CN101139435A - Polyester having excellent fire-retardancy and preparation method thereof - Google Patents
Polyester having excellent fire-retardancy and preparation method thereof Download PDFInfo
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- CN101139435A CN101139435A CNA2006100414958A CN200610041495A CN101139435A CN 101139435 A CN101139435 A CN 101139435A CN A2006100414958 A CNA2006100414958 A CN A2006100414958A CN 200610041495 A CN200610041495 A CN 200610041495A CN 101139435 A CN101139435 A CN 101139435A
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- Prior art keywords
- polyester
- monomer
- excellent fire
- organophosphorus
- retardancy
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- 229920000728 polyester Polymers 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000178 monomer Substances 0.000 claims abstract description 23
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 71
- -1 polyethylene terephthalate Polymers 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 230000032050 esterification Effects 0.000 claims description 11
- 238000005886 esterification reaction Methods 0.000 claims description 11
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 10
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 10
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 7
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 4
- 229920002215 polytrimethylene terephthalate Polymers 0.000 claims description 4
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 3
- 125000003545 alkoxy group Chemical group 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 229940058344 antitrematodals organophosphorous compound Drugs 0.000 claims description 3
- 150000005840 aryl radicals Chemical class 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 150000002903 organophosphorus compounds Chemical class 0.000 claims description 3
- 150000001282 organosilanes Chemical class 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- 239000003063 flame retardant Substances 0.000 abstract description 24
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 18
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000835 fiber Substances 0.000 abstract description 4
- 229910052710 silicon Inorganic materials 0.000 abstract description 4
- 239000010703 silicon Substances 0.000 abstract description 4
- 238000007334 copolymerization reaction Methods 0.000 abstract description 3
- 239000004744 fabric Substances 0.000 abstract description 3
- 239000004753 textile Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000002759 woven fabric Substances 0.000 abstract description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract 2
- 229920001577 copolymer Polymers 0.000 abstract 1
- 229910052698 phosphorus Inorganic materials 0.000 abstract 1
- 239000011574 phosphorus Substances 0.000 abstract 1
- 229920001296 polysiloxane Polymers 0.000 abstract 1
- 238000009941 weaving Methods 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 14
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 14
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 239000004408 titanium dioxide Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- OLLFKUHHDPMQFR-UHFFFAOYSA-N dihydroxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](O)(O)C1=CC=CC=C1 OLLFKUHHDPMQFR-UHFFFAOYSA-N 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical class OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 229920004935 Trevira® Polymers 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 2
- XQSFXFQDJCDXDT-UHFFFAOYSA-N hydroxysilicon Chemical compound [Si]O XQSFXFQDJCDXDT-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UXFQFBNBSPQBJW-UHFFFAOYSA-N 2-amino-2-methylpropane-1,3-diol Chemical compound OCC(N)(C)CO UXFQFBNBSPQBJW-UHFFFAOYSA-N 0.000 description 1
- ISPYQTSUDJAMAB-UHFFFAOYSA-N 2-chlorophenol Chemical compound OC1=CC=CC=C1Cl ISPYQTSUDJAMAB-UHFFFAOYSA-N 0.000 description 1
- UFMBOFGKHIXOTA-UHFFFAOYSA-N 2-methylterephthalic acid Chemical compound CC1=CC(C(O)=O)=CC=C1C(O)=O UFMBOFGKHIXOTA-UHFFFAOYSA-N 0.000 description 1
- WMRCTEPOPAZMMN-UHFFFAOYSA-N 2-undecylpropanedioic acid Chemical compound CCCCCCCCCCCC(C(O)=O)C(O)=O WMRCTEPOPAZMMN-UHFFFAOYSA-N 0.000 description 1
- HSSYVKMJJLDTKZ-UHFFFAOYSA-N 3-phenylphthalic acid Chemical compound OC(=O)C1=CC=CC(C=2C=CC=CC=2)=C1C(O)=O HSSYVKMJJLDTKZ-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 150000001263 acyl chlorides Chemical class 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 description 1
- 125000005907 alkyl ester group Chemical group 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical class C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- QYQADNCHXSEGJT-UHFFFAOYSA-N cyclohexane-1,1-dicarboxylate;hydron Chemical class OC(=O)C1(C(O)=O)CCCCC1 QYQADNCHXSEGJT-UHFFFAOYSA-N 0.000 description 1
- PDXRQENMIVHKPI-UHFFFAOYSA-N cyclohexane-1,1-diol Chemical class OC1(O)CCCCC1 PDXRQENMIVHKPI-UHFFFAOYSA-N 0.000 description 1
- QSAWQNUELGIYBC-UHFFFAOYSA-N cyclohexane-1,2-dicarboxylic acid Chemical compound OC(=O)C1CCCCC1C(O)=O QSAWQNUELGIYBC-UHFFFAOYSA-N 0.000 description 1
- ZKVIBMMEAFGRNQ-UHFFFAOYSA-N dioctyl benzene-1,2-dicarboxylate terephthalic acid Chemical compound C(C=1C(C(=O)OCCCCCCCC)=CC=CC1)(=O)OCCCCCCCC.C(C1=CC=C(C(=O)O)C=C1)(=O)O ZKVIBMMEAFGRNQ-UHFFFAOYSA-N 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- OJURWUUOVGOHJZ-UHFFFAOYSA-N methyl 2-[(2-acetyloxyphenyl)methyl-[2-[(2-acetyloxyphenyl)methyl-(2-methoxy-2-oxoethyl)amino]ethyl]amino]acetate Chemical compound C=1C=CC=C(OC(C)=O)C=1CN(CC(=O)OC)CCN(CC(=O)OC)CC1=CC=CC=C1OC(C)=O OJURWUUOVGOHJZ-UHFFFAOYSA-N 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- UWJJYHHHVWZFEP-UHFFFAOYSA-N pentane-1,1-diol Chemical compound CCCCC(O)O UWJJYHHHVWZFEP-UHFFFAOYSA-N 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 238000007665 sagging Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 150000003504 terephthalic acids Chemical class 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- FCVNATXRSJMIDT-UHFFFAOYSA-N trihydroxy(phenyl)silane Chemical compound O[Si](O)(O)C1=CC=CC=C1 FCVNATXRSJMIDT-UHFFFAOYSA-N 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
Landscapes
- Artificial Filaments (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The present invention discloses excellent flame-retardant polyester and preparation method of the flame-retardant polyester. The product comprises polyester and the organic silicone copolymer as well as organic phosphorus copolymer contained in the polyester. The preparation process comprises the synthesis of the polyester, etherifying of the synthesized polyester or the polycondensation phase during which organic silicon monomer and organic phosphor monomer are added. The present invention takes use of silicon monomer and organic phosphor monomer for copolymerization with the polyester. The polyester is endowed with excellent flame-retardant performance. The polyester can meet the no-drop requirements during the flame-retardant process. The product by the present invention is no-drop-typed flame-retardant polyester, which can be used to manufacture polyester fiber and correspondent woven fabric or weaving fabric textile or nonwoven cloth and so on.
Description
Technical field:
The present invention relates to a kind of polyester and production method, is a kind of flame retardant polyester and production method.
Background technology:
Polyester product particularly polyethylene terephthalate has become the product of chemical fibre industry output maximum in the world owing to the field that its excellent performance is widely used in making fiber and goods thereof.Along with the mankind to the raising of the requirement of quality of life with to the enhancing of autoprotection consciousness; requirement to polyester product is also more and more higher; the particularly requirement of safety in utilization aspect; as require polyester product to have good flame retardancy; so that under the situation of catching fire; can not bring bigger disaster, so the polyester that the numerous and confused exploitation of each company has flame retardant properties to the mankind.
The flame-retarded technology of each company's use mainly contains post-treatment technology, copolymerization, blending technology etc. at present.The post-treatment technology is mainly carried out coating processing etc. to trevira or polyester textile, but has a unabiding shortcoming of flame retardant effect, and aspects such as the dyeing of product, feel are produced a lot of influences.
Chinese patent 02817032.6 adopts the method for blend to obtain fire-retardant PET, is to use brominated based flame retardant, though reached flame retardant properties, brominated flame-retardant can produce toxic smog in combustion processes, banned use of by many countries gradually.Other companies also adopt non-halogen fire retardant to be used for blend, but blending technology is that the polyester of producing is carried out secondary processing, need extra production to product to increase cost.
Each company also develops the copolymerization flame-retarded technology, gives polyester good combustion-supporting performance from essential structure.It is that comonomer adds the pet reaction system in polycondensation phase that Chinese patent 00804393.0, Chinese patent 02109909.X are to use organophosphorus, thereby obtain the copoly type flame retardant polyester, but this type polyester is the drippage type when fire-retardant, the polyester of drippage causes spot fire easily, so be only limited to the use of low-end product.
Summary of the invention:
The object of the present invention is to provide a kind of flame retardant properties good have polyester of excellent fire-retardancy and preparation method thereof.
Technical solution of the present invention is:
A kind of polyester with excellent fire-retardancy is characterized in that: comprise polyester, contain Organosiliconcopolymere and organophosphorus multipolymer in the polyester.
Contain the Organosiliconcopolymere of 2-20 weight part and the organophosphorus multipolymer of 0.5-12 weight part in the polyester of per 100 weight parts.
Polyester is a kind of or its multipolymer in polyethylene terephthalate, polybutylene terephthalate, the Poly(Trimethylene Terephthalate).Preferred polyethylene terephthalate.
Wherein the monomer of Organosiliconcopolymere is organosilicon glycol or triol, has following structural formula:
Wherein n is 1～20 integer, R
1, R
2Be hydrogen atom, hydroxyl, aryl radical, saturated alkyl or alkoxyl group.
Wherein the monomer of organophosphorus multipolymer is to have one of the compound of following structural formula or the derivative after these compound esterifications:
Contain the Organosiliconcopolymere of 3-15 weight part and the organophosphorus multipolymer of 0.8-10 weight part in the polyester of per 100 weight parts.The organosilicon addition is less than 2%, can not play the effect of fine fire-retardant and anti-drippage, and addition then can influence the performances such as intensity of the synthetic reaction process and the polyester of polyester greater than 20%.The organophosphorus addition is less than 0.5%, then influences the flame retardant properties of product, and addition then influences the production performance and the mechanical property of product greater than 11%.
A kind of preparation method with polyester of excellent fire-retardancy comprises the synthetic of polyester, it is characterized in that: esterification or polycondensation phase at synthesizing polyester add organosilane monomer and organophosphorus monomer, make after the reaction.
A kind of preparation method with polyester of excellent fire-retardancy is characterized in that: the organophosphorus monomer is at first made the ethylene glycol solution that concentration is the organo phosphorous compounds of 40-70% with glycol reaction, adds the pet reaction system in Esterification Stage or polycondensation phase then.
The present invention adopts silicon-containing monomer and phosphorous-containing monomers and polyethylene terephthalate copolymer, gives the polyester excellent flame-retardant, and reaches the requirement of not having drippage in fire-retardant process.
The polyester that the present invention uses is polyethylene terephthalate, polybutylene terephthalate, Poly(Trimethylene Terephthalate) a kind of or its multipolymer wherein.Remove basic synthesis material, terephthalic acid, dimethyl terephthalate (DMT), ethylene glycol, 1, ammediol, 1, outside the 4-butyleneglycol, interpolymer can be selected following diacid for use: m-phthalic acid, phthalic acid, the methyl terephthalic acid, the naphthalene diacid, the aryl dicarboxylic acid's class and the hexanodioic acid of aromatic carboxylic acids such as biphenyl dicarboxylic acid and ester derivative thereof, pimelic acid, suberic acid, nonane diacid, aliphatic carboxylic acid and ester derivative and cyclohexane dicarboxylic acids such as dodecanedicarboxylic acid, the hexahydro-m-phthalic acid, alicyclic dicarboxylic acid and ester derivatives thereof such as hexahydro-phthalic acid.Be meant materials such as lower alkyl esters, acid anhydrides, acyl chlorides such as dimethyl ester in the described derivative.These dicarboxylic acid can two or more alone or in combination uses, the glycol that polyethylene terephthalate copolymer uses can be aklylene glycol class component and cyclohexanediols, 1 such as a chain such as pentanediol, 1,6-hexylene glycol or a catenate aklylene glycol, alicyclic diols such as 4-cyclohexanedimethanol, Hydrogenated Bisphenol A; And the polyoxyalkylene diols class of glycol ether, triglycol, polyoxyethylene glycol, polypropylene glycol, polytetramethylene glycol etc.
Polyester use is known altogether in synthetic method and catalyzer, compounds such as catalyst system therefor such as cobalt, magnesium, sodium, lithium, antimony, titanium, method such as polymerization of still formula or successive polymerization etc. that the present invention is used.
Under the prerequisite that does not influence flame retardant properties of the present invention, can also in polyester, add functional aids such as antioxidant, white dyes, static inhibitor.
The present invention adopts silicon-containing monomer and phosphorous-containing monomers and polyethylene terephthalate copolymer, gives the polyester excellent flame-retardant, and reaches the requirement of not having drippage in fire-retardant process.Product of the present invention is a kind of no drippage type flame retardant polyester, can be used for making trevira and relevant woven fabrics or goods such as knitted fabrics textiles or non-woven fabrics.
The invention will be further described below in conjunction with embodiment:
Embodiment:
Embodiment and evaluation method thereof:
Embodiment 1:
1.5 the Diphenylsilanediol of part, 12.32 the terephthalic acid of part, 5.63 the ethylene glycol of part joins in the serial reaction device that has vaporizer and vacuum unit, be heated to about 250 degree and carry out esterification, esterification proceeds to 90% when above, in reaction system, add concentration and be 0.98 part of the ethylene glycol solution of 60%PHP, 0.006 part of The catalytic antimony trioxide, 0.053 the titanium dioxide of part, progressively reduce pressure below 200 pascals, carry out polycondensation under the temperature 290 degree conditions, reacted about three hours, and finished reaction, make fire-retardant slice, and carry out conventional melt-spinning, or carry out next step processing and make fiber.
Embodiment 2:
The addition of raw material is as follows: 2.25 parts hydroxy silicon oil (hydroxy radical content 8%), 12.75 parts terephthalic acid, 5.83 parts ethylene glycol, 0.053 part 0.006 part of titanium dioxide, The catalytic antimony trioxide, concentration are 3 parts of the ethylene glycol solutions of 70% DDP.All the other are with embodiment 1.
Embodiment 3:
Device is with embodiment 1, and the addition of raw material is as follows: 1.5 parts Diphenylsilanediol, 15 parts dimethyl terephthalate (DMT), 9.79 parts ethylene glycol, 0.004 part of Cobaltous diacetate are as transesterification catalyst, 0.053 part 1 part of the ethylene glycol solution of BCPPO of 0.006 part 65% of titanium dioxide, The catalytic antimony trioxide.
Embodiment 4:
Device is with embodiment 1, and the addition of raw material is as follows: 0.75 part phenyl silanetriol oligopolymer (about molecular weight 600), 15.07 parts of terephthalic acids, 9.84 parts of ethylene glycol, 0.053 part 3 parts of the ethylene glycol solutions of 0.006 part of titanium dioxide, The catalytic antimony trioxide, 60%DDP.
Embodiment 5:
Device is with embodiment 1, and the addition of raw material is as follows: 0.75 part Diphenylsilanediol, 0.75 part hydroxy silicon oil (hydroxy radical content 8%), 14.68 parts terephthalic acid dioctyl phthalate, 9.6 parts of ethylene glycol, 0.053 part the ethylene glycol solution of 60%CMP of 0.006 part, 0.6 part of titanium dioxide, The catalytic antimony trioxide.
Embodiment 6:
A kind of preparation method with polyester of excellent fire-retardancy comprises the synthetic of polyester, it is characterized in that: esterification or polycondensation phase at synthesizing polyester add organosilane monomer and organophosphorus monomer, make after the reaction.Wherein the organophosphorus monomer is at first made the ethylene glycol solution that concentration is the organo phosphorous compounds of 40-70% (example 40%, 50%, 60%, 70%) with glycol reaction, adds the pet reaction system in Esterification Stage or polycondensation phase then.
Described polyester is a kind of or its multipolymer in polyethylene terephthalate, polybutylene terephthalate, the Poly(Trimethylene Terephthalate).The addition of raw material satisfies in product, contains the Organosiliconcopolymere of 2-20 weight part (example 2,3,10,15,20 weight parts) and the organophosphorus multipolymer of 0.5-11 weight part (example 0.5,0.8,5,10) in the polyester of per 100 weight parts.
Wherein the monomer of Organosiliconcopolymere is organosilicon glycol or triol, has following structural formula:
Wherein n is 1～20 integer (example 1,5,10,15,20), R
1, R
2Be hydrogen atom, hydroxyl, aryl radical, saturated alkyl or alkoxyl group.
Wherein the monomer of organophosphorus multipolymer is to have one of the compound of following structural formula or the derivative after these compound esterifications:
Comparative example 1:
Device is with embodiment 1, and the addition of raw material is as follows: 1.5 parts Diphenylsilanediol, 12.32 parts terephthalic acid, 5.63 parts ethylene glycol, 0.053 part 0.006 part of titanium dioxide, The catalytic antimony trioxide.
Comparative example 2;
Device is with embodiment 1, and raw material is composed as follows: 13 parts terephthalic acid, 5.57 parts ethylene glycol, 0.053 part the ethylene glycol solution of 60% PHP of 0.006 part, 1.5 parts of titanium dioxide, The catalytic antimony trioxide.
The result of embodiment and comparative example is as shown in the table:
| IV | L | b | Incendivity | Anti-drippage | Intensity | |
| Embodiment 1 | 0.655 | 74 | 5 | ○ | ◎ | 3.6 |
| Embodiment 2 | 0.640 | 70 | 4 | ○ | ○ | 3.5 |
| Embodiment 3 | 0.660 | 73 | 5 | ◎ | ○ | 3.8 |
| Embodiment 4 | 0.658 | 69 | 3 | ◎ | ◎ | 3.6 |
| Embodiment 5 | 0.650 | 76 | 4 | ◎ | ◎ | 3.6 |
| Comparative example 1 | 0.660 | 77 | 3 | △ | ○ | 3.9 |
| Comparative example 2 | 0.653 | 75 | 7 | ○ | △ | 3.7 |
Limiting viscosity (IV) (dL/g)
With the ortho chloro phenol is solvent, measures under 25 ℃.
Tone L, b value
Measure by GB GB/T 14190-1993.
Flame retardancy
The long filament of 50dtex is cut into a section of 150mm, gets the 0.7g bundle together, a head-clamp is lived sagging being fixed on the iron stand of nature.The long filament that is fixed into useful length 120mm is estimated with the high flame ignition of 20mm 3 seconds.
Incendivity
◎: the residual flame time is 0 second (missing of ignition)
Zero: less than 3 seconds.
△：3～10。
*: more than 10 seconds.
Anti-drippage
◎: dripping back number is 0.
Below zero: 5.
△：6～10。
*: more than 11.
Claims (8)
1. the polyester with excellent fire-retardancy is characterized in that: comprise polyester, contain Organosiliconcopolymere and organophosphorus multipolymer in the polyester.
2. the polyester with excellent fire-retardancy according to claim 1 is characterized in that: contain the Organosiliconcopolymere of 2-20 weight part and the organophosphorus multipolymer of 0.5-12 weight part in the polyester of per 100 weight parts.
3. the polyester with excellent fire-retardancy according to claim 1 and 2 is characterized in that: polyester is a kind of or its multipolymer in polyethylene terephthalate, polybutylene terephthalate, the Poly(Trimethylene Terephthalate).
4. the polyester with excellent fire-retardancy according to claim 1 and 2 is characterized in that: wherein the monomer of Organosiliconcopolymere is organosilicon glycol or triol, has following structural formula:
Wherein n is 1～20 integer, R
1, R
2Be hydrogen atom, hydroxyl, aryl radical, saturated alkyl or alkoxyl group.
5. the polyester with excellent fire-retardancy according to claim 1 and 2 is characterized in that: wherein the monomer of organophosphorus multipolymer is to have one of the compound of following structural formula or the derivative after these compound esterifications:
6. the polyester with excellent fire-retardancy according to claim 2 is characterized in that: contain the Organosiliconcopolymere of 3-15 weight part and the organophosphorus multipolymer of 0.8-10 weight part in the polyester of per 100 weight parts.
7. the preparation method with polyester of excellent fire-retardancy comprises the synthetic of polyester, it is characterized in that: esterification or polycondensation phase at synthesizing polyester add organosilane monomer and organophosphorus monomer, make after the reaction.
8. the preparation method with polyester of excellent fire-retardancy according to claim 7, it is characterized in that: the organophosphorus monomer is at first made the ethylene glycol solution that concentration is the organo phosphorous compounds of 40-70% with glycol reaction, adds the pet reaction system in Esterification Stage or polycondensation phase then.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100414958A CN101139435A (en) | 2006-09-08 | 2006-09-08 | Polyester having excellent fire-retardancy and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100414958A CN101139435A (en) | 2006-09-08 | 2006-09-08 | Polyester having excellent fire-retardancy and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101139435A true CN101139435A (en) | 2008-03-12 |
Family
ID=39191553
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006100414958A Pending CN101139435A (en) | 2006-09-08 | 2006-09-08 | Polyester having excellent fire-retardancy and preparation method thereof |
Country Status (1)
| Country | Link |
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| CN (1) | CN101139435A (en) |
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