CN112812473B - Low-thermal-conductivity-coefficient rigid crosslinked polyvinyl chloride foam material and preparation method thereof - Google Patents
Low-thermal-conductivity-coefficient rigid crosslinked polyvinyl chloride foam material and preparation method thereof Download PDFInfo
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- CN112812473B CN112812473B CN202110173491.XA CN202110173491A CN112812473B CN 112812473 B CN112812473 B CN 112812473B CN 202110173491 A CN202110173491 A CN 202110173491A CN 112812473 B CN112812473 B CN 112812473B
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- 229920000915 polyvinyl chloride Polymers 0.000 title claims abstract description 39
- 239000004800 polyvinyl chloride Substances 0.000 title claims abstract description 39
- 239000006261 foam material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229920005989 resin Polymers 0.000 claims abstract description 18
- 239000011347 resin Substances 0.000 claims abstract description 18
- 239000003822 epoxy resin Substances 0.000 claims abstract description 13
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 13
- 239000004088 foaming agent Substances 0.000 claims abstract description 5
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 3
- 239000003085 diluting agent Substances 0.000 claims abstract description 3
- 239000012760 heat stabilizer Substances 0.000 claims abstract description 3
- 239000012948 isocyanate Substances 0.000 claims abstract description 3
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 3
- 239000004094 surface-active agent Substances 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 20
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims description 19
- 239000002994 raw material Substances 0.000 claims description 17
- 238000005187 foaming Methods 0.000 claims description 15
- -1 polymethylene Polymers 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 11
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 235000012424 soybean oil Nutrition 0.000 claims description 10
- 239000003549 soybean oil Substances 0.000 claims description 10
- 229920001400 block copolymer Polymers 0.000 claims description 8
- 150000007942 carboxylates Chemical class 0.000 claims description 5
- 229920001328 Polyvinylidene chloride Polymers 0.000 claims description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 4
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 4
- 239000005033 polyvinylidene chloride Substances 0.000 claims description 4
- 239000005056 polyisocyanate Substances 0.000 claims description 3
- 229920001228 polyisocyanate Polymers 0.000 claims description 3
- 229920006389 polyphenyl polymer Polymers 0.000 claims description 3
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 2
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 2
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- 239000004593 Epoxy Substances 0.000 claims description 2
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 2
- 235000013539 calcium stearate Nutrition 0.000 claims description 2
- 239000008116 calcium stearate Substances 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 2
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 2
- 235000019359 magnesium stearate Nutrition 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 2
- 239000013638 trimer Substances 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims 2
- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 239000006260 foam Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 11
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 description 8
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 8
- YSUQLAYJZDEMOT-UHFFFAOYSA-N 2-(butoxymethyl)oxirane Chemical compound CCCCOCC1CO1 YSUQLAYJZDEMOT-UHFFFAOYSA-N 0.000 description 8
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 8
- 239000004246 zinc acetate Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000012360 testing method Methods 0.000 description 5
- 239000012774 insulation material Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- NXFJXKDZEKNNRK-UHFFFAOYSA-N furan-2,5-dione;methyl 2-methylprop-2-enoate Chemical compound COC(=O)C(C)=C.O=C1OC(=O)C=C1 NXFJXKDZEKNNRK-UHFFFAOYSA-N 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- KMOUUZVZFBCRAM-OLQVQODUSA-N (3as,7ar)-3a,4,7,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C=CC[C@@H]2C(=O)OC(=O)[C@@H]21 KMOUUZVZFBCRAM-OLQVQODUSA-N 0.000 description 1
- NVSXSBBVEDNGPY-UHFFFAOYSA-N 1,1,1,2,2-pentafluorobutane Chemical compound CCC(F)(F)C(F)(F)F NVSXSBBVEDNGPY-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 description 1
- RCXHRHWRRACBTK-UHFFFAOYSA-N 3-(oxiran-2-ylmethoxy)propane-1,2-diol Chemical compound OCC(O)COCC1CO1 RCXHRHWRRACBTK-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- MWRWFPQBGSZWNV-UHFFFAOYSA-N Dinitrosopentamethylenetetramine Chemical compound C1N2CN(N=O)CN1CN(N=O)C2 MWRWFPQBGSZWNV-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- NVFYKZBOLSIHEI-UHFFFAOYSA-N furan-2,5-dione;2-methylprop-2-enoic acid Chemical compound CC(=C)C(O)=O.O=C1OC(=O)C=C1 NVFYKZBOLSIHEI-UHFFFAOYSA-N 0.000 description 1
- VNZYHVPAPZNCBZ-UHFFFAOYSA-N furan-2,5-dione;methyl prop-2-enoate Chemical compound COC(=O)C=C.O=C1OC(=O)C=C1 VNZYHVPAPZNCBZ-UHFFFAOYSA-N 0.000 description 1
- OSIMQZHJCXQJDX-UHFFFAOYSA-N furan-2,5-dione;prop-2-enenitrile Chemical compound C=CC#N.O=C1OC(=O)C=C1 OSIMQZHJCXQJDX-UHFFFAOYSA-N 0.000 description 1
- JPZROSNLRWHSQQ-UHFFFAOYSA-N furan-2,5-dione;prop-2-enoic acid Chemical compound OC(=O)C=C.O=C1OC(=O)C=C1 JPZROSNLRWHSQQ-UHFFFAOYSA-N 0.000 description 1
- WOLATMHLPFJRGC-UHFFFAOYSA-N furan-2,5-dione;styrene Chemical compound O=C1OC(=O)C=C1.C=CC1=CC=CC=C1 WOLATMHLPFJRGC-UHFFFAOYSA-N 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- MSSNHSVIGIHOJA-UHFFFAOYSA-N pentafluoropropane Chemical compound FC(F)CC(F)(F)F MSSNHSVIGIHOJA-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229920006132 styrene block copolymer Polymers 0.000 description 1
- 229940014800 succinic anhydride Drugs 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
-
- 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
- C08J9/12—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
- C08J9/141—Hydrocarbons
-
- 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
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
-
- 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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
-
- 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
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
-
- 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
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
- C08J2463/02—Polyglycidyl ethers of bis-phenols
-
- 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
- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention belongs to the technical field of foam materials, and particularly relates to a low-thermal-conductivity-coefficient hard cross-linked polyvinyl chloride foam material and a preparation method thereof, which solve the problems that the cross-linked polyvinyl chloride foam material is long in production period, high in thermal conductivity coefficient and greatly increased in thermal conductivity coefficient along with time in the prior art. The formula of the foam material comprises 100 parts of polyvinyl chloride, 20-50 parts of isocyanate, 0-30 parts of epoxy resin, 10-50 parts of reactive diluent, 5-50 parts of modified resin, 5-50 parts of foaming agent, 5-20 parts of heat stabilizer, 1-5 parts of surfactant, 0.1-5 parts of vulcanizing agent and 0.1-5 parts of accelerator. The foam has short production period, meets the performance requirements of high strength, high toughness, high flame retardance, high closed cell rate, low density and the like at the temperature of between 170 ℃ below zero and 40 ℃, has a heat conductivity coefficient of less than or equal to 30mW/mk, and meets the use requirement of low heat conductivity coefficient for a long time.
Description
Technical Field
The invention belongs to the technical field of foam materials, and particularly relates to a low-thermal conductivity rigid crosslinked polyvinyl chloride foam material and a preparation method thereof.
Background
The special marine thermal insulation material is required to be capable of maintaining high strength, high toughness, high flame retardance, low density and low heat conductivity coefficient at the ambient temperature of minus 170-40 ℃ for a long time. The traditional heat insulation materials such as PU foam and PIR foam only have the heat conductivity coefficient meeting the requirements, and the mechanical property can not meet the use requirements. The only foam material meeting the performance requirements and having a lower price is the cross-linked polyvinyl chloride foam material.
Currently, only one of the swedish DIAB companies in the world is capable of providing a special marine rigid cross-linked polyvinyl chloride foam product. The reasons are mainly two: firstly, the hard cross-linked polyvinyl chloride foam material with high strength, high toughness, high flame retardance, high closed cell rate and low density has larger production technical difficulty, long production period which is about 15-30d, and can be produced by a few companies such as DIAB in Sweden, Maricell in Italy and the like; secondly, the existing hard cross-linked polyvinyl chloride foam is a water foaming process, and the gas in foam material foam holes is CO 2 ，CO 2 High heat conductivity coefficient, easy permeation from foam, high initial heat conductivity coefficient, greatly increased heat conductivity coefficient in short time, and no heat insulating abilityAnd the service life of the heat-insulating material is extremely short. Can not meet the use requirements of special marine thermal insulation materials.
Although the technology disclosed in patent CN106867140A has a low initial thermal conductivity, a comparative test proves that the foam material cannot maintain a low thermal conductivity for a long time, the thermal insulation property is lost quickly, and the foaming process adopts a traditional water foaming process, so that the production cycle is long. The invention not only keeps the excellent mechanical property and flame retardant property of the rigid cross-linked polyvinyl chloride foam product, but also greatly reduces the production period of the foam material, reduces the heat conductivity coefficient, prolongs the heat preservation life and is expected to break the monopoly of foreign technologies.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a low-thermal conductivity rigid crosslinked polyvinyl chloride foam material and a preparation method thereof, which can effectively shorten the production period of the rigid crosslinked polyvinyl chloride foam material; and the heat conductivity coefficient is less than or equal to 30mW/mk while meeting the performance requirements of high strength, high toughness, high flame retardance, high closed porosity, low density and the like at the temperature of between 170 ℃ below zero and 40 ℃, thereby meeting the use requirement of low heat conductivity coefficient for a long time.
The technical scheme of the invention is as follows: according to a first aspect of the present invention, there is provided a low thermal conductivity rigid crosslinked polyvinyl chloride foam material, which comprises the following raw materials in parts by mass:
Preferably, the polyvinyl chloride is PVC paste resin with the particle size of less than 100 μm and the molecular weight of 2000-20000.
Preferably, the isocyanate is at least one of toluene diisocyanate, diphenylmethane diisocyanate, hexamethylene diisocyanate trimer, and polymethylene polyphenyl polyisocyanate.
Preferably, the epoxy resin is at least one of bisphenol a type, bisphenol F type, and bisphenol S type epoxy resins.
Preferably, the reactive diluent is at least one of a glycidyl ether or ester having a viscosity of less than 500 mPas.
Preferably, the modified resin is at least one of maleic anhydride styrene block copolymer, maleic anhydride acrylate block copolymer, maleic anhydride methacrylate block copolymer, polyvinylidene chloride and poly (trimethylene naphthalate).
Preferably, the foaming agent is at least one of cyclopentane, n-pentane, cyclohexane, pentafluoropropane and pentafluorobutane.
Preferably, the heat stabilizer is at least one of epoxy soybean oil, zinc stearate, calcium stearate, barium stearate, magnesium stearate and sodium dodecyl sulfate.
Preferably, the surfactant is a polyether poly-siloxane block copolymer.
Preferably, the vulcanizing agent is an organic peroxide compound.
Preferably, the promoter is at least one of 2, 4, 6-tris (dimethylaminomethyl) phenol and its carboxylate and carboxylate or carboxylate of manganese, calcium, cobalt, zinc.
According to a second aspect of the present invention, there is provided a method for preparing a low thermal conductivity rigid crosslinked polyvinyl chloride foam material, for preparing the above low thermal conductivity crosslinked polyvinyl chloride foam material, comprising the following steps:
s1: introducing the liquid raw materials into a planetary stirring kettle by using a metering pump, and mixing for 20min at 20-30 ℃;
s2: adding the solid powder into a stirring kettle, mixing at 20-30 deg.C for 20min, keeping the temperature, standing for 30min to remove bubbles;
s3: pressurizing the stirred tank to 0.1-0.2MPa by using dry air, and putting the materials into a mold through a bottom discharge valve;
s4: placing the mould on a flat vulcanizing machine, pressurizing to 25-35MPa, raising the temperature to 150-200 ℃, and keeping the temperature and the pressure for 10-40 min;
s5: cooling the plate vulcanizing machine to 40-80 ℃, decompressing, opening the die and taking out the green body;
s6: placing the green body into an oven with the temperature of 80-130 ℃ for foaming for 1-4h, and curing in the oven with the temperature of 40-80 ℃ for 4-10 days to obtain a foamed product.
Compared with the prior art, the invention has the beneficial effects that:
1) by adopting the foaming-curing system and the preparation process, the production period is shortened by more than half compared with the prior art while the good mechanical properties of high strength, high toughness, high closed cell rate, low density and the like of the foam material are kept, and the production efficiency is greatly improved;
2) in order to meet the long-term use requirement in the environment of-170-40 ℃, the initial thermal conductivity of the foam material is greatly reduced by adopting a physical foaming agent with low thermal conductivity; meanwhile, the permeation-resistant modified resin is used to generate a complex synergistic effect, so that the foam material can keep a low thermal conductivity coefficient for a long time, and the service life of the heat-insulating material is greatly prolonged.
Detailed Description
For a further understanding of the invention, preferred embodiments of the invention are described below in conjunction with the examples, but it should be understood that these descriptions are included merely to further illustrate the features and advantages of the invention and are not intended to limit the invention to the claims. The starting materials used in the examples are all commercially available.
Example 1
The formula comprises 100 parts of PVC paste resin, 35 parts of Wanhua PM200, 28 parts of epoxy resin E51, 10 parts of allyl glycidyl ether, 25 parts of butyl glycidyl ether, 46 parts of maleic anhydride methyl methacrylate block copolymer, 46 parts of cyclopentane, 15 parts of epoxidized soybean oil, 5 parts of AK8805, 5 parts of dicumyl peroxide, 3 parts of DMP-30 carboxylic ester and 2 parts of zinc acetate. The process comprises the following steps:
1) Introducing the liquid raw materials into a planetary stirring kettle by using a metering pump, and mixing for 20min at 30 ℃;
2) adding the solid powder into a stirring kettle, mixing for 20min at 30 ℃, preserving heat, standing for 30min to remove bubbles;
3) pressurizing the stirred tank to 0.1-0.2MPa by using dry air, and putting the materials into a mold through a bottom discharge valve;
4) the mold is placed on a flat vulcanizing machine, the pressure is increased by 30MPa, the temperature is increased to 170 ℃, and the temperature and the pressure are maintained for 10 min.
5) And cooling the plate vulcanizing machine to 60 ℃, decompressing, opening the die and taking out the green body.
6) And (3) placing the green bodies into an oven at 115 ℃ for foaming for 2h, and curing in an oven at 80 ℃ for 6 days to obtain foamed products.
Example 2
The formula comprises 100 parts of PVC paste resin, 35 parts of Wanhua PM200, 28 parts of epoxy resin E51, 10 parts of allyl glycidyl ether, 25 parts of butyl glycidyl ether, 46 parts of maleic anhydride methyl acrylate block copolymer, 46 parts of cyclopentane, 15 parts of epoxidized soybean oil, 5 parts of AK8805, 5 parts of dicumyl peroxide, 3 parts of DMP-30 carboxylic ester and 2 parts of zinc acetate. The process comprises the following steps:
1) introducing the liquid raw materials into a planetary stirring kettle by using a metering pump, and mixing for 20min at 30 ℃;
2) adding the solid powder into a stirring kettle, mixing for 20min at 30 ℃, preserving heat, standing for 30min to remove bubbles;
3) Pressurizing the stirred tank to 0.1-0.2MPa by using dry air, and putting the materials into a mold through a bottom discharge valve;
4) the mold is placed on a flat vulcanizing machine, the pressure is increased by 30MPa, the temperature is increased to 170 ℃, and the temperature and the pressure are maintained for 10 min.
5) And cooling the plate vulcanizing machine to 60 ℃, decompressing, opening the die and taking out the green body.
6) And (3) placing the green bodies into an oven at 115 ℃ for foaming for 2h, and curing in an oven at 80 ℃ for 6 days to obtain foamed products.
Example 3
The formula comprises 100 parts of PVC paste resin, 35 parts of Wanhua PM200, 28 parts of epoxy resin E51, 10 parts of allyl glycidyl ether, 25 parts of butyl glycidyl ether, 46 parts of maleic anhydride acrylonitrile block copolymer, 46 parts of cyclopentane, 15 parts of epoxidized soybean oil, 5 parts of AK8805, 5 parts of dicumyl peroxide, 3 parts of DMP-30 carboxylic ester and 2 parts of zinc acetate. The process comprises the following steps:
1) introducing the liquid raw materials into a planetary stirring kettle by using a metering pump, and mixing for 20min at 30 ℃;
2) adding the solid powder into a stirring kettle, mixing for 20min at 30 ℃, preserving heat, standing for 30min to remove bubbles;
3) pressurizing the stirred tank to 0.1-0.2MPa by using dry air, and putting the materials into a mold through a bottom discharge valve;
4) the mold is placed on a flat vulcanizing machine, the pressure is increased by 30MPa, the temperature is increased to 170 ℃, and the temperature and the pressure are maintained for 10 min.
5) And cooling the plate vulcanizing machine to 60 ℃, decompressing, opening the die and taking out the green body.
6) And (3) placing the green bodies into an oven at 115 ℃ for foaming for 2h, and curing in an oven at 80 ℃ for 6 days to obtain foamed products.
Example 4
The formula comprises 100 parts of PVC paste resin, 35 parts of Wanhua PM200, 28 parts of epoxy resin E51, 10 parts of allyl glycidyl ether, 25 parts of butyl glycidyl ether, 46 parts of polyvinylidene chloride, 46 parts of cyclopentane, 15 parts of epoxidized soybean oil, 5 parts of AK8805, 5 parts of dicumyl peroxide, 3 parts of DMP-30 carboxylic ester and 2 parts of zinc acetate. The process comprises the following steps:
1) introducing the liquid raw materials into a planetary stirring kettle by using a metering pump, and mixing for 20min at 30 ℃;
2) adding the solid powder into a stirring kettle, mixing for 20min at 30 ℃, preserving heat, standing for 30min to remove bubbles;
3) pressurizing the stirred tank to 0.1-0.2MPa by using dry air, and putting the materials into a mold through a bottom discharge valve;
4) the mold is placed on a flat vulcanizing machine, the pressure is increased by 30MPa, the temperature is increased to 170 ℃, and the temperature and the pressure are maintained for 10 min.
5) And cooling the plate vulcanizing machine to 60 ℃, decompressing, opening the die and taking out the green body.
6) And (3) placing the green blank into an oven at 115 ℃ for foaming for 2h, and curing in the oven at 80 ℃ for 6 days to obtain a foamed product.
Example 5
The formula comprises 100 parts of PVC paste resin, 35 parts of Wanhua PM200, 28 parts of epoxy resin E51, 10 parts of allyl glycidyl ether, 25 parts of butyl glycidyl ether, 46 parts of polytrimethylene naphthalate, 46 parts of cyclopentane, 15 parts of epoxidized soybean oil, 5 parts of AK8805, 5 parts of dicumyl peroxide, 3 parts of DMP-30 carboxylic ester and 2 parts of zinc acetate. The process comprises the following steps:
1) introducing the liquid raw materials into a planetary stirring kettle by using a metering pump, and mixing for 20min at 30 ℃;
2) adding the solid powder into a stirring kettle, mixing for 20min at 30 ℃, preserving heat, standing for 30min to remove bubbles;
3) pressurizing the stirred tank to 0.1-0.2MPa by using dry air, and putting the materials into a mold through a bottom discharge valve;
4) the mold was placed on a press vulcanizer and pressurized at 30MPa, the temperature was raised to 170 ℃ and the temperature and pressure were maintained for 10 min.
5) And cooling the plate vulcanizing machine to 60 ℃, decompressing, opening the die and taking out the green body.
6) And (3) placing the green bodies into an oven at 115 ℃ for foaming for 2h, and curing in an oven at 80 ℃ for 6 days to obtain foamed products.
Example 6
The formula comprises 100 parts of PVC paste resin, 35 parts of Wanhua PM200, 28 parts of epoxy resin E51, 10 parts of allyl glycidyl ether, 25 parts of butyl glycidyl ether, 26 parts of maleic anhydride methyl methacrylate block copolymer, 20 parts of polyvinylidene chloride, 46 parts of cyclopentane, 15 parts of epoxidized soybean oil, 5 parts of AK8805, 5 parts of dicumyl peroxide, 3 parts of DMP-30 carboxylic ester and 2 parts of zinc acetate. The process comprises the following steps:
1) Introducing the liquid raw materials into a planetary stirring kettle by using a metering pump, and mixing for 20min at 30 ℃;
2) adding the solid powder into a stirring kettle, mixing for 20min at 30 ℃, preserving heat, standing for 30min to remove bubbles;
3) pressurizing the stirred tank to 0.1-0.2MPa by using dry air, and putting the materials into a mold through a bottom discharge valve;
4) the mold is placed on a flat vulcanizing machine, the pressure is increased by 30MPa, the temperature is increased to 170 ℃, and the temperature and the pressure are maintained for 10 min.
5) And cooling the plate vulcanizing machine to 60 ℃, decompressing, opening the die and taking out the green body.
6) And (3) placing the green bodies into an oven at 115 ℃ for foaming for 2h, and curing in an oven at 80 ℃ for 6 days to obtain foamed products.
Comparative example 1
The formula comprises 100 parts of PVC paste resin, 35 parts of Wanhua PM200, 28 parts of epoxy resin E51, 10 parts of allyl glycidyl ether, 25 parts of butyl glycidyl ether, 46 parts of cyclopentane, 15 parts of epoxidized soybean oil, 5 parts of AK8805, 5 parts of dicumyl peroxide, 3 parts of DMP-30 carboxylic ester and 2 parts of zinc acetate. The process comprises the following steps:
1) introducing the liquid raw materials into a planetary stirring kettle by using a metering pump, and mixing for 20min at 30 ℃;
2) adding the solid powder into a stirring kettle, mixing for 20min at 30 ℃, preserving heat, standing for 30min to remove bubbles;
3) pressurizing the stirred tank to 0.1-0.2MPa by using dry air, and putting the materials into a mold through a bottom discharge valve;
4) The mold is placed on a flat vulcanizing machine, the pressure is increased by 30MPa, the temperature is increased to 170 ℃, and the temperature and the pressure are maintained for 10 min.
5) And cooling the plate vulcanizing machine to 60 ℃, decompressing, opening the die and taking out the green body.
6) And (3) placing the green bodies into an oven at 115 ℃ for foaming for 2h, and curing in an oven at 80 ℃ for 6 days to obtain foamed products.
Comparative example 2
The formula comprises 100 parts of PVC paste resin, 35 parts of Wanhua PM200, 28 parts of epoxy resin E51, 10 parts of allyl glycidyl ether, 25 parts of butyl glycidyl ether, 26 parts of maleic anhydride, 20 parts of methyl methacrylate, 46 parts of cyclopentane, 15 parts of epoxidized soybean oil, 5 parts of AK8805, 5 parts of dicumyl peroxide, 3 parts of DMP-30 carboxylic ester and 2 parts of zinc acetate. The process comprises the following steps:
1) introducing the liquid raw materials into a planetary stirring kettle by using a metering pump, and mixing for 20min at 30 ℃;
2) adding the solid powder into a stirring kettle, mixing for 20min at 30 ℃, preserving heat, standing for 30min to remove bubbles;
3) pressurizing the stirred tank to 0.1-0.2MPa by using dry air, and putting the materials into a mold through a bottom discharge valve;
4) the mold was placed on a press vulcanizer and pressurized at 30MPa, the temperature was raised to 170 ℃ and the temperature and pressure were maintained for 10 min.
5) And cooling the plate vulcanizing machine to 60 ℃, decompressing, opening the die and taking out the green body.
6) And (3) placing the green bodies into an oven at 115 ℃ for foaming for 2h, and curing in an oven at 80 ℃ for 6 days to obtain foamed products.
Comparative example 3
The test was carried out according to example 3 of patent CN106867140A, the formulation being 100 parts of PVC paste resin, 50 parts of succinic anhydride, 10 parts of tetrahydrophthalic anhydride, 10 parts of glycerol glycidyl ether, 60 parts of polymethylene polyphenyl polyisocyanate (PAPI), 10 parts of N, N-dinitrosopentamethylenetetramine, 3 parts of Tween 80, 5 parts of antimony trioxide, 0.1 part of graphite powder (400 mesh).
The preparation process comprises the following steps: uniformly mixing the raw materials, adding the raw materials into a mold, preheating the raw materials at 90 ℃ for 20min, boosting the pressure to 15MPa, raising the temperature to 180 ℃, carrying out mold pressing for 40s/mm, cooling the raw materials to 110 ℃, opening the mold, foaming the raw materials in water at 100 ℃ for 2h, solidifying a sample 3-1 in 70 ℃ water for 6 days, solidifying a sample 3-2 in 70 ℃ water for 10 days, solidifying a sample 3-3 in 70 ℃ water for 10 days, and drying the sample in an oven at 70 ℃ for 5 days.
Performance testing and results demonstration
To further illustrate the gain effect of the present invention, examples 1-6 and comparative examples 1-3 were tested for performance by:
compressive strength ASTM D1621, compressive modulus ASTM D1621-B-73, thermal conductivity ASTM D C581, accelerated aging to 70 ℃ 0D, 7D, 14D, 21D, 28D, apparent density ASTM D1622, closed cell rate ASTM D6226, pore size by slice with scale optical microscope measurement. The measurement results are shown in table 1.
Comparing table 1 the results of the strength modulus tests, it can be seen that the mechanical properties of the foams of examples 1-6 and comparative examples 1-2 using the foam-cure system of the present invention are far superior to those of comparative example 3 of the prior art.
Compared with the 0d thermal conductivity of the comparative examples 1-6 and 1-3, the introduction of the physical foaming agent with low thermal conductivity can effectively reduce the initial thermal conductivity of the foam. The results of comparing the thermal conductivity coefficients of examples 1 to 6 and comparative examples 1 to 3 after accelerated aging show that the heat preservation life of the foam material is greatly prolonged by introducing the permeation resistant modified resin, and the permeation resistant resin has to have a specific structure, so that the monomer of the resin is directly added into the formula, and the effect of prolonging the heat preservation life of the foam material cannot be achieved. The test results of the comparative example 1 and the comparative examples 3-1 to 3-3 show that the traditional water foaming process needs long-time curing and drying, but the method greatly shortens the production period, improves the production efficiency and reduces the production cost.
TABLE 1 sample Performance test results
Claims (9)
1. The hard cross-linked polyvinyl chloride foam material with low thermal conductivity is characterized by comprising the following raw materials in parts by mass:
the modified resin is at least one of polyvinylidene chloride and poly (trimethylene naphthalate);
The foaming agent is cyclopentane;
the preparation method of the hard crosslinked polyvinyl chloride foam material with the low thermal conductivity coefficient comprises the following steps:
s1: introducing the liquid raw materials into a planetary stirring kettle by using a metering pump, and mixing for 20min at 20-30 ℃;
s2: adding the solid powder into a stirring kettle, mixing at 20-30 deg.C for 20min, keeping the temperature, standing for 30min to remove bubbles;
s3: pressurizing the stirred tank to 0.1-0.2MPa by using dry air, and putting the materials into a mold through a bottom discharge valve;
s4: placing the mould on a flat vulcanizing machine, pressurizing to 25-35MPa, raising the temperature to 150-200 ℃, and keeping the temperature and the pressure for 10-40 min;
s5: cooling the plate vulcanizing machine to 40-80 ℃, decompressing, opening the die and taking out a green body;
s6: placing the green body into an oven with the temperature of 80-130 ℃ for foaming for 1-4h, and curing in the oven with the temperature of 40-80 ℃ for 4-10 days to obtain a foamed product.
2. The rigid cross-linked polyvinyl chloride foam material of claim 1, wherein: the polyvinyl chloride is PVC paste resin with the particle size of less than 100 mu m and the molecular weight of 2000-20000.
3. The rigid cross-linked polyvinyl chloride foam material of claim 1, wherein: the isocyanate is at least one of toluene diisocyanate, diphenylmethane diisocyanate, hexamethylene diisocyanate trimer and polymethylene polyphenyl polyisocyanate.
4. The rigid cross-linked polyvinyl chloride foam material of claim 1, wherein: the epoxy resin is at least one of bisphenol A type, bisphenol F type and bisphenol S type epoxy resin.
5. The rigid cross-linked polyvinyl chloride foam material of claim 1, wherein: the reactive diluent is at least one of glycidyl ether or glycidyl ester with viscosity less than 500 mPas.
6. A low thermal conductivity rigid crosslinked polyvinyl chloride foam material according to claim 1 wherein: the heat stabilizer is at least one of epoxy soybean oil, zinc stearate, calcium stearate, barium stearate, magnesium stearate and sodium dodecyl sulfate.
7. The crosslinked polyvinyl chloride foam material with low thermal conductivity of claim 1, wherein: the surfactant is polyether poly-siloxane block copolymer.
8. The crosslinked polyvinyl chloride foam material with low thermal conductivity of claim 1, wherein: the vulcanizing agent is an organic peroxide compound.
9. The crosslinked polyvinyl chloride foam material with low thermal conductivity of claim 1, wherein: the promoter is at least one of 2, 4, 6-tri (dimethylaminomethyl) phenol and carboxylate thereof or carboxylate of manganese, calcium, cobalt and zinc.
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