CN102978735B - Preparation method of flame-retardant droplet-resistant terylene - Google Patents
Preparation method of flame-retardant droplet-resistant terylene Download PDFInfo
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- CN102978735B CN102978735B CN201210488858.8A CN201210488858A CN102978735B CN 102978735 B CN102978735 B CN 102978735B CN 201210488858 A CN201210488858 A CN 201210488858A CN 102978735 B CN102978735 B CN 102978735B
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34924—Triazines containing cyanurate groups; Tautomers thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
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- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
- D01F6/84—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyesters
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- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/023—Silicon
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/026—Phosphorus
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
- C08K2003/3063—Magnesium sulfate
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
Abstract
The invention discloses a preparation method of flame-retardant droplet-resistant terylene. The preparation method comprises the following steps of: A) evenly mixing four materials including a flame-retardant droplet resistant basic magnesium sulfate whisker, a beta-type silicon nitride whisker, a tetrapod-like zinc oxide whisker and a magnesium salt whisker, baking the mixture in a vacuum furnace; stirring and dispersing the mixture in a sodium hexametaphosphate solution, carrying out atmospheric pressure plasma treatment, and then filtering and baking the solution by a filter with 200 meshes; B) mixing the whiskers obtained from the step A) with flame-retardant melamine cyanurate, a microencapsulated red phosphorus retardant, and a silane coupling agent under the condition of 75 DEG C; C) preparing a flame-retardant droplet resistant whisker ethylene glycol solution by a flame-retardant droplet resistant whisker obtained in the step B); and D) preparing a flame-retardant droplet resistant polyester from the flame-retardant droplet resistant whisker in a blending or copolyester manner, and preparing the sheath-core flame-retardant droplet resistant terylene of taking the flame-retardant droplet resistant polyester as a skin layer by using a compound spinning technology.
Description
Technical field
The present invention relates to a kind of manufacture method of flame-retardant and anti-dripping terylene, described flame-retardant and anti-dripping terylene comprises polyester (PET), melamine cyanurate, microencapsulation red phosphorus combustion inhibitor, four acicular type zinc oxide crystal whisker, β type silicon nitride crystal whisker, alkali magnesium sulfate crystal whisker, magnesium salt whisker; Belong to textile fabric manufacturing technology field.
Background technology
Terylene is to be made by polyethylene terephthalate (PET).It is the first kind of current synthetic fiber.Because the rigidity of fiber macromolecular chain is larger, elastic modelling quantity is high, and fiber is not yielding, after its fabric washing, does not wrinkle, and can not press, strongly very scrapes, easily washes easily dry.Also having good heat-resisting, cold-resistant, sun-proof and ABRASION RESISTANCE, is a kind of more satisfactory textile raw material.Terylene is widely used in that dress ornament, decoration, family are spun, building and industrial circle.
In the modern life, to get rid of outside natural disaster and war, main disaster is exactly fire, as the saying goes " floods and fires have no mercy ".The basic material of terylene is oil, and the limited oxygen index of terylene only has 21 left and right, belongs to meltbility easy firing fiber.When terylene provides rich and varied material conditions to the mankind thus, also to the mankind, hidden a lot of disaster hidden-troubles.More seriously can there is melting drippage in terylene goods under burning or high temperature, causes the more conflagration that scald and kindling material migration cause.For safety, must improve the flame-retardant and anti-dripping of terylene.The demand of flame-retardant and anti-dripping terylene is had no precedent as today and is increased sharply.
Manufacture flame-retardant and anti-dripping terylene, conventionally introduce containing fire proofing, as add the compounds such as chloride, bromine, phosphorus, antimony, anti-molten drop agent, make blending type or copoly type flame-retardant and anti-dripping terylene, in order to subtract low-fiber inflammability and anti-molten drop.The flame-retardant and anti-dripping terylene that this kind of method manufactured, generally, the acquisition of flame-retardant and anti-dripping is that to take other performance of sacrificial fiber be cost, along with adding fire-retardant, anti-molten drop agent, fibre strength, degree of stretching tend to become weak; Feel variation; Spinning, weave difficulty.
Whisker is the diameter very little (0.1～10um), length atomic arrangement high-sequential, the intensity that form with the monocrystalline form growth theoretical value that approaches perfect crystal, the fibrous material that has certain draw ratio (5～1000), and the length of whisker is several times to tens times of macromolecular material macromolecular chain length.In macromolecular material, add a small amount of whisker, just can strengthen, toughness reinforcing, also can improve heat resistance etc.Be a kind of desirable macromolecular material reinforced modifier, have a wide range of applications field.
Inorganic crystal whisker fusing point is very high, conventionally all more than 1000 ℃, has just in time made up the deficiency of macromolecular material aspect heat-resisting, makes the glass transition temperature of system and heat distortion temperature all have rising, has fire resistance.What be most widely used is alkali magnesium sulfate crystal whisker, because the crystallization water in its molecule, when burning, dehydration occurs, can absorb the temperature that a large amount of heat energy reduces base material.In addition, the water vapour of generation can dilute the concentration of flame-zone reaction gas, can absorb smog again, plays effect fire-retardant and that eliminate smoke.
Magnesium salt whisker, four acicular type zinc oxide crystal whisker all have good flame-retardant and anti-dripping effect, more more superior than conventional flame-retardant and anti-dripping material.
Summary of the invention
The object of the invention is to overcome the deficiency that prior art exists, provide a kind of intensity high, good toughness, flame-retardant and anti-dripping, is specially adapted to the manufacture method of the flame-retardant and anti-dripping terylene of public area fire safety requirement.
The object of the invention is to complete by following technical solution, the manufacture method of described flame-retardant and anti-dripping terylene, it adopts following steps:
A) by mass fraction, getting 4-8 part characterization parameter diameter is the alkali magnesium sulfate crystal whisker that 0.1-1um, length are 5-12um, 2-6 part characterization parameter diameter is the four acicular type zinc oxide crystal whisker that 0.1-0.8um, length are 6-10um, 4-8 part characterization parameter diameter is the magnesium salt whisker that 0.2-0.8um, length are 6-10um, and 2-6 part characterization parameter diameter is the β type silicon nitride crystal whisker that 0.1-0.6um, length are 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 4-6h in 350-450 ℃ of vacuum drying oven, after cooling, containing stirring in the absolute ethyl alcohol of calgon to shear, disperseing 30-45min, then atmospheric plasma is processed 10-20min, in the 60-70 ℃ of deionized water for ultrasonic wavelength-division containing calcium stearate dispersion, fall apart, clean again 25-35min, getting solution upper strata suspension whisker filters through 200 orders, get modified crystal whiskers mixed liquor, and repeat 3-5 time until filtering, after filtering, at vacuum drying oven, dry, obtain modified crystal whiskers;
B) by mass fraction, get steps A) modified crystal whiskers 6-10 part of obtaining, under expansion type flame retardant melamine cyanurate 4-8 part, microencapsulation red phosphorus combustion inhibitor 1-2 part, KH-550 silane coupler 0.5-1.5 part, the condition that exists at 70-80 ℃ of a small amount of nonionic surface active agent, in mixer, airtight high-speed stirred reaction 45-60min, obtains flame-retardant and anti-dripping whisker;
C) by mass fraction, be to be made into flame-retardant and anti-dripping whisker ethylene glycol liquid with 6-4 part ethylene glycol under the condition that exists at micro-calgon of the flame-retardant and anti-dripping whisker of 4-6 part, temperature is controlled at ultrasonic wave under 50-60 ℃ of condition and disperses 2.5-5h, obtains flame-retardant and anti-dripping whisker ethylene glycol;
D) the flame-retardant and anti-dripping whisker ethylene glycol of getting 30-40 part by mass fraction adds in the polycondensation vessel that has 70-60 part terephthalate, until copolyesters flame-retardant and anti-dripping polyester is made in esterification, polymerization;
Or E) get step B) the flame-retardant and anti-dripping whisker that obtains and normal polyester in mass ratio 25-35 ﹕ 75-65 blended melting make the anti-molten drop polyester of blending fire retardant;
F) by step D) the copolyesters flame-retardant and anti-dripping polyester or the step e that obtain) the anti-molten drop polyester of blending fire retardant that obtains and PET, PTT, PBT polyester, take flame-retardant and anti-dripping component as cortex, and 20-40 ﹕ 80-60 makes a kind of core-skin type flame-retardant and anti-dripping terylene through composite spinning technology in mass ratio.
The preferred technical scheme of the present invention is:
A) by mass fraction, getting 6 parts of characterization parameter diameters is the alkali magnesium sulfate crystal whisker that 0.1-1um, length are 5-12um, 4 parts of characterization parameter diameters are the four acicular type zinc oxide crystal whisker that 0.1-0.8um, length are 6-10um, 6 parts of characterization parameter diameters are the magnesium salt whisker that 0.2-0.8um, length are 6-10um, and 4 parts of characterization parameter diameters are the β type silicon nitride crystal whisker that 0.1-0.6um, length are 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 5h in 400 ℃ of vacuum drying ovens, after cooling, containing stirring in the absolute ethyl alcohol of calgon to shear, disperseing 38min, then atmospheric plasma is processed 15min, then, cleaning 30min loose in 65 ℃ of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion, gets solution upper strata suspension whisker and filters through 200 orders, get modified crystal whiskers mixed liquor, and repeat 4 times until filtering is dried at vacuum drying oven after filtering, obtain modified crystal whiskers;
B) by mass fraction, get A) 8 parts of the modified crystal whiskers that obtain, with 6 parts of expansion type flame retardant melamine cyanurates, 1.5 parts of microencapsulation red phosphorus combustion inhibitors, 1 part of KH-550 silane coupler, under the condition existing at 75 ℃ of a small amount of nonionic surface active agent, in mixer, airtight high-speed stirred reaction 55min, obtains flame-retardant and anti-dripping whisker;
C) by mass fraction, be to be made into flame-retardant and anti-dripping whisker ethylene glycol liquid with 5 parts of ethylene glycol under the condition that exists at micro-calgon of the flame-retardant and anti-dripping whisker of 5 parts, temperature is controlled at ultrasonic wave under 55 ℃ of conditions and disperses 3.5h, obtains flame-retardant and anti-dripping whisker ethylene glycol;
D) by mass fraction, get the flame-retardant and anti-dripping whisker ethylene glycol of 35 parts and add in the polycondensation vessel that has 65 parts of terephthalates, until copolyesters flame-retardant and anti-dripping polyester is made in esterification, polymerization;
F) by step D) the copolyesters flame-retardant and anti-dripping polyester that obtains and PET, PTT, PBT polyester, take flame-retardant and anti-dripping component as cortex, 30 ﹕ 70 make a kind of core-skin type flame-retardant and anti-dripping terylene through composite spinning technology in mass ratio.
The another kind of preferred technical scheme of the present invention is:
A) by mass fraction, getting 6 parts of characterization parameter diameters is the alkali magnesium sulfate crystal whisker that 0.1-1um, length are 5-12um, 4 parts of characterization parameter diameters are the four acicular type zinc oxide crystal whisker that 0.1-0.8um, length are 6-10um, 6 parts of characterization parameter diameters are the magnesium salt whisker that 0.2-0.8um, length are 6-10um, and 4 parts of characterization parameter diameters are the β type silicon nitride crystal whisker that 0.1-0.6um, length are 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 5h in 400 ℃ of vacuum drying ovens, after cooling, containing stirring in the absolute ethyl alcohol of calgon to shear, disperseing 38min, then atmospheric plasma is processed 15min, then, cleaning 30min loose in 65 ℃ of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion, gets solution upper strata suspension whisker and filters through 200 orders, get modified crystal whiskers mixed liquor, and repeat 4 times until filtering is dried at vacuum drying oven after filtering, obtain modified crystal whiskers;
B) by mass fraction, get steps A) 8 parts of the modified crystal whiskers that obtain, with 6 parts of expansion type flame retardant melamine cyanurates, 1.5 parts of microencapsulation red phosphorus combustion inhibitors, 1 part of KH-550 silane coupler, under the condition existing at 75 ℃ of a small amount of nonionic surface active agent, in mixer, airtight high-speed stirred reaction 55min, obtains flame-retardant and anti-dripping whisker;
E) get step B) the flame-retardant and anti-dripping whisker that obtains and normal polyester in mass ratio 30 ﹕ 70 blended meltings make the anti-molten drop polyester of blending fire retardant;
F) by step e) the anti-molten drop polyester of blending fire retardant that obtains and PET, PTT, PBT polyester, take flame-retardant and anti-dripping component as cortex, 30 ﹕ 70 make a kind of core-skin type flame-retardant and anti-dripping terylene through composite spinning technology in mass ratio.
The present invention is at described step D) in: in polyethylene terephthalate polymerization process, when esterification yield reaches 85-90%, the flame-retardant and anti-dripping whisker ethylene glycol of getting 35 parts by mass fraction adds in the polycondensation vessel that has 65 parts of terephthalates, until copolyesters flame-retardant and anti-dripping polyester is made in esterification, polymerization.
Flame-retardant and anti-dripping polyester of the present invention is spun into PDY, DTY, BCF, BSY, nonwoven fabric through blend or complex technique; Or described flame-retardant and anti-dripping polyester adopts blend or complex technique to make flame-retardant and anti-dripping polyester sheet, tubing, bar, wire rod.
The present invention adds and has humidification in polyester, there is melamine cyanurate, microencapsulation red phosphorus combustion inhibitor, four acicular type zinc oxide crystal whisker, alkali magnesium sulfate crystal whisker, magnesium salt whisker, β type silicon nitride crystal whisker of flame-retardant and anti-dripping function etc. simultaneously, by melt composite spinning means, make and take the core-skin type flame-retardant and anti-dripping terylene that flame-retardant and anti-dripping component is cortex; When terylene goods are under burning or high temperature, polyester is melted, the fracture of thermal cracking, macromolecular chain, but the whisker being dispersed in polyester can not be melted, can thermal cracking yet, and whisker can not rupture, can not burn yet; Whisker and fire retardant obstruct burning and the drippage of polyester fondant as flame-retardant and anti-dripping muscle silk screen, have the anti-molten drop effect of fabulous flame resistance.This whisker adds the flame-retardant and anti-dripping terylene of fire retardant, and intensity is high, good toughness, and flame-retardant and anti-dripping, can be widely used in decorating, family is spun, building and fire-fighting, thermal technology, military industry field, is specially adapted to the fire safety requirement of public area.
The specific embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail: the manufacture method of a kind of flame-retardant and anti-dripping terylene of the present invention, and this manufacture method adopts following steps:
A) by mass fraction, getting 4-8 part characterization parameter diameter is the alkali magnesium sulfate crystal whisker that 0.1-1um, length are 5-12um, 2-6 part characterization parameter diameter is the four acicular type zinc oxide crystal whisker that 0.1-0.8um, length are 6-10um, 4-8 part characterization parameter diameter is the magnesium salt whisker that 0.2-0.8um, length are 6-10um, and 2-6 part characterization parameter diameter is the β type silicon nitride crystal whisker that 0.1-0.6um, length are 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 4-6h in 350-450 ℃ of vacuum drying oven, after cooling, containing stirring in the absolute ethyl alcohol of calgon to shear, disperseing 30-45min, then atmospheric plasma is processed 10-20min, in the 60-70 ℃ of deionized water for ultrasonic wavelength-division containing calcium stearate dispersion, fall apart, clean again 25-35min, getting solution upper strata suspension whisker filters through 200 orders, get modified crystal whiskers mixed liquor, and repeat 3-5 time until filtering, after filtering, at vacuum drying oven, dry, obtain modified crystal whiskers;
B) by mass fraction, get steps A) modified crystal whiskers 6-10 part of obtaining, under expansion type flame retardant melamine cyanurate 4-8 part, microencapsulation red phosphorus combustion inhibitor 1-2 part, KH-550 silane coupler 0.5-1.5 part, the condition that exists at 70-80 ℃ of a small amount of nonionic surface active agent, in mixer, airtight high-speed stirred reaction 45-60min, obtains flame-retardant and anti-dripping whisker;
C) by mass fraction, be to be made into flame-retardant and anti-dripping whisker ethylene glycol liquid with 6-4 part ethylene glycol under the condition that exists at micro-calgon of the flame-retardant and anti-dripping whisker of 4-6 part, temperature is controlled at ultrasonic wave under 50-60 ℃ of condition and disperses 2.5-5h, obtains flame-retardant and anti-dripping whisker ethylene glycol;
D) the flame-retardant and anti-dripping whisker ethylene glycol of getting 30-40 part by mass fraction adds in the polycondensation vessel that has 70-60 part terephthalate, until copolyesters flame-retardant and anti-dripping polyester is made in esterification, polymerization;
Or E) get step B) the flame-retardant and anti-dripping whisker that obtains and normal polyester in mass ratio 25-35 ﹕ 75-65 blended melting make the anti-molten drop polyester of blending fire retardant;
F) by step D) the copolyesters flame-retardant and anti-dripping polyester or the step e that obtain) the anti-molten drop polyester of blending fire retardant that obtains and PET, PTT, PBT polyester, take flame-retardant and anti-dripping component as cortex, and 20-40 ﹕ 80-60 makes a kind of core-skin type flame-retardant and anti-dripping terylene through composite spinning technology in mass ratio.
Described step D) in: in polyethylene terephthalate polymerization process, when esterification yield reaches 85-90%, the flame-retardant and anti-dripping whisker ethylene glycol of getting 35 parts by mass fraction adds in the polycondensation vessel that has 65 parts of terephthalates, until copolyesters flame-retardant and anti-dripping polyester is made in esterification, polymerization.
Described flame-retardant and anti-dripping polyester is spun into PDY, DTY, BCF, BSY, nonwoven fabric through blend or complex technique; Or described flame-retardant and anti-dripping polyester adopts blend or complex technique to make flame-retardant and anti-dripping polyester sheet, tubing, bar, wire rod.
Embodiment 1: the manufacture method of flame-retardant and anti-dripping terylene of the present invention, and it adopts following steps:
A) by mass fraction, getting 6 parts of characterization parameter diameters is the alkali magnesium sulfate crystal whisker that 0.1-1um, length are 5-12um, 4 parts of characterization parameter diameters are the four acicular type zinc oxide crystal whisker that 0.1-0.8um, length are 6-10um, 6 parts of characterization parameter diameters are the magnesium salt whisker that 0.2-0.8um, length are 6-10um, and 4 parts of characterization parameter diameters are the β type silicon nitride crystal whisker that 0.1-0.6um, length are 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 5h in 400 ℃ of vacuum drying ovens, after cooling, containing stirring in the absolute ethyl alcohol of calgon to shear, disperseing 38min, then atmospheric plasma is processed 15min, then, cleaning 30min loose in 65 ℃ of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion, gets solution upper strata suspension whisker and filters through 200 orders, get modified crystal whiskers mixed liquor, and repeat 4 times until filtering is dried at vacuum drying oven after filtering, obtain modified crystal whiskers;
B) by mass fraction, get A) 8 parts of the modified crystal whiskers that obtain, with 6 parts of expansion type flame retardant melamine cyanurates, 1.5 parts of microencapsulation red phosphorus combustion inhibitors, 1 part of KH-550 silane coupler, under the condition existing at 75 ℃ of a small amount of nonionic surface active agent, in mixer, airtight high-speed stirred reaction 55min, obtains flame-retardant and anti-dripping whisker;
C) by mass fraction, be to be made into flame-retardant and anti-dripping whisker ethylene glycol liquid with 5 parts of ethylene glycol under the condition that exists at micro-calgon of the flame-retardant and anti-dripping whisker of 5 parts, temperature is controlled at ultrasonic wave under 55 ℃ of conditions and disperses 3.5h, obtains flame-retardant and anti-dripping whisker ethylene glycol;
D) by mass fraction, get the flame-retardant and anti-dripping whisker ethylene glycol of 35 parts and add in the polycondensation vessel that has 65 parts of terephthalates, until copolyesters flame-retardant and anti-dripping polyester is made in esterification, polymerization;
F) by step D) the copolyesters flame-retardant and anti-dripping polyester that obtains and PET, PTT, PBT polyester, take flame-retardant and anti-dripping component as cortex, 30 ﹕ 70 make a kind of core-skin type flame-retardant and anti-dripping terylene through composite spinning technology in mass ratio.
Embodiment 2: the manufacture method of flame-retardant and anti-dripping terylene of the present invention, and it adopts following steps:
A) by mass fraction, getting 6 parts of characterization parameter diameters is the alkali magnesium sulfate crystal whisker that 0.1-1um, length are 5-12um, 4 parts of characterization parameter diameters are the four acicular type zinc oxide crystal whisker that 0.1-0.8um, length are 6-10um, 6 parts of characterization parameter diameters are the magnesium salt whisker that 0.2-0.8um, length are 6-10um, and 4 parts of characterization parameter diameters are the β type silicon nitride crystal whisker that 0.1-0.6um, length are 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 5h in 400 ℃ of vacuum drying ovens, after cooling, containing stirring in the absolute ethyl alcohol of calgon to shear, disperseing 38min, then atmospheric plasma is processed 15min, then, cleaning 30min loose in 65 ℃ of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion, gets solution upper strata suspension whisker and filters through 200 orders, get modified crystal whiskers mixed liquor, and repeat 4 times until filtering is dried at vacuum drying oven after filtering, obtain modified crystal whiskers;
B) by mass fraction, get steps A) 8 parts of the modified crystal whiskers that obtain, with 6 parts of expansion type flame retardant melamine cyanurates, 1.5 parts of microencapsulation red phosphorus combustion inhibitors, 1 part of KH-550 silane coupler, under the condition existing at 75 ℃ of a small amount of nonionic surface active agent, in mixer, airtight high-speed stirred reaction 55min, obtains flame-retardant and anti-dripping whisker;
E) get step B) the flame-retardant and anti-dripping whisker that obtains and normal polyester in mass ratio 30 ﹕ 70 blended meltings make the anti-molten drop polyester of blending fire retardant;
F) by step e) the anti-molten drop polyester of blending fire retardant that obtains and PET, PTT, PBT polyester, take flame-retardant and anti-dripping component as cortex, 30 ﹕ 70 make a kind of core-skin type flame-retardant and anti-dripping terylene through composite spinning technology in mass ratio.
Embodiment 3: a kind of manufacture method of flame-retardant and anti-dripping terylene, and this manufacture method adopts following steps:
A) by mass fraction, getting 4 parts of characterization parameter diameters is the alkali magnesium sulfate crystal whisker that 0.1-1um, length are 5-12um, 2 parts of characterization parameter diameters are the four acicular type zinc oxide crystal whisker that 0.1-0.8um, length are 6-10um, 4 parts of characterization parameter diameters are the magnesium salt whisker that 0.2-0.8um, length are 6-10um, and 2 parts of characterization parameter diameters are the β type silicon nitride crystal whisker that 0.1-0.6um, length are 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 4h in 350 ℃ of vacuum drying ovens, after cooling, containing stirring in the absolute ethyl alcohol of calgon to shear, disperseing 30min, then atmospheric plasma is processed 10min, then, cleaning 25min loose in 60 ℃ of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion, gets solution upper strata suspension whisker and filters through 200 orders, get modified crystal whiskers mixed liquor, and repeat 3 times until filtering is dried at vacuum drying oven after filtering, obtain modified crystal whiskers;
B) by mass fraction, get steps A) 6 parts of the modified crystal whiskers that obtain, under 4 parts of expansion type flame retardant melamine cyanurates, 1 part of microencapsulation red phosphorus combustion inhibitor, 0.5 part of KH-550 silane coupler, the condition that exists at 70 ℃ of a small amount of nonionic surface active agent, in mixer, airtight high-speed stirred reaction 45min, obtains flame-retardant and anti-dripping whisker;
C) by mass fraction, be to be made into flame-retardant and anti-dripping whisker ethylene glycol liquid with 6 parts of ethylene glycol under the condition that exists at micro-calgon of the flame-retardant and anti-dripping whisker of 4 parts, temperature is controlled at ultrasonic wave under 50 ℃ of conditions and disperses 2.5h, obtains flame-retardant and anti-dripping whisker ethylene glycol;
D) by mass fraction, get the flame-retardant and anti-dripping whisker ethylene glycol of 30 parts and add in the polycondensation vessel that has 70 parts of terephthalates, until copolyesters flame-retardant and anti-dripping polyester is made in esterification, polymerization;
Or E) get step B) the flame-retardant and anti-dripping whisker that obtains and normal polyester in mass ratio 25 ﹕ 75 blended meltings make the anti-molten drop polyester of blending fire retardant;
F) by step D) the copolyesters flame-retardant and anti-dripping polyester or the step e that obtain) the anti-molten drop polyester of blending fire retardant that obtains and PET, PTT, PBT polyester, take flame-retardant and anti-dripping component as cortex, and 20 ﹕ 80 make a kind of core-skin type flame-retardant and anti-dripping terylene through composite spinning technology in mass ratio.
Embodiment 4: a kind of manufacture method of flame-retardant and anti-dripping terylene, and this manufacture method adopts following steps:
A) by mass fraction, getting 8 parts of characterization parameter diameters is the alkali magnesium sulfate crystal whisker that 0.1-1um, length are 5-12um, 6 parts of characterization parameter diameters are the four acicular type zinc oxide crystal whisker that 0.1-0.8um, length are 6-10um, 8 parts of characterization parameter diameters are the magnesium salt whisker that 0.2-0.8um, length are 6-10um, and 6 parts of characterization parameter diameters are the β type silicon nitride crystal whisker that 0.1-0.6um, length are 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 6h in 450 ℃ of vacuum drying ovens, after cooling, containing stirring in the absolute ethyl alcohol of calgon to shear, disperseing 45min, then atmospheric plasma is processed 20min, then, cleaning 35min loose in 70 ℃ of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion, gets solution upper strata suspension whisker and filters through 200 orders, get modified crystal whiskers mixed liquor, and repeat 5 times until filtering is dried at vacuum drying oven after filtering, obtain modified crystal whiskers;
B) by mass fraction, get steps A) 10 parts of the modified crystal whiskers that obtain, under 8 parts of expansion type flame retardant melamine cyanurates, 2 parts of microencapsulation red phosphorus combustion inhibitors, 1.5 parts of KH-550 silane couplers, the condition that exists at 80 ℃ of a small amount of nonionic surface active agent, in mixer, airtight high-speed stirred reaction 60min, obtains flame-retardant and anti-dripping whisker;
C) by mass fraction, be to be made into flame-retardant and anti-dripping whisker ethylene glycol liquid with 4 parts of ethylene glycol under the condition that exists at micro-calgon of the flame-retardant and anti-dripping whisker of 6 parts, temperature is controlled at ultrasonic wave under 60 ℃ of conditions and disperses 5h, obtains flame-retardant and anti-dripping whisker ethylene glycol;
D) by mass fraction, get the flame-retardant and anti-dripping whisker ethylene glycol of 40 parts and add in the polycondensation vessel that has 60 parts of terephthalates, until copolyesters flame-retardant and anti-dripping polyester is made in esterification, polymerization;
Or E) get step B) the flame-retardant and anti-dripping whisker that obtains and normal polyester in mass ratio 35 ﹕ 65 blended meltings make the anti-molten drop polyester of blending fire retardant;
F) by step D) the copolyesters flame-retardant and anti-dripping polyester or the step e that obtain) the anti-molten drop polyester of blending fire retardant that obtains and PET, PTT, PBT polyester, take flame-retardant and anti-dripping component as cortex, and 40 ﹕ 60 make a kind of core-skin type flame-retardant and anti-dripping terylene through composite spinning technology in mass ratio.
Embodiment of the present invention is not limited to the above four embodiment, by aforementioned disclosed number range, in specific embodiment, replaces arbitrarily, thereby can obtain numerous embodiment, and this is not exemplified one by one.
Claims (5)
1. the manufacture method of a flame-retardant and anti-dripping terylene, it is characterized in that this manufacture method adopts following steps: A) by mass fraction, getting 4-8 part characterization parameter diameter is that 0.1-1 μ m, length are the alkali magnesium sulfate crystal whisker of 5-12 μ m, 2-6 part characterization parameter diameter is that 0.1-0.8 μ m, length are the four acicular type zinc oxide crystal whisker of 6-10 μ m, 4-8 part characterization parameter diameter is that 0.2-0.8 μ m, length are the magnesium salt whisker of 6-10 μ m, and 2-6 part characterization parameter diameter is that 0.1-0.6 μ m, length are the β type silicon nitride crystal whisker of 5-10 μ m; After above-mentioned four kinds of whiskers are mixed, calcination 4-6h in 350-450 ℃ of vacuum drying oven, after cooling, containing stirring in the absolute ethyl alcohol of calgon to shear, disperseing 30-45min, then atmospheric plasma is processed 10-20min, in the 60-70 ℃ of deionized water for ultrasonic wavelength-division containing calcium stearate dispersion, fall apart, clean again 25-35min, getting solution upper strata suspension whisker filters through 200 orders, get modified crystal whiskers mixed liquor, and repeat 3-5 time until filtering, after filtering, at vacuum drying oven, dry, obtain modified crystal whiskers; B) by mass fraction, get steps A) modified crystal whiskers 6-10 part of obtaining, with expansion type flame retardant melamine cyanurate 4-8 part, microencapsulation red phosphorus combustion inhibitor 1-2 part, KH-550 silane coupler 0.5-1.5 part, under the condition existing at 70-80 ℃ of a small amount of nonionic surface active agent, in mixer, airtight high-speed stirred reaction 45-60min, obtains flame-retardant and anti-dripping whisker; C) by mass fraction, be to be made into flame-retardant and anti-dripping whisker ethylene glycol liquid with 6-4 part ethylene glycol under the condition that exists at micro-calgon of the flame-retardant and anti-dripping whisker of 4-6 part, temperature is controlled at ultrasonic wave under 50-60 ℃ of condition and disperses 2.5-5h, obtains flame-retardant and anti-dripping whisker ethylene glycol; D) the flame-retardant and anti-dripping whisker ethylene glycol of getting 30-40 part by mass fraction adds in the polycondensation vessel that has 70-60 part terephthalate, until copolyesters flame-retardant and anti-dripping polyester is made in esterification, polymerization; Or E) get step B) the flame-retardant and anti-dripping whisker that obtains and normal polyester in mass ratio 25-35:75-65 blended melting make the anti-molten drop polyester of blending fire retardant; F) by step D) the copolyesters flame-retardant and anti-dripping polyester or the step e that obtain) the anti-molten drop polyester of blending fire retardant that obtains and PET, PTT, PBT polyester, take flame-retardant and anti-dripping component as cortex, and 20-40:80-60 makes a kind of core-skin type flame-retardant and anti-dripping terylene through composite spinning technology in mass ratio.
2. the manufacture method of flame-retardant and anti-dripping terylene according to claim 1, is characterized in that in described step:
A) by mass fraction, getting 6 parts of characterization parameter diameters is that 0.1-1 μ m, length are the alkali magnesium sulfate crystal whisker of 5-12 μ m, 4 parts of characterization parameter diameters are that 0.1-0.8 μ m, length are the four acicular type zinc oxide crystal whisker of 6-10 μ m, 6 parts of characterization parameter diameters are that 0.2-0.8 μ m, length are the magnesium salt whisker of 6-10 μ m, and 4 parts of characterization parameter diameters are that 0.1-0.6 μ m, length are the β type silicon nitride crystal whisker of 5-10 μ m; After above-mentioned four kinds of whiskers are mixed, calcination 5h in 400 ℃ of vacuum drying ovens, after cooling, containing stirring in the absolute ethyl alcohol of calgon to shear, disperseing 38min, then atmospheric plasma is processed 15min, then, cleaning 30min loose in 65 ℃ of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion, gets solution upper strata suspension whisker and filters through 200 orders, get modified crystal whiskers mixed liquor, and repeat 4 times until filtering is dried at vacuum drying oven after filtering, obtain modified crystal whiskers; B) by mass fraction, get A) 8 parts of the modified crystal whiskers that obtain, with 6 parts of expansion type flame retardant melamine cyanurates, 1.5 parts of microencapsulation red phosphorus combustion inhibitors, 1 part of KH-550 silane coupler, under the condition existing at 75 ℃ of a small amount of nonionic surface active agent, in mixer, airtight high-speed stirred reaction 55min, obtains flame-retardant and anti-dripping whisker; C) by mass fraction, be to be made into flame-retardant and anti-dripping whisker ethylene glycol liquid with 5 parts of ethylene glycol under the condition that exists at micro-calgon of the flame-retardant and anti-dripping whisker of 5 parts, temperature is controlled at ultrasonic wave under 55 ℃ of conditions and disperses 3.5h, obtains flame-retardant and anti-dripping whisker ethylene glycol; D) by mass fraction, get the flame-retardant and anti-dripping whisker ethylene glycol of 35 parts and add in the polycondensation vessel that has 65 parts of terephthalates, until copolyesters flame-retardant and anti-dripping polyester is made in esterification, polymerization; F) by step D) the copolyesters flame-retardant and anti-dripping polyester that obtains and PET, PTT, PBT polyester, take flame-retardant and anti-dripping component as cortex, 30:70 makes a kind of core-skin type flame-retardant and anti-dripping terylene through composite spinning technology in mass ratio.
3. according to the manufacture method of the flame-retardant and anti-dripping terylene described in claim 1, it is characterized in that in described step: A) by mass fraction, getting 6 parts of characterization parameter diameters is that 0.1-1 μ m, length are the alkali magnesium sulfate crystal whisker of 5-12 μ m, 4 parts of characterization parameter diameters are that 0.1-0.8 μ m, length are the four acicular type zinc oxide crystal whisker of 6-10 μ m, 6 parts of characterization parameter diameters are that 0.2-0.8 μ m, length are the magnesium salt whisker of 6-10 μ m, and 4 parts of characterization parameter diameters are that 0.1-0.6 μ m, length are the β type silicon nitride crystal whisker of 5-10 μ m; After above-mentioned four kinds of whiskers are mixed, calcination 5h in 400 ℃ of vacuum drying ovens, after cooling, containing stirring in the absolute ethyl alcohol of calgon to shear, disperseing 38min, then atmospheric plasma is processed 15min, then, cleaning 30min loose in 65 ℃ of deionized water for ultrasonic wavelength-divisions containing calcium stearate dispersion, gets solution upper strata suspension whisker and filters through 200 orders, get modified crystal whiskers mixed liquor, and repeat 4 times until filtering is dried at vacuum drying oven after filtering, obtain modified crystal whiskers; B) by mass fraction, get A) 8 parts of the modified crystal whiskers that obtain, with 6 parts of expansion type flame retardant melamine cyanurates, 1.5 parts of microencapsulation red phosphorus combustion inhibitors, 1 part of KH-550 silane coupler, under the condition existing at 75 ℃ of a small amount of nonionic surface active agent, in mixer, airtight high-speed stirred reaction 55min, obtains flame-retardant and anti-dripping whisker; E) get step B) the flame-retardant and anti-dripping whisker that obtains and normal polyester in mass ratio 30:70 blended melting make the anti-molten drop polyester of blending fire retardant;
F) by step e) the anti-molten drop polyester of blending fire retardant that obtains and PET, PTT, PBT polyester, take flame-retardant and anti-dripping component as cortex, 30:70 makes a kind of core-skin type flame-retardant and anti-dripping terylene through composite spinning technology in mass ratio.
4. the manufacture method of flame-retardant and anti-dripping terylene according to claim 2, it is characterized in that described step D) in: in polyethylene terephthalate polymerization process, when esterification yield reaches 85-90%, the flame-retardant and anti-dripping whisker ethylene glycol of getting 35 parts by mass fraction adds in the polycondensation vessel that has 65 parts of terephthalates, until copolyesters flame-retardant and anti-dripping polyester is made in esterification, polymerization.
5. according to the manufacture method of the flame-retardant and anti-dripping terylene described in claim 2 or 3, it is characterized in that described flame-retardant and anti-dripping polyester is spun into PDY, DTY, BCF, BSY, nonwoven fabric through blend or complex technique; Or described flame-retardant and anti-dripping polyester adopts blend or complex technique to make flame-retardant and anti-dripping polyester sheet, tubing, bar, wire rod.
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| CN201210488858.8A CN102978735B (en) | 2012-11-26 | 2012-11-26 | Preparation method of flame-retardant droplet-resistant terylene |
| CA2895255A CA2895255C (en) | 2012-11-26 | 2013-11-26 | Method for preparing flame-retardant melt droplet-resistant polyester |
| PCT/CN2013/087806 WO2014079393A1 (en) | 2012-11-26 | 2013-11-26 | Method for preparing flame-retardant melt droplet-resistant polyester |
| GB1510225.4A GB2526441B (en) | 2012-11-26 | 2013-11-26 | Method for preparing flame-retardant and melt droplet-resistant polyester |
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| CN102978735B (en) * | 2012-11-26 | 2014-08-13 | 浙江盛元化纤有限公司 | Preparation method of flame-retardant droplet-resistant terylene |
| CN105646939A (en) * | 2014-11-10 | 2016-06-08 | 合肥杰事杰新材料股份有限公司 | Application of basic magnesium sulfate whiskers as flame-retardant anti-dripping agent of composition |
| CN104538105A (en) * | 2014-12-03 | 2015-04-22 | 常州市拓源电缆成套有限公司 | Flame-retardant capacitance type composite insulated bus |
| CN105624825B (en) * | 2016-03-15 | 2018-06-29 | 张家港骏马无纺布有限公司 | A kind of fire-retardant melt-blown non-woven material and preparation method thereof |
| CN106336504A (en) * | 2016-08-31 | 2017-01-18 | 浙江省现代纺织工业研究院 | Manufacturing method of flame-retardant anti-ageing PET (polyester) and fibers |
| CN108440743A (en) * | 2018-01-23 | 2018-08-24 | 浙江省现代纺织工业研究院 | A kind of preparation method of preposition modified EG |
| CN108341939A (en) * | 2018-01-23 | 2018-07-31 | 浙江省现代纺织工业研究院 | A kind of preparation method of hydridization paraxylene |
| CN110158174B (en) * | 2019-06-20 | 2021-10-22 | 宜宾屏山辉瑞油脂有限公司 | Flame retardant, flame-retardant synthetic fiber and manufacturing method thereof |
| CN113512248B (en) * | 2021-04-25 | 2023-05-09 | 常熟市中联光电新材料有限责任公司 | Whisker synergistic multielement flame-retardant ethylene-vinyl acetate copolymer/low density polyethylene composite material and preparation method thereof |
| CN113512249B (en) * | 2021-04-25 | 2023-05-02 | 常熟市中联光电新材料有限责任公司 | Zinc hydroxide borate and whisker synergistic flame-retardant ethylene-vinyl acetate copolymer/low-density polyethylene composite material and preparation method thereof |
| CN114957949B (en) * | 2022-06-30 | 2023-03-21 | 宁波昌亚新材料科技股份有限公司 | High-heat-resistance high-rigidity polylactic acid composite material and preparation method and application thereof |
| CN115710755B (en) * | 2022-11-30 | 2024-02-06 | 潍坊迅纺新材料科技有限公司 | Flame-retardant tooling fabric without molten drops |
| CN115896967B (en) * | 2022-12-13 | 2023-06-13 | 泰安亚荣生物科技有限公司 | Degradable environment-friendly flame retardant and preparation method thereof |
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| CN1203219C (en) * | 2003-07-29 | 2005-05-25 | 东华大学 | Method for preparing whisker material to make modification treatment of spinning chemical fibre |
| US20060157882A1 (en) * | 2004-12-10 | 2006-07-20 | Simona Percec | Filled ultramicrocellular structures |
| CN1814697A (en) * | 2006-02-21 | 2006-08-09 | 南通瑞森科技合成材料有限公司 | Sub-nano silica-magnesia whisker halogen-less flame-retardant agent |
| CN101402753B (en) * | 2008-10-31 | 2011-03-16 | 浙江七色鹿色母粒有限公司 | Begin-color flame-proof antistatic polyolefin master batch |
| CN101423666B (en) * | 2008-10-31 | 2011-04-27 | 广东新会美达锦纶股份有限公司 | Halogen-free flame retardant polyamide 6 composition |
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| CN102731996A (en) * | 2012-06-15 | 2012-10-17 | 苏州宇度医疗器械有限责任公司 | Preparation method of calcium sulfate whisker filled flame-retardant polyamide high polymer material |
| CN102978735B (en) * | 2012-11-26 | 2014-08-13 | 浙江盛元化纤有限公司 | Preparation method of flame-retardant droplet-resistant terylene |
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| CA2895255C (en) | 2017-01-17 |
| GB201510225D0 (en) | 2015-07-29 |
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| CN102978735A (en) | 2013-03-20 |
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