CN117430780A - 阻燃硬质聚氨酯泡沫及其制备方法 - Google Patents
阻燃硬质聚氨酯泡沫及其制备方法 Download PDFInfo
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- CN117430780A CN117430780A CN202311756565.8A CN202311756565A CN117430780A CN 117430780 A CN117430780 A CN 117430780A CN 202311756565 A CN202311756565 A CN 202311756565A CN 117430780 A CN117430780 A CN 117430780A
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- polyurethane foam
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- 229920005830 Polyurethane Foam Polymers 0.000 title claims abstract description 80
- 239000011496 polyurethane foam Substances 0.000 title claims abstract description 80
- 239000003063 flame retardant Substances 0.000 title claims abstract description 69
- 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 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title abstract description 20
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- 150000003077 polyols Chemical class 0.000 claims abstract description 21
- 239000012948 isocyanate Substances 0.000 claims abstract description 18
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 18
- 239000001506 calcium phosphate Substances 0.000 claims abstract description 17
- 229910000389 calcium phosphate Inorganic materials 0.000 claims abstract description 17
- 235000011010 calcium phosphates Nutrition 0.000 claims abstract description 17
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 17
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical group [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims abstract description 17
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical group O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000009736 wetting Methods 0.000 claims abstract description 16
- 239000002270 dispersing agent Substances 0.000 claims abstract description 15
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 13
- 239000010452 phosphate Substances 0.000 claims abstract description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 13
- 239000003381 stabilizer Substances 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 239000004088 foaming agent Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000005187 foaming Methods 0.000 claims description 27
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 22
- 238000001746 injection moulding Methods 0.000 claims description 12
- FRCHKSNAZZFGCA-UHFFFAOYSA-N 1,1-dichloro-1-fluoroethane Chemical compound CC(F)(Cl)Cl FRCHKSNAZZFGCA-UHFFFAOYSA-N 0.000 claims description 11
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 11
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 11
- VONWDASPFIQPDY-UHFFFAOYSA-N dimethyl methylphosphonate Chemical compound COP(C)(=O)OC VONWDASPFIQPDY-UHFFFAOYSA-N 0.000 claims description 10
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims description 6
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
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- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 claims description 3
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 3
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 claims description 3
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 claims description 3
- MSSNHSVIGIHOJA-UHFFFAOYSA-N pentafluoropropane Chemical compound FC(F)CC(F)(F)F MSSNHSVIGIHOJA-UHFFFAOYSA-N 0.000 claims description 3
- UKODFQOELJFMII-UHFFFAOYSA-N pentamethyldiethylenetriamine Chemical compound CN(C)CCN(C)CCN(C)C UKODFQOELJFMII-UHFFFAOYSA-N 0.000 claims description 3
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 3
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 3
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 3
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 3
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- 229920000538 Poly[(phenyl isocyanate)-co-formaldehyde] Polymers 0.000 claims description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- YYQRGCZGSFRBAM-UHFFFAOYSA-N Triclofos Chemical compound OP(O)(=O)OCC(Cl)(Cl)Cl YYQRGCZGSFRBAM-UHFFFAOYSA-N 0.000 claims description 2
- 239000007858 starting material Substances 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
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- OXFUXNFMHFCELM-UHFFFAOYSA-N tripropan-2-yl phosphate Chemical compound CC(C)OP(=O)(OC(C)C)OC(C)C OXFUXNFMHFCELM-UHFFFAOYSA-N 0.000 claims description 2
- 239000004604 Blowing Agent Substances 0.000 claims 1
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- 150000002367 halogens Chemical class 0.000 abstract 1
- 229910052698 phosphorus Inorganic materials 0.000 abstract 1
- 239000011574 phosphorus Substances 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 17
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 12
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- 238000002485 combustion reaction Methods 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 230000000704 physical effect Effects 0.000 description 4
- 239000002341 toxic gas Substances 0.000 description 4
- 239000000080 wetting agent Substances 0.000 description 4
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- 239000000126 substance Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910052918 calcium silicate Inorganic materials 0.000 description 2
- 239000000378 calcium silicate Substances 0.000 description 2
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 2
- 239000013065 commercial product Substances 0.000 description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
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- 239000002245 particle Substances 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UPYPTOCXMIWHSG-UHFFFAOYSA-N 1-dodecylsulfanyldodecane Chemical compound CCCCCCCCCCCCSCCCCCCCCCCCC UPYPTOCXMIWHSG-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- SVYKKECYCPFKGB-UHFFFAOYSA-N N,N-dimethylcyclohexylamine Chemical compound CN(C)C1CCCCC1 SVYKKECYCPFKGB-UHFFFAOYSA-N 0.000 description 1
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- 239000000919 ceramic Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 description 1
- ASMQGLCHMVWBQR-UHFFFAOYSA-M diphenyl phosphate Chemical compound C=1C=CC=CC=1OP(=O)([O-])OC1=CC=CC=C1 ASMQGLCHMVWBQR-UHFFFAOYSA-M 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
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- 238000004062 sedimentation Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
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- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6681—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6685—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3225—Polyamines
- C08G18/3228—Polyamines acyclic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/143—Halogen containing compounds
- C08J9/144—Halogen containing compounds containing carbon, halogen and hydrogen only
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
本发明属于阻燃聚氨酯泡沫技术领域,具体涉及阻燃硬质聚氨酯泡沫及其制备方法。所述阻燃硬质聚氨酯泡沫由黑料和白料制得,所述白料包括以下原料:聚醚多元醇、磷酸酯类阻燃剂、无机粉末填料、泡沫稳定剂、发泡剂、催化剂、润湿分散剂、所述黑料为异氰酸酯;所述无机粉末填料由阻燃无机粉末和促进剂组成;所述阻燃无机粉末为磷酸钙、碳化硅,所述促进剂为氧化铝。无机粉末填料在高温下反应生成阻燃膜,并与磷酸酯类阻燃剂起到促进作用,较于传统的含磷含卤阻燃,更好的提高了聚氨酯泡沫的阻燃性、力学性能和环保性能,并且制备方法简单,生产成本低,较好的解决了现有技术中的短板,可用于硬质聚氨酯泡沫阻燃的工业应用中。
Description
技术领域
本发明属于阻燃聚氨酯泡沫技术领域,具体涉及阻燃硬质聚氨酯泡沫及其制备方法。
背景技术
聚氨酯泡沫是一种极易燃烧的材料、并且在燃烧的过程中会发生滴落现象,并且释放大量的热和一氧化碳、氰化氢等有毒气体,这些有毒气体对人体健康和环境都有明显的危害,在实际应用中存在极大的安全隐患。特别是在房屋建筑和汽车内饰等多个领域对聚氨酯泡沫的阻燃性和力学性能提出了一定的要求,这就需要提供一种高阻燃、物理性能优异环保的聚氨酯材料用于这些领域,有效的阻燃性能够降低聚氨酯泡沫燃烧释放的有毒气体。因此市场亟需一种新的阻燃剂,既能提高聚氨酯泡沫的阻燃性又可以提高其固有的机械属性。
专利CN116515070A公开了一种硬质阻燃聚氨酯泡沫及其制备方法,所述硬质阻燃聚氨酯泡沫包括白料和黑料;白料包括以下质量份数的组分:50份~55份的聚醚多元醇、8份~10份的磷酸酯类阻燃剂、48份~50份的膨胀型阻燃剂、2份~5份的无机陶瓷填料、0.8份~1份的发泡剂、0.5份~0.9份的泡沫稳定剂和0.1份~0.2份的催化剂;黑料包括异氰酸酯。此专利阻燃剂的添加为简单的物理混合,难以快速、均匀、稳定的分散在体系中,且使用的阻燃剂膨胀石墨和氧化铝、氮化铝或六方氮化硼在体系中只是单一的起着各自的阻燃效果,并无法产生“一加一大于二”的协同效果,且其实施例使用全水发泡体系,发泡剂水用量极少,制得的成品密度较高的前提下,机械属性和阻燃性能依然没有较好的改善。
传统添加阻燃剂的方法不仅阻燃效果不佳,还会影响聚氨酯泡沫的力学性能和热稳定性,同时燃烧时释放有害剧毒气体对人员和环境的危害较大。
发明内容
针对现有技术的不足,本发明的目的是提供一种阻燃硬质聚氨酯泡沫,有效提高聚氨酯泡沫的阻燃性、自熄性、力学性能及热稳定性。
本发明还提供其制备方法,简单易行,适合大规模生产。
本发明所述的阻燃硬质聚氨酯泡沫,由质量比为1:(1-1.6)的白料和黑料制得,所述白料包括以下质量份数的原料:
聚醚多元醇50-100份;
磷酸酯类阻燃剂5-20份;
无机粉末填料45-55份;
泡沫稳定剂1-5份;
发泡剂10-25份;
催化剂0.8-1.5份;
润湿分散剂0.45-0.55份;
所述黑料为异氰酸酯;
其中:
所述无机粉末填料由质量比为(90-99):(1-10)的阻燃无机粉末和促进剂组成。
所述阻燃无机粉末为磷酸钙、碳化硅,所述促进剂为氧化铝,所述磷酸钙、碳化硅、氧化铝的质量比为(70-75):(20-24):(1-10),所述无机粉末填料的粒度为10-15微米;将上述原料混合均匀后,即得无机粉末填料。
所述磷酸酯类阻燃剂为甲基磷酸二甲酯、磷酸三氯乙酯、磷酸三乙酯、磷酸三甲苯酯、磷酸三苯酯、磷酸三异丙苯酯、磷酸三丁酯、磷酸三辛酯、甲苯基二苯基磷酸酯中的一种或多种。
所述发泡剂为正戊烷、HCFC-141b、HFC-245fa和环戊烷中的一种。
所述泡沫稳定剂为有机硅泡沫稳定剂。
所述催化剂为辛酸亚锡、二月桂酸二丁基锡、二(十二烷基硫)二丁基锡、二醋酸二丁基锡、三乙烯二胺、五甲基二亚乙基三胺、N,N-二甲基环己胺和N,N-二甲基苄胺中的两种。
所述聚醚多元醇为以蔗糖起始剂体系的硬泡聚醚多元醇。
所述异氰酸酯为多亚甲基多苯基异氰酸酯。
本发明所述的阻燃硬质聚氨酯泡沫的制备方法,将白料的原料搅拌混匀,得到白料,再将黑料加入到白料中搅拌混匀,得混合液注模并进行发泡,得到发泡成型的泡沫;等泡沫熟化后进行脱模,得到阻燃硬质聚氨酯泡沫。
聚氨酯泡沫制备的过程中要经过发泡、熟化和脱模。在白料和黑料混合的过程中会放出大量的热,白料中无机粉末填料在反应热的相互作用下发生自反应,生成物会提高聚氨酯泡沫的阻燃性和物理性能。
与现有技术相比,本发明有益效果如下:
(1)本发明通过选用无机粉末填料和磷酸酯类阻燃剂的促进作用,使得到的聚氨酯泡沫阻燃性明显提高。
(2)润湿分散剂联合碳化硅、磷酸钙、氧化铝协同起到两个作用:
a.润湿分散剂能够降低体系的黏度使填料快速且均匀的分散在体系中,润湿分散剂帮助无机粉末填料润湿与稳定,避免了物料长时间搁置产生沉淀。
b.润湿分散剂不仅可以降低液体的表面张力,还能降低液体与填料间的界面张力,将无机粉末填料吸附的空气完全置换掉,粒子从而被液体介质完全的包围。
c.润湿分散剂分子带有的基团或者链段,可以通过离子键,偶极作用或者氢键,与填料表面产生很强的作用力,润湿分散剂牢牢地吸附在填料表面,所以稳定了良好的填料分布。
润湿分散剂的加入能够加快填料的润湿速度同时降低黏度、快速分散从而降低填料沉降,可添加更多的无机粉末填料,由于促进剂的加入使阻燃无机粉末可以利用发泡过程中的自反应热,在较低的温度下进行化学反应分解,分解后的产物硅酸钙和碳单质形成较厚的多孔碳层覆盖在聚氨酯泡沫表面,磷酸酯类阻燃剂在受热后黏度变大,覆盖在多孔碳层表面,降低有毒气体的挥发,以此来达到其阻燃的目的,本发明专利选用的无机粉末填料和磷酸酯类阻燃剂在较低的温度下分解的产物不含有有害物质,减少对环境的危害。
(3)无机粉末填料在低温下分解后的产物可以镶嵌在聚氨酯泡沫空隙中,提高了多孔碳层的密度,达到较好的隔热保温性能和隔绝空气的作用,因此其阻燃性能进一步提升。其次无机粉末填料在较低的温度下自反应生成的各种小颗粒分散在聚氨酯泡沫中,无机粉末填料自反应生成的硅酸钙和碳单质具有很高的耐火限度,从而使得聚氨酯泡沫的阻燃性能进一步提高,同时使得聚氨酯泡沫的强度和刚性提高,提高结构的整体稳定性。
(4)本发明在提高了阻燃效果的同时还使聚氨酯泡沫着火自熄,保证了聚氨酯泡沫的物理性能、热稳定性和环保性能,并且制备方法简单,具有实用性和经济效益。
(5)本发明做到了不用大幅提高聚氨酯泡沫材料密度的前提下,使得其机械性能和阻燃性能达到一个较高的水平。
具体实施方式
以下结合实施例对本发明作进一步说明。
实施例中用到的所有原料除特殊说明外,均为市购。
润湿分散剂BYK-W968为德国毕克公司的市售产品;
聚醚多元醇R4110为宏顺化工科技有限公司的市售产品;
泡沫稳定剂AK8805为山东同蓝化工公司的市售产品;
PM200为万华化学集团股份有限公司的市售产品。
实施例1
所述的阻燃硬质聚氨酯泡沫包括100g的聚醚多元醇R4110(羟值:440mgKOH/g,粘度:3800mPa·s)、1g的二月桂酸二丁基锡、0.5g的三乙烯二胺、2g的AK8805、5g的甲基磷酸二甲酯、45g的无机粉末填料(10微米)、15g的HCFC-141b、0.45g的BYK-W968,以上混合均匀为白料,黑料为异氰酸酯PM200。
所述无机粉末填料为质量比为75:24:1的磷酸钙、碳化硅、氧化铝的混合物。
所述的聚氨酯泡沫的制备方法如下:
黑料和白料各取100g,黑料加入到所述白料中,进行二次搅拌,得到混合液;然后将混合液注模并进行发泡,得到发泡成型的泡沫;等泡沫熟化后进行脱模,得到所述聚氨酯泡沫。
实施例2
实施例2与实施例1相比,区别仅在于:无机粉末填料和润湿分散剂的含量不同,具体如下:
所述的阻燃硬质聚氨酯泡沫包括100g的聚醚多元醇R4110(羟值:440mgKOH/g,粘度:3800mPa·s)、1g的二月桂酸二丁基锡、0.5g的三乙烯二胺、2g的AK8805、5g的甲基磷酸二甲酯、50g的无机粉末填料(10微米)、15g的HCFC-141b、0.5g的BYK-W968,以上混合均匀为白料,黑料为异氰酸酯PM200。
所述无机粉末填料为质量比为75:24:1的磷酸钙、碳化硅、氧化铝的混合物。
实施例3
实施例3与实施例1相比,区别仅在于:无机粉末填料和润湿分散剂的含量不同,具体如下:
所述的阻燃硬质聚氨酯泡沫包括100g的聚醚多元醇R4110(羟值:440mgKOH/g,粘度:3800mPa·s)、1g的二月桂酸二丁基锡、0.5g的三乙烯二胺、2g的AK8805、5g的甲基磷酸二甲酯、55g的无机粉末填料(10微米)、15g的HCFC-141b、0.55g的BYK-W968,以上混合均匀为白料,黑料为异氰酸酯PM200。
所述无机粉末填料为质量比为75:24:1的磷酸钙、碳化硅、氧化铝的混合物。
实施例4
所述的阻燃硬质聚氨酯泡沫包括50g的聚醚多元醇R4110(羟值:440mgKOH/g,粘度:3800mPa·s)、1.2g的N,N-二甲基苄胺、0.3g的五甲基二亚乙基三胺、5g的AK8805、15g的磷酸三丁酯、5g的磷酸三辛酯、45g的无机粉末填料(10微米)、10g的HFC-245fa、0.45g的BYK-W968,以上混合均匀为白料,黑料为异氰酸酯PM200。
所述无机粉末填料为质量比为70:20:10的磷酸钙、碳化硅、氧化铝的混合物。
所述的聚氨酯泡沫的制备方法如下:
黑料和白料各取100g,黑料加入到所述白料中,进行二次搅拌,得到混合液;然后将混合液注模并进行发泡,得到发泡成型的泡沫;等泡沫熟化后进行脱模,得到所述聚氨酯泡沫。
实施例5
所述的阻燃硬质聚氨酯泡沫包括80g的聚醚多元醇R4110(羟值:440mgKOH/g,粘度:3800mPa·s)、0.8g的二醋酸二丁基锡、0.5g的N,N-二甲基环己胺、3g的AK8805、1g的磷酸三苯酯、2g磷酸三甲苯酯、5g磷酸三乙酯、50g的无机粉末填料(12微米)、18g的正戊烷、0.5g的BYK-W968,以上混合均匀为白料,黑料为异氰酸酯PM200。
所述无机粉末填料为质量比为73:22:5的磷酸钙、碳化硅、氧化铝的混合物。
所述的聚氨酯泡沫的制备方法如下:
黑料取110g,白料取100g,黑料加入到所述白料中,进行二次搅拌,得到混合液;然后将混合液注模并进行发泡,得到发泡成型的泡沫;等泡沫熟化后进行脱模,得到所述聚氨酯泡沫。
实施例6
所述的阻燃硬质聚氨酯泡沫包括100g的聚醚多元醇R4110(羟值:440mgKOH/g,粘度:3800mPa·s)、0.3g的二(十二烷基硫)二丁基锡、0.5g的辛酸亚锡、1g的AK8805、2g的磷酸三辛酯、2g甲苯基二苯基磷酸酯、1g磷酸三异丙苯酯、55g的无机粉末填料(15微米)、25g的环戊烷、0.55g的BYK-W968,以上混合均匀为白料,黑料为异氰酸酯PM200。
所述无机粉末填料为质量比为75:24:1的磷酸钙、碳化硅、氧化铝的混合物。
所述的聚氨酯泡沫的制备方法如下:
黑料取160g,白料取100g,黑料加入到所述白料中,进行二次搅拌,得到混合液;然后将混合液注模并进行发泡,得到发泡成型的泡沫;等泡沫熟化后进行脱模,得到所述聚氨酯泡沫。
对比例1
对比例1与实施例2相比,区别仅在于:不添加无机粉末填料和润湿分散剂,具体如下:
所述的阻燃硬质聚氨酯泡沫包括100g的聚醚多元醇R4110(羟值:440mgKOH/g,粘度:3800mPa·s)、1g的二月桂酸二丁基锡、0.5g的三乙烯二胺、2g的AK8805、5g的甲基磷酸二甲酯、15g的HCFC-141b,以上混合均匀为白料,黑料为异氰酸酯PM200。
所述的聚氨酯泡沫的制备方法如下:
黑料和白料各取100g,黑料加入到所述白料中,进行二次搅拌,得到混合液;然后将混合液注模并进行发泡,得到发泡成型的泡沫;等泡沫熟化后进行脱模,得到所述聚氨酯泡沫。
对比例2
对比例2与实施例2相比,区别仅在于:无机粉末填料中不加促进剂氧化铝,具体如下:
所述的阻燃硬质聚氨酯泡沫包括100g的聚醚多元醇R4110(羟值:440mgKOH/g,粘度:3800mPa·s)、1g的二月桂酸二丁基锡、0.5g的三乙烯二胺、2g的AK8805、5g的甲基磷酸二甲酯、50g的无机粉末填料(10微米)、15g的HCFC-141b、0.5g的BYK-W968,以上混合均匀为白料,黑料为异氰酸酯PM200。
所述的聚氨酯泡沫的制备方法如下:
黑料和白料各取100g,黑料加入到所述白料中,进行二次搅拌,得到混合液;然后将混合液注模并进行发泡,得到发泡成型的泡沫;等泡沫熟化后进行脱模,得到所述聚氨酯泡沫。
对比例3
对比例3与实施例2相比,区别仅在于:无机粉末填料中不加磷酸钙,具体如下:
所述的阻燃硬质聚氨酯泡沫包括100g的聚醚多元醇R4110(羟值:440mgKOH/g,粘度:3800mPa·s)、1g的二月桂酸二丁基锡、0.5g的三乙烯二胺、2g的AK8805、5g的甲基磷酸二甲酯、50g的无机粉末填料(10微米)、15g的HCFC-141b、0.5g的BYK-W968,以上混合均匀为白料,黑料为异氰酸酯PM200。
所述的聚氨酯泡沫的制备方法如下:
黑料和白料各取100g,黑料加入到所述白料中,进行二次搅拌,得到混合液;然后将混合液注模并进行发泡,得到发泡成型的泡沫;等泡沫熟化后进行脱模,得到所述聚氨酯泡沫。
对比例4
对比例4与实施例2相比,区别仅在于:无机粉末填料中不加碳化硅,具体如下:
所述的阻燃硬质聚氨酯泡沫包括100g的聚醚多元醇R4110(羟值:440mgKOH/g,粘度:3800mPa·s)、1g的二月桂酸二丁基锡、0.5g的三乙烯二胺、2g的AK8805、5g的甲基磷酸二甲酯、50g的无机粉末填料(10微米)、15g的HCFC-141b、0.5g的BYK-W968,以上混合均匀为白料,黑料为异氰酸酯PM200。
所述的聚氨酯泡沫的制备方法如下:
黑料和白料各取100g,黑料加入到所述白料中,进行二次搅拌,得到混合液;然后将混合液注模并进行发泡,得到发泡成型的泡沫;等泡沫熟化后进行脱模,得到所述聚氨酯泡沫。
对比例5
对比例5与实施例2相比,区别仅在于:体系中不加润湿分散剂,具体如下:
所述的阻燃硬质聚氨酯泡沫包括100g的聚醚多元醇R4110(羟值:440mgKOH/g,粘度:3800mPa·s)、1g的二月桂酸二丁基锡、0.5g的三乙烯二胺、2g的AK8805、5g的甲基磷酸二甲酯、50g的无机粉末填料(10微米)、15g的HCFC-141b,以上混合均匀为白料,黑料为异氰酸酯PM200。
所述的聚氨酯泡沫的制备方法如下:
黑料和白料各取100g,黑料加入到所述白料中,进行二次搅拌,得到混合液;然后将混合液注模并进行发泡,得到发泡成型的泡沫;等泡沫熟化后进行脱模,得到所述聚氨酯泡沫。
对比例6
无机粉末填料超出设定值范围,具体如下:
所述的阻燃硬质聚氨酯泡沫包括100g的聚醚多元醇R4110(羟值:440mgKOH/g,粘度:3800mPa·s)、1g的二月桂酸二丁基锡、0.5g的三乙烯二胺、2g的AK8805、5g的甲基磷酸二甲酯、65g的无机粉末填料(10微米)、15g的HCFC-141b、0.5g的BYK-W968,以上混合均匀为白料,黑料为异氰酸酯PM200。
所述的聚氨酯泡沫的制备方法如下:
黑料和白料各取100g,黑料加入到所述白料中,进行二次搅拌,得到混合液;然后将混合液注模并进行发泡,得到发泡成型的泡沫;等泡沫熟化后进行脱模,得到所述聚氨酯泡沫。
分别对实施例1-实施例6、对比例1-对比例6所制备的聚氨酯泡沫进行压缩强度测试、极限氧指数测试和着火自熄测试,相关性能测试结果见表1。
力学性能测试:将实施例1-实施例6、对比例1-对比例6已经熟化好的聚氨酯泡沫进行切块,切割成50mm×50mm×50mm立方体,进行压缩性能测试。
极限氧指数测试:采用WK5155A数显氧指数测定仪依据GB-T2406-1993标准对样品进行氧指数测试,将实施例1-实施例6、对比例1-对比例6已经熟化好的聚氨酯泡沫进行切块,切割成100mm×20mm×20mm立方体。
自熄测试:将实施例1-实施例6、对比例1-对比例6已经熟化好的聚氨酯泡沫进行切块,切割成100mm×20mm×20mm立方体,根据下述的测试方法,通过垂直燃烧测试来测定它们的自熄能力(在火焰自熄之前它们燃烧了多长时间)表现,样品竖直地夹持在架子上,同时下端自由悬挂,每个样本在相对于该样本约90°取向并且朝向其下端的火焰作用下进行燃烧,然后记录自熄时间(如果发生自熄的话)。
表1实施例和对比例的性能测试结果
由表1可知,在加入无机粉末填料的情况下,通过实施例1-实施例6、对比例1-对比例6比较,在加入无机粉末填料后各方面性能比不添加无机粉末填料的各方面性能显著提高,说明在聚氨酯泡沫燃烧时产生的无机阻燃隔膜有较好的自熄和阻燃效果,由对比例6可知无机粉末填料并不是越多越好,无机粉末填料填充量太大反而会破坏泡沫基体的性能,使得物性降低,并且填料掺量大时操作困难,当添加无机粉末填料在50份时各方面性能最佳。
由以上实施例可知,本发明提供的制备方法步骤简单,容易操作,无机粉末填料和磷酸酯类阻燃剂的相互促进作用,提高了聚氨酯泡沫的阻燃性能以及改善了力学性能和热稳定性。
Claims (8)
1.一种阻燃硬质聚氨酯泡沫,其特征在于,由质量比为1:(1-1.6)的白料和黑料制得,所述白料包括以下质量份数的原料:
聚醚多元醇50-100份;
磷酸酯类阻燃剂5-20份;
无机粉末填料45-55份;
泡沫稳定剂1-5份;
发泡剂10-25份;
催化剂0.8-1.5份;
润湿分散剂0.45-0.55份;
所述黑料为异氰酸酯;
其中:
所述无机粉末填料由质量比为(90-99):(1-10)的阻燃无机粉末和促进剂组成;
所述阻燃无机粉末为磷酸钙、碳化硅,所述促进剂为氧化铝,所述磷酸钙、碳化硅、氧化铝的质量比为(70-75):(20-24):(1-10),所述无机粉末填料的粒度为10-15微米。
2.根据权利要求1所述的阻燃硬质聚氨酯泡沫,其特征在于,所述磷酸酯类阻燃剂为甲基磷酸二甲酯、磷酸三氯乙酯、磷酸三乙酯、磷酸三甲苯酯、磷酸三苯酯、磷酸三异丙苯酯、磷酸三丁酯、磷酸三辛酯、甲苯基二苯基磷酸酯中的一种或多种。
3.根据权利要求1所述的阻燃硬质聚氨酯泡沫,其特征在于,所述发泡剂为正戊烷、HCFC-141b、HFC-245fa和环戊烷中的一种。
4.根据权利要求1所述的阻燃硬质聚氨酯泡沫,其特征在于,所述泡沫稳定剂为有机硅泡沫稳定剂。
5.根据权利要求1所述的阻燃硬质聚氨酯泡沫,其特征在于,所述催化剂为辛酸亚锡、二月桂酸二丁基锡、二(十二烷基硫)二丁基锡、二醋酸二丁基锡、三乙烯二胺、五甲基二亚乙基三胺、N,N-二甲基环己胺和N,N-二甲基苄胺中的两种。
6.根据权利要求1所述的阻燃硬质聚氨酯泡沫,其特征在于,所述聚醚多元醇为以蔗糖起始剂体系的硬泡聚醚多元醇。
7.根据权利要求1所述的阻燃硬质聚氨酯泡沫,其特征在于,所述异氰酸酯为多亚甲基多苯基异氰酸酯。
8.一种权利要求1-7任一所述的阻燃硬质聚氨酯泡沫的制备方法,其特征在于,将白料的原料搅拌混匀,得到白料,再将黑料加入到白料中搅拌混匀,得混合液注模并进行发泡,得到发泡成型的泡沫;等泡沫熟化后进行脱模,得到阻燃硬质聚氨酯泡沫。
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