CN107353385A - The preparation method of High-temperature-respolyurethane polyurethane foam material - Google Patents
The preparation method of High-temperature-respolyurethane polyurethane foam material Download PDFInfo
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- CN107353385A CN107353385A CN201710568796.4A CN201710568796A CN107353385A CN 107353385 A CN107353385 A CN 107353385A CN 201710568796 A CN201710568796 A CN 201710568796A CN 107353385 A CN107353385 A CN 107353385A
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- parts
- temperature
- polyurethane foam
- crosslinking agent
- foam material
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- 239000000463 material Substances 0.000 title claims abstract description 23
- 229920005830 Polyurethane Foam Polymers 0.000 title claims abstract description 19
- 239000011496 polyurethane foam Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000012948 isocyanate Substances 0.000 claims abstract description 28
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 20
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000010792 warming Methods 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- 229920001228 polyisocyanate Polymers 0.000 claims abstract description 9
- 239000005056 polyisocyanate Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000004970 Chain extender Substances 0.000 claims abstract description 7
- 150000001244 carboxylic acid anhydrides Chemical group 0.000 claims abstract description 6
- 230000018044 dehydration Effects 0.000 claims abstract description 6
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 6
- 229920005862 polyol Polymers 0.000 claims abstract description 6
- 150000003077 polyols Chemical class 0.000 claims abstract description 6
- -1 hexylene glycol ester Chemical class 0.000 claims description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- 239000006260 foam Substances 0.000 claims description 11
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 11
- 229920000734 polysilsesquioxane polymer Polymers 0.000 claims description 10
- 229920002635 polyurethane Polymers 0.000 claims description 7
- 239000004814 polyurethane Substances 0.000 claims description 7
- ALQLPWJFHRMHIU-UHFFFAOYSA-N 1,4-diisocyanatobenzene Chemical compound O=C=NC1=CC=C(N=C=O)C=C1 ALQLPWJFHRMHIU-UHFFFAOYSA-N 0.000 claims description 6
- SJRJJKPEHAURKC-UHFFFAOYSA-N N-Methylmorpholine Chemical compound CN1CCOCC1 SJRJJKPEHAURKC-UHFFFAOYSA-N 0.000 claims description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- 229920001610 polycaprolactone Polymers 0.000 claims description 6
- 239000004632 polycaprolactone Substances 0.000 claims description 6
- 239000003381 stabilizer Substances 0.000 claims description 6
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 6
- PISLZQACAJMAIO-UHFFFAOYSA-N 2,4-diethyl-6-methylbenzene-1,3-diamine Chemical compound CCC1=CC(C)=C(N)C(CC)=C1N PISLZQACAJMAIO-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920002545 silicone oil Polymers 0.000 claims description 4
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 claims description 3
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 3
- 150000008065 acid anhydrides Chemical class 0.000 claims description 3
- WNLRTRBMVRJNCN-UHFFFAOYSA-L adipate(2-) Chemical compound [O-]C(=O)CCCCC([O-])=O WNLRTRBMVRJNCN-UHFFFAOYSA-L 0.000 claims description 3
- NIHJEJFQQFQLTK-UHFFFAOYSA-N butanedioic acid;hexanedioic acid Chemical compound OC(=O)CCC(O)=O.OC(=O)CCCCC(O)=O NIHJEJFQQFQLTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004872 foam stabilizing agent Substances 0.000 claims description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-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
- RJDVGKCBHFINOK-UHFFFAOYSA-N tris(2-methylphenoxy)-sulfanylidene-$l^{5}-phosphane Chemical compound CC1=CC=CC=C1OP(=S)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C RJDVGKCBHFINOK-UHFFFAOYSA-N 0.000 claims description 3
- IBOFVQJTBBUKMU-UHFFFAOYSA-N 4,4'-methylene-bis-(2-chloroaniline) Chemical compound C1=C(Cl)C(N)=CC=C1CC1=CC=C(N)C(Cl)=C1 IBOFVQJTBBUKMU-UHFFFAOYSA-N 0.000 claims description 2
- 241001112258 Moca Species 0.000 claims description 2
- QORUGOXNWQUALA-UHFFFAOYSA-N N=C=O.N=C=O.N=C=O.C1=CC=C(C(C2=CC=CC=C2)C2=CC=CC=C2)C=C1 Chemical group N=C=O.N=C=O.N=C=O.C1=CC=C(C(C2=CC=CC=C2)C2=CC=CC=C2)C=C1 QORUGOXNWQUALA-UHFFFAOYSA-N 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 239000012965 benzophenone Substances 0.000 claims description 2
- HGQSXVKHVMGQRG-UHFFFAOYSA-N dioctyltin Chemical compound CCCCCCCC[Sn]CCCCCCCC HGQSXVKHVMGQRG-UHFFFAOYSA-N 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 2
- 229940051250 hexylene glycol Drugs 0.000 claims description 2
- SVTBMSDMJJWYQN-UHFFFAOYSA-N hexylene glycol Natural products CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 claims description 2
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- ZXHZWRZAWJVPIC-UHFFFAOYSA-N 1,2-diisocyanatonaphthalene Chemical compound C1=CC=CC2=C(N=C=O)C(N=C=O)=CC=C21 ZXHZWRZAWJVPIC-UHFFFAOYSA-N 0.000 claims 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims 1
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims 1
- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims 1
- 229920001451 polypropylene glycol Polymers 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 238000005829 trimerization reaction Methods 0.000 claims 1
- 150000002148 esters Chemical class 0.000 description 5
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical class OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- VQVIHDPBMFABCQ-UHFFFAOYSA-N 5-(1,3-dioxo-2-benzofuran-5-carbonyl)-2-benzofuran-1,3-dione Chemical compound C1=C2C(=O)OC(=O)C2=CC(C(C=2C=C3C(=O)OC(=O)C3=CC=2)=O)=C1 VQVIHDPBMFABCQ-UHFFFAOYSA-N 0.000 description 1
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- OWIKHYCFFJSOEH-UHFFFAOYSA-N Isocyanic acid Chemical compound N=C=O OWIKHYCFFJSOEH-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- KXBFLNPZHXDQLV-UHFFFAOYSA-N [cyclohexyl(diisocyanato)methyl]cyclohexane Chemical compound C1CCCCC1C(N=C=O)(N=C=O)C1CCCCC1 KXBFLNPZHXDQLV-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-N anhydrous cyanic acid Natural products OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005090 crystal field Methods 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- RAABOESOVLLHRU-UHFFFAOYSA-N diazene Chemical group N=N RAABOESOVLLHRU-UHFFFAOYSA-N 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- GWLJTAJEHRYMCA-UHFFFAOYSA-N phospholane Chemical compound C1CCPC1 GWLJTAJEHRYMCA-UHFFFAOYSA-N 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000011495 polyisocyanurate Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- YFIAVMMGSRDLLG-UHFFFAOYSA-N tert-butyl 3-benzylpiperazine-1-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCNC1CC1=CC=CC=C1 YFIAVMMGSRDLLG-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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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
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- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/77—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur
- C08G18/78—Nitrogen
- C08G18/79—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates
- C08G18/797—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing carbodiimide and/or uretone-imine groups
-
- C—CHEMISTRY; METALLURGY
- 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
- C08J9/06—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 chemical blowing agent
- C08J9/08—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 chemical blowing agent developing carbon dioxide
-
- 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
- C08G2101/00—Manufacture of cellular products
-
- C—CHEMISTRY; METALLURGY
- 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
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The present invention discloses a kind of preparation method of High-temperature-respolyurethane polyurethane foam material, is characterized in：High-temperature-respolyurethane polyurethane foam material, the first step are synthesized using polymerisation in bulk two-step method：5 20 parts of polyisocyanates are weighed, are warming up to 60 100 DEG C, add 0.1 1 parts of catalyst 1, react 20 100min, obtain polycondensation isocyanates；Second step：Weigh 1 20 parts of macromolecular polyols, in 100 120 DEG C of 4h of vacuum dehydration 2, it is cooled to 50 100 DEG C, add 5 45 parts of POSS, 5 20 parts of polyisocyanates, the 5h of stirring reaction 1, add 8 30 parts of carboxylic acid anhydrides chain extender, react 1 5h, it is warming up to 120 140 DEG C, add 1 15 parts, 0.1 5 parts above-mentioned polycondensation isocyanates, 1 15 parts of polyfunctional isocyanate's crosslinking agent, chain extension-crosslinking agent catalyst 2, poured into after stirring in warmed-up mould, product is obtained within 2 10 hours in 100 160 DEG C of vacuum bakings.
Description
First, technical field
The present invention relates to a kind of preparation method of High-temperature-respolyurethane polyurethane foam material, belong to Macroscopic single crystal field.
2nd, background technology
Polyurethane foamed material (PUF) is one of principal item of polyurethane synthetic material.Due to its porous, low heat conduction
The features such as coefficient, show the excellent properties such as excellent wear-resisting, tear-resistant, resistant to chemical etching, antidetonation resistance to compression, heat-insulated.When its work
Be structural material applications when the fields such as armament systems, space flight and aviation, in addition to it need to have excellent mechanical property, should also have compared with
Good thermodynamic stability.But raised with temperature, the decay of its mechanical property is very fast, and usual PUF long-term uses temperature is no more than
85 DEG C, so that its application is by a definite limitation.
At present, mainly by introducing heat-resisting organic group and hybrid inorganic-organic the methods of improve its heat resistance.Li Yan,
Zhou Bing et al., Chinese papermaking journal, 2008,23 (3), the lignin (AAL) in Acetic pulping waste liquor is extracted, its is substituted into portion
Divide polyethylene glycol synthesis PUF, TG analysis results show that the PUF initial decomposition temperatures containing AAL are slightly above the PUF for being not added with AAL,
PUF residual qualities fraction is raised to 4.46% from 3.68% at 797 DEG C.Tang Mingjing, Tian Chunrong et al., plastics industry, 2010,
38 (10), by introducing isocyanates ring into polyurethane foam, polyurethane-modified poly- isocyanuric acid is prepared for using one-step method
Ester (PU-PIR) foam, TG analysis shows PU-PIR are less than conventional PUF in the thermal weight loss rate of high-temperature region (350-550 DEG C).Chen Ke
Equality people, J.APPL.POLYM.SCI.2016,133 (13), by regulating and controlling isocyanates (PAPI) and epoxy resin (E-51)
Mol ratio, the resistant to elevated temperatures epoxy resin modification poly-isocyanurate (EP-PIR) of series is prepared for, in appropriate molar ratios, can be obtained
Obtain optimal machinery and heat resistance, its glass transition temperature are substantially improved.Chinese invention patent ZL201610148679.8
A kind of preparation method of thermal polyurethane composite thermo-insulating wall board is disclosed, and preparing aerosil by using waterglass improves
The thermal insulation and compression strength of polyurethane foam；Improved by using light porous mullite powder, floating bead, nonionic borate
The heat resistance of foam, resistance to ag(e)ing and crushing resistance.But above method is to improving PUF heat-resisting quantities and thermodynamic stability effect
It is not very notable.
3rd, the content of the invention
The purpose of the present invention is in view of the shortcomings of the prior art and provides a kind of preparation of High-temperature-respolyurethane polyurethane foam material
Method, it is characterized according to molecular design theory, by polyisocyanates polycondensation generation containing high heat-resisting carbodiimides structure
Isocyanate compound；It is simultaneously that high temperature resistant, high intensity polyhedral oligomeric silsesquioxane (abbreviation POSS) and macromolecular is polynary
Alcohol is compound to be used as polyurethane soft segment, and the two is matched for regulation, using carboxylic acid anhydrides as chain extender, using polyfunctional isocyanate as crosslinking agent,
By to PUF Study on Preparation, preparing high temperature resistant and thermodynamically stable PUF materials.
The purpose of the present invention is realized by following technical measures, wherein the raw material fraction is unless otherwise specified, it is weight
Number.
The initiation material recipe ingredient of High-temperature-respolyurethane polyurethane foam material is：
Wherein, polyisocyanates 4,4'- methyl diphenylene diisocyanates (MDI), toluene di-isocyanate(TDI) (TDI),
In 1,5- naphthalene diisocyanates (NDI), PPDI (PPDI), 1,4- cyclohexane diisocyanates (CHDI) at least
It is a kind of；
Macromolecular polyol is terminal hydroxy group polyethylene glycol adipate (PEA), terminal hydroxy group polycaprolactone (PCL), terminal hydroxy group
Polyadipate hexylene glycol ester (PHA), terminal hydroxy group poly adipate succinic acid ester (PBA), polytetramethylene ether diol (PTHF), poly- third
At least one of glycol, its mean molecule quantity are 500-3000；
POSS is amine propyl group cage modle polysilsesquioxane, trihydroxy cage modle polysilsesquioxane, poly- times of eight anilino- cage modles
At least one of half siloxanes, epoxy cage type polysilsesquioxane；
Chain extension-crosslinking agent is 3,3 '-two chloro- 4,4 '-MDAs (MOCA), diethyl toluene diamine
(DETDA), at least one of triethanolamine, trimethylolpropane, pentaerythrite；
Polyfunctional isocyanate's crosslinking agent is triphenylmethane triisocyanate, tri o cresyl thiophosphate phenyl isocyanate, TDI tri-
At least one of aggressiveness, MDI tripolymers；
Carboxylic acid anhydrides chain extender be pyromellitic dianhydride, 3,3,4,4- biphenyl tetracarboxylics acid anhydrides, 1,4,5,8 naphthalenetetracarbacidic acidic acid anhydrides, 3,
At least one of 3,4,4- benzophenone tetracarboxylic dianhydrides；
Foam stabiliser is that B8462 silicone oil types foam stabiliser, B8404 silicone oil types foam stabiliser, SD-601 foams are steady
Determine at least one of agent, L-580 foam stabilisers；
Catalyst 1 is 1- methyl -3- methyl -3- Phospholes -1- oxides, 1- methyl isophthalic acids-oxygen Phospholes, 6-
At least one of phospholane, trichloromethyl phosphorous oxide；
Catalyst 2 be triethylenediamine, N-methylmorpholine, triethylamine, stannous octoate, in mercaptan dioctyl tin at least
It is a kind of.
The preparation method of High-temperature-respolyurethane polyurethane foam material：
High-temperature-respolyurethane polyurethane foam material, the first step are synthesized using polymerisation in bulk two-step method：Weigh 5-20 part polyisocyanic acid
Ester, 60-100 DEG C is warming up to, adds 0.1-1 parts catalyst 1, react 20-100min, obtain polycondensation isocyanates；Second step：Claim
1-20 part macromolecular polyols are taken, in 100-120 DEG C of vacuum dehydration 2-4h, 50-100 DEG C is cooled to, adds 5-45 parts POSS, 5-
20 parts of polyisocyanates, stirring reaction 1-5h, carboxylic acid anhydrides chain extender 8-30 parts are added, react 1-5h, be warming up to 120-140 DEG C,
Add above-mentioned polycondensation isocyanates, polyfunctional isocyanate crosslinking agent 1-15 parts, chain extension-crosslinking agent 1-15 parts, the catalysis of 0.1-5 parts
Agent 2, poured into after stirring in warmed-up mould, product is obtained in 100-160 DEG C of vacuum baking 2-10 hour.
The performance of High-temperature-respolyurethane polyurethane foam material：
Turned using High-temperature-respolyurethane polyurethane foam material normal temperature modulus prepared by the above method up to 400-600MPa, vitrifying
Temperature is up to 200-400 DEG C, and thermal weight loss final temperature is up to 600-700 DEG C.
4th, the invention has the advantages that
The present invention introduces heat-resisting molecular radical, and strengthen system crosslinking by MOLECULE DESIGN in segmented polyurethane, soft segment
Degree, so as to greatly improve PUF heat-resisting quantities and thermodynamic stability, i.e., polyisocyanates polycondensation is generated containing high heat-resisting carbon
Change the isocyanate compound of diimine structure；High temperature resistant, high intensity polysilsesquioxane (abbreviation POSS) are introduced into polyurethane
Soft segment, and macromolecular polyol is added, by regulation, the two is matched, and assigns the preferable heat endurances of PUF and pliability；With carboxylic acid
Acid anhydride is chain extender, and using the reaction of isocyanates and acid anhydrides, acid imide heterocycle is introduced into PUF hard sections；Simultaneously using multifunctional different
Cyanate can improve PUF system crosslinking degrees, and introduce heat-resisting benzene ring structure, so as to be obviously improved PUF material resistances to elevated temperatures.
PUF system crosslinked foaming techniques are studied, are not required to applied foam agent, the carbon dioxide gas generated using isocyanates and anhydride reaction
Body is foamed, and forms foam structure.
5th, embodiment
The present invention is specifically described below by embodiment, it is necessary to it is pointed out here that be that the present embodiment is served only for pair
The present invention is further described, it is impossible to is interpreted as limiting the scope of the invention, the person skilled in the art in the field can
Some nonessential modifications and adaptations are made to the present invention with the content according to the invention described above.
Embodiment 1
High-temperature-respolyurethane polyurethane foam material, the first step are synthesized using polymerisation in bulk two-step method：Weigh 1kg toluene diisocynates
Ester (TDI), 60 DEG C are warming up to, add 0.02kg 1- methyl -3- methyl -3- Phospholes -1- oxides, react 30min,
Obtain polycondensation isocyanates；Second step：Terminal hydroxy group polyethylene glycol adipate (PEA, molecular weight 2000) 2kg is weighed, in 120 DEG C
Vacuum dehydration 3h, 60 DEG C are cooled to, add 2kg amine propyl group cage modle polysilsesquioxanes (POSS, molecular weight 1267.32), 2.5kg
Toluene di-isocyanate(TDI) (TDI), stirring reaction 2h, pyromellitic dianhydride 1.499kg is added, react 1h, be warming up to 120 DEG C, add
Enter above-mentioned polycondensation isocyanates, TDI tripolymers 0.5kg, trimethylolpropane 0.5kg and triethylenediamine 0.01kg, stir
Poured into after uniformly in warmed-up mould, product is obtained within 8 hours in 120 DEG C of vacuum bakings.
Embodiment 2
High-temperature-respolyurethane polyurethane foam material, the first step are synthesized using polymerisation in bulk two-step method：Weigh 2kg 4,4'- hexichol
Dicyclohexylmethane diisocyanate (MDI), 70 DEG C are warming up to, add 0.02kg 1- methyl isophthalic acids-oxygen Phospholes, react 30min,
Obtain polycondensation isocyanates；Second step：Terminal hydroxy group poly adipate succinic acid ester (PBA, molecular weight 2000) 1kg is weighed, in 120 DEG C
Vacuum dehydration 2h, 70 DEG C are cooled to, add 2kg trihydroxy cage modles polysilsesquioxane (POSS, molecular weight 931), 2.944kg
4,4'- methyl diphenylene diisocyanates (MDI), stirring reaction 3h, 3,3,4,4- benzophenone tetracarboxylic dianhydride 0.556kg are added,
1.5h is reacted, 100 DEG C is warming up to, adds above-mentioned polycondensation isocyanates, MDI tripolymers 1kg, pentaerythrite 0.5kg and mercaptan two
Tin octylate 0.01kg, poured into after stirring in warmed-up mould, product is obtained within 10 hours in 100 DEG C of vacuum bakings.
Embodiment 3
High-temperature-respolyurethane polyurethane foam material, the first step are synthesized using polymerisation in bulk two-step method：2kg is weighed to the isocyanic acid of benzene two
Ester (PPDI), 80 DEG C are warming up to, add 0.02kg 6- phospholanes, react 40min, obtain polycondensation isocyanates；Second
Step：Terminal hydroxy group polycaprolactone (PCL, molecular weight 2000) 1.5kg is weighed, in 120 DEG C of vacuum dehydration 3h, 80 DEG C is cooled to, adds
2kg epoxy cage types polysilsesquioxane (POSS, molecular weight 1490.58), 1.989kg PPDIs (PPDI), are stirred
Reaction 2h is mixed, adds 3,3,4,4- biphenyl tetracarboxylic acid anhydrides 1.511kg, 1h is reacted, is warming up to 110 DEG C, adds above-mentioned polycondensation isocyanide
Acid esters, tri o cresyl thiophosphate phenyl isocyanate 0.5kg, triethanolamine 0.5kg and stannous octoate 0.01kg, are poured into after stirring
In warmed-up mould, product is obtained within 6 hours in 110 DEG C of vacuum bakings.
Claims (2)
1. a kind of High-temperature-respolyurethane polyurethane foam material, it is characterised in that the raw material of the polyurethane foamed material is by following components group
Into by weight：
Wherein, polyisocyanates 4,4'- methyl diphenylene diisocyanates (MDI), toluene di-isocyanate(TDI) (TDI), 1,5-
At least one in naphthalene diisocyanate (NDI), PPDI (PPDI), 1,4- cyclohexane diisocyanates (CHDI)
Kind；
Macromolecular polyol is terminal hydroxy group polyethylene glycol adipate (PEA), terminal hydroxy group polycaprolactone (PCL), and terminal hydroxy group gathers oneself
Diacid hexylene glycol ester (PHA), terminal hydroxy group poly adipate succinic acid ester (PBA), polytetramethylene ether diol (PTHF), polypropylene glycol
At least one of, its mean molecule quantity is 500-3000；
POSS is amine propyl group cage modle polysilsesquioxane, trihydroxy cage modle polysilsesquioxane, the poly- sesquialter silicon of eight anilino- cage modles
At least one of oxygen alkane, epoxy cage type polysilsesquioxane；
Chain extension-crosslinking agent is 3,3 '-two chloro- 4,4 '-MDAs (MOCA), diethyl toluene diamine (DETDA), three
At least one of monoethanolamine, trimethylolpropane, pentaerythrite；
Polyfunctional isocyanate's crosslinking agent is triphenylmethane triisocyanate, tri o cresyl thiophosphate phenyl isocyanate, TDI trimerizations
At least one of body, MDI tripolymers；
Carboxylic acid anhydrides chain extender be pyromellitic dianhydride, 3,3,4,4- biphenyl tetracarboxylics acid anhydrides, 1,4,5,8 naphthalenetetracarbacidic acidic acid anhydrides, 3,3,4,
At least one of 4- benzophenone tetracarboxylic dianhydrides；
Foam stabiliser be B8462 silicone oil types foam stabiliser, B8404 silicone oil types foam stabiliser, SD-601 foam stabilisers,
At least one of L-580 foam stabilisers；
Catalyst 1 is 1- methyl -3- methyl -3- Phospholes -1- oxides, 1- methyl isophthalic acids-oxygen Phospholes, 6- phosphas
At least one of pentamethylene, trichloromethyl phosphorous oxide；
Catalyst 2 is at least one in triethylenediamine, N-methylmorpholine, triethylamine, stannous octoate, mercaptan dioctyl tin
Kind.
2. the preparation method of High-temperature-respolyurethane polyurethane foam material as claimed in claim 1, it is characterised in that this method includes following
Step：
High-temperature-respolyurethane polyurethane foam material, the first step are synthesized using polymerisation in bulk two-step method：5-20 part polyisocyanates is weighed, is risen
Temperature adds 0.1-1 parts catalyst 1 to 60-100 DEG C, reacts 20-100min, obtains polycondensation isocyanates；Second step：Weigh 1-
20 parts of macromolecular polyols, in 100-120 DEG C of vacuum dehydration 2-4h, 50-100 DEG C is cooled to, adds 5-45 part POSS, 5-20 parts
Polyisocyanates, stirring reaction 1-5h, carboxylic acid anhydrides chain extender 8-30 parts are added, react 1-5h, be warming up to 120-140 DEG C, added
Above-mentioned polycondensation isocyanates, polyfunctional isocyanate crosslinking agent 1-15 parts, chain extension-crosslinking agent 1-15 parts, 0.1-5 parts catalyst 2,
Poured into after stirring in warmed-up mould, product is obtained in 100-160 DEG C of vacuum baking 2-10 hour.
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Cited By (5)
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| CN111848903A (en) * | 2019-10-16 | 2020-10-30 | 宁波途锐达休闲用品有限公司 | Microporous polyurethane foam material and its production process |
| CN113801293A (en) * | 2021-08-13 | 2021-12-17 | 浙江工业大学 | Method for preparing high-temperature-resistant foaming adhesive by using polyurethane foam degradation product |
| CN114989560A (en) * | 2022-07-20 | 2022-09-02 | 浙江南塑合成材料有限公司 | High-performance composite material based on modified phenolic resin and preparation method thereof |
| CN116872592A (en) * | 2023-01-10 | 2023-10-13 | 南通北风橡塑制品有限公司 | High-strength wear-resistant polyurethane composite board and processing technology thereof |
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| CN113801293A (en) * | 2021-08-13 | 2021-12-17 | 浙江工业大学 | Method for preparing high-temperature-resistant foaming adhesive by using polyurethane foam degradation product |
| CN114989560A (en) * | 2022-07-20 | 2022-09-02 | 浙江南塑合成材料有限公司 | High-performance composite material based on modified phenolic resin and preparation method thereof |
| CN114989560B (en) * | 2022-07-20 | 2023-07-28 | 浙江南塑合成材料有限公司 | High-performance composite material based on modified phenolic resin and preparation method thereof |
| CN116872592A (en) * | 2023-01-10 | 2023-10-13 | 南通北风橡塑制品有限公司 | High-strength wear-resistant polyurethane composite board and processing technology thereof |
| CN116872592B (en) * | 2023-01-10 | 2023-12-12 | 南通北风橡塑制品有限公司 | High-strength wear-resistant polyurethane composite board and processing technology thereof |
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