viscose rayon, the specifically manufacturing method and manufacture of flame retardant cellulose fiber
Spinning head used in process.
Background method
Cellulose is the most abundant natural high molecular substance that nature assigns the mankind, is that nature is presented to the mankind
Rich gift, its not only abundance, but also be reproducible resource, in petroleum resources increasingly depleted today, cellulose is got over
To be more valued by people.The cellulose fibre made of cellulose has good hygroscopicity, and gas permeability is strong, and dyeability is good, wears
Comfortable, the features such as being easy to textile process and biodegradability, be that other synthetic fibers cannot compare.However cellulose
Limit oxygen index (LOI) value of fiber is 19 or so, meets fire and easily burns, seriously limits it in fields such as life, industry
Use.
Existing viscose rayon preparation process are as follows: pure alpha-cellulose (pulp) is extracted by cellulosic material, with burning
Alkali, carbon disulfide processing, obtain orange-yellow sodium cellulose xanthate, are re-dissolved in diluted sodium hydroxide solution, become sticky
Spinning solution, referred to as viscose glue, viscose glue (places about 18-30h, at a certain temperature through filtering, maturation to reduce cellulose xanthan
The esterification degree of acid esters), after deaeration, carry out wet spinning, coagulating bath is made of sulfuric acid, sodium sulphate and zinc sulfate, the fibre in viscose glue
It ties up plain sodium xanthogenate and the effect of sulfuric acid in coagulating bath and decomposes, it is cellulose regenerated and be precipitated, gained cellulose fibre washed,
Become viscose rayon after desulfurization, bleaching, drying.
CN102965750A discloses a kind of manufacturing method of flame retardant viscose fiber, and this method is by receiving with flame retarding function
In 400 DEG C of kiln roastings after rice fiber-alkali magnesium sulfate crystal whisker, basic magnesium chloride whisker, magnesium salt whisker mixing, then inclined containing six
Disperse in the dehydrated alcohol of sodium phosphate, atmospheric plasma processing, then through ultrasonic wave dispersion, cleaning, 400 mesh screens, drying；
Above-mentioned whisker and titanate coupling agent are mixed later, drying, antimony oxide hexabromocyclododecane, (HDPE+ is then added
SEBS) after-g-MAH, calcium stearate mixing；It adds cellulose spinning viscose and fire-retardant cellulose spinning viscose is made；Using wet
Fire resistant viscose acetal fibre is made in method or dry spinning processes.This method preparation process is complicated, inefficiency, and gained flame-retardant fiber
It is unknown with mechanical property.
CN103147145A then discloses a kind of method that reactive extrursion prepares modified cellulose fire resistance fibre.This method is first
First uniform mixture is made in fire retardant, cellulose, solvent and acid binding agent according to a certain mass ratio, then again feeds mixture
Enter double screw extruder, by reactive extrursion method, modified flame-retardant cellulose fibre is made.Although this method is squeezed using twin-screw
Machine out, it is synchronous to implement dissolution, reaction and spinning technique, shorten process flow, production efficiency is higher.But fire-retardant fibre in this method
The plain ester degree of substitution of dimension is lower, and flame retardant effect is mainly derived from unreacted fire retardant, and gaseousness pair is also easy to produce in reaction process
Product, product application in residual fire retardant it is easy to fall off.
Summary of the invention
Above-mentioned existing flame retardant cellulose fiber poor flame retardant properties, poor mechanical property, and it is also easy to produce gas during the reaction
The shortcomings that body contact scar object.
The purpose of the present invention is to provide spinning head used in the manufacturing method of flame retardant cellulose fiber and manufacturing process,
The following steps are included:
(1) by calcium sulfate crystal whiskers and magnesium sulfate crystal whisker microcapsules processing method, microcapsule-type fire retardant is obtained；
(2) microcapsule flame retardant is added in atoleine, obtains mixed liquor A, calcium sulfate crystal whiskers and magnesium sulfate crystal whisker it is total
The mass ratio that quality accounts for atoleine is 16%-24%；
(3) mixed liquor A is added in viscose glue with syringe pump, is uniformly mixed in static mixer later, obtains mixed liquid B,
Calcium sulfate crystal whiskers and magnesium sulfate crystal whisker gross mass account for the 1%-15% of first fibre mass ratio in viscose glue；
(4) spinning head, spinning coagulation forming in the acid bath in acid bath groove is added in mixed liquid B metering pump；
(5) strand after coagulation forming passes through first wash, desulfurization, second wash, soft treatment, dries fire-retardant
Cellulose fibre.
In the technical solution of the application: calcium sulfate crystal whiskers and magnesium sulfate crystal whisker being obtained after the processing of microcapsules processing method micro-
Capsule-type fire retardant adds it to obtain mixed liquor A in atoleine later, and mixed liquor A is added in viscose glue and is uniformly mixed
Mixed liquid B is obtained, spinning head, the spinning coagulation forming in acid bath is added in mixed liquid B metering pump, rear strand passes through first time water
It washes, desulfurization, second wash, soft treatment, dry to obtain flame retardant cellulose fiber, be cellulose fibre long filament or short silk, product
It is a kind of renewable environment-friendly materials for capableing of natural degradation, there is the features such as excellent anti-flammability, superhigh intensity, be widely used in
Craftwork packing rope, indoor wallpaper, carpet and handbag rope etc.；Manufacturing method is simple, will not generate gaseousness during the reaction
Pollutant solves above-mentioned existing flame retardant cellulose fiber poor flame retardant properties, poor mechanical property, and easily produces during the reaction
The shortcomings that angry body contact scar object.
Magnesium sulfate crystal whisker with flame retarding function can since in burning dehydration occurs for the crystallization water in its molecule
A large amount of thermal energy is absorbed to reduce the temperature of substrate, in addition, the water vapour generated can dilute the concentration of flame-zone reaction gas,
Smog can be absorbed again, play the role of fire-retardant and eliminated smoke；Magnesium sulfate crystal whisker dispersion in system is preferable, magnesium sulfate crystal whisker
Outside energy can be absorbed in the presence of one side, improves the stress value cracked, on the other hand since magnesium sulfate crystal whisker has height
Deformability and tensile strength, it can acceleration energy loss and inhibit the extension of crackle, to improve cellulose fibre
Tensile strength；Enhancing component of the calcium sulfate crystal whiskers as flame retardant cellulose fiber, after calcium sulfate crystal whiskers are added in viscose glue, with sulphur
Sour magnesium whisker one works, and since the length and diameter of the two make a big difference, calcium sulfate crystal whiskers are filled with magnesium sulfate crystal whisker
Between gap, and be inorganic matter and with micron-sized formal distribution, the good dispersion in microcapsules is not easy to reunite, makes
Mechanical strength, heat resistance, anti-flammability and the excellent stability of cellulose fibre.
Preferably, in step (1) microcapsules processing method the following steps are included:
A mixes Nano chitosan, gelatin, sodium alginate, and is dissolved, is stirred evenly with water, Nano chitosan, gelatin,
The mass ratio of sodium alginate is 3-5: 3-4: 2-3；
Calcium sulfate crystal whiskers and magnesium sulfate crystal whisker are added in step A products therefrom by B after mixing, calcium sulfate crystal whiskers and
The mass ratio of magnesium sulfate crystal whisker is 1-5: 1-5, and microcapsule flame retardant is made.Magnesium sulfate crystal whisker and calcium sulfate crystal whiskers are uniformly mixed
Afterwards, it places it in Nano chitosan, gelatin and mixed solution of sodium alginate, it is wrapped up, it can be in cellulose fibre
Surface forms film, provides certain mechanical strength, in addition, Nano chitosan, gelatin and sodium alginate have moisture absorption, it is moisture-proof
Function also has the function of certain absorption pernicious gas, reduces fire retardant damage caused by environment in fire retardant burning
Evil, Nano chitosan, gelatin and sodium alginate are natural plant composition, environment friendly and pollution-free.
Preferably, in step (4) acid bath be sulfuric acid 80-160g/l, sodium sulphate 100-300g/l, zinc sulfate 10-100g/l,
The temperature of acid bath is 50-60 DEG C.
Preferably, first wash crosses the washing of drainage room temperature in step (5).
Preferably, desulfurization is to be washed with the sodium hydroxide solution in alkaline bath in step (5), and the concentration of sodium hydroxide is 5-
50g/l, wash temperature are 50-60 DEG C.
Preferably, second wash includes a deionized water washing, and temperature is 60-85 DEG C, secondary deionized water washing,
Temperature is room temperature.
Preferably, in step (5) when soft treatment, film concentration is 5-50g/l, and temperature is 35-45 DEG C.
Preferably, it is dried using hot-air in step (5), temperature when drying is 100-130 DEG C.
More preferably, it is dried using hot-air in step (5), temperature when drying is 120 DEG C.
Preferably, the calcium sulfate crystal whiskers are anhydrous calcium sulfate whisker, and the magnesium sulfate crystal whisker is alkali magnesium sulfate crystal whisker,
The characterization parameter diameter of the anhydrous calcium sulfate whisker is 1-4 μm, and length is 10-200 μm, the table of the alkali magnesium sulfate crystal whisker
Parameter diameter is levied less than 1.0 μm, 10-60 μm of length.The average aspect ratio of anhydrous calcium sulfate whisker is 20-80, absolute density
2.69-3.50g/cm3, loose density 0.1-0.5g/cm3, 1450 DEG C of fusing point, heat-resisting 1000 DEG C, pH value 6-8, calcium sulphate content >=
95%, whiteness >=85%, refraction index (25 DEG C) 1.400-1.600, arsenic, lead content≤3mg/kg, attached water≤1.5%, knot
Brilliant water≤1%；Alkali magnesium sulfate crystal whisker, appearance: white powder or discrete particles, microstructure: raphioid fiber, draw ratio >
30, specific gravity 2.3g/cm3, water content < 1.0%, pH value: 9-9.5 (2% over dry aqueous dispersion), whiteness >=93 (fluorescent whiteness).
A kind of spinning head for the manufacturing method, spinning head shape size are ￠ 10-100mm × 10-25mm, institute
The shape for stating spinneret orifice on spinning head is a straight line spray orifice, multiple straight line spray orifices, camber line spray orifice, single round spray orifice or multiple
Round spray orifice.
Preferably, the size of straight line spray orifice is 5-50mm × 0.07mm, the size of camber line spray orifice be 51-95mm ×
0.07mm, the size of round spray orifice are ￠ 5-50mm × ￠ 0.08mm.
A kind of flat cellulose fiber filament or flat cellulose short fibre obtained for the manufacturing method.
In the present processes scheme:
Compared with existing method, the beneficial effects of the present invention are:
(1) calcium sulfate crystal whiskers and magnesium sulfate crystal whisker are obtained into microcapsule-type fire retardant after the processing of microcapsules processing method, it
After add it in atoleine to obtain mixed liquor A, be added in viscose glue and be uniformly mixed mixed liquor A to obtain mixed liquid B, will mix
Spinning head, the coagulation forming in acid bath is added in liquid B metering pump, and rear spinning, soft treatment, dries to obtain fire-retardant cellulose at washing
Fiber is cellulose fibre long filament or short silk, and product is a kind of renewable environment-friendly materials for capableing of natural degradation, is had excellent
The features such as anti-flammability, superhigh intensity, is widely used in craftwork packing rope, indoor wallpaper, carpet and handbag rope etc.；Manufacturing method
Simply, gaseousness pollutant will not be generated during the reaction, solve above-mentioned existing flame retardant cellulose fiber flame retardant property
Difference, poor mechanical property, and the shortcomings that be also easy to produce gaseousness pollutant during the reaction；
(2) with the magnesium sulfate crystal whisker of flame retarding function, since in burning dehydration occurs for the crystallization water in its molecule
A large amount of thermal energy is can absorb to reduce the temperature of substrate, in addition, the water vapour generated can dilute the dense of flame-zone reaction gas
Degree, and smog can be absorbed, play the role of fire-retardant and eliminated smoke；Magnesium sulfate crystal whisker dispersion in system is preferable, and magnesium sulfate is brilliant
On the one hand the presence of palpus can absorb outside energy, improve the stress value cracked, on the other hand since magnesium sulfate crystal whisker has
There are high deformability and tensile strength, the loss of its energy acceleration energy and the extension for inhibiting crackle, to improve cellulose fiber
The tensile strength of dimension；Enhancing component of the calcium sulfate crystal whiskers as flame retardant cellulose fiber, after calcium sulfate crystal whiskers are added in viscose glue,
It works with magnesium sulfate crystal whisker one, since the length and diameter of the two make a big difference, calcium sulfate crystal whiskers are filled with magnesium sulfate
Gap between whisker, and be inorganic matter and with micron-sized formal distribution, the good dispersion in microcapsules, the group of being not easy
It is poly-, make mechanical strength, heat resistance, anti-flammability and the excellent stability of cellulose fibre；
(3) present invention by magnesium sulfate crystal whisker and calcium sulfate crystal whiskers after mixing, place it in Nano chitosan, gelatin and
In mixed solution of sodium alginate, it is wrapped up, film can be formed in cellulose fiber surface, it is strong to provide certain machinery
Degree, in addition, Nano chitosan, gelatin and sodium alginate have moisture absorption, moisture-proof function also has one in fire retardant burning
The function of fixed absorption pernicious gas, reduces fire retardant damage caused by environment, Nano chitosan, gelatin and sodium alginate
It is natural plant composition, it is environment friendly and pollution-free；
(4) shape of spinneret orifice is a straight line spray orifice, multiple straight line spray orifices, camber line spray orifice, single circle on spinning head
Spray orifice or multiple round spray orifices；
(5) spun product is one or more silk；
(6) product obtained is flat cellulose fiber filament or flat cellulose short fibre.
Detailed description of the invention
Fig. 1 is the flow diagram of the manufacturing method of herein described flame retardant cellulose fiber；
Fig. 2 is that the shape of spinneret orifice on the application spinning head is the structural schematic diagram of a straight line spray orifice；
Fig. 3 is that the shape of spinneret orifice on the application spinning head is camber line jet orifice structure schematic diagram；
Fig. 4 is that the shape of spinneret orifice on the application spinning head is multiple straight line jet orifice structure schematic diagrames；
Fig. 5 is that the shape of spinneret orifice on the application spinning head is single round jet orifice structure schematic diagram；
Fig. 6 is that the shape of spinneret orifice on the application spinning head is multiple round jet orifice structure schematic diagrames.
Marked in the figure: 1- syringe pump, 2- static mixer, 3- metering pump, 4- acid bath groove, 5- spinning head, 6- alkaline bath.
In flow chart: A indicates whisker pretreatment, includes the steps that in the manufacturing method of flame retardant cellulose fiber (1) and walks
Suddenly (2), B are viscose glue, and C is strand, and D is filtering washing, and E is a deionization washing, and F washes for secondary deionized water, and G is softness
Processing, H are drying.
Specific embodiment
It is right combined with specific embodiments below for the method personnel that make this field methods of this invention will be better understood scheme
The present invention is described in further detail.
Embodiment 1
Such as Fig. 1-2, the manufacturing method of flame retardant cellulose fiber, comprising the following steps:
(1) by calcium sulfate crystal whiskers and magnesium sulfate crystal whisker microcapsules processing method, microcapsule-type fire retardant is obtained,
Microcapsules processing method the following steps are included:
A mixes Nano chitosan, gelatin, sodium alginate, and is dissolved, is stirred evenly with water, Nano chitosan, gelatin,
The mass ratio of sodium alginate is 3: 3: 2；
Calcium sulfate crystal whiskers and magnesium sulfate crystal whisker are added in step A products therefrom by B after mixing, calcium sulfate crystal whiskers and
The mass ratio of magnesium sulfate crystal whisker is 1: 5, microcapsule flame retardant is made, the calcium sulfate crystal whiskers are anhydrous calcium sulfate whisker, described
Magnesium sulfate crystal whisker is alkali magnesium sulfate crystal whisker, and the characterization parameter diameter of the anhydrous calcium sulfate whisker is 1-4 μm, length 10-
200 μm, the characterization parameter diameter of the alkali magnesium sulfate crystal whisker is less than 1.0 μm, 10-60 μm of length；
(2) microcapsule flame retardant is added in atoleine, obtains mixed liquor A, calcium sulfate crystal whiskers and magnesium sulfate crystal whisker it is total
The mass ratio that quality accounts for atoleine is 16%；
(3) mixed liquor A is added in viscose glue with syringe pump 1, is uniformly mixed in static mixer 2 later, obtains mixed liquor
B, calcium sulfate crystal whiskers and magnesium sulfate crystal whisker gross mass account for 1% of first fibre mass ratio in viscose glue；
(4) spinning head 5 is added in mixed liquid B metering pump 3, the coagulation forming in the acid bath in acid bath groove 4, acid bath is sulphur
Sour 80g/l, sodium sulphate 100g/l, zinc sulfate 10g/l, the temperature of acid bath are 50 DEG C；
(5) strand after coagulation forming passes through first wash, desulfurization, second wash, soft treatment, dries fire-retardant
Cellulose fibre, first wash cross the washing of drainage room temperature；Desulfurization is to be washed with the sodium hydroxide solution in alkaline bath 6, hydrogen-oxygen
The concentration for changing sodium is 5g/l, and wash temperature is 50 DEG C；Second wash includes the washing of deionized water, and temperature is 60 DEG C, and two
Secondary deionized water washing, temperature is room temperature；When soft treatment, film concentration is 50g/l, and temperature is 35 DEG C；It is dried using hot-air
Dry, temperature when drying is 100 DEG C.
A kind of spinning head 5 for the manufacturing method, 5 shape size of spinning head are ￠ 10mm × 10mm or ￠ 55mm
× 18mm or ￠ 100mm × 25mm, the shape of spinneret orifice is a straight line spray orifice, the size of straight line spray orifice on the spinning head 5
For 5mm × 0.07mm or 25mm × 0.07mm or 50mm × 0.07mm.
A kind of cellulose fibre long filament obtained for the manufacturing method.
In the present embodiment, strand intensity is 9.0cn/dtex, and limit oxygen index (LOI) is 38.
Embodiment 2
Such as the manufacturing method of Fig. 1 and Fig. 3 flame retardant cellulose fiber, comprising the following steps:
(1) by calcium sulfate crystal whiskers and magnesium sulfate crystal whisker microcapsules processing method, microcapsule-type fire retardant is obtained,
Microcapsules processing method the following steps are included:
A mixes Nano chitosan, gelatin, sodium alginate, and is dissolved, is stirred evenly with water, Nano chitosan, gelatin,
The mass ratio of sodium alginate is 4: 3.5: 2.5；
Calcium sulfate crystal whiskers and magnesium sulfate crystal whisker are added in step A products therefrom by B after mixing, calcium sulfate crystal whiskers and
The mass ratio of magnesium sulfate crystal whisker is 1: 1, microcapsule flame retardant is made, the calcium sulfate crystal whiskers are anhydrous calcium sulfate whisker, described
Magnesium sulfate crystal whisker is alkali magnesium sulfate crystal whisker, and the characterization parameter diameter of the anhydrous calcium sulfate whisker is 1-4 μm, length 10-
200 μm, the characterization parameter diameter of the alkali magnesium sulfate crystal whisker is less than 1.0 μm, 10-60 μm of length；
(2) microcapsule flame retardant is added in atoleine, obtains mixed liquor A, calcium sulfate crystal whiskers and magnesium sulfate crystal whisker it is total
The mass ratio that quality accounts for atoleine is 20%；
(3) mixed liquor A is added in viscose glue with syringe pump 1, is uniformly mixed in static mixer 2 later, obtains mixed liquor
B, calcium sulfate crystal whiskers and magnesium sulfate crystal whisker gross mass account for 10% of first fibre mass ratio in viscose glue；
(4) spinning head 5 is added in mixed liquid B metering pump 3, the coagulation forming in the acid bath in acid bath groove 4, acid bath is sulphur
Sour 120g/l, sodium sulphate 200g/l, zinc sulfate 55g/l, the temperature of acid bath are 55 DEG C；
(5) strand of coagulation forming passes through first wash, desulfurization, second wash, soft treatment, dries to obtain fire-retardant fibre
Cellulose fiber, first wash cross the washing of drainage room temperature；Desulfurization is to be washed with the sodium hydroxide solution in alkaline bath 6, hydroxide
The concentration of sodium is 27g/l, and wash temperature is 55 DEG C；Second wash includes a deionized water washing, and temperature is 72 DEG C, secondary
Deionized water washing, temperature is room temperature；When soft treatment, film concentration is 30g/l, and temperature is 40 DEG C；It is dried using hot-air,
Temperature when drying is 115 DEG C.
A kind of spinning head 5 for the manufacturing method, 5 shape size of spinning head are ￠ 10mm × 10mm or ￠ 55mm
× 18mm or ￠ 100mm × 25mm, the shape of spinneret orifice is multiple straight line spray orifices, the size of straight line spray orifice on the spinning head 5
For 5mm × 0.07mm or 25mm × 0.07mm or 50mm × 0.07mm.
A kind of cellulose fibre long filament obtained for the manufacturing method.
In the present embodiment, strand intensity is 9.8cn/dtex, and limit oxygen index (LOI) is 39.
Embodiment 3
Such as Fig. 1 and Fig. 4, the manufacturing method of flame retardant cellulose fiber, comprising the following steps:
(1) by calcium sulfate crystal whiskers and magnesium sulfate crystal whisker microcapsules processing method, microcapsule-type fire retardant is obtained, at microcapsules
Reason method the following steps are included:
A mixes Nano chitosan, gelatin, sodium alginate, and is dissolved, is stirred evenly with water, Nano chitosan, gelatin,
The mass ratio of sodium alginate is 5: 4: 3；
Calcium sulfate crystal whiskers and magnesium sulfate crystal whisker are added in step A products therefrom by B after mixing, calcium sulfate crystal whiskers and
The mass ratio of magnesium sulfate crystal whisker is 1: 2, microcapsule flame retardant is made, the calcium sulfate crystal whiskers are anhydrous calcium sulfate whisker, described
Magnesium sulfate crystal whisker is alkali magnesium sulfate crystal whisker, and the characterization parameter diameter of the anhydrous calcium sulfate whisker is 1-4 μm, length 10-
200 μm, the characterization parameter diameter of the alkali magnesium sulfate crystal whisker is less than 1.0 μm, 10-60 μm of length；
(2) microcapsule flame retardant is added in atoleine, obtains mixed liquor A, calcium sulfate crystal whiskers and magnesium sulfate crystal whisker it is total
The mass ratio that quality accounts for atoleine is 24%；
(3) mixed liquor A is added in viscose glue with syringe pump 1, is uniformly mixed in static mixer 2 later, obtains mixed liquor
B, calcium sulfate crystal whiskers and magnesium sulfate crystal whisker gross mass account for 15% of first fibre mass ratio in viscose glue；
(4) spinning head 5 is added in mixed liquid B metering pump 3, the coagulation forming in the acid bath in acid bath groove 4, acid bath is sulphur
Sour 160g/l, sodium sulphate 300g/l, zinc sulfate 100g/l, the temperature of acid bath are 60 DEG C；
(5) strand of coagulation forming passes through first wash, desulfurization, second wash, soft treatment, dries to obtain fire-retardant fibre
Cellulose fiber, first wash cross the washing of drainage room temperature；Desulfurization is to be washed with the sodium hydroxide solution in alkaline bath 6, hydroxide
The concentration of sodium is 50g/l, and wash temperature is 60 DEG C；Second wash includes a deionized water washing, and temperature is 85 DEG C, secondary
Deionized water washing, temperature is room temperature；When soft treatment, film concentration is 5g/l, and temperature is 45 DEG C；It is dried using hot-air,
Temperature when drying is 130 DEG C.
A kind of spinning head 5 for the manufacturing method, 5 shape size of spinning head are ￠ 10mm × 10mm or ￠ 55mm
× 18mm or ￠ 100mm × 25mm, the shape of spinneret orifice is camber line spray orifice on the spinning head 5, and the size of camber line spray orifice is
51mm × 0.07mm or 72mm × 0.07mm or 95mm × 0.07mm.
A kind of cellulose fibre long filament obtained for the manufacturing method.
In the present embodiment, strand intensity is 9.0cn/dtex, and limit oxygen index (LOI) is 37.
Embodiment 4
In the present embodiment, the mass ratio of calcium sulfate crystal whiskers and magnesium sulfate crystal whisker is 2: 1, the shape of spinneret orifice on spinning head 5
For single round spray orifice, the size of round spray orifice is ￠ 5mm × ￠ 0.08mm or ￠ 25mm × ￠ 0.08mm or ￠ 50mm × ￠
0.08mm, remaining is the same as described in embodiment 2.
A kind of short silk of cellulose fibre obtained for the manufacturing method.
Embodiment 5
In the present embodiment, the mass ratio of calcium sulfate crystal whiskers and magnesium sulfate crystal whisker is 5: 1, the shape of spinneret orifice on spinning head 5
For multiple round spray orifices, the size of round spray orifice is ￠ 5mm × ￠ 0.08mm or ￠ 25mm × ￠ 0.08mm or ￠ 50mm × ￠
0.08mm, remaining is the same as described in embodiment 1.
A kind of short silk of cellulose fibre obtained for the manufacturing method.
The specific embodiment of the application above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
The limitation to the application protection scope therefore cannot be interpreted as.It should be pointed out that for the commonsense method personnel of this field
For, under the premise of not departing from the application method plan plot, various modifications and improvements can be made, these belong to this
The protection scope of application.
Claims (10)
1. the manufacturing method of flame retardant cellulose fiber, which comprises the following steps:
(1) by calcium sulfate crystal whiskers and magnesium sulfate crystal whisker microcapsules processing method, microcapsule-type fire retardant is obtained；
(2) microcapsule flame retardant is added in atoleine, obtains mixed liquor A, the gross mass of calcium sulfate crystal whiskers and magnesium sulfate crystal whisker
The mass ratio for accounting for atoleine is 16%-24%；
(3) mixed liquor A is added in viscose glue with syringe pump (1), is uniformly mixed in static mixer (2) later, obtains mixed liquor
B, calcium sulfate crystal whiskers and magnesium sulfate crystal whisker gross mass account for the 1%-15% of first fibre mass ratio in viscose glue；
(4) spinning head, the spinning coagulation forming in the acid bath in acid bath groove (4) is added with metering pump (3) in mixed liquid B；
(5) strand after coagulation forming passes through first wash, desulfurization, second wash, soft treatment, dries to obtain fire resistance fibre
Cellulose fiber.
2. the manufacturing method of the flame retardant cellulose fiber according to requiring 1, which is characterized in that microcapsules are handled in step (1)
Method the following steps are included:
Nano chitosan, gelatin, sodium alginate are mixed, and are dissolved with water by A, are stirred evenly, Nano chitosan, gelatin, seaweed
The mass ratio of sour sodium is 3-5: 3-4: 2-3；
Calcium sulfate crystal whiskers and magnesium sulfate crystal whisker are added in step A products therefrom by B after mixing, calcium sulfate crystal whiskers and sulfuric acid
The mass ratio of magnesium whisker is 1-5: 1-5, and microcapsule flame retardant is made.
3. the manufacturing method of the flame retardant cellulose fiber according to requiring 1, which is characterized in that first wash in step (5)
Cross the washing of drainage room temperature.
4. the manufacturing method of the flame retardant cellulose fiber according to requiring 1, which is characterized in that desulfurization is to use alkali in step (5)
Sodium hydroxide solution washing in washing trough (6), the concentration of sodium hydroxide are 5-50g/l, and wash temperature is 50-60 DEG C.
5. the manufacturing method of the flame retardant cellulose fiber according to requiring 1, which is characterized in that second wash includes once going
Ion water washing, temperature are 60-85 DEG C, and secondary deionized water washing, temperature is room temperature.
6. the manufacturing method of the flame retardant cellulose fiber according to requiring 1, which is characterized in that in step (5) when soft treatment,
Film concentration is 5-50g/l, and temperature is 35-45 DEG C.
7. the manufacturing method of the flame retardant cellulose fiber according to requiring 1 or 2, which is characterized in that the calcium sulfate crystal whiskers are
Anhydrous calcium sulfate whisker, the magnesium sulfate crystal whisker are alkali magnesium sulfate crystal whisker, and the characterization parameter of the anhydrous calcium sulfate whisker is straight
Diameter is 1-4 μm, and length is 10-200 μm, and the characterization parameter diameter of the alkali magnesium sulfate crystal whisker is less than 1.0 μm, length 10-60 μ
m。
8. a kind of spinning head for the described in any item manufacturing methods of claim 1-7, which is characterized in that spinning head (5) is outside
Shape size is ￠ 10-100mm × 10-25mm, and the shape of spinneret orifice is straight line spray orifice, a Duo Gezhi on the spinning head (5)
Line spray orifice, camber line spray orifice, single round spray orifice or multiple round spray orifices.
9. a kind of spinning head for the described in any item manufacturing methods of claim 8, which is characterized in that the size of straight line spray orifice
For 5-50mm × 0.07mm, the size of camber line spray orifice is 51-95mm × 0.07mm, and the size of round spray orifice is ￠ 5-50mm × ￠
0.08mm。
10. a kind of cellulose fibre long filament or short silk obtained for the described in any item manufacturing methods of claim 1-7.
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| CN110747528A (en) * | 2019-11-29 | 2020-02-04 | 河北科技大学 | Flame-retardant microcapsule and preparation method and application thereof |
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| CN110184666B (en) | 2021-11-16 |
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