CN101631910A - Flameproofing agent, flame-retardant fiber and method for producing the same - Google Patents
Flameproofing agent, flame-retardant fiber and method for producing the same Download PDFInfo
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- CN101631910A CN101631910A CN200880003918.4A CN200880003918A CN101631910A CN 101631910 A CN101631910 A CN 101631910A CN 200880003918 A CN200880003918 A CN 200880003918A CN 101631910 A CN101631910 A CN 101631910A
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- fire retardant
- textile material
- phosphorus compound
- surfactant
- polyoxyalkylene
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/06—Organic materials
- C09K21/12—Organic materials containing phosphorus
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
- D06M13/285—Phosphines; Phosphine oxides; Phosphine sulfides; Phosphinic or phosphinous acids or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/52—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment combined with mechanical treatment
- D06M13/53—Cooling; Steaming or heating, e.g. in fluidised beds; with molten metals
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Fireproofing Substances (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
Disclosed is a flameproofing agent which is used for imparting a fiber material with flame retardancy and capable of providing good flame retardancy even in a small amount. This flameproofing agent enables to suppress deterioration of other physical properties, while having excellent product stability. Specifically disclosed is a flameproofing agent containing a phosphorus compound (A), a surfactant (B) composed of an anionic surfactant and/or a nonionic surfactant and water, which is used for imparting a fiber material with flame retardancy. The phosphorus compound (A) has a median particle size (D50) of not more than 1 [mu]m.
Description
Technical field
The present invention relates to fire retardant, anti-flammability textile material and preparation method thereof.
Background technology
In conventional method, be normally used for giving textile material with flame-retardant nature by dispersion or emulsification halogen compounds such as the prepared fire retardant of hexabromo-Cyclododecane in water.Have flame-retardant nature although be coated with the textile material of halogen compounds, when this material combustion, may produce poison gas.For this reason and motion, there is the trend of avoiding using halogen compounds as far as possible away from halogen compounds in order to increase based on environmental consideration.
Although organic phosphorus compound is used as the substitute of halogen compounds, owing to a spot of phosphorus contained in each molecule of those compounds, they can't give enough flame-retardant natures.Therefore, must on textile material, apply a large amount of organic phosphorus compounds to give sufficient flame-retardant nature.On textile material coating so a large amount of organic phosphorus compounds caused problem, for example, the textile material feel of difference and by friction and the color fastness that is exposed to the dyed textile material that light causes reduce.In addition, the molecular weight of organic phosphorus compound is too little and thermo-labile, and therefore described compound causes being coated with the textile material transparent article atomizing on every side of this compound sometimes.In order to address these problems, advised that the diphosphonic acid that molecular weight is high is used for fire retardant.References 1 to 3 discloses use resorcinol two (diphenyl phosphoester) gives the textile material flame-retardant nature as the example of phosphonium flame retardant method.
References 4 discloses the method for using fire retardant to give the textile material flame-retardant nature, described fire retardant be by will as four (2, the 6-3,5-dimethylphenyl) of fire retardant with phosphorus compound--the phenylene phosphate disperses and the solution of preparation.References 5 discloses the method for using fire retardant to give the textile material flame-retardant nature, and described fire retardant is the solution for preparing by disperseing as the naphthyl diphenyl phosphoester of phosphonium flame retardant.
[references 1] JP A 2000-328445
[references 2] JP A 2002-88368
[references 3] JP A 2005-15947
[references 4] JP A 2001-254268
[references 5] JP A 2006-70417
Yet disclosed resorcinol two (diphenyl phosphoester) is owing to phosphorus contained in its chemical constitution-oxygen singly-bound (phosphate-based) is easy to hydrolysis, and the phosphoric acid that produces in hydrolysis makes the textile material deterioration in references 1 to 3.In addition, the color fastness of two (diphenyl phosphoester) deterioration dyed textile material of resorcinol is such as the color fastness loss owing to friction, because this compound is liquid under normal temperature.But disclosed fire retardant in references 3 is not easy to hydrolysis owing to used the resorcinol two (diphenyl phosphoester) of self-emulsifying.Yet when being coated on fire retardant on the textile material, it becomes and is easier to hydrolysis, and thereby As time goes on and the deterioration textile material.For making flame-retardant properties, in dye bath, described fire retardant is coated on the textile material usually washing and dry-cleaning durable purpose.In this process, resorcinol two (diphenyl phosphoester) can not give textile material with enough flame-retardant natures, because this material fully can't be coated on the textile material owing to its high molecular.Although in above-mentioned references 4 in the disclosed fire retardant contained four (2, the 6-3,5-dimethylphenyl)--the phenylene phosphate has resistance to hydrolysis, but the high molecular of phosphate and three-dimensional bulk properties stop it to be coated on the textile material fully and suppress to obtain durable flame-retardant nature.Contained naphthyl diphenyl phosphoester has about 60 ℃ fusing point in the disclosed fire retardant in references 5, and when the textile material that is coated with described fire retardant was processed to goods such as automotive seat, described fire retardant may fusion and reduce the color fastness of textile material to friction.In addition, this fire retardant has poor light resistance and impracticable.
As mentioned above, conventional flame retardants has merits and demerits simultaneously at its aspect of performance.
Summary of the invention
Technical problem
The purpose of this invention is to provide a kind of fire retardant, it is used to give the textile material flame-retardant nature, reaches sufficient flame-retardant nature with a small amount of fire retardant, will the deterioration of other textiles character be minimized, and has excellent stability; A kind of method for preparing the anti-flammability textile material, described method comprise fire retardant are coated to step on the textile material; With a kind of anti-flammability textile material with described method preparation.
Technical solution
The present inventor deeply and carefully studies to achieve the above object, and find, reducing particle diameter as some phosphorus compound of flame retardant compositions helps at deterioration flame-retardant nature not and makes to reduce the amount that is coated on the fire retardant on the textile material under the minimized condition of other textiles character deterioration, and the surfactant that adds in the fire retardant improves the stability of fire retardant, thereby achieves the above object.Therefore the inventor has obtained the present invention.
Fire retardant of the present invention comprises phosphorus compound (A), surfactant (B) and water, and described phosphorus compound (A) is by following formula (1) expression, and described surfactant (B) comprises anion surfactant and/or non-ionic surface active agent; And fire retardant of the present invention is used to give the textile material flame-retardant nature, and wherein phosphorus compound (A) has the median particle diameter (D below 1 micron
50).
[Chemical formula 1]
(R wherein
1, R
2And R
3Can be mutually the same or differ from one another, and expression can have substituent C
1-24Alkyl, C
2-22Thiazolinyl, C
5-6Alcyl, and aryl or aralkyl.)
Fire retardant of the present invention should preferably meet the following conditions 1) to 5) at least one.
1) surfactant (B) contains and is selected from least a in the group of being made up of the following: polyoxyalkylene alkyl aryl ether sulfate class, alkylaryl sulfonates class, alkyl aromatic ether disulfonic acid salt (alkylaryl oxide disulfonates), aromatic sulphonate-formaldehyde (formalin) condensation product class, polyoxyalkylene alkylaryl ethers, polyoxyalkylene castor oil ethers, polyoxyalkylene rilanit special ethers and polyoxyalkylene fatty acid ester.
2) surfactant (B) contains and is selected from least a in the group of being made up of the following: aromatic sulphonate-formaldehyde condensation products class, polyoxyalkylene castor oil ethers, polyoxyalkylene rilanit special ethers and polyoxyalkylene fatty acid ester.
3) respectively, the ratio of phosphorus compound (A) is in the scope of 20 to 70 weight % of fire retardant integral body, and the ratio of surfactant (B) is in the scope of 3 to 20 weight % of fire retardant integral body, and phosphorus compound (A) is dispersed in the water by surfactant (B).
4) respectively, the ratio of phosphorus compound (A) is in the scope of 30 to 60 weight % of fire retardant integral body, and the ratio of surfactant (B) is in the scope of 5 to 15 weight % of fire retardant integral body, and phosphorus compound (A) is dispersed in the water by surfactant (B).
5) textile material comprises the fiber with higher crystalline region rate at least, and can comprise the fiber with higher amorphous regions ratio.
The method for preparing the anti-flammability textile material of the present invention comprises above-mentioned fire retardant is coated to method on the textile material.
The method that the prepares the anti-flammability textile material of the present invention A that should preferably meet the following conditions) and/or B).
A) textile material comprises the fiber with higher crystalline region rate at least, and can comprise the fiber with higher amorphous regions ratio.
B) above-mentioned coating is to carry out in 2 to 120 minutes by dipping in the solution that textile material is being contained fire retardant in temperature more than 80 ℃.
Anti-flammability textile material of the present invention obtains with above-mentioned preparation method.
Advantageous effects
Fire retardant of the present invention is used to give the textile material flame-retardant nature, and reaches sufficient flame-retardant nature with a small amount of fire retardant.Describedly contribute to minimizing on a small quantity by other textiles character deterioration that phosphorus compound caused in the fire retardant.Fire retardant of the present invention is coated to unlikely causes textile material, their feel and their color fastness to comprise deterioration on the textile material the friction or the color fastness of light.Described fire retardant reaches washing and dry-cleans durable flame-retardant nature, has reduced the burden to environment and human body, and has excellent stability.
As mentioned above, the method for preparing anti-flammability textile material of the present invention utilizes fire retardant to handle textile material, thereby obtains sufficient flame-retardant nature and the deterioration of other textiles character that is caused by phosphorus compound is minimized.
Implement best mode of the present invention
(fire retardant)
Fire retardant of the present invention is the composition that is used to give the textile material flame-retardant nature.
To being not particularly limited with the textile material of fire retardant coating, and the textile material that preferably contains the higher fiber of crystal region ratio at least, for example, but the copolymer of aromatic polyester, CATION-dyeing polyester, aromatic polyamides, aromatic polyimide, diacetate, triacetate and their monomers, because the flame-retardant nature of triphenylphosphine oxide that these textile materials absorb in the fire retardant fully to be contained to be improved.In described material, but more preferably comprise the textile material of aromatic polyester or CATION-dyeing polyester at least, reason is that it absorbs the high-performance of following phosphorus compound (A).
But the example of aromatic polyester and CATION-dyeing polyester comprises: polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate (PBT), PEN, PBN, poly terephthalic acid/ethylene isophthalate and poly terephthalic acid/5-(sodium sulfo group (sodium sulfo)) ethylene isophthalate.
Textile material can contain the higher fiber of above-mentioned crystal region ratio and the higher fiber of above-mentioned amorphous regions ratio simultaneously, and (for example, natural fabric comprises cotton, flax, wool; And nylon).
As mentioned herein crystal region be such as the physical treatment in the synthetic fiber production process as polymer chain formed in stretching, that wherein form fiber relatively with the zone of fiber of rule state orientation, and amorphous regions is opposite with the former, wherein form the relative zone of fiber with the stochastic regime orientation of polymer chain of fiber.
Textile material can comprise a kind of fibre variant or multiple fibre variant.The textile material that comprises the fiber that contains the higher rate crystal region simultaneously and contain the fiber of higher rate amorphous regions can or be united weaving (combined weaving) by blending and be formed.The form of textile material can adopt yarn, woven fabric, knit goods, nonwoven fabric, rope and mesh bag (code) without limits.
Fire retardant of the present invention comprises phosphorus compound (A), surfactant (B) and water, and described surfactant (B) comprises anion surfactant and/or non-ionic surface active agent.Described component is not halogen-containing, thereby the burden to environment and human body is minimized.
The phosphorus compound (A) that uses in the present invention is coated on the textile material to improve their flame-retardant nature.Phosphorus compound (A) has the molecular structure of unlikely hydrolysis, and can not cause the deterioration of the textile material found in the textile material that is coated with phosphate flame retardant as described in the background art.Phosphorus compound (A) is that fusing point is not less than 130 ℃ solid, and this character makes this compound can keep stable dispersiveness in solution, is used for giving flame-retardant nature under the temperature more than 80 ℃.In addition, the phosphorus compound (A) that is coated on textile material can not cause dye migration outside textile material, therefore contributes to excellent color fastness as the color fastness to friction.
Molecular weight to phosphorus compound (A) is not particularly limited, and should be preferably in 250 to 500, more preferably 250 to 400 scope, to give washing and to dry-clean durable flame-retardant nature.
Phosphorus compound (A) is represented by above-mentioned chemical formula (1).In chemical formula (1), R
1, R
2And R
3In at least one should be preferably aryl or aralkyl, so that described compound fully is coated on the textile material.More preferably R
1, R
2And R
3It all is aryl or aralkyl.This phosphorus compound (A) comprises, for example, triphenylphosphine oxide, oxidation three (2-aminomethyl phenyl) phosphine, oxidation three (4-aminomethyl phenyl) phosphine, oxidation three (2, the 6-3,5-dimethylphenyl) phosphine, oxidation three (2, the 6-Dimethoxyphenyl) phosphine, tribenzylphosphine oxide and 2-(two phenenyl phosphinyl) quinhydrones.
Median particle diameter (the D of phosphorus compound (A)
50) should be below 1 micron, preferred below 0.8 micron, more preferably 0.2 to 0.6 micron, with the long-time stability of the excellence that obtains the invention described above and unique effect.Not preferred median particle diameter (D
50) greater than 1 micron phosphorus compound (A), because this compound can not obtain effect of the present invention and have poor long-time stability.
Median particle diameter (the D that mentions in the present invention
50) expression forms the intermediate value of whole particle grain size of the whole volume of phosphorus compound (A).
The ratio of contained phosphorus compound (A) is not particularly limited in fire retardant of the present invention, and should be preferably at 20 to 70 weight % of fire retardant integral body, more preferably in the scope of 30 to 60 weight %.The ratio that is lower than the phosphorus compound (A) of 20 weight % may be because the water of excessive ratio and other composition and cause problem at preparation, storage, stability and the aspect of performance of fire retardant.On the other hand, being higher than the ratio of the phosphorus compound (A) of 70 weight % possibly can't prepare stable fire retardant.
Surfactant (B) comprises anion surfactant and/or non-ionic surface active agent, and improves the dispersiveness of phosphorus compound (A).Phosphorus compound (A) is easy to usually reunite and is difficult for being made into particulate.Surfactant (B) plays the surface tension that reduces between phosphorus compound (A) and the water and the effect of moistening phosphorus compound (A), thereby effectively phosphorus compound (A) is made particulate.In addition, surfactant (B) control phosphorus compound (A) particulate is along with the reunion of time, thereby improves the stability of resulting fire retardant.Contained surfactant (B) makes and phosphorus compound (A) can be made particulate and be dispersed in the water in the fire retardant of the present invention.
Anion surfactant is not particularly limited, and for example can comprise: the alkylsurfuric acid salt, the alkyl aryl sulfate class, the polyoxyalkylene alkyl Sulfates, polyoxyalkylene alkyl aryl ether sulfate class (polyoxyalkylene three (2-phenylethyl) phenyl ether Sulfates, two (2-phenylethyl) the phenyl ether Sulfateses of polyoxyalkylene, polyoxyalkylene 2-phenyl ethyl phenyl ether sulfate class, polyoxyalkylene nonylplenyl ether Sulfates etc.), polyoxyalkylene alkyl polyols ether sulfate class, alkyl sulfonates, alkylaryl sulfonates class (xylenesulfonate, toluene fulfonate, cumene sulfonate etc.), alkyl aromatic ether disulfonic acid salt (alkyl diphenyl ether disulfonate class etc.), the alkyl sulfo succinate class, the alkyl phosphoric acid salt, the alkylaryl phosphoric acid salt, the polyoxyalkylene alkyl phosphoric acid salt, polyoxyalkylene alkyl aryl ether phosphoric acid salt, polyoxyalkylene alkyl polyols ether phosphoric acid salt, aromatic sulphonate-formaldehyde condensation products salt (naphthalene sulfonate-formaldehyde condensation products salt etc.), the polyoxyalkylene alkyl metal carboxylate, the polycarboxylic acid salt, turkey red oil and lignosulphonates.Be selected under the situation of salt preferred as alkali salt, alkaline-earth metal salt, ammonium salt class and organic amine salt at anion surfactant.Can use a kind of in the anion surfactant or at least two kinds.
In described anion surfactant, because theirs is excellent dispersed, preferred polyoxyalkylene alkyl aryl ether sulfate class, alkylaryl sulfonates class, alkyl aromatic ether disulfonic acid salt and aromatic sulphonate-formaldehyde condensation products salt, and except their excellent dispersiveness, because they make phosphorus compound (A) performance of particulate, more preferably polyoxyalkylene alkyl aryl ether sulfate class, alkylaryl sulfonates class and aromatic sulphonate-formaldehyde condensation products salt effectively in the preparation of fire retardant.More preferably aromatic sulphonate-formaldehyde condensation products salt again because the reunion in time of described salt control phosphorus compound (A) particulate, thereby improves the stability of fire retardant.
Non-ionic surface active agent is not particularly limited, and for example comprise polyoxyalkylene alkyl class, polyoxyalkylene alkylaryl ethers (polyoxyalkylene three (2-phenylethyl) phenyl ether, two (2-phenylethyl) phenyl ethers of polyoxyalkylene, polyoxyalkylene (2-phenylethyl) phenyl ether, polyoxyalkylene nonylplenyl ether etc.), polyoxyalkylene alkyl amine, polyoxyalkylene alkylamide, polyoxyalkylene fatty acid ester, polyoxyalkylene castor oil ethers, polyoxyalkylene rilanit special ethers and polyoxyalkylene polyol ethers.Can use a kind of in the described non-ionic surface active agent or at least two kinds.
In described non-ionic surface active agent, because theirs is excellent dispersed, preferred polyoxyalkylene alkylaryl ethers, polyoxyalkylene castor oil ethers, polyoxyalkylene rilanit special ethers and polyoxyalkylene fatty acid ester, and because phosphorus compound (A) is made the reunion that particulate and control phosphorus compound (A) particulate are passed in time effectively in their excellences dispersed and they in the preparation of fire retardant, thereby improve the performance of fire retardant stability, more preferably polyoxyalkylene castor oil ethers, polyoxyalkylene rilanit special ethers and polyoxyalkylene fatty acid ester.
Contained non-ionic surface active agent integral body should preferably have by the definite HLB in 11 to 15 scopes of lattice Lifei method (Griffin ' s method) in fire retardant of the present invention, and form 1% aqueous solution that clouding point is not less than 10 ℃, because this non-ionic surface active agent has the excellent performance that phosphorus compound (A) is disperseed.
The ratio of the surfactant in fire retardant of the present invention (B) is not particularly limited, should be preferably at 3 to 20 weight % of fire retardant, more preferably in the scope of 5 to 15 weight %.The ratio that is lower than the surfactant (B) of 3 weight % possibly can't be prepared stable fire retardant.On the other hand, the ratio that is higher than 20 weight % may deterioration be coated with fire retardant textile material color fastness or quicken dyestuff depression effect when adding to fire retardant in the dye bath.
The prescription of fire retardant of the present invention is not particularly limited, as long as its phosphorus-containing compound (A), surfactant (B) and water.Fire retardant can contain other component that can influence effect of the present invention sharply.
Component except above-mentioned those components comprises, for example: solvent (methyl alcohol, ethanol, isopropyl alcohol, ethylene glycol, propylene glycol, butanediol, benzylalcohol, 3-methoxyl group-3-methyl isophthalic acid-butanols, BC, poly alkylene glycol etc.), water-soluble polymer (polyvinyl alcohol, polyacrylate, methylcellulose, Carboxymethyl Cellulose, hydroxyethylcellulose, carboxymethyl cellulose, xanthans, gum Arabic, gelatin, PVP, poly(ethylene oxide), polyacrylamide, poly styrene sulfonate, the polystyrene-maleic copolymer, methoxy-ethylene-copolymer-maleic anhydride, the soluble starch class, the cationic starch class, carboxymethyl starch class etc.); Carrier (aromatic halide class, N-alkyl phthalimide, aromatic carbonate, methyl naphthalene, biphenyl, diphenyl ester, naphthol ester, phenol ether, xenol etc.); Other fire retardant (phosphoric acid ester, comprise triphenyl phosphate, tricresyl phosphate hydroxy toluene ester, trixylyl phosphate, phosphoric acid cresyl phenyl ester, di(2-ethylhexyl)phosphate tolyl phenyl ester, phosphoric acid cresyl diformazan phenyl ester, adjacent biphenyl ester of phosphoric acid phenyl and Naphthyl phosphate, the condensed phosphoric acid esters class comprises resorcinol two (diphenyl phosphoester), bisphenol-A two (diphenyl phosphoester) and resorcinol two (xylyl phosphate), phosphite, hypophosphites, phosphine oxide, the phosphoamide ester, chloride phosphoric acid ester, chloride condensed phosphoric acid esters class, the phosphorous-containing polyester resin, the phosphorus azane, the bromide fire retardant comprises hexabromo-Cyclododecane, deca-BDE, ethylenebis (pentabromo-biphenyl), ethylenebis (tetrabromo phthalimide) and three (tribromophenoxy) triazine); And ultra-violet absorber, comprise benzotriazole UV absorbers (2-(2 '-hydroxyl-the 3 '-tert-butyl group-5 '-aminomethyl phenyl)-5-chlorobenzotriazole and 2-(2 '-hydroxyl-5 '-aminomethyl phenyl) benzotriazole), benzophenone UV-absorber (2-hydroxyl-4-methoxy benzophenone and 2,2 ' 4,4 '-tetrahydroxybenzophenone), (2-(4 for triazine uv absorber, 6-diphenyl-1,3,5-triazine-2-yl)-5-(own oxygen base)-phenol and 2,4-two (2, the 4-3,5-dimethylphenyl)-6-(2-hydroxyl-4-octyloxyphenyl)-1,3, the 5-triazine) benzoxazinone ultra-violet absorber (2,2 '-(to phenylene) two-3,1-benzoxazine-4-ketone), cyanoacrylate ultra-violet absorber (ethyl-2-cyano group-3,3-diphenylacrylate ester and (2-ethylhexyl)-2-cyano group-3,3-diphenylacrylate ester) and salicylate ultra-violet absorber (p-t-butylphenyl salicylate).
The ratio of said components is not particularly limited.Thereby but the viscosity of the solvent of little ratio reduction fire retardant is improved stability, dispersiveness and emulsibility under operating efficiency, the low temperature.Yet the solvent of big ratio may cause preparing and storing the problem of fire retardant aspect, and ratio should be preferably below the 20 weight % of fire retardant.
Fire retardant of the present invention prepare by phosphorus compound (A), surfactant (B) and water are mixed, and is used to mix the method for described component and is not particularly limited in proper order.The method for preparing fire retardant of the present invention comprises that for example, a kind of method wherein prepares median particle diameter (D in advance
50) be not more than 1 micron phosphorus compound (A), and it is mixed (method 1) with surfactant (B) and water; With a kind of method, wherein phosphorus compound (C) is mixed with surfactant (B) and water, described phosphorus compound (C) is except median particle diameter (D
50) greater than beyond 1 micron, have the identical character of character with phosphorus compound (A), use micro-granulating device that phosphorus compound (C) is dispersed into particulate (method 2) then.In method 2, can use phosphorus compound (A) to replace phosphorus compound (C) so that the median particle diameter (D of phosphorus compound
50) littler.
In method 2, micronizer comprises a grinding machine, sand mill and grater (grinder).In addition, in method 2, can randomly add some additives, such as non-drying agent (non-dryingagent), defoamer and viscosity improver.Can use commercially available phosphorus compound as phosphorus compound (C), and can before mixing, they be made particulate roughly.
Said method 1 or method 2 can be used as the method for preparing fire retardant of the present invention, and method for optimizing 2, because in method 1, the reunion particulate of the phosphorus compound (A) of particle diameter below 1 micron may not separate, and may cause the instability in the resulting fire retardant to be disperseed.
Fire retardant of the present invention is used to give flame-retardant nature to textile material.The form of the fire retardant that uses is not particularly limited, and usually it is diluted in the water and coating.
[anti-flammability textile material and preparation method thereof]
The method for preparing anti-flammability textile material of the present invention comprises above-mentioned fire retardant is coated to step (finishing (finishing) step) on the textile material.
In the finishing step, fire retardant and textile material are in contact with one another so that the phosphorus compound in the fire retardant (A) is coated on the textile material.The finishing step comprises, for example, wherein textile material contained 2 to 120 minutes step (step 1) of dipping in the bath of fire retardant in the temperature more than 80 ℃; With another method, wherein fire retardant is coated on the textile material, then textile material is heated so that phosphorus compound (A) is penetrated into (step 2) in the textile material at 100 to 220 ℃.
In step 1, phosphorus compound (A) is coated on the textile material by following method usually: textile material is immersed in by in the prepared bath of dilute with water fire retardant, thereby (A) is coated on the textile material with phosphorus compound, and will be immersed in the textile material heating 2 to 120 minutes in the bath of the temperature more than 80 ℃, so that flame-retardant nature is durable.The thinner ratio of fire retardant is not particularly limited, but is generally 10 to 10000 times water.The treatment temperature of textile material in bath should be preferably more than 80 ℃, more preferably 90 ℃ to 150 ℃, because the amorphous regions of textile material is lax or expansion, thereby quickens the coating of phosphorus compound (A) to textile material.Step 1 can operative installations for example jet dyeing machine, beam dyeing machine and yarn package dyeing machine carry out.
In step 2, by textile material being immersed in by in the prepared bath of dilute with water fire retardant and phosphorus compound (A) is coated on the textile material, and the textile material that will behind dipping, be dried sometimes heating, so that phosphorus compound (A) is penetrated in the textile material, thereby make flame-retardant nature durable.Heating-up temperature should be preferably 100 to 220 ℃, more preferably in 160 ℃ to 200 ℃ the scope,, thereby quicken the coating of phosphorus compound (A) to textile material because the amorphous regions of textile material is lax or expand.Preferably be not lower than 100 ℃ heating-up temperature,, thereby give the flame-retardant nature of poor durability sometimes because so low temperature can't obtain the abundant infiltration of phosphorus compound (A) in textile material.On the other hand, preferably be not higher than 220 ℃ heating-up temperature, because excessive heat possibility deterioration textile material, thereby the toughness of reduction textile material.Can use dip-dye, spray or be coated with fire retardant is coated on the textile material.Heating can be by xeothermic or damp and hot carrying out.This coating and heating means comprise sprays and dried cure system, dip-dye and net gas steaming system, dip-dye and decatize system and dip-dye and dried cure system.
The preparation method of anti-flammability textile material of the present invention can comprise at least one in above-mentioned steps 1 and the step 2.Repeat identical step or can give textile material better flame-retardant nature step 1 and step 2 combination.In addition, the preparation method of anti-flammability textile material of the present invention can also comprise the finishing step that another uses the fire retardant different with fire retardant of the present invention.
In the preparation method of anti-flammability textile material of the present invention, fiber finishing agent and the fiber finishing auxiliary agent that is different from fire retardant of the present invention can be used for textile material is carried out finishing.Other fiber finishing agent and fiber finishing auxiliary agent comprise, for example, the fire retardant, dyestuff (basic-dyeable fibre and DISPERSE DYES), carrier (aromatic halide class, N-alkyl phthalimide, aromatic carbonate, methyl naphthalene, biphenyl, biphenyl ester, naphthol ester, phenol ether, xenol etc.), deodorant, antiseptic, softening agent, antistatic additive, waterproofing agent, oil-proofing agent, curing agent, ultra-violet absorber, anti-fouling agent and the hydrophilizing agent that are different from phosphorus compound (A).Can use a kind of in the described reagent or at least two kinds.
In the preparation method of anti-flammability textile material of the present invention, fire retardant on the textile material, the amount (amount of obtaining (pickup)) that is phosphorus compound (A) is not particularly limited, because it changes according to following condition, such as, the variant of textile material and structure and the variant and the amount of obtaining that are coated on other fiber finishing agent on the textile material.Preferably the amount of obtaining should be at 0.1 to 30 weight % of textile material, more preferably in the scope of 1 to 20 weight %.The amount of obtaining less than the phosphorus compound (A) of 1 weight % possibly can't give textile material sufficient flame-retardant nature.On the other hand, greater than the amount of obtaining of 30 weight % may the resulting anti-flammability textile material of deterioration feel, also may be uneconomic the fire retardant of the amount of obtaining just no longer further improves flame retardant effect because surpass necessarily.
Embodiment
With following embodiment and comparative example the present invention is carried out specific explanations, although the invention is not restricted in the scope of described embodiment.
[method of testing]
(1) median particle diameter (D
50) and average volume diameter
To fire retardant sampling and use laser diffraction and scattering particle size analyzer LA-910 (producing) analysis, to determine its median particle diameter (D by Horiba Co., Ltd by the micronize preparation
50) and average volume diameter.
(2) product stability
Visual inspection is 40 ℃ of outward appearances that store 1 month fire retardant.To show not that precipitation or the fire retardant that separates are evaluated as " well ", and will show that precipitation or the fire retardant that separates are evaluated as " bad ".
(3) flame-retardant nature
In the anti-flammability finishing, woven fabric is carried out finishing with fire retardant.According to JIS L-1091 A-1 (microlamp method (microburner method)) and JIS L 1091 D (coil method (coil method)) to testing through the fabric of finishing and the flame-retardant nature of two fabric samples, in described two fabric samples one is by will washing 5 preparations through the fabric of finishing with water, and in described two fabric samples another is by with following method will be through 5 preparations of dry cleaning fabric of finishing.
In " microlamp method ", add heating fabric: heated for 3 seconds with microlamp with microlamp heating 1 minute with in fabric burning back with two kinds of methods.In both cases, such fabric is evaluated as " well ", promptly on described fabric, flame keeps no longer than 5 seconds after heating no longer than 3 seconds, residual vehement (afterglow) in maintenance after the heating, and generation is not more than 30cm
2The carbonization area, be evaluated as " poor " and will show the flammable fabric that surpasses the described limit.In " coil method ", will contact the fabric that can be burned to preset distance more than 3 times with flame and be evaluated as " well ", be evaluated as " poor " and will contact the fabric that can be burned to preset distance below 2 times with flame.
In water, wash
According to JIS K 3371 laundering of textile fabrics, wherein at first with fabric in the detergent solution that contains alkalescent 1 class (group 1) washing agent that 1g/ rises, with 1: 40 the fabric and the ratio of detergent solution, washed 15 minutes down at 60 ± 2 ℃, rinsing 5 minutes 3 times in water under 40 ± 2 ℃ then, with centrifugal dehydrator dehydration 2 minutes, and dry in hot-air under 60 ± 5 ℃.The process of washing is carried out 5 times altogether.
Dry-cleaning
The woven fabric that 1 gram is coated with fire retardant was handled 15 minutes down at 30 ± 2 ℃ with the electric charge soap (charge soap) (non-ionic surface active agent, anion surfactant and the water that contain 10: 10: 1 weight ratios) of 12.6 milliliters of tetrachloroethanes and 0.265g.Handle and carry out altogether 5 times.
(4) color fastness to rubbing
Prepare the polyester woven fabric of the dyeing of fire retardant finishing by in dye bath, adding fire retardant, and test according to JIS L 0849 usefulness friction analyzer II.By grading the result is estimated, and higher number of degrees is represented the better color fastness to rubbing.
(5) to the color fastness of light
According to the method for definition among the JIS L 0842, make polyester textile be exposed to carbon arc lamp 100 hours, and estimate by grading with the dyeing of method for preparing.Higher number of degrees is represented better color fastness to light.
[embodiment 1 to 4]
The component of every kind of prescription shown in the table 1 is placed in the agitator, and stirs with abundant dispersion.In 4 hours, resulting slurries are processed into particulate with the preparation fire retardant then with grain grinding machine ZRS (producing) by Ashizawa Finetech Co., Ltd.POE (20) three (2-phenylethyl) phenyl ether sodium sulphate described in the table 1 is polyoxyethylene three (2-phenylethyl) the phenyl ether sodium sulphate that contains 20 oxygen ethylene repeating units.
Determine the median particle diameter and the average volume diameter of resulting fire retardant, and the stability of visual inspection fire retardant.In the anti-flammability finishing, textile material is carried out finishing then with resulting fire retardant and following parameter (comprise dyeing and soap), and determine the flame-retardant nature of resulting anti-flammability textile material, to the color fastness of friction with to the color fastness of light.
[anti-flammability finishing]
With small-sized dyeing machine (producing) by Texam Co., Ltd, with undyed polyester 100% top-weight fabric in dye bath, with the ratio of 1: 15 fabric and bath and 4.5 bath pH, handled 30 minutes at 130 ℃, described dye bath contains each of fire retardant (with their %owf in the table 1) of description in the Kayalon Polyester Black AL 167 (a kind of DISPERSE DYES, by Nippon Kayaku Co., Ltd produce) of 6 fibre weight % and the table 1.Then in soaping with fabric in the solution that contains the caustic soda that soaping agent (being produced by Matsumoto Yushi-Seiyaku Co., Ltd) that 1g/ rises, bisulfites that 2g/ rises and 2g/ rise, with the ratio of 1: 15 fabric with solution, handled 20 minutes at 80 ℃, rinsing in water, and, thereby be prepared into the fire-retardant polyester fabric 170 ℃ of dryings 1 minute.
Table 1
Comparative example 1 to 6
Except the component described in using table 2, with embodiment 1 to 4 in identical method prepare fire retardant.Then with the method identical, each resulting relatively fire retardant is used for anti-flammability finishing (comprise dyeing and soap) with embodiment 1 to 4.Determine the flame-retardant nature of resulting textile material, to the color fastness of friction with to the color fastness of light.
Table 2
The fire retardant of embodiment 1 to 4 caused after the anti-flammability finishing textile material, after the anti-flammability finishing in water the textile material of washing 5 times and after the anti-flammability finishing, dry-clean 5 times textile material and have highly durable flame-retardant nature; Color fastness through the excellence of the textile material of finishing to friction; Stability with excellence.On the contrary, the fire retardant of comparative example 1 to 6 has poor stability and separates.Although as under the situation of comparative example 3, the flame-retardant nature that will be given by the fire retardant of comparative example by the amount of obtaining that increases fire retardant has been improved to the similar degree of improvement with embodiment 1 to 4, but the fire retardant of comparative example 3 cause the wet spinning fabric difference to the color fastness of friction and the color fastness to light of difference.Comparative example 4 and 5 fire retardant cause the flame-retardant nature of difference and to the color fastness of friction.The fire retardant of comparative example 6 causes the color fastness to light of difference.
Industrial usability
Fire retardant of the present invention is suitable for giving the textile material flame-retardant nature. Be coated to the basis on the textile material The invention fire retardant least is easy to deterioration textile material, its feel and color fastness thereof, comprise to the friction and Fastness to light. Described fire retardant can obtain washing with the burden to environment and human body of minimum The flame-retardant nature durable with dry-cleaning, and have excellent stability.
Claims (according to the modification of the 19th of treaty)
Modification statement according to the 19th of PCT treaty
Being revised as of claim 1: described surfactant (B) comprises the anion surfactant as key component, and described anion surfactant contains and is selected from least a in the group of being made up of the following: polyoxyalkylene alkyl aryl ether sulfate class, alkyl aromatic ether disulfonic acid salt and aromatic sulphonate-formaldehyde condensation products salt.Therefore, show that described fire retardant comprises specific phosphorus compound (A) and specific anion surfactant.Described anion surfactant and described non-ionic surface active agent further limit in claim 2 and 3.
Both not open these anion surfactants of also not advising of existing document 1.On the other hand, existing document 2 and 3 does not disclose fire retardant.In addition, the function of employed surfactant is different from the function of the surfactant that is used for further showing flame-retardant nature in the present invention fully.Therefore, both not open also suggestion of existing document 1 to 3 used these specific anion surfactants with the specific phosphorus compound (A) that is not less than 130 ℃ by chemical formula (1) expression and fusing point, and existing document does not provide enlightenment.
1. (modification) a kind of fire retardant, described fire retardant is used to give the textile material flame-retardant nature, and described fire retardant comprises:
Phosphorus compound (A), described phosphorus compound (A) is represented by chemical formula shown below (1), and is had the fusing point that is not less than 130 ℃;
Surfactant (B), described surfactant (B) comprises anion surfactant; Or anion surfactant and non-ionic surface active agent; With
Water;
Wherein said phosphorus compound has the median particle diameter (D that is not more than 1 micron
50); And wherein said anion surfactant is selected from least a in the group of being made up of the following: polyoxyalkylene alkyl aryl ether sulfate class, alkyl aromatic ether disulfonic acid salt and aromatic sulphonate-formaldehyde condensation products salt.
(R wherein
1, R
2And R
3Can be same to each other or different to each other, and expression can have substituent C
1-24Alkyl, C
2-22Thiazolinyl, C
5-6Alcyl, and aryl or aralkyl.)
2. (modification) fire retardant according to claim 1, wherein said anion surfactant contains described aromatic sulphonate-formaldehyde condensation products salt as key component.
3. (modification) fire retardant according to claim 1 and 2, wherein said non-ionic surface active agent contain and are selected from least a in the group of being made up of the following: polyoxyalkylene alkylaryl ethers, polyoxyalkylene castor oil ethers, polyoxyalkylene rilanit special ethers and polyoxyalkylene aliphatic acid ethers.
4. according to each described fire retardant in the claim 1,2 and 3, the ratio of wherein said phosphorus compound (A) and described surfactant (B) is respectively in the scope of 20 to 70 weight % of described fire retardant integral body and 3 to 20 weight %, and described phosphorus compound (A) is dispersed in the water by described surfactant (B).
5. according to each described fire retardant in the claim 1,2,3 and 4, the ratio of wherein said phosphorus compound (A) and described surfactant (B) is respectively in the scope of 30 to 60 weight % of described fire retardant integral body and 5 to 15 weight %, and described phosphorus compound (A) is dispersed in the water by described surfactant (B).
6. according to each described fire retardant in the claim 1,2,3,4 and 5, wherein said textile material comprises a kind of fiber with higher crystalline region rate at least, and can comprise the fiber that another kind has higher amorphous regions ratio.
7. method for preparing the anti-flammability textile material, described method comprises the step of using according to each the described fire retardant finishing of textile materials in the claim 1,2,3,4,5 and 6.
8. the method for preparing the anti-flammability textile material according to claim 7, wherein said textile material comprise a kind of fiber with higher crystalline region rate at least, and can comprise the fiber that another kind has higher amorphous regions ratio.
9. according to claim 7 or the 8 described methods that prepare the anti-flammability textile material, wherein said finishing step is by in the temperature more than 80 ℃, described textile material was flooded in the bath that contains described fire retardant 2 to 120 minutes and carries out.
10. anti-flammability textile material, described anti-flammability textile material is with according to each described method preparation in the claim 7,8 and 9.
Claims (10)
1. fire retardant, described fire retardant is used to give the textile material flame-retardant nature, and described fire retardant comprises:
Phosphorus compound (A), described phosphorus compound (A) is represented by chemical formula shown below (1), and is had the fusing point that is not less than 130 ℃;
Surfactant, described surfactant comprises anion surfactant and/or non-ionic surface active agent; With
Water; Wherein said phosphorus compound has the median particle diameter (D that is not more than 1 micron
50).
(R wherein
1, R
2And R
3Can be same to each other or different to each other, and expression can have substituent C
1-24Alkyl, C
2-22Thiazolinyl, C
5-6Alcyl, and aryl or aralkyl.)
2. fire retardant according to claim 1, wherein said surfactant (B) contain and are selected from least a in the group of being made up of the following: polyoxyalkylene alkyl aryl ether sulfate class, alkylaryl sulfonates class, alkyl aromatic ether disulfonic acid salt, aromatic sulphonate-formaldehyde condensation products salt, polyoxyalkylene alkylaryl ethers, polyoxyalkylene castor oil ethers, polyoxyalkylene rilanit special ethers and polyoxyalkylene aliphatic acid ethers.
3. fire retardant according to claim 1 and 2, wherein said surfactant (B) contain and are selected from least a in the group of being made up of the following: aromatic sulphonate-formaldehyde condensation products salt, polyoxyalkylene castor oil ethers, polyoxyalkylene rilanit special ethers and polyoxyalkylene aliphatic acid ethers.
4. according to each described fire retardant in the claim 1,2 and 3, the ratio of wherein said phosphorus compound (A) and described surfactant (B) is respectively in the scope of 20 to 70 weight % of described fire retardant integral body and 3 to 20 weight %, and described phosphorus compound (A) is dispersed in the water by described surfactant (B).
5. according to each described fire retardant in the claim 1,2,3 and 4, the ratio of wherein said phosphorus compound (A) and described surfactant (B) is respectively in the scope of 30 to 60 weight % of described fire retardant integral body and 5 to 15 weight %, and described phosphorus compound (A) is dispersed in the water by described surfactant (B).
6. according to each described fire retardant in the claim 1,2,3,4 and 5, wherein said textile material comprises a kind of fiber with higher crystalline region rate at least, and can comprise the fiber that another kind has higher amorphous regions ratio.
7. method for preparing the anti-flammability textile material, described method comprises the step of using according to each the described fire retardant finishing of textile materials in the claim 1,2,3,4,5 and 6.
8. the method for preparing the anti-flammability textile material according to claim 7, wherein said textile material comprise a kind of fiber with higher crystalline region rate at least, and can comprise the fiber that another kind has higher amorphous regions ratio.
9. according to claim 7 or the 8 described methods that prepare the anti-flammability textile material, wherein said finishing step is by in the temperature more than 80 ℃, described textile material was flooded in the bath that contains described fire retardant 2 to 120 minutes and carries out.
10. anti-flammability textile material, described anti-flammability textile material is with according to each described method preparation in the claim 7,8 and 9.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2007048438 | 2007-02-28 | ||
| JP048438/2007 | 2007-02-28 | ||
| PCT/JP2008/000169 WO2008105140A1 (en) | 2007-02-28 | 2008-02-07 | Flameproofing agent, flame-retardant fiber and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101631910A true CN101631910A (en) | 2010-01-20 |
| CN101631910B CN101631910B (en) | 2013-05-22 |
Family
ID=39720983
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200880003918.4A Expired - Fee Related CN101631910B (en) | 2007-02-28 | 2008-02-07 | Flameproofing agent, flame-retardant fiber and method for producing the same |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP4348407B2 (en) |
| CN (1) | CN101631910B (en) |
| WO (1) | WO2008105140A1 (en) |
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2008
- 2008-02-07 WO PCT/JP2008/000169 patent/WO2008105140A1/en active Application Filing
- 2008-02-07 JP JP2009501115A patent/JP4348407B2/en not_active Expired - Fee Related
- 2008-02-07 CN CN200880003918.4A patent/CN101631910B/en not_active Expired - Fee Related
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Also Published As
| Publication number | Publication date |
|---|---|
| CN101631910B (en) | 2013-05-22 |
| JP4348407B2 (en) | 2009-10-21 |
| WO2008105140A1 (en) | 2008-09-04 |
| JPWO2008105140A1 (en) | 2010-06-03 |
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