CN116655877A - Wall heat-insulating composite material and production process thereof - Google Patents
Wall heat-insulating composite material and production process thereof Download PDFInfo
- Publication number
- CN116655877A CN116655877A CN202310731281.7A CN202310731281A CN116655877A CN 116655877 A CN116655877 A CN 116655877A CN 202310731281 A CN202310731281 A CN 202310731281A CN 116655877 A CN116655877 A CN 116655877A
- Authority
- CN
- China
- Prior art keywords
- parts
- insulation composite
- flame retardant
- stirring
- linking agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title abstract description 11
- 239000003063 flame retardant Substances 0.000 claims abstract description 45
- 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 claims abstract description 43
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 30
- 238000009413 insulation Methods 0.000 claims abstract description 29
- 239000004088 foaming agent Substances 0.000 claims abstract description 24
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 20
- 229920000570 polyether Polymers 0.000 claims abstract description 20
- 229920005862 polyol Polymers 0.000 claims abstract description 20
- 150000003077 polyols Chemical class 0.000 claims abstract description 20
- 239000000126 substance Substances 0.000 claims abstract description 16
- 239000011256 inorganic filler Substances 0.000 claims abstract description 15
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 239000012948 isocyanate Substances 0.000 claims abstract description 4
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 59
- 238000006243 chemical reaction Methods 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 13
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 12
- 238000005187 foaming Methods 0.000 claims description 11
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical group CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 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 6
- 239000004156 Azodicarbonamide Substances 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 6
- BHIIGRBMZRSDRI-UHFFFAOYSA-N [chloro(phenoxy)phosphoryl]oxybenzene Chemical compound C=1C=CC=CC=1OP(=O)(Cl)OC1=CC=CC=C1 BHIIGRBMZRSDRI-UHFFFAOYSA-N 0.000 claims description 6
- XOZUGNYVDXMRKW-AATRIKPKSA-N azodicarbonamide Chemical compound NC(=O)\N=N\C(N)=O XOZUGNYVDXMRKW-AATRIKPKSA-N 0.000 claims description 6
- 235000019399 azodicarbonamide Nutrition 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- 239000004917 carbon fiber Substances 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 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 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 5
- BPYFPNZHLXDIGA-UHFFFAOYSA-N diphenylsilicon Chemical compound C=1C=CC=CC=1[Si]C1=CC=CC=C1 BPYFPNZHLXDIGA-UHFFFAOYSA-N 0.000 claims description 5
- 235000011187 glycerol Nutrition 0.000 claims description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 5
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 4
- KXBFLNPZHXDQLV-UHFFFAOYSA-N [cyclohexyl(diisocyanato)methyl]cyclohexane Chemical compound C1CCCCC1C(N=C=O)(N=C=O)C1CCCCC1 KXBFLNPZHXDQLV-UHFFFAOYSA-N 0.000 claims description 4
- 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 4
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 4
- 125000005442 diisocyanate group Chemical group 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 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 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 239000004604 Blowing Agent Substances 0.000 claims 1
- 239000002666 chemical blowing agent Substances 0.000 claims 1
- 229920002635 polyurethane Polymers 0.000 abstract description 11
- 239000004814 polyurethane Substances 0.000 abstract description 11
- 239000012774 insulation material Substances 0.000 abstract description 8
- CMPQUABWPXYYSH-UHFFFAOYSA-N phenyl phosphate Chemical group OP(O)(=O)OC1=CC=CC=C1 CMPQUABWPXYYSH-UHFFFAOYSA-N 0.000 abstract description 5
- 229920005830 Polyurethane Foam Polymers 0.000 abstract description 3
- HIVGXUNKSAJJDN-UHFFFAOYSA-N [Si].[P] Chemical compound [Si].[P] HIVGXUNKSAJJDN-UHFFFAOYSA-N 0.000 abstract description 3
- 239000011496 polyurethane foam Substances 0.000 abstract description 3
- 229910052710 silicon Inorganic materials 0.000 abstract description 3
- 239000010703 silicon Substances 0.000 abstract description 3
- 239000002243 precursor Substances 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 239000011810 insulating material Substances 0.000 description 18
- 230000000694 effects Effects 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 239000006260 foam Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical group C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000004970 Chain extender Substances 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 238000007792 addition Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000010425 asbestos Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 2
- 150000002926 oxygen Chemical class 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 229910052895 riebeckite Inorganic materials 0.000 description 2
- 238000007142 ring opening reaction Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000013049 sediment 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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- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
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- C08G18/6511—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen the low-molecular compounds being compounds of group C08G18/32 or polyamines of C08G18/38 compounds of group C08G18/3203
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B30/00—Energy efficient heating, ventilation or air conditioning [HVAC]
- Y02B30/90—Passive houses; Double facade technology
Abstract
The invention relates to the technical field of heat insulation materials and discloses a wall heat insulation composite material and a production process thereof, wherein the heat insulation composite material comprises polyether polyol, binary isocyanate, a branched flame retardant cross-linking agent, a catalyst, a physical foaming agent, a chemical foaming agent and an inorganic filler, wherein the branched flame retardant cross-linking agent contains rich organic silicon and phenyl phosphate structures, and is used as a cross-linking agent to enter a polyurethane molecular chain to form a polyurethane foam heat insulation material precursor containing a phosphorus-silicon synergistic flame retardant in the structure.
Description
Technical Field
The invention relates to the technical field of heat insulation materials, in particular to a wall heat insulation composite material and a production process thereof.
Background
In modern buildings, heat insulation materials are often required to be used for heat insulation treatment of building outer walls, so that energy exchange between the indoor and the outdoor is blocked, and further, a heat insulation effect is achieved. At present, the wall heat-insulating material is mainly divided into an organic heat-insulating material and an inorganic heat-insulating material, wherein the inorganic heat-insulating material is mainly foam asbestos heat-insulating material, and the foam asbestos heat-insulating material has high water absorption rate, is waterproof and easy to be damp and is gradually eliminated by the market. The organic heat-insulating material is mainly prepared by taking high polymer materials such as polystyrene, polyurethane, phenolic resin and the like as base materials through a foaming process, and the high polymer foam heat-insulating material has lower heat conductivity coefficient, so that the high polymer foam heat-insulating material can show higher heat-insulating effect, but has extremely poor flame retardant property, is extremely easy to burn when encountering fire, and in recent years, the high-rise building has fire disaster, and the rescue difficulty is increased due to the specificity of the high-rise building, so that people have higher requirements on the flame retardant property of the building material, and the traditional high polymer foam heat-insulating material is required to be modified, so that the high polymer foam heat-insulating material is easier to popularize and use in the market.
The Chinese patent application No. CN202210134254.7 discloses a rock wool-polyurethane composite flame-retardant heat-insulating material, a preparation method and application thereof, wherein the heat-insulating material is subjected to flame retardant modification by adding compounded expanded graphite and phosphoric acid flame retardant into a polyurethane base material, and the flame retardant property of the heat-insulating material can be effectively improved, but materials with different phases are mutually mixed in a physical addition mode, and phase separation can be generated due to the problem of interface incompatibility, so that the mechanical properties and other aspects of the heat-insulating material are weakened, and therefore, the polymer heat-insulating base material is subjected to filling modification in a simple physical addition mode is avoided.
Disclosure of Invention
The invention aims to provide a wall heat-insulating composite material and a production process thereof, which solve the problem of poor flame retardant property of polyurethane foam heat-insulating materials.
The aim of the invention can be achieved by the following technical scheme:
a wall thermal insulation composite material comprises the following raw materials in parts by weight: 40-60 parts of polyether polyol, 20-35 parts of binary isocyanate, 2-5 parts of branched flame retardant cross-linking agent, 1-3 parts of catalyst, 2-4 parts of physical foaming agent, 0.4-1 part of chemical foaming agent and 1-4 parts of inorganic filler;
the preparation method of the branched flame retardant cross-linking agent comprises the following steps:
the first step: dissolving diphenyl chlorophosphate and 1, 3-diglycidyl ether glycerol in N, N-dimethylformamide, adding an acid binding agent, uniformly mixing, introducing nitrogen for protection, raising the temperature of the system to 70-85 ℃, stirring for 4-8 hours, removing nitrogen, pouring the materials into methanol for precipitation, separating the precipitate, and washing and drying to obtain an intermediate;
and a second step of: adding the intermediate and diphenyl silicon glycol into N, N-dimethylformamide, stirring uniformly, introducing nitrogen for protection, placing the system in a temperature condition of 120-135 ℃ for stirring for 12-18 hours, filtering and separating a solid sample after the reaction is finished, and washing and vacuum drying to obtain the branched flame retardant cross-linking agent.
According to the technical scheme, under the action of an acid binding agent, a P-C l bond in a diphenyl chlorophosphate structure can react with a hydroxyl group in a 1, 3-diglycidyl ether glycerin structure to obtain a phenyl phosphate intermediate containing two equivalents of epoxy groups, and under the high-temperature condition, the epoxy groups in the phenyl phosphate intermediate structure can undergo a ring-opening addition reaction with S i-OH in a diphenyl silicon glycol structure and gradually polymerize to obtain a branched flame-retardant cross-linking agent, wherein the branched flame-retardant cross-linking agent not only contains abundant organosilicon and phenyl phosphate structures, but also contains a large number of active hydroxyl groups generated by the ring-opening reaction.
Further, the polyether polyol has a number average molecular weight of 400 to 500 and a hydroxyl value of 350 to 500mg KOH/g.
Further, the diisocyanate is any one of toluene-2, 4-diisocyanate, diphenylmethane diisocyanate or dicyclohexylmethane diisocyanate.
Further, the catalyst is any one of dibutyl tin dilaurate, stannous octoate or dibutyl tin diacetate.
Further, the physical foaming agent is any one of cyclopentane or n-hexane.
Further, the chemical foaming agent is any one of azodicarbonamide or water.
Further, the inorganic filler is any one of carbon fiber and calcium carbonate.
Further, in the first step, the acid binding agent is triethylamine.
Further, in the first step, the molar ratio of the diphenyl chlorophosphate to the 1, 3-diglycidyl ether glycerin is 1:1; in the second step, the molar ratio of the intermediate to the diphenyl silicon glycol is 1:1.
A production process of a wall heat-insulating composite material comprises the following production steps:
step one: mixing polyether polyol, diisocyanate and a catalyst in parts by weight, placing the mixture in a temperature environment of 50-60 ℃, and stirring the mixture for reaction for 1-2 hours to obtain a pre-reaction material (1);
step two: adding the branched flame retardant cross-linking agent in parts by weight into the pre-reaction material (1) for mixing, and continuously stirring for 30-60min to obtain a pre-reaction material (2);
step three: adding physical foaming agent, chemical foaming agent and inorganic filler in parts by weight into the pre-reaction material (2), stirring and mixing to form a uniform material, injecting the material into a mold, foaming for 20-40min at 50-60 ℃, then placing the material into a normal temperature environment for curing for 1-2h, and finally placing the material into a temperature of 70-80 ℃ for curing for 2-4h to obtain the wall heat insulation composite material.
According to the technical scheme, polyether polyol and binary isocyanate are used for reaction to prepare the pre-reaction material (1) with the end group of isocyanate groups, and the branched flame-retardant cross-linking agent structure contains active hydroxyl groups, so that the pre-reaction material (2) with a branched cross-linked network structure can be obtained by reacting with the isocyanate groups of the end group of the pre-reaction material (1), and then foaming, curing and solidifying are carried out to obtain the wall thermal insulation composite material.
The invention has the beneficial effects that:
(1) According to the invention, the branched flame retardant cross-linking agent with rich organic silicon and phenyl phosphate structures and active hydroxyl groups is prepared, and then is introduced into polyurethane molecular chains in a chemical connection mode, so that the prepared polyurethane molecular chains contain silicon-phosphorus synergistic composite flame retardants, after foaming, the prepared polyurethane foaming heat-insulating material contains rich composite flame retardants, when the heat-insulating material burns, phosphorus elements can be burnt to generate oxygen acids of phosphorus, and the catalysis effect of the oxygen acids of phosphorus can be utilized to quickly catalyze the surface of the heat-insulating composite material to form a compact carbon layer, so that the combustion is difficult to continue, meanwhile, the silicon elements can be combined with the carbon layer in a sediment form after being burnt, so that the density of the carbon layer is higher, the strength of the carbon layer is enhanced, the thermal insulation effect of the carbon layer is better, and a good flame-retardant effect is realized. Meanwhile, the precipitation of the flame retardant can be avoided in a chemical grafting mode, and a long-acting flame retardant effect is achieved.
(2) According to the invention, the branched flame-retardant cross-linking agent is added in the polyurethane preparation process, so that the cross-linking density of polyurethane molecular chains can be effectively improved, the structure of the polyurethane foam heat-insulation composite material has higher density, the mechanical strength of the heat-insulation composite material can be effectively enhanced, and meanwhile, the heat-insulation composite material can show lower heat conductivity coefficient due to the improvement of the density, so that a more excellent heat-insulation effect is generated.
Of course, it is not necessary for any one product to practice the invention to achieve all of the advantages set forth above at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an infrared spectrum of a branched flame retardant cross-linking agent prepared in example 1 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A wall thermal insulation composite material comprises the following raw materials in parts by weight: 40 parts of polyether polyol, 10 parts of toluene-2, 4-diisocyanate, 2 parts of branched flame retardant cross-linking agent, 1 part of catalyst dibutyl tin dilaurate, 2 parts of physical foaming agent cyclopentane, 0.4 part of chemical foaming agent azodicarbonamide and 1 part of inorganic filler carbon fiber;
the production method of the wall heat insulation material comprises the following steps:
step one: mixing polyether polyol, toluene-2, 4-diisocyanate and dibutyltin dilaurate serving as a catalyst in parts by weight, placing the mixture in a temperature environment of 50 ℃, and stirring the mixture for reaction for 1h to obtain a pre-reaction material (1), wherein the number average molecular weight of the polyether polyol is 440, and the hydroxyl value is 390mg KOH/g;
step two: adding the branched flame retardant cross-linking agent in parts by weight into the pre-reaction material (1) for mixing, and continuously stirring for 30 min to obtain a pre-reaction material (2);
step three: adding the physical foaming agent cyclopentane, the chemical foaming agent azodicarbonamide and the inorganic filler carbon fiber in parts by weight into the pre-reaction material (2), stirring and mixing to form a uniform material, injecting the material into a mold, foaming the material in a temperature environment of 50 ℃ for 20 min, then placing the material in a normal temperature environment for curing for 1h, and finally placing the material at a temperature of 70 ℃ for curing for 2h to obtain the wall heat-insulating composite material.
Wherein the preparation method of the branched flame retardant cross-linking agent comprises the following steps:
the first step: dissolving 2.5g of diphenyl chlorophosphate and 1.9g of 1, 3-diglycidyl ether glycerol in N, N-dimethylformamide, adding 0.5mL of triethylamine, uniformly mixing, introducing nitrogen for protection, raising the temperature of the system to 75 ℃, stirring for 6 hours, removing nitrogen, pouring the materials into methanol for precipitation, separating the precipitate, and obtaining an intermediate through washing and drying processes;
and a second step of: adding 1.8g of intermediate and 0.9g of diphenyl silicon glycol into N, N-dimethylformamide, stirring uniformly, introducing nitrogen for protection, placing the system in a temperature condition of 130 ℃ for stirring for 16 hours, filtering and separating a solid sample after the reaction is finished, and washing and vacuum drying to obtain the branched flame retardant cross-linking agent.
The branched flame retardant cross-linking agent is tested by using a Tensor27 type Fourier transform infrared spectrometer, and the scanning range is 4000-500 cm -1 The test results are shown in FIG. 1, and the branched flame retardant cross-linking agent is 3408cm as shown in FIG. 1 -1 The absorption peak of the hydroxyl group appears at 3071cm -1 The unsaturated carbon-hydrogen bond stretching vibration peak of benzene ring appears at 1780-2000 cm -1 The frequency multiplication peak of the bending vibration outside the unsaturated carbon-hydrogen bond surface of the benzene ring appears at 1602cm -1 The characteristic peak of S i-Ph (benzene ring) appears at 1319cm -1 The absorption peak of P=O bond appears at 1050-1120 cm -1 There appears an absorption peak of S i-O bond.
Example 2
A wall thermal insulation composite material comprises the following raw materials in parts by weight: 50 parts of polyether polyol, 30 parts of diphenylmethane diisocyanate, 4 parts of branched flame retardant cross-linking agent, 2 parts of catalyst stannous octoate, 3 parts of physical foaming agent n-hexane, 0.5 part of chemical foaming agent water and 2 parts of inorganic filler calcium carbonate;
the production method of the wall heat insulation material comprises the following steps:
step one: mixing polyether polyol, diphenylmethane diisocyanate and stannous octoate serving as catalysts in parts by weight, placing the mixture in a temperature environment of 55 ℃, and stirring the mixture for reaction for 1 hour to obtain a pre-reaction material (1), wherein the number average molecular weight of the polyether polyol is 440, and the hydroxyl value is 390mg KOH/g;
step two: adding the branched flame retardant cross-linking agent in parts by weight into the pre-reaction material (1) for mixing, and continuously stirring for 40min to obtain a pre-reaction material (2);
step three: adding the physical foaming agent n-hexane, the chemical foaming agent water and the inorganic filler calcium carbonate into the pre-reaction material (2), stirring and mixing to form a uniform material, injecting the material into a mold, foaming for 30 min at the temperature of 55 ℃, then placing the material into a normal temperature environment for curing for 1h, and finally placing the material at the temperature of 75 ℃ for curing for 3h to obtain the wall heat-insulating composite material.
Wherein the branched flame retardant cross linking agent was prepared in the same manner as in example 1.
Example 3
A wall thermal insulation composite material comprises the following raw materials in parts by weight: 60 parts of polyether polyol, 35 parts of dicyclohexylmethane diisocyanate, 5 parts of branched flame retardant cross-linking agent, 3 parts of catalyst dibutyltin diacetate, 4 parts of physical foaming agent cyclopentane, 1 part of chemical foaming agent azodicarbonamide and 4 parts of inorganic filler carbon fiber;
the production method of the wall heat insulation material comprises the following steps:
step one: mixing polyether polyol, dicyclohexylmethane diisocyanate and dibutyltin diacetate serving as a catalyst in parts by weight, placing in a temperature environment of 60 ℃, and stirring for 2 hours to obtain a pre-reaction material (1), wherein the number average molecular weight of the polyether polyol is 440, and the hydroxyl value is 390mg KOH/g;
step two: adding the branched flame retardant cross-linking agent in parts by weight into the pre-reaction material (1) for mixing, and continuously stirring for 60min to obtain a pre-reaction material (2);
step three: adding the physical foaming agent cyclopentane, the chemical foaming agent azodicarbonamide and the inorganic filler carbon fiber in parts by weight into the pre-reaction material (2), stirring and mixing to form a uniform material, injecting the material into a mold, foaming 40min in a temperature environment of 60 ℃, then placing the material into a normal temperature environment for curing for 2 hours, and finally placing the material into a temperature of 80 ℃ for curing for 4 hours to obtain the wall heat-insulating composite material.
Wherein the branched flame retardant cross linking agent was prepared in the same manner as in example 1.
Comparative example 1
A wall thermal insulation composite material comprises the following raw materials in parts by weight: 50 parts of polyether polyol, 30 parts of diphenylmethane diisocyanate, 4 parts of chain extender 1, 4-butanediol, 2 parts of stannous octoate catalyst, 3 parts of n-hexane as a physical foaming agent, 0.5 part of water as a chemical foaming agent and 2 parts of calcium carbonate as an inorganic filler;
the production method of the wall heat insulation material comprises the following steps:
step one: mixing polyether polyol, diphenylmethane diisocyanate and stannous octoate serving as catalysts in parts by weight, placing the mixture in a temperature environment of 55 ℃, and stirring the mixture for reaction for 1 hour to obtain a pre-reaction material (1), wherein the number average molecular weight of the polyether polyol is 440, and the hydroxyl value is 390mg KOH/g;
step two: adding 1, 4-butanediol serving as a chain extender in parts by weight into the pre-reaction material (1), mixing, and continuously stirring for 40min to obtain a pre-reaction material (2);
step three: adding the physical foaming agent n-hexane, the chemical foaming agent water and the inorganic filler calcium carbonate into the pre-reaction material (2), stirring and mixing to form a uniform material, injecting the material into a mold, foaming for 30 min at the temperature of 55 ℃, then placing the material into a normal temperature environment for curing for 1h, and finally placing the material at the temperature of 75 ℃ for curing for 3h to obtain the wall heat-insulating composite material.
Performance detection
Cutting the heat-insulating composite material prepared in the embodiment 1-3 into test samples meeting the test specification, and testing the tensile strength of the samples by referring to the national standard GB/T9641-1988; testing the compressive strength of the sample by referring to the national standard GB/T8813-2020; the thermal conductivity of the sample is tested by referring to the national standard GB/T3399-1982; the limiting oxygen index of the sample is tested by referring to the national standard GB/T2406.2-2008, and the test results are shown in the following table:
| example 1 | Example 2 | Example 3 | Comparative example 1 | |
| Tensile Strength/MPa | 1.6 | 1.9 | 1.8 | 0.9 |
| Compressive Strength/kPa | 183.1 | 187.5 | 185.2 | 131.7 |
| Thermal conductivity/W/m.k | 0.0248 | 0.0236 | 0.0241 | 0.0273 |
| Limiting oxygen index/% | 32.3 | 33.0 | 32.8 | 20.6 |
As can be seen from the above table, the thermal insulation composite materials prepared in the examples 1-3 of the invention have good mechanical properties, flame retardant properties and thermal insulation properties. In the preparation process of the heat-insulating composite material prepared in the comparative example 1, the conventional 1, 4-butanediol chain extender is used for preparing polyurethane, and the branched flame retardant cross-linking agent is not used as a raw material, so that the prepared polyurethane foaming precursor has low cross-linking density, and the structure does not contain phosphorus-silicon flame retardant elements, so that the mechanical property, the heat-insulating effect and the flame retardant property are poor.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (10)
1. The wall heat-insulating composite material is characterized by comprising the following raw materials in parts by weight: 40-60 parts of polyether polyol, 20-35 parts of binary isocyanate, 2-5 parts of branched flame retardant cross-linking agent, 1-3 parts of catalyst, 2-4 parts of physical foaming agent, 0.4-1 part of chemical foaming agent and 1-4 parts of inorganic filler;
the preparation method of the branched flame retardant cross-linking agent comprises the following steps:
the first step: dissolving diphenyl chlorophosphate and 1, 3-diglycidyl ether glycerol in N, N-dimethylformamide, adding an acid binding agent, uniformly mixing, introducing nitrogen for protection, raising the temperature of the system to 70-85 ℃, stirring for 4-8 hours, removing nitrogen, pouring the materials into methanol for precipitation, separating the precipitate, and washing and drying to obtain an intermediate;
and a second step of: adding the intermediate and diphenyl silicon glycol into N, N-dimethylformamide, stirring uniformly, introducing nitrogen for protection, placing the system in a temperature condition of 120-135 ℃ for stirring for 12-18 hours, filtering and separating a solid sample after the reaction is finished, and washing and vacuum drying to obtain the branched flame retardant cross-linking agent.
2. The wall insulation composite of claim 1, wherein the polyether polyol has a number average molecular weight of 400-500 and a hydroxyl number of 350-500mgKOH/g.
3. The wall insulation composite of claim 1, wherein the diisocyanate is any one of toluene-2, 4-diisocyanate, diphenylmethane diisocyanate or dicyclohexylmethane diisocyanate.
4. The wall insulation composite of claim 1, wherein the catalyst is any one of dibutyltin dilaurate, stannous octoate, and dibutyltin diacetate.
5. The wall insulation composite of claim 1, wherein the physical blowing agent is any one of cyclopentane or n-hexane.
6. The wall insulation composite of claim 1, wherein the chemical blowing agent is either azodicarbonamide or water.
7. The wall insulation composite of claim 1, wherein the inorganic filler is any one of carbon fiber or calcium carbonate.
8. The wall insulation composite of claim 1, wherein in the first step, the acid binding agent is triethylamine.
9. The wall insulation composite of claim 1, wherein in the first step, the molar ratio of diphenyl chlorophosphate to 1, 3-diglycidyl ether glycerin is 1:1; in the second step, the molar ratio of the intermediate to the diphenyl silicon glycol is 1:1.
10. A process for producing a wall insulation composite according to claim 1, comprising the following steps:
step one: mixing polyether polyol, diisocyanate and a catalyst in parts by weight, placing the mixture in a temperature environment of 50-60 ℃, and stirring the mixture for reaction for 1-2 hours to obtain a pre-reaction material (1);
step two: adding the branched flame retardant cross-linking agent in parts by weight into the pre-reaction material (1) for mixing, and continuously stirring for 30-60min to obtain a pre-reaction material (2);
step three: adding physical foaming agent, chemical foaming agent and inorganic filler in parts by weight into the pre-reaction material (2), stirring and mixing to form a uniform material, injecting the material into a mold, foaming for 20-40min at 50-60 ℃, then placing the material into a normal temperature environment for curing for 1-2h, and finally placing the material into a temperature of 70-80 ℃ for curing for 2-4h to obtain the wall heat insulation composite material.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2023106877016 | 2023-06-12 | ||
| CN202310687701 | 2023-06-12 |
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| CN116655877A true CN116655877A (en) | 2023-08-29 |
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| CN202310731281.7A Withdrawn CN116655877A (en) | 2023-06-12 | 2023-06-20 | Wall heat-insulating composite material and production process thereof |
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