CN102978735A - Preparation method of flame-retardant droplet-resistant terylene - Google Patents
Preparation method of flame-retardant droplet-resistant terylene Download PDFInfo
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- CN102978735A CN102978735A CN2012104888588A CN201210488858A CN102978735A CN 102978735 A CN102978735 A CN 102978735A CN 2012104888588 A CN2012104888588 A CN 2012104888588A CN 201210488858 A CN201210488858 A CN 201210488858A CN 102978735 A CN102978735 A CN 102978735A
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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
- 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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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-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
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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
- 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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- 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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- 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
- D01F6/78—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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- 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
- D01F6/88—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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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—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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- 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
- C08K2003/026—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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- 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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- C—CHEMISTRY; METALLURGY
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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
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, does not wrinkle behind its fabric washing, can not press, strongly very scrapes, easily washes easily and do.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 the 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 about 21, belongs to meltbility easy firing fiber.When terylene provides rich and varied material conditions to the mankind thus, also hidden a lot of disaster hidden-troubles to the mankind.More seriously the melting drippage can occur in the terylene goods under burning or high temperature, causes the more conflagration that the migration of scald and kindling material causes.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.
Make the flame-retardant and anti-dripping terylene, usually introduce and contain 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 method is made, generally, the acquisition of flame-retardant and anti-dripping is take other performance of sacrificial fiber as cost, along with adding fire-retardant, anti-molten drop agent, fibre strength, degree of stretching tend to become weak; The feel variation; Spinning, weave difficulty.
Whisker be the diameter that forms with monocrystalline form growth very little (0.1～10um), length atomic arrangement high-sequential, intensity near the theoretical value of perfect crystal, the fibrous material of certain draw ratio (5～1000) is arranged, 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 widely Application Areas.
The inorganic crystal whisker fusing point is very high, usually all more than 1000 ℃, has just in time remedied the deficiency of macromolecular material aspect heat-resisting, makes the glass transition temperature of system and heat distortion temperature that rising all be arranged, and 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, again can absorbing smoke, play 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, and be more more superior than flame-retardant and anti-dripping material commonly used.
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 objective of the invention is to finish by following technical solution, the manufacture method of described flame-retardant and anti-dripping terylene, it adopts following steps:
A) getting 4-8 part characterization parameter diameter by mass fraction is that 0.1-1um, length are the alkali magnesium sulfate crystal whisker of 5-12um, 2-6 part characterization parameter diameter is that 0.1-0.8um, length are the four acicular type zinc oxide crystal whisker of 6-10um, 4-8 part characterization parameter diameter is that 0.2-0.8um, length are the magnesium salt whisker of 6-10um, and 2-6 part characterization parameter diameter is that 0.1-0.6um, length are the β type silicon nitride crystal whisker of 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 4-6h in 350-450 ℃ of vacuum drying oven, in containing the absolute ethyl alcohol of calgon, stir after the cooling to shear and disperse 30-45min, then atmospheric plasma is processed 10-20min, fall apart, clean again 25-35min the 60-70 that contains calcium stearate dispersion ℃ of deionized water for ultrasonic wavelength-division, getting solution upper strata suspension whisker filters through 200 orders, get the modified crystal whiskers mixed liquor, and repetitive operation 3-5 time is until filtering, in the vacuum drying oven oven dry, obtain modified crystal whiskers after the filtering;
B) get steps A by mass fraction) 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 that 70-80 ℃ of a small amount of nonionic surface active agent exists, airtight high-speed stirred reaction 45-60min obtains the flame-retardant and anti-dripping whisker in mixer;
C) be that the flame-retardant and anti-dripping whisker of 4-6 part is made into flame-retardant and anti-dripping whisker ethylene glycol liquid with 6-4 part ethylene glycol with mass fraction under the condition that micro-calgon exists, temperature is controlled at ultrasonic wave dispersion 2.5-5h under the 50-60 ℃ of condition, 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 70-60 part terephthalate is arranged, 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) with 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 the flame-retardant and anti-dripping component as cortex, 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) getting 6 parts of characterization parameter diameters by mass fraction is that 0.1-1um, length are the alkali magnesium sulfate crystal whisker of 5-12um, 4 parts of characterization parameter diameters are that 0.1-0.8um, length are the four acicular type zinc oxide crystal whisker of 6-10um, 6 parts of characterization parameter diameters are that 0.2-0.8um, length are the magnesium salt whisker of 6-10um, and 4 parts of characterization parameter diameters are that 0.1-0.6um, length are the β type silicon nitride crystal whisker of 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 5h in 400 ℃ of vacuum drying ovens, in containing the absolute ethyl alcohol of calgon, stir after the cooling to shear and disperse 38min, then atmospheric plasma is processed 15min, and, cleaning 30min loose in 65 ℃ of deionized water for ultrasonic wavelength-divisions that contain calcium stearate dispersion gets solution upper strata suspension whisker and filter through 200 orders again, get the modified crystal whiskers mixed liquor, and repetitive operation 4 times is until filtering in the vacuum drying oven oven dry, obtains modified crystal whiskers after the filtering;
B) get A by mass fraction) 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 that 75 ℃ of a small amount of nonionic surface active agent exist, airtight high-speed stirred reaction 55min obtains the flame-retardant and anti-dripping whisker in mixer;
C) be that 5 parts flame-retardant and anti-dripping whisker is made into flame-retardant and anti-dripping whisker ethylene glycol liquid with 5 parts of ethylene glycol with mass fraction under the condition that micro-calgon exists, temperature is controlled at ultrasonic wave dispersion 3.5h under 55 ℃ of conditions, obtains flame-retardant and anti-dripping whisker ethylene glycol;
D) get 35 parts flame-retardant and anti-dripping whisker ethylene glycol by mass fraction and add in the polycondensation vessel that 65 parts of terephthalates are arranged, until copolyesters flame-retardant and anti-dripping polyester is made in esterification, polymerization;
F) with step D) the copolyesters flame-retardant and anti-dripping polyester that obtains and PET, PTT, PBT polyester, take the 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) getting 6 parts of characterization parameter diameters by mass fraction is that 0.1-1um, length are the alkali magnesium sulfate crystal whisker of 5-12um, 4 parts of characterization parameter diameters are that 0.1-0.8um, length are the four acicular type zinc oxide crystal whisker of 6-10um, 6 parts of characterization parameter diameters are that 0.2-0.8um, length are the magnesium salt whisker of 6-10um, and 4 parts of characterization parameter diameters are that 0.1-0.6um, length are the β type silicon nitride crystal whisker of 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 5h in 400 ℃ of vacuum drying ovens, in containing the absolute ethyl alcohol of calgon, stir after the cooling to shear and disperse 38min, then atmospheric plasma is processed 15min, and, cleaning 30min loose in 65 ℃ of deionized water for ultrasonic wavelength-divisions that contain calcium stearate dispersion gets solution upper strata suspension whisker and filter through 200 orders again, get the modified crystal whiskers mixed liquor, and repetitive operation 4 times is until filtering in the vacuum drying oven oven dry, obtains modified crystal whiskers after the filtering;
B) get steps A by mass fraction) 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 that 75 ℃ of a small amount of nonionic surface active agent exist, airtight high-speed stirred reaction 55min obtains the flame-retardant and anti-dripping whisker in mixer;
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) with step e) the anti-molten drop polyester of blending fire retardant that obtains and PET, PTT, PBT polyester, take the 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 the 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 65 parts of terephthalates are arranged, 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 to have humidification in polyester, have simultaneously 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., by the melt composite spinning means, make the core-skin type flame-retardant and anti-dripping terylene take the flame-retardant and anti-dripping component as cortex; When the terylene goods under burning or high temperature, polyester is melted, the fracture of thermal cracking, macromolecular chain, but the whisker that is dispersed in the polyester can not be melted, can thermal cracking yet, whisker can not rupture, can not burn yet; Whisker and fire retardant have the anti-molten drop effect of fabulous flame resistance as burning and the drippage of flame-retardant and anti-dripping muscle silk screen obstruction polyester fondant.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
The present invention will be described in detail below in conjunction with specific embodiment: 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) getting 4-8 part characterization parameter diameter by mass fraction is that 0.1-1um, length are the alkali magnesium sulfate crystal whisker of 5-12um, 2-6 part characterization parameter diameter is that 0.1-0.8um, length are the four acicular type zinc oxide crystal whisker of 6-10um, 4-8 part characterization parameter diameter is that 0.2-0.8um, length are the magnesium salt whisker of 6-10um, and 2-6 part characterization parameter diameter is that 0.1-0.6um, length are the β type silicon nitride crystal whisker of 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 4-6h in 350-450 ℃ of vacuum drying oven, in containing the absolute ethyl alcohol of calgon, stir after the cooling to shear and disperse 30-45min, then atmospheric plasma is processed 10-20min, fall apart, clean again 25-35min the 60-70 that contains calcium stearate dispersion ℃ of deionized water for ultrasonic wavelength-division, getting solution upper strata suspension whisker filters through 200 orders, get the modified crystal whiskers mixed liquor, and repetitive operation 3-5 time is until filtering, in the vacuum drying oven oven dry, obtain modified crystal whiskers after the filtering;
B) get steps A by mass fraction) 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 that 70-80 ℃ of a small amount of nonionic surface active agent exists, airtight high-speed stirred reaction 45-60min obtains the flame-retardant and anti-dripping whisker in mixer;
C) be that the flame-retardant and anti-dripping whisker of 4-6 part is made into flame-retardant and anti-dripping whisker ethylene glycol liquid with 6-4 part ethylene glycol with mass fraction under the condition that micro-calgon exists, temperature is controlled at ultrasonic wave dispersion 2.5-5h under the 50-60 ℃ of condition, 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 70-60 part terephthalate is arranged, 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) with 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 the flame-retardant and anti-dripping component as cortex, 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 the 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 65 parts of terephthalates are arranged, 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) getting 6 parts of characterization parameter diameters by mass fraction is that 0.1-1um, length are the alkali magnesium sulfate crystal whisker of 5-12um, 4 parts of characterization parameter diameters are that 0.1-0.8um, length are the four acicular type zinc oxide crystal whisker of 6-10um, 6 parts of characterization parameter diameters are that 0.2-0.8um, length are the magnesium salt whisker of 6-10um, and 4 parts of characterization parameter diameters are that 0.1-0.6um, length are the β type silicon nitride crystal whisker of 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 5h in 400 ℃ of vacuum drying ovens, in containing the absolute ethyl alcohol of calgon, stir after the cooling to shear and disperse 38min, then atmospheric plasma is processed 15min, and, cleaning 30min loose in 65 ℃ of deionized water for ultrasonic wavelength-divisions that contain calcium stearate dispersion gets solution upper strata suspension whisker and filter through 200 orders again, get the modified crystal whiskers mixed liquor, and repetitive operation 4 times is until filtering in the vacuum drying oven oven dry, obtains modified crystal whiskers after the filtering;
B) get A by mass fraction) 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 that 75 ℃ of a small amount of nonionic surface active agent exist, airtight high-speed stirred reaction 55min obtains the flame-retardant and anti-dripping whisker in mixer;
C) be that 5 parts flame-retardant and anti-dripping whisker is made into flame-retardant and anti-dripping whisker ethylene glycol liquid with 5 parts of ethylene glycol with mass fraction under the condition that micro-calgon exists, temperature is controlled at ultrasonic wave dispersion 3.5h under 55 ℃ of conditions, obtains flame-retardant and anti-dripping whisker ethylene glycol;
D) get 35 parts flame-retardant and anti-dripping whisker ethylene glycol by mass fraction and add in the polycondensation vessel that 65 parts of terephthalates are arranged, until copolyesters flame-retardant and anti-dripping polyester is made in esterification, polymerization;
F) with step D) the copolyesters flame-retardant and anti-dripping polyester that obtains and PET, PTT, PBT polyester, take the 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) getting 6 parts of characterization parameter diameters by mass fraction is that 0.1-1um, length are the alkali magnesium sulfate crystal whisker of 5-12um, 4 parts of characterization parameter diameters are that 0.1-0.8um, length are the four acicular type zinc oxide crystal whisker of 6-10um, 6 parts of characterization parameter diameters are that 0.2-0.8um, length are the magnesium salt whisker of 6-10um, and 4 parts of characterization parameter diameters are that 0.1-0.6um, length are the β type silicon nitride crystal whisker of 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 5h in 400 ℃ of vacuum drying ovens, in containing the absolute ethyl alcohol of calgon, stir after the cooling to shear and disperse 38min, then atmospheric plasma is processed 15min, and, cleaning 30min loose in 65 ℃ of deionized water for ultrasonic wavelength-divisions that contain calcium stearate dispersion gets solution upper strata suspension whisker and filter through 200 orders again, get the modified crystal whiskers mixed liquor, and repetitive operation 4 times is until filtering in the vacuum drying oven oven dry, obtains modified crystal whiskers after the filtering;
B) get steps A by mass fraction) 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 that 75 ℃ of a small amount of nonionic surface active agent exist, airtight high-speed stirred reaction 55min obtains the flame-retardant and anti-dripping whisker in mixer;
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) with step e) the anti-molten drop polyester of blending fire retardant that obtains and PET, PTT, PBT polyester, take the 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) getting 4 parts of characterization parameter diameters by mass fraction is that 0.1-1um, length are the alkali magnesium sulfate crystal whisker of 5-12um, 2 parts of characterization parameter diameters are that 0.1-0.8um, length are the four acicular type zinc oxide crystal whisker of 6-10um, 4 parts of characterization parameter diameters are that 0.2-0.8um, length are the magnesium salt whisker of 6-10um, and 2 parts of characterization parameter diameters are that 0.1-0.6um, length are the β type silicon nitride crystal whisker of 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 4h in 350 ℃ of vacuum drying ovens, in containing the absolute ethyl alcohol of calgon, stir after the cooling to shear and disperse 30min, then atmospheric plasma is processed 10min, and, cleaning 25min loose in 60 ℃ of deionized water for ultrasonic wavelength-divisions that contain calcium stearate dispersion gets solution upper strata suspension whisker and filter through 200 orders again, get the modified crystal whiskers mixed liquor, and repetitive operation 3 times is until filtering in the vacuum drying oven oven dry, obtains modified crystal whiskers after the filtering;
B) get steps A by mass fraction) 6 parts of the modified crystal whiskers that obtain, with 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, under the condition that 70 ℃ of a small amount of nonionic surface active agent exist, airtight high-speed stirred reaction 45min obtains the flame-retardant and anti-dripping whisker in mixer;
C) be that 4 parts flame-retardant and anti-dripping whisker is made into flame-retardant and anti-dripping whisker ethylene glycol liquid with 6 parts of ethylene glycol with mass fraction under the condition that micro-calgon exists, temperature is controlled at ultrasonic wave dispersion 2.5h under 50 ℃ of conditions, obtains flame-retardant and anti-dripping whisker ethylene glycol;
D) get 30 parts flame-retardant and anti-dripping whisker ethylene glycol by mass fraction and add in the polycondensation vessel that 70 parts of terephthalates are arranged, 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) with 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 the flame-retardant and anti-dripping component as cortex, 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) getting 8 parts of characterization parameter diameters by mass fraction is that 0.1-1um, length are the alkali magnesium sulfate crystal whisker of 5-12um, 6 parts of characterization parameter diameters are that 0.1-0.8um, length are the four acicular type zinc oxide crystal whisker of 6-10um, 8 parts of characterization parameter diameters are that 0.2-0.8um, length are the magnesium salt whisker of 6-10um, and 6 parts of characterization parameter diameters are that 0.1-0.6um, length are the β type silicon nitride crystal whisker of 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 6h in 450 ℃ of vacuum drying ovens, in containing the absolute ethyl alcohol of calgon, stir after the cooling to shear and disperse 45min, then atmospheric plasma is processed 20min, and, cleaning 35min loose in 70 ℃ of deionized water for ultrasonic wavelength-divisions that contain calcium stearate dispersion gets solution upper strata suspension whisker and filter through 200 orders again, get the modified crystal whiskers mixed liquor, and repetitive operation 5 times is until filtering in the vacuum drying oven oven dry, obtains modified crystal whiskers after the filtering;
B) get steps A by mass fraction) 10 parts of the modified crystal whiskers that obtain, with 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, under the condition that 80 ℃ of a small amount of nonionic surface active agent exist, airtight high-speed stirred reaction 60min obtains the flame-retardant and anti-dripping whisker in mixer;
C) be that 6 parts flame-retardant and anti-dripping whisker is made into flame-retardant and anti-dripping whisker ethylene glycol liquid with 4 parts of ethylene glycol with mass fraction under the condition that micro-calgon exists, temperature is controlled at that ultrasonic wave disperses 5h under 60 ℃ of conditions, obtains flame-retardant and anti-dripping whisker ethylene glycol;
D) get 40 parts flame-retardant and anti-dripping whisker ethylene glycol by mass fraction and add in the polycondensation vessel that 60 parts of terephthalates are arranged, 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) with 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 the flame-retardant and anti-dripping component as cortex, 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, replaces arbitrarily in specific embodiment, 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 is characterized in that this manufacture method adopts following steps:
A) getting 4-8 part characterization parameter diameter by mass fraction is that 0.1-1um, length are the alkali magnesium sulfate crystal whisker of 5-12um, 2-6 part characterization parameter diameter is that 0.1-0.8um, length are the four acicular type zinc oxide crystal whisker of 6-10um, 4-8 part characterization parameter diameter is that 0.2-0.8um, length are the magnesium salt whisker of 6-10um, and 2-6 part characterization parameter diameter is that 0.1-0.6um, length are the β type silicon nitride crystal whisker of 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 4-6h in 350-450 ℃ of vacuum drying oven, in containing the absolute ethyl alcohol of calgon, stir after the cooling to shear and disperse 30-45min, then atmospheric plasma is processed 10-20min, fall apart, clean again 25-35min the 60-70 that contains calcium stearate dispersion ℃ of deionized water for ultrasonic wavelength-division, getting solution upper strata suspension whisker filters through 200 orders, get the modified crystal whiskers mixed liquor, and repetitive operation 3-5 time is until filtering, in the vacuum drying oven oven dry, obtain modified crystal whiskers after the filtering;
B) get steps A by mass fraction) 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 that 70-80 ℃ of a small amount of nonionic surface active agent exists, airtight high-speed stirred reaction 45-60min obtains the flame-retardant and anti-dripping whisker in mixer;
C) be that the flame-retardant and anti-dripping whisker of 4-6 part is made into flame-retardant and anti-dripping whisker ethylene glycol liquid with 6-4 part ethylene glycol with mass fraction under the condition that micro-calgon exists, temperature is controlled at ultrasonic wave dispersion 2.5-5h under the 50-60 ℃ of condition, 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 70-60 part terephthalate is arranged, 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) with 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 the flame-retardant and anti-dripping component as cortex, 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 the described step:
A) getting 6 parts of characterization parameter diameters by mass fraction is that 0.1-1um, length are the alkali magnesium sulfate crystal whisker of 5-12um, 4 parts of characterization parameter diameters are that 0.1-0.8um, length are the four acicular type zinc oxide crystal whisker of 6-10um, 6 parts of characterization parameter diameters are that 0.2-0.8um, length are the magnesium salt whisker of 6-10um, and 4 parts of characterization parameter diameters are that 0.1-0.6um, length are the β type silicon nitride crystal whisker of 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 5h in 400 ℃ of vacuum drying ovens, in containing the absolute ethyl alcohol of calgon, stir after the cooling to shear and disperse 38min, then atmospheric plasma is processed 15min, and, cleaning 30min loose in 65 ℃ of deionized water for ultrasonic wavelength-divisions that contain calcium stearate dispersion gets solution upper strata suspension whisker and filter through 200 orders again, get the modified crystal whiskers mixed liquor, and repetitive operation 4 times is until filtering in the vacuum drying oven oven dry, obtains modified crystal whiskers after the filtering;
B) get A by mass fraction) 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 that 75 ℃ of a small amount of nonionic surface active agent exist, airtight high-speed stirred reaction 55min obtains the flame-retardant and anti-dripping whisker in mixer;
C) be that 5 parts flame-retardant and anti-dripping whisker is made into flame-retardant and anti-dripping whisker ethylene glycol liquid with 5 parts of ethylene glycol with mass fraction under the condition that micro-calgon exists, temperature is controlled at ultrasonic wave dispersion 3.5h under 55 ℃ of conditions, obtains flame-retardant and anti-dripping whisker ethylene glycol;
D) get 35 parts flame-retardant and anti-dripping whisker ethylene glycol by mass fraction and add in the polycondensation vessel that 65 parts of terephthalates are arranged, until copolyesters flame-retardant and anti-dripping polyester is made in esterification, polymerization;
F) with step D) the copolyesters flame-retardant and anti-dripping polyester that obtains and PET, PTT, PBT polyester, take the 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.
3. the manufacture method of flame-retardant and anti-dripping terylene according to claim 1 is characterized in that in the described step:
A) getting 6 parts of characterization parameter diameters by mass fraction is that 0.1-1um, length are the alkali magnesium sulfate crystal whisker of 5-12um, 4 parts of characterization parameter diameters are that 0.1-0.8um, length are the four acicular type zinc oxide crystal whisker of 6-10um, 6 parts of characterization parameter diameters are that 0.2-0.8um, length are the magnesium salt whisker of 6-10um, and 4 parts of characterization parameter diameters are that 0.1-0.6um, length are the β type silicon nitride crystal whisker of 5-10um; After above-mentioned four kinds of whiskers are mixed, calcination 5h in 400 ℃ of vacuum drying ovens, in containing the absolute ethyl alcohol of calgon, stir after the cooling to shear and disperse 38min, then atmospheric plasma is processed 15min, and, cleaning 30min loose in 65 ℃ of deionized water for ultrasonic wavelength-divisions that contain calcium stearate dispersion gets solution upper strata suspension whisker and filter through 200 orders again, get the modified crystal whiskers mixed liquor, and repetitive operation 4 times is until filtering in the vacuum drying oven oven dry, obtains modified crystal whiskers after the filtering;
B) get A by mass fraction) 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 that 75 ℃ of a small amount of nonionic surface active agent exist, airtight high-speed stirred reaction 55min obtains the flame-retardant and anti-dripping whisker in mixer;
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) with step e) the anti-molten drop polyester of blending fire retardant that obtains and PET, PTT, PBT polyester, take the 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.
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 the 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 65 parts of terephthalates are arranged, until copolyesters flame-retardant and anti-dripping polyester is made in esterification, polymerization.
5. according to claim 2 or the manufacture method of 3 described flame-retardant and anti-dripping terylene, 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.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210488858.8A CN102978735B (en) | 2012-11-26 | 2012-11-26 | Preparation method of flame-retardant droplet-resistant terylene |
| GB1510225.4A GB2526441B (en) | 2012-11-26 | 2013-11-26 | Method for preparing flame-retardant and melt droplet-resistant polyester |
| 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 |
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| CN201210488858.8A CN102978735B (en) | 2012-11-26 | 2012-11-26 | Preparation method of flame-retardant droplet-resistant terylene |
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| CN102978735B CN102978735B (en) | 2014-08-13 |
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| Country | Link |
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| CN (1) | CN102978735B (en) |
| CA (1) | CA2895255C (en) |
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| WO2014079393A1 (en) * | 2012-11-26 | 2014-05-30 | 浙江盛元化纤有限公司 | Method for preparing flame-retardant melt droplet-resistant polyester |
| 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 |
| CN105624825A (en) * | 2016-03-15 | 2016-06-01 | 张家港骏马无纺布有限公司 | Flame-retardant melt-blowing nonwoven material and preparation method thereof |
| 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 |
| 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 |
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| 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 |
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| GB2526441A (en) * | 2012-11-26 | 2015-11-25 | Zhejiang Shengyuan Chemical Fibre Co Ltd | Method for preparing flame-retardant melt droplet-resistant polyester |
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| 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 |
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| Publication number | Publication date |
|---|---|
| GB2526441B (en) | 2019-01-09 |
| GB2526441A (en) | 2015-11-25 |
| WO2014079393A1 (en) | 2014-05-30 |
| CA2895255C (en) | 2017-01-17 |
| GB201510225D0 (en) | 2015-07-29 |
| CN102978735B (en) | 2014-08-13 |
| CA2895255A1 (en) | 2014-05-30 |
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