CN105064016A - Flame retardant for textile materials, preparation method thereof and prepared flame-retardant textile material - Google Patents
Flame retardant for textile materials, preparation method thereof and prepared flame-retardant textile material Download PDFInfo
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Abstract
The invention provides a flame retardant for textile materials, a preparation method thereof and a prepared flame-retardant textile material. Sufficient flame-retardant property can be achieved with a small amount of flame retardant on the textile material, the decrease of the other properties of the textile material is minimized, and moreover, the flame retardant has excellent stability. The flame retardant contains phosphorus compound, surfactants and water, and the surfactants include anionic surfactant and/or nonionic surfactant; moreover, the flame retardant is used for giving flame-retardant property to the textile material, and furthermore, the phosphorus compound has median size (D50) which is not greater than 1 microns.
Description
Technical field
The invention belongs to fire retardant and textile material technical field, relate to the flame-retardant textile material of a kind of fire retardant for textile material, its preparation method and preparation.
Background technology
In conventional method, be normally used for giving textile material with flame-retardant nature by dispersion or the fire retardant of emulsification halogen compounds prepared by hexabromo-Cyclododecane in water.Although the textile material being coated with halogen compounds has flame-retardant nature, poison gas may be produced when this material combustion., there is the trend avoiding as far as possible using halogen compounds in the motion away from halogen compounds for this reason and in order to increase based on environmental consideration.
Although organic phosphorus compound is used as the substitute of halogen compounds, due to a small amount of phosphorus contained in each molecule of those compounds, they cannot give enough flame-retardant natures.Therefore, a large amount of organic phosphorus compound must be applied to give sufficient flame-retardant nature on textile material.Textile material applies so a large amount of organic phosphorus compounds and result in problem, such as, difference textile material feel and by rub and be exposed to the dyed textile material that light causes color fastness reduce.In addition, the molecular weight of organic phosphorus compound is too little and thermo-labile, and therefore described compound causes the transparent article be coated with around the textile material of this compound to be atomized sometimes.In order to address these problems, advise diphosphonic acid high for molecular weight to be used for fire retardant.References 1 to 3 discloses and uses resorcinol two (diphenyl phosphoester) to give the method for textile material flame-retardant nature as the example of phosphonium flame retardant.
References 4 discloses the method using fire retardant to give textile material flame-retardant nature, described fire retardant is by being disperseed and the solution of preparation by four (2,6-the 3,5-dimethylphenyls)-m-phenylene phosphate as the fire retardant with phosphorus compound.
References 5 discloses the method using fire retardant to give textile material flame-retardant nature, and described fire retardant is the solution by the naphthyl diphenyl phosphoester dispersion as phosphonium flame retardant being prepared.
[references 1] JPA2000-328445
[references 2] JPA2002-88368
[references 3] JPA2005-15947
[references 4] JPA2001-254268
[references 5] JPA2006-70417
But, resorcinol disclosed in references 1 to 3 two (diphenyl phosphoester) is easy to hydrolysis due to phosphorus-oxygen singly-bound (phosphate-based) contained in its chemical constitution, and the phosphoric acid produced in hydrolysis makes textile material deterioration.In addition, the color fastness of two (diphenyl phosphoester) the deteriorated dyed textile material of resorcinol, such as owing to the color fastness loss of friction, because this compound is liquid at a normal temperature.Fire retardant disclosed in references 3 due to employ can self-emulsifying resorcinol two (diphenyl phosphoester) and be comparatively not easy to hydrolysis.But when being coated on textile material by fire retardant, it becomes and is easier to hydrolysis, and thus As time goes on deteriorated textile material.For making flame-retardant properties to washing and dry-cleaning durable object, usually in dye bath, described fire retardant is coated on textile material.In this process, resorcinol two (diphenyl phosphoester) can not give textile material with enough flame-retardant natures, because this material fully cannot be coated on textile material owing to its high molecular.Although contained by fire retardant disclosed in above-mentioned references 4 four (2,6-3,5-dimethylphenyl)-m-phenylene phosphate has resistance to hydrolysis, but the high molecular of phosphate and steric bulk character stop it to be coated to fully on textile material and suppress to obtain durable flame-retardant nature.Naphthyl diphenyl phosphoester contained in fire retardant disclosed in references 5 has the fusing point of about 60 DEG C, and when the textile material being coated with described fire retardant is processed to goods as automotive seat, described fire retardant may melting 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 at its aspect of performance simultaneously.
CN101631910B discloses a kind of fire retardant and flame-retardant textile material and preparation method thereof, described fire retardant comprises phosphorus compound (A), surfactant and water, and described surfactant comprises anion surfactant and/or non-ionic surface active agent; And described fire retardant is used to give textile material flame-retardant nature, and described phosphorus compound (A) has the median particle diameter (D50) being not more than 1 micron.Described phosphorus compound has following structural formula
wherein, R
1, R
2and R
3for substituent C1-24 alkyl, C2-22 thiazolinyl, C5-6 alcyl, aryl or aralkyl can be had.But the performance of described fire retardant is desirable not enough, need further to be studied.
Summary of the invention
An object of the present invention is to provide a kind of fire retardant, described fire retardant can give textile material flame-retardant nature, textile material can be made to reach sufficient flame-retardant nature with a small amount of fire retardant, the deterioration of described fire retardant to textile properties minimizes, and has excellent stability; Two of object of the present invention is to provide a kind of anti-flammability textile material; Three of object of the present invention is the preparation method providing a kind of anti-flammability textile material, and described method is simple, easy to operate.
Fire retardant provided by the invention comprises phosphorus compound (A), surfactant (B) and water, described phosphorus compound (A) is represented by following formula (1), and described surfactant is: the composition of a kind of in polyoxyalkylene alkyl aryl ether Sulfates, alkylaryl sulfonates class or alkyl aromatic ether disulfonic acid salt or at least two kinds; And fire retardant of the present invention is used to give textile material flame-retardant nature, wherein phosphorus compound (A) has the median particle diameter (D50) of less than 1 micron.
[chemical formula 1]
Wherein, R
1, R
2and R
3be respectively C6 alcyl, aryl and C5 alcyl.
The present invention uses specific phosphorus compound, make textiles under the minimized condition of its property-deterioration, reduce the amount being coated on the fire retardant on textile material, and the surfactant added in fire retardant can improve the stability of fire retardant.
As preferred technical scheme, described surfactant (B) is: polyoxyalkylene alkyl aryl ether Sulfates.
The mass percentage that described phosphorus compound (A) accounts for fire retardant entirety is 20 ~ 70%, as 30%, 40%50,60% or 65% etc.; The mass percentage that surfactant (B) accounts for fire retardant entirety is 3 ~ 20%, and as 5,10,12,14,15,16,18% or 19% etc., and phosphorus compound (A) is dispersed in water by surfactant (B).
As preferred technical scheme, the mass percentage that described phosphorus compound (A) accounts for fire retardant entirety is 30 ~ 60%, and the mass percentage that described surfactant (B) accounts for fire retardant entirety is 5 ~ 15%.
On the other hand, the invention provides a kind of flame-retardant textile material, containing fire retardant as above in described flame-retardant textile material.
Described flame-retardant textile material at least comprises a kind of fiber with higher crystalline region rate.
Described flame-retardant textile material also comprises the fiber with higher amorphous regions ratio.
Present invention also offers the preparation method of described flame-retardant textile material, described method is: use fire retardant finishing of textile materials.
Described finishing is: the temperature more than 80 DEG C, as 85 DEG C, 90 DEG C, 95 DEG C, 100 DEG C, 110 DEG C, 120 DEG C or 130 DEG C etc., textile material is flooded 2 ~ 120min in the bath containing described fire retardant, as 5min, 10min, 20min, 30min, 50min, 70min, 80min, 100min, 110min or 115min etc.; bath raio 1:10 ~ 25, as 1:12,1:15,1:18,1:20,1:22,1:23 or 1:24 etc.
The textile material of fire retardant coating is not particularly limited, preferably at least contain the textile material of the higher fiber of a kind of crystal region ratio, such as, aromatic polyester, CATION-can the copolymer of dyeing polyester, aromatic polyamides, aromatic polyimide, diacetate, triacetate and their monomers, because these textile materials absorb triphenylphosphine oxide contained in fire retardant fully with the flame-retardant nature be improved.In the material, more preferably at least comprise aromatic polyester or CATION-can the textile material of dyeing polyester, reason is that it absorbs the high-performance of following phosphorus compound (A).
Aromatic polyester and CATION-can the example of dyeing polyester comprise: polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate (PBT), PEN, PBN, poly terephthalic acid/ethylene isophthalate and poly terephthalic acid/5-(sodium sulfo group (sodiumsulfo)) ethylene isophthalate.
Textile material can simultaneously containing the higher fiber of above-mentioned crystal region ratio and the higher fiber of above-mentioned amorphous regions ratio, and such as, natural fabric comprises cotton, flax, wool and nylon.
As mentioned herein crystal region be physical treatment in synthetic fiber production process as in stretching formed, the polymer chain that wherein forms fiber relatively with the zone of fiber of rule state orientation, and amorphous regions is contrary with the former, it is relative to the zone of fiber of stochastic regime orientation wherein to form the polymer chain of fiber.
Textile material can comprise a kind of fibre variant or multiple fibre variant.The textile material that also simultaneously can comprise the fiber containing higher rate crystal region and the fiber containing higher rate amorphous regions or can be combined weaving (combinedweaving) and be formed by blending.The form of textile material does not limit, and can adopt yarn, woven fabric, knit goods, nonwoven fabric, rope and mesh bag (code).
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, thus makes to minimize the burden of environment and human body.
The phosphorus compound used in the present invention (A) is coated on textile material to improve their flame-retardant nature.Phosphorus compound (A) has the molecular structure of unlikely hydrolysis, and can not cause in the deterioration being coated with the textile material found in the textile material of phosphate flame retardant as described in the background art.Phosphorus compound (A) is the solid that fusing point is not less than 130 DEG C, and this character makes this compound can keep stable dispersiveness in the solution, for giving flame-retardant nature at the temperature more than 80 DEG C.In addition, the phosphorus compound (A) being coated on textile material can not cause dye migration to outside textile material, therefore contributes to excellent color fastness as the color fastness to friction.
The median particle diameter (D50) of phosphorus compound (A) should be less than 1 micron, preferably less than 0.8 micron, more preferably 0.2 to 0.6 micron, to obtain the long-time stability of the excellence of the invention described above and unique effect.The phosphorus compound (A) that not preferred median particle diameter (D50) is greater than 1 micron, because this compound can not obtain effect of the present invention and have poor long-time stability.
The median particle diameter (D50) mentioned in the present invention represents the intermediate value of the particle diameter of whole particles of composition phosphorus compound (A) whole volume.
Phosphorus compound (A) contained in fire retardant of the present invention is preferably 20 ~ 70%, more preferably 30 ~ 60% of fire retardant total quality.The ratio of the phosphorus compound (A) lower than 20% may cause problem due to the water of excessive ratio and other composition at the preparation of fire retardant, storage, stability and aspect of performance.On the other hand, the ratio higher than the phosphorus compound (A) of 70% possibly cannot prepare stable fire retardant.
Described surfactant (B) is: the composition of a kind of in polyoxyalkylene alkyl aryl ether Sulfates, alkylaryl sulfonates class or alkyl aromatic ether disulfonic acid salt or at least two kinds, is preferably polyoxyalkylene alkyl aryl ether Sulfates.
Phosphorus compound (A) is easy to reunite and be not easily made into particulate usually.Surfactant (B) plays and reduces surface tension between phosphorus compound (A) and water and the effect of moistening phosphorus compound (A), thus effectively phosphorus compound (A) is made particulate.In addition, surfactant (B) controls the reunion of phosphorus compound (A) particulate along with the time, thus improves the stability of the fire retardant obtained.Surfactant (B) contained in fire retardant of the present invention makes it possible to phosphorus compound (A) make particulate and be dispersed in water.
Surfactant (B) in fire retardant of the present invention is preferably 3 ~ 20%, more preferably 5 ~ 15% of fire retardant quality.The ratio of the surfactant (B) lower than 3% possibly cannot prepare stable fire retardant.On the other hand, deterioration may be coated with the color fastness of the textile material of fire retardant or accelerate dyestuff depression effect when being added in dye bath by fire retardant higher than the ratio of 20%.
The formula 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 containing other component that can not adversely affect effect of the present invention.
Component except those components above-mentioned comprises, such as: solvent (methyl alcohol, ethanol, isopropyl alcohol, ethylene glycol, propylene glycol, butanediol, benzylalcohol, MMB, 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, polystyrene-maleic copolymer, methoxy-ethylene-copolymer-maleic anhydride, soluble starch class, cationic starch class, carboxymethyl starch class etc.), carrier (aromatic halide class, N-alkylphthalimide, 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, the adjacent Biphenyl Ester of phosphoric acid phenyl and Naphthyl phosphate, condensed phosphoric acid esters class comprises resorcinol two (diphenyl phosphoester), bisphenol-A two (diphenyl phosphoester) and resorcinol two (dixylenyl phosphate), phosphite, hypophosphites, phosphine oxide, phosphoamide ester, chloride phosphoric acid ester, chloride condensed phosphoric acid esters class, phosphorous-containing polyester resin, phosphorus azane, bromide flame retardant, comprise 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-3 '-the tert-butyl group-5 '-aminomethyl phenyl)-5-chlorobenzotriazole and 2-(2 '-hydroxyl-5 '-aminomethyl phenyl) benzotriazole), benzophenone UV-absorber (ESCALOL 567 and 2, 2 ' 4, 4 '-tetrahydroxybenzophenone), triazine uv absorber (2-(4, 6-diphenyl-1, 3, 5-triazine-2-base)-5-(own oxygen base)-phenol and 2, 4-two (2, 4-3,5-dimethylphenyl)-6-(2-hydroxyl-4-octyloxyphenyl)-1, 3, 5-triazine), benzoxazinone ultra-violet absorber (2, 2 '-(to phenylene) two-3, 1-benzoxazine-4-ketone), cyanoacrylate ultraviolet absorbent (ethyl-2-cyano group-3, 3-diphenylacrylate ester and (2-ethylhexyl)-2-cyano group-3, 3-diphenylacrylate ester) and salicylate UV light absorbers (p-t-butylphenyl salicylate).
Fire retardant of the present invention, by the mixing of phosphorus compound (A), surfactant (B) and water being prepared, is not particularly limited for the method and order mixing described component.The method preparing fire retardant of the present invention comprises, such as, one method, wherein previously prepared median particle diameter (D50) is not more than the phosphorus compound (A) of 1 micron, 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 greater than except 1 micron except median particle diameter (D50); there is the character identical with the character of phosphorus compound (A), then use micro-granulating device that phosphorus compound (C) is dispersed into particulate (method 2).In method 2, phosphorus compound (A) can be used to replace phosphorus compound (C) to make the median particle diameter of phosphorus compound (D50) less.
In method 2, micronizer comprises a grinding machine, sand mill and grater (grinder).In addition, some additives can optionally be added in method 2, such as non-drying agent (non-dryingagent), defoamer and viscosity-improving agents.Commercially available phosphorus compound can be used as phosphorus compound (C), and before combination they can be made particulate roughly.
Said method 1 or method 2 can be used as the method preparing fire retardant of the present invention, and method for optimizing 2, because in method 1, the agglomerated microparticles of the phosphorus compound (A) that particle diameter is less than 1 micron may not be separated, and the instability in obtained fire retardant may be caused to disperse.
Fire retardant of the present invention is used to give flame-retardant nature to textile material.The form of fire retardant used is not particularly limited, and to be usually diluted in water and to apply.
Flame-retardant textile material and preparation method thereof
The method preparing anti-flammability textile material of the present invention comprises the step (finishing (finishing) step) be coated to by above-mentioned fire retardant on textile material.
In correction step, fire retardant and textile material is made to contact with each other to be coated on textile material by the phosphorus compound (A) in fire retardant.Correction step comprises, and such as, the temperature wherein more than 80 DEG C is by textile material dipping step (step 1) of 2 ~ 120 minutes in containing the bath of fire retardant; With another method, wherein fire retardant is coated on textile material, then textile material is heated to make phosphorus compound (A) penetrate into (step 2) in textile material at 100 ~ 220 DEG C.
In step 1, phosphorus compound (A) is coated on textile material by following method usually: be immersed in by textile material by the bath prepared by dilute with water fire retardant, thus phosphorus compound (A) is coated on textile material, and by be immersed in more than 80 DEG C temperature bath in textile material heating 2 ~ 120 minutes, to make flame-retardant nature durable; bath raio 1:10 ~ 25.The thinner ratio of fire retardant is not particularly limited, but is generally the water of 10 to 10000 times.The treatment temperature of textile material in bath should be preferably more than 80 DEG C, is more preferably 90 DEG C ~ 150 DEG C, because the amorphous regions of textile material is lax or expand, thus accelerates the coating of phosphorus compound (A) to textile material.Step 1 can operative installations such as jet dyeing machine, beam dyeing machine and yarn package dyeing machine be carried out.
In step 2, by textile material being immersed in by phosphorus compound (A) being coated on textile material in the bath prepared by dilute with water fire retardant, and sometimes dried after impregnating textile material is heated, to make phosphorus compound (A) penetrate in textile material, thus make flame-retardant nature durable.Heating-up temperature preferably in the scope of 100 ~ 220 DEG C, more preferably 160 DEG C ~ 200 DEG C, because the amorphous regions of textile material is lax or expand, thus should accelerate the coating of phosphorus compound (A) to textile material.Not preferably lower than the heating-up temperature of 100 DEG C, because so low temperature cannot obtain phosphorus compound (A) to the abundant infiltration in textile material, thus sometimes give the flame-retardant nature of poor durability.On the other hand, not preferably higher than the heating-up temperature of 220 DEG C, because the excessive deteriorated textile material of heat possibility, thus reduce the toughness of textile material.Dip-dye, injection or coating can be used to be coated on textile material by fire retardant.Heating can by xeothermic or damp and hotly to carry out.This coating and heating means comprise injection and dry cure system, dip-dye and net gas and steam system, dip-dye and decatize system and dip-dye and dry 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 step 2.Repeat identical step or step 1 and step 2 combined to give textile material better flame-retardant nature.In addition, the preparation method of anti-flammability textile material of the present invention can also comprise the correction step that another uses the fire retardant different from fire retardant of the present invention.
In the preparation method of anti-flammability textile material of the present invention, the fiber finishing agent and fiber finishing auxiliary agent that are different from fire retardant of the present invention can be used for carrying out finishing to textile material.Other fiber finishing agent and fiber finishing auxiliary agent comprise, such as, the fire retardant of phosphorus compound (A), dyestuff (basic-dyeable fibre and DISPERSE DYES), carrier (aromatic halide class, N-alkylphthalimide, 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 hydrophilizing agent is different from.The one in described reagent or at least two kinds can be used.
In the preparation method of anti-flammability textile material of the present invention, fire retardant on textile material, namely the amount (amount to obtain (pickup)) of phosphorus compound (A) is not particularly limited, because it changes according to following condition, such as, the variant of textile material and structure and be coated on variant and the amount to obtain of other fiber finishing agent on textile material.Bath of preference is than 1:10 ~ 25, and the flame retardant effect now obtained is best.
Compared with prior art, beneficial effect of the present invention is:
Fire retardant character of the present invention is good, can reach sufficient flame-retardant nature, and the deterioration of textile properties can be made to minimize for textile material with a small amount of fire retardant.Fire retardant of the present invention is coated to textile material can not cause textile material feel, color fastness or the deterioration of color fastness to friction or light.Described fire retardant reaches washing and dry-cleans durable flame-retardant nature, reduces the burden of environment and human body, and has excellent stability.
Detailed description of the invention
Technical scheme of the present invention is further illustrated below by detailed description of the invention.
With following examples and comparative example, specific explanations is carried out to the present invention, although the invention is not restricted in the scope of described embodiment.
Method of testing
(1) median particle diameter (D50) and average volume diameter
The fire retardant prepared by micronize is sampled and uses laser diffraction and scattering particle size analyzer LA-910 (being produced by Horiba Co., Ltd) to analyze, to determine its median particle diameter (D50) and average volume diameter.
(2) product stability
Visual inspection stores the outward appearance of the fire retardant of 1 month at 40 DEG C.The fire retardant not showing precipitation or separation is evaluated as " well ", and the fire retardant of display precipitation or separation is evaluated as " bad ".
(3) flame-retardant nature
In anti-flammability finishing, with fire retardant, finishing is carried out to woven fabric.Test through the fabric of finishing and the flame-retardant nature of two fabric samples according to JISL-1091A-1 (microlamp method (microburnermethod)) and JISL1091D (coil method (coilmethod)), one in described two fabric samples is by the fabric through finishing being washed with water 5 preparations, and another in described two fabric samples is by being prepared for 5 times by the dry cleaning fabric through finishing with following method.
In " microlamp method ", heated web in two ways: heat 1 minute with microlamp, and heated for 3 seconds with microlamp after fabric burning.In both cases, be " well " by such fabric evaluation, namely on the fabric, flame keeps keeping after the heating no longer than 5 seconds no longer than 3 seconds, residual vehement (afterglow) after the heating, and generation is not more than 30cm
2carbonization area, and the flammable fabric evaluation that will exhibit greater than the described limit is " poor ".In " coil method ", the fabric evaluation of preset distance can be burned to for more than 3 times for " well " by with flame contact, and the fabric evaluation of preset distance can be burned to for less than 2 times for " poor " by with flame contact.
Wash in water
According to JISK3371 laundering of textile fabrics, wherein first by fabric containing 1g/ rise alkalescent 1 class (group1) washing agent detergent solution in, with the fabric of 1: 40 and the ratio of detergent solution, wash 15 minutes at 60 ± 2 DEG C, then rinsing 5 minutes 3 times in water at 40 ± 2 DEG C, dewater 2 minutes with centrifugal dehydrator, and dry in hot-air at 60 ± 5 DEG C.The process of washing carries out 5 times altogether.
Dry-cleaning
The electric charge soap (chargesoap) (containing the non-ionic surface active agent of 10: 10: 1 weight ratios, anion surfactant and water) 1 gram being coated with woven fabric 12.6 milliliters of tetrachloroethanes of fire retardant and 0.265g processes 15 minutes at 30 ± 2 DEG C.Process carries out 5 times altogether.
(4) to the color fastness of friction
By adding the polyester woven fabric that the dyeing of fire retardant finishing prepared by fire retardant in dye bath, and test according to JISL0849 friction analyzer II.By grading, result is evaluated, and higher number of degrees represents better to the color fastness of friction.
(5) to the color fastness of light
According to the method defined in JISL0842, make the polyester textile of the dyeing prepared with said method be exposed to carbon arc lamp 100 hours, and evaluated by grading.Higher number of degrees represents the color fastness better to light.
Embodiment 1
Get phosphorus compound 500 parts, 30 parts, POE (20) three (2-phenylethyl) phenyl ether sodium sulphate (polyoxyethylene three (2-phenylethyl) the phenyl ether sodium sulphate containing 20 oxygen ethylene repeating units), 30 parts, POE (25) castor oil ether, the sodium salt of naphthalene sulfonate-formaldehyde condensation product 20 parts, 420 parts, water, place it in agitator, stir 4h fully to disperse, then use a grinding machine ZRS (being produced by AshizawaFinetech Co., Ltd) that obtained slurries are processed into particulate to prepare fire retardant.Determine median particle diameter and the average volume diameter of obtained fire retardant, and the stability of visual inspection fire retardant.
With described fire retardant, finishing is carried out to textile material:
With small-sized dyeing machine (being produced by Texam Co., Ltd), by undyed polyester 100% top-weight fabric in dye bath, with the fabric of 1: 15 and the ratio of bath and 4.5 bath pH, 130 DEG C of process 30 minutes, described dye bath contains each of the fire retardant (with their %owf in table 1) described in the KayalonPolyesterBlackAL167 (a kind of DISPERSE DYES is produced by NipponKayaku Co., Ltd) of 6 fibre weight % and table 1.Then in soaping by fabric containing 1g/ rise soaping agent (being produced by MatsumotoYushi-Seiyaku Co., Ltd), 2g/ rise bisulfites and 2g/ rise caustic soda solution in, the ratio of the fabric with 1: 15 and solution, 80 DEG C of process 20 minutes, rinsing in water, and 170 DEG C of dryings 1 minute, thus be prepared into fire-retardant polyester fabric.
Determine the flame-retardant nature of obtained anti-flammability textile material, to the color fastness of friction and the color fastness to light.
Embodiment 2
The formula of described fire retardant is: get phosphorus compound 500 parts, 30 parts, POE (20) three (2-phenylethyl) phenyl ether sodium sulphate (polyoxyethylene three (2-phenylethyl) the phenyl ether sodium sulphate containing 20 oxygen ethylene repeating units), the sodium salt of naphthalene sulfonate-formaldehyde condensation product 20 parts, POE (20) laurate 30 parts, 420 parts, water.
The preparation method of described fire retardant is identical with embodiment 1.
Described fire retardant is identical with embodiment 1 to the finishing of textile material, and difference is, the bath raio of fabric and fire retardant is 1:10.
Embodiment 3
The formula of described fire retardant is: get phosphorus compound 500 parts, 30 parts, POE (20) three (2-phenylethyl) phenyl ether sodium sulphate (polyoxyethylene three (2-phenylethyl) the phenyl ether sodium sulphate containing 20 oxygen ethylene repeating units), 30 parts, POE (25) rilanit special ether, the sodium salt of naphthalene sulfonate-formaldehyde condensation product 20 parts, 420 parts, water.
The preparation method of described fire retardant is identical with embodiment 1.
Described fire retardant is identical with embodiment 1 to the finishing of textile material, and difference is, the bath raio of fabric and fire retardant is 1:25.
Embodiment 4
The formula of described fire retardant is: get phosphorus compound 500 parts, 30 parts, POE (25) castor oil ether, sodium xylene sulfonate 30 parts, the sodium salt of naphthalene sulfonate-formaldehyde condensation product 30 parts, (2-(2 '-hydroxyl-3 '-the tert-butyl group-5 '-aminomethyl phenyl)-5-chlorobenzotriazole 20 parts, 420 parts, water.
The preparation method of described fire retardant is identical with embodiment 1.
Described fire retardant is identical with embodiment 1 to the finishing of textile material, and difference is, the bath raio of fabric and fire retardant is 1:15.
The structural formula of the phosphorus compound in embodiment 1 ~ 4 is
Wherein, R
1, R
2and R
3be respectively C6 alcyl, aryl and C alcyl.
The performance test results is as shown in table 1.
Table 1
Comparative example 1
Comparative example 1 is the embodiment 1 in CN101631910B.
Comparative example 2
Described comparative example 2 is identical with embodiment 1, and difference is, R in phosphide
1for methyl.
Comparative example 3
Described comparative example 3 is identical with embodiment 1, and difference is, R in phosphide
2for vinyl.
Comparative example 4
Described comparative example 4 is identical with embodiment 1, and difference is, R in phosphide
3for aryl.
Comparative example 5
Described comparative example 5 is identical with embodiment 1, and difference is, bath raio when fire retardant carries out finishing to fabric is 1:9.
Comparative example 6
Described comparative example 6 is identical with embodiment 1, and difference is, bath raio when fire retardant carries out finishing to fabric is 1:26.
Comparative example 7
Described comparative example 7 is identical with embodiment 1, and difference is, described surfactant uses polyoxyalkylene hydrogenated castor oil ethers and polyoxyalkylene fatty acid ethers.
Test as described in Example 1 comparative example 1 ~ 7, test result is as shown in table 2.
Table 2
The textile material that the fire retardant of embodiment 1 ~ 4 result in textile material after anti-flammability finishing, wash the textile material of 5 times and dry-clean 5 times after anti-flammability finishing in water after anti-flammability finishing has highly durable flame-retardant nature; Through the color fastness to friction of the excellence of the textile material of finishing; With the stability of excellence.On the contrary, the fire retardant of comparative example 1 ~ 7 has poor stability and is separated.
Industrial usability
The present invention selects fire retardant containing specific phosphorus compound for textile material, and the burden of described fire retardant to environment and human body is minimum.The textile material being coated with described fire retardant is not easy to deterioration, its feel and color fastness (comprising friction and the fastness to light) thereof by force, and the anti-flammability of described fabric is to washing and dry-clean durable, and has excellent stability.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. a fire retardant, described fire retardant is used for giving textile material flame-retardant nature, and described fire retardant is prepared from primarily of following raw material:
Phosphorus compound, described phosphorus compound has chemical formula (1) as follows, and has the fusing point being not less than 130 DEG C;
Wherein, R
1, R
2and R
3be respectively C6 alcyl, aryl and C5 alcyl;
Described phosphorus compound has the median particle diameter being not more than 1 micron;
Described surfactant is: the composition of a kind of in polyoxyalkylene alkyl aryl ether Sulfates, alkylaryl sulfonates class or alkyl aromatic ether disulfonic acid salt or at least two kinds;
And water.
2. fire retardant according to claim 1, described surfactant is polyoxyalkylene alkyl aryl ether Sulfates surfactant.
3. fire retardant according to claim 1 and 2, described phosphorus compound and the mass percentage of described surfactant in described fire retardant are respectively 20 ~ 70% and 3 ~ 20%, and described phosphorus compound by described surfactant-dispersed in water.
4. the fire retardant according to any one of claim 1-3, described phosphorus compound and the mass percentage of described surfactant in described fire retardant are respectively 30 ~ 60% and 5 ~ 15%.
5. a flame-retardant textile material, containing the fire retardant described in any one of claim 1-4 in described flame-retardant textile material.
6. flame-retardant textile material according to claim 5, at least comprises a kind of fiber with higher crystalline region rate in described flame-retardant textile material.
7. the flame-retardant textile material according to claim 5 or 6, is characterized in that, described flame-retardant textile material also comprises a kind of fiber with higher amorphous regions ratio.
8. a preparation method for the flame-retardant textile material according to any one of claim 5-7, is characterized in that, described method is: with described fire retardant finishing of textile materials.
9. preparation method according to claim 8, is characterized in that, described finishing is: the temperature more than 80 DEG C, is flooded by textile material and carries out for 2 ~ 120 minutes, bath raio 1:30 ~ 50 in the bath containing described fire retardant.
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| CN201510577901.1A CN105064016A (en) | 2015-09-11 | 2015-09-11 | Flame retardant for textile materials, preparation method thereof and prepared flame-retardant textile material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108882760A (en) * | 2016-04-05 | 2018-11-23 | 帝人株式会社 | Cloth and silk, multilayered structure cloth and silk and fibre |
| CN110438577A (en) * | 2019-07-26 | 2019-11-12 | 温多利遮阳材料（德州）股份有限公司 | Polypropylene flame redardant composite material and its product |
| CN115109601A (en) * | 2022-06-30 | 2022-09-27 | 广东电网有限责任公司 | Environment-friendly flame retardant and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101631910A (en) * | 2007-02-28 | 2010-01-20 | 松本油脂制药株式会社 | Flameproofing agent, flame-retardant fiber and method for producing the same |
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2015
- 2015-09-11 CN CN201510577901.1A patent/CN105064016A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101631910A (en) * | 2007-02-28 | 2010-01-20 | 松本油脂制药株式会社 | Flameproofing agent, flame-retardant fiber and method for producing the same |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108882760A (en) * | 2016-04-05 | 2018-11-23 | 帝人株式会社 | Cloth and silk, multilayered structure cloth and silk and fibre |
| CN110438577A (en) * | 2019-07-26 | 2019-11-12 | 温多利遮阳材料（德州）股份有限公司 | Polypropylene flame redardant composite material and its product |
| CN115109601A (en) * | 2022-06-30 | 2022-09-27 | 广东电网有限责任公司 | Environment-friendly flame retardant and preparation method and application thereof |
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Application publication date: 20151118 |