CN114479007A - Structural flame-retardant polyurethane heat-insulation foam material for refrigeration house terrace - Google Patents
Structural flame-retardant polyurethane heat-insulation foam material for refrigeration house terrace Download PDFInfo
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- CN114479007A CN114479007A CN202210109285.7A CN202210109285A CN114479007A CN 114479007 A CN114479007 A CN 114479007A CN 202210109285 A CN202210109285 A CN 202210109285A CN 114479007 A CN114479007 A CN 114479007A
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- foam material
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- insulation foam
- flame retardant
- polyol
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000003063 flame retardant Substances 0.000 title claims abstract description 57
- 239000000463 material Substances 0.000 title claims abstract description 36
- 239000004814 polyurethane Substances 0.000 title claims abstract description 31
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 31
- 239000002937 thermal insulation foam Substances 0.000 title claims abstract description 20
- 238000005057 refrigeration Methods 0.000 title abstract description 15
- 229920005862 polyol Polymers 0.000 claims abstract description 56
- 150000003077 polyols Chemical class 0.000 claims abstract description 55
- 239000012948 isocyanate Substances 0.000 claims abstract description 39
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 39
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 35
- 229920000570 polyether Polymers 0.000 claims abstract description 35
- 239000006260 foam Substances 0.000 claims description 31
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 19
- 239000000600 sorbitol Substances 0.000 claims description 19
- 239000003999 initiator Substances 0.000 claims description 18
- 239000004088 foaming agent Substances 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 10
- 239000012752 auxiliary agent Substances 0.000 claims description 9
- 229920002545 silicone oil Polymers 0.000 claims description 9
- 239000004094 surface-active agent Substances 0.000 claims description 9
- 238000006757 chemical reactions by type Methods 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 8
- 230000000379 polymerizing effect Effects 0.000 claims description 7
- 150000001412 amines Chemical class 0.000 claims description 6
- MRVZORUPSXTRHD-UHFFFAOYSA-N bis(hydroxymethyl)phosphorylmethanol Chemical compound OCP(=O)(CO)CO MRVZORUPSXTRHD-UHFFFAOYSA-N 0.000 claims description 6
- 239000006261 foam material Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- -1 polydimethylsiloxane Polymers 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- FRCHKSNAZZFGCA-UHFFFAOYSA-N 1,1-dichloro-1-fluoroethane Chemical group CC(F)(Cl)Cl FRCHKSNAZZFGCA-UHFFFAOYSA-N 0.000 claims description 3
- DKRWGRQBYLWNKR-UHFFFAOYSA-N OC(O)(O)[PH2]=O Chemical compound OC(O)(O)[PH2]=O DKRWGRQBYLWNKR-UHFFFAOYSA-N 0.000 claims description 3
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 3
- 238000001308 synthesis method Methods 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims description 3
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical group C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 24
- 238000007906 compression Methods 0.000 abstract description 4
- 230000006835 compression Effects 0.000 abstract description 4
- 238000005507 spraying Methods 0.000 abstract description 3
- 229920005830 Polyurethane Foam Polymers 0.000 description 11
- 230000007613 environmental effect Effects 0.000 description 11
- 239000011496 polyurethane foam Substances 0.000 description 11
- 238000013461 design Methods 0.000 description 7
- 239000000654 additive Substances 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 5
- 238000004132 cross linking Methods 0.000 description 5
- HHDUMDVQUCBCEY-UHFFFAOYSA-N 4-[10,15,20-tris(4-carboxyphenyl)-21,23-dihydroporphyrin-5-yl]benzoic acid Chemical compound OC(=O)c1ccc(cc1)-c1c2ccc(n2)c(-c2ccc(cc2)C(O)=O)c2ccc([nH]2)c(-c2ccc(cc2)C(O)=O)c2ccc(n2)c(-c2ccc(cc2)C(O)=O)c2ccc1[nH]2 HHDUMDVQUCBCEY-UHFFFAOYSA-N 0.000 description 4
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 4
- 229930006000 Sucrose Natural products 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 125000003636 chemical group Chemical group 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 229960004793 sucrose Drugs 0.000 description 4
- 150000005846 sugar alcohols Polymers 0.000 description 4
- 125000001951 carbamoylamino group Chemical group C(N)(=O)N* 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 239000012774 insulation material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000004014 plasticizer Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000005720 sucrose Substances 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N anhydrous diethylene glycol Natural products OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 150000004985 diamines Chemical group 0.000 description 2
- 230000009970 fire resistant effect Effects 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229920000582 polyisocyanurate Polymers 0.000 description 2
- 239000011495 polyisocyanurate Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- KVMPUXDNESXNOH-UHFFFAOYSA-N tris(1-chloropropan-2-yl) phosphate Chemical compound ClCC(C)OP(=O)(OC(C)CCl)OC(C)CCl KVMPUXDNESXNOH-UHFFFAOYSA-N 0.000 description 2
- 239000004604 Blowing Agent Substances 0.000 description 1
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 229920002396 Polyurea Polymers 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- PZBFGYYEXUXCOF-UHFFFAOYSA-N TCEP Chemical compound OC(=O)CCP(CCC(O)=O)CCC(O)=O PZBFGYYEXUXCOF-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000004620 low density foam Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000011513 prestressed concrete Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—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
- C08G18/776—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur phosphorus
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3225—Polyamines
- C08G18/3237—Polyamines aromatic
- C08G18/3243—Polyamines aromatic containing two or more aromatic rings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4829—Polyethers containing at least three hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6681—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6685—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
-
- 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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/143—Halogen containing compounds
- C08J9/144—Halogen containing compounds containing carbon, halogen and hydrogen only
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/08—Polyurethanes from polyethers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- 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
- C08J2203/02—CO2-releasing, e.g. NaHCO3 and citric acid
-
- 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
- C08J2203/142—Halogenated saturated hydrocarbons, e.g. H3C-CF3
-
- 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
- C08J2203/18—Binary blends of expanding agents
- C08J2203/184—Binary blends of expanding agents of chemical foaming agent and physical blowing agent, e.g. azodicarbonamide and fluorocarbon
-
- 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
- C08J2375/08—Polyurethanes from polyethers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- General Chemical & Material Sciences (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention relates to a structural flame-retardant polyurethane heat-insulation foam material for a refrigeration house terrace, belonging to the technical field of polyurethane materials. The invention makesThe polyurethane thermal insulation foam material is produced by using the combined polyether polyol and the 3-functionality modified isocyanate according to the weight ratio of 100 (100-150). The density after sprayed by high-pressure inorganic spraying equipment is 45-50 kg/m3The compression strength is more than or equal to 500kPa, the flame retardance is grade B1, the odor grade (80 ℃) is less than or equal to 3.5, and the fog test is less than or equal to 5 mg.
Description
Technical Field
The invention relates to a structural flame-retardant polyurethane heat-insulation foam material for a refrigeration house terrace, belonging to the technical field of polyurethane materials.
Background
In the traditional design and construction process of a refrigeration house, the bearing design of the ground generally requires more than or equal to 350KPa, and some of the bearing design even achieves more than or equal to 500KPa, in order to meet the requirement of cargo carrying walking of transport vehicles such as forklifts and the like, the ground which can preserve heat and bear load is mostly paved layer by adopting polystyrene extruded sheets (XPS). The heat insulation performance of the XPS plate is poorer than that of polyurethane foam, a gap formed by layer-by-layer paving has a cold bridge hidden danger, a certain gap correction coefficient is required to assist, and meanwhile, the existence of the gap is beneficial to the permeation of small molecular water vapor, so that the phenomenon of 'cold running' is frequently caused. It is no problem that the polyurethane foam reaches 350KPa or more and even 500KPa or more, but the density is generally at least 50kg/m when the polyurethane foam reaches 350KPa or more3Above, the general density of the product is 65kg/m when the product reaches more than or equal to 500KPa3In the above, the B1 grade flame retardant foam needs to be added with a large amount of physical flame retardant, such as TCPP, TCEP and the like, so it is more difficult to achieve the same strength, and the density is generally increased by 20% or more, which greatly increases the cost of the refrigerator.
Patent CN104672420, a high-strength polyurethane rigid foam, a preparation method and application thereof, discloses a technology that the compressive strength reaches 200KPa, and does not meet the requirement that the bearing design is more than or equal to 350 KPa.
CN107033327B patent of "a high compression resistance polyurethane combined material for freezer floor and its preparation method", adopts phthalic anhydride, aromatic dibasic acid polyol PS3152 and ethylenediamine polyol BH403 to match, effectively combines PIR structure and PUR structure, utilizes highly symmetrical and high content rigid benzene ring in its structure to reach higher foam mechanical strength, and in its example, the product density is reached to 46.8kg/m3The highest compressive strength is 403KPa, the requirement of the load-bearing design is more than or equal to 350KPa is met, but the requirement of the distance more than or equal to 500KPa is far.
In the aspect of flame retardance, the large space, the high wall surface and the few safe exits are the building characteristics of a refrigeration house, and the large space causes the toxic gas of fire smoke to spread rapidly after a fire disaster occurs, so that the fire-resistant wall is very unfavorable for workers in dense smoke to escape. Meanwhile, the large span of the structure space of the refrigeration house determines that the collapse of the building can be caused once a fire disaster occurs, and the large-span structure needs corresponding building components for supporting, so that the selection of a steel structure and a prestressed concrete slab or a light component becomes a preferred object. And the fire-resistant collapse limit of the steel structure is only 8 minutes, so that the whole collapse of the building is easily caused.
Polyurethane foams are formed by reacting an isocyanate with a polyol component and are inherently flammable if a flame retardant is not added. For many years, significant fire related to polyurethane foams such as Jilin Baoyuan Feng, shou Guang, Beijing great-rise cold storage and the like is continuous, and GB50016-2014 'fire prevention code for building design' stipulates that the internal and external heat insulation systems of the building are not suitable for adopting B2-grade heat insulation materials, and strictly forbidden for adopting B3-grade heat insulation materials. The B1 grade flame-retardant rigid polyurethane foam material for walls requires an oxygen index of more than or equal to 30 percent, so that a large amount of flame retardant is required to be added into the foam (the foam strength is reduced due to the plasticizing effect), and the strength of the rigid polyurethane foam material for B1 grade is much poorer than that of rigid polyurethane foam materials for B3 and B2 grade due to the use of flame-retardant polyester or polyether polyol (the strength is reduced compared with that of conventional polyol).
The more flame retardant is added, the poorer the environmental protection performance of the foam material such as taste, TVOC, fog and the like. Because the physically added flame retardant is one of the most environmentally contributing factors to the flame retardant foam. Most of the cold storages are food storages, and the requirement on environmental protection is higher than that of the common environment.
Therefore, in the current stage, the ground of the refrigeration house in the construction of the refrigeration house urgently needs a polyurethane heat-insulating terrace foam material which has low density foam, can achieve B1-grade flame retardance, has the compressive strength meeting the design requirement of the refrigeration house (more than or equal to 500KPa) and has excellent environmental protection performance.
Disclosure of Invention
The invention aims to solve the problems of the prior artIt is sufficient to produce polyurethane insulation foams using a combination polyether polyol and a 3-functionality modified isocyanate. The density after sprayed by high-pressure inorganic spraying equipment is 45-50 kg/m3The compression strength is more than or equal to 500kPa, the flame retardant grade B1 is realized, the odor grade (80 ℃) is less than or equal to 3.5, and the fog test is less than or equal to 5mg (no physical additive flame retardant diffuses to the environment).
The invention discloses a structural flame-retardant refrigeration house terrace polyurethane thermal insulation foam material, which is formed by polymerizing an isocyanate component and a polyol component, and is characterized in that the mass ratio of the isocyanate component to the polyol component is (100-:
the 3-functionality modified isocyanate had a P content of 4.7%, an N content of 12.7%, and an NCO% content of 19%.
The polyol component includes: polyether glycol taking sorbitol with the functionality of 6 as an initiator, 4' -bis-sec-butylaminodiphenylmethane, a chemical foaming agent, a reactive auxiliary agent and a physical foaming agent. Wherein the polyether polyol having sorbitol as an initiator with a functionality of 6 is present in an amount of 45 to 55% by weight based on the total weight of the polyol component; 4,4' -bis-sec-butylaminodiphenylmethane accounts for 25-35% of the total weight of the polyol component; the chemical foaming agent accounts for 0.2 to 1 percent of the total weight of the polyol component; the reaction type auxiliary agent accounts for 4.5-6.5% of the total weight of the polyol component, and the physical foaming agent accounts for 10-20% of the total weight of the polyol component;
the polyether polyol taking sorbitol with the functionality of 6 as an initiator is high-activity polyether taking sorbitol as an initiator and propylene oxide as a polymerization monomer;
the polyether polyol taking the sorbitol with the functionality of 6 as an initiator adopts YD6482 of the chemical group Limited in Asia east of Hebei province or NJ-6207 of the new material development Limited in Shinewanning province;
the 4,4' -bis-sec-butylaminodiphenylmethane is a liquid secondary diamine;
the chemical foaming agent is mainly water, can effectively participate in the reaction of isocyanate, and improves the hard chain component in the foam;
the auxiliary agent comprises a foam surfactant and a reactive catalyst, wherein the surfactant accounts for 1-3% of the total weight of the polyhydric alcohol, and the reactive catalyst accounts for 3-5% of the total weight of the polyhydric alcohol;
the foam surfactant is silicone oil, the silicone oil is polydimethylsiloxane, and the silicone oil can adopt L6950 of a new material group in a My diagram;
the non-emission amine catalyst is mainly Dabco T and the like which win special chemistry (Shanghai) Limited company;
the physical foaming agent is monofluorodichloroethane.
The invention also aims to provide a structural flame-retardant synthesis method of the polyurethane heat-insulating foam material for the floor of the refrigeration house, which is formed by polymerizing an isocyanate component and a polyol component, wherein the isocyanate component is 3-functionality modified isocyanate, and is characterized in that the 3-functionality modified isocyanate is obtained by polymerizing trihydroxymethyl phosphine oxide and TDI, and the reaction equation is as follows:
the synthesis process of the 3-functionality modified isocyanate comprises the following steps:
1) heating the reaction kettle to 48-52 ℃;
2) according to the following tris (hydroxymethyl) phosphine oxide (available from Hubei Xingsheng chemical group Ltd.): adding all TDI with the molar ratio of (4-8) first, and then adding all the tris (hydroxymethyl) phosphine oxide at a constant speed;
3) heating the reaction kettle to 78-82 ℃, and then reacting for 1.9-2.2 h;
4) removing unreacted excessive TDI by using a thin film evaporator;
5) then cooling the reaction kettle to 48-52 ℃, taking out of the kettle and packaging to obtain a product with the P content of 4.7%, the N content of 12.7% and the NCO% content of 19%.
Hair brushObviously in order to make freezer terrace polyurethane insulation foam material use the inorganic spraying equipment of high pressure after spouting, satisfy simultaneously: the density is 45-50 kg/m3The compression strength is more than or equal to 500kPa, the flame retardant grade B1 is flame retardant grade B1, the odor grade (80 ℃) is less than or equal to 3.5, and the fog test is less than or equal to 5mg (no physical additive flame retardant diffuses to the environment), and the following technical schemes are adopted simultaneously and used simultaneously to achieve the aim of the invention:
1. according to the invention, sorbitol polyether polyol with functionality of about 6 and 4,4' -bis-sec-butyl amino diphenylmethane are effectively matched in the combined polyether polyol component to react with 3-functionality modified isocyanate, so that the requirement of high compressive strength of the polyurethane thermal insulation foam material for the refrigeration house floor is met. The main reasons are as follows:
the polyether polyol which takes sorbitol as an initiator and has the functionality of about 6 can generate enough crosslinking degree and rigidity when reacting with isocyanate, so that the polyurethane foam has higher compressive strength and dimensional stability and has the following 2 obvious advantages compared with the conventional high-functionality polyether which takes sucrose as an initiator and also meets the functionality of 6: 1. the self functionality of the sorbitol is 6, the functionality of the sorbitol polyether with the functionality of about 6 is uniform, and the foam crosslinking density is high; the 6-functionality-degree sucrose polyether functionality is 67% of 8-functionality-degree sucrose, 33% of 2-functionality-degree water, ethylene glycol and diethylene glycol compound initiator, 33% of 2-functionality-degree can only play a role in chain extension and does not play a role in crosslinking, and the foam crosslinking density is small; 2. the sorbitol polyether polyol with the functionality of about 6 has lower viscosity which is lower by more than 30 percent on average compared with the conventional high-functionality polyether with the functionality of 6 and taking cane sugar as an initiator, the lower viscosity is beneficial to mixing and conveying raw materials, and particularly, the viscosity can be reduced without adding a small amount of plasticizer and flame retardant;
the invention adopts 4,4' -bis-sec-butyl aminodiphenylmethane in the combined polyether polyol component, the equivalent weight (molecular weight/functionality) is 155, and a smaller equivalent weight obtains more ureido group hard segments, compared with carbamate (polyurethane), the hydrogen bonding acting force in the ureido group is much stronger, the intermolecular (namely interchain) interaction acting force in the polyurea structure is much stronger, the phase separation of hard chains such as the ureido group and the polyisocyanurate group and soft segments such as polyether amine is more obvious, the melting temperature of the hard segment region of the polymer is higher than that of the polyurethane structure, and the compressive strength is also higher.
According to the invention, no physical flame retardant is added in the combined polyether polyol component, so that the plasticizing effect caused by the physical flame retardant can be avoided, and the compressive strength of the polyurethane foam is improved.
2. The 3-functionality modified isocyanate is used for replacing the conventional polymeric MDI, the P content of the 3-functionality modified isocyanate is 4.7 percent, and the phosphorus content of the foam obtained by combining polyether polyol in the proportion of (100) 150: 100 is 2.35-2.82 percent, which is equivalent to the phosphorus content obtained by adding 25-30 percent of TCPP into the system, so that the problem of smell increase caused by adding a physical halogen phosphate flame retardant into the system is avoided while a good flame retardant effect is obtained; no additive physical flame retardant and other plasticizer are added in the system, so that a very low fog test value is obtained. The lower the fog test result is, the phenomenon that no physical additive flame retardant diffuses to the environment exists in the thermal insulation foam, and the phenomenon that the flame retardance of the thermal insulation material is reduced along with the change of time does not occur later.
The fact that no physical flame retardant is added is more important to improve the compressive strength of the heat-insulating material, on one hand, the reason is to avoid the plasticizing effect caused by the addition type physical flame retardant; the second reason is that the foam density increase caused by the addition type physical flame retardant is avoided (the foam density is passively increased by about 15% by adding 30% of flame retardant into the combined polyether polyol in the common bi-component raw material 1:1 ratio B1 grade foam);
compared with common polymeric MDI such as Rowa chemical PM200, the functionality of the 3-functionality modified isocyanate is improved by 15.4 percent by the functionality of HUNTSMAN5005 with the average functionality of 2.6, namely, even if the weight of the physical addition flame retardant is not considered, the crosslinking density in the foam is also increased by 15.4 percent, and the compressive strength of the foam can be effectively improved.
3. The structural flame-retardant polyurethane heat-insulating foam material for the terrace of the refrigeration house has lower odor and fog value. The main reasons are as follows:
according to the invention, no physical flame retardant is added into the refrigeration house terrace polyurethane heat-insulating foam bi-component material, so that the problem of smell increase caused by adding a flame retardant into a system is avoided, no additive flame retardant or plasticizer diffuses into the environment in the heat-insulating foam, and the flame retardant property of the heat-insulating material cannot be reduced along with the change of time. Meanwhile, the catalysts used in the invention are all reaction type catalysts, so that the odor value in the foam is greatly reduced.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The structural flame-retardant freezer terrace polyurethane heat preservation foam material of the embodiment is formed by polymerizing an isocyanate component and a polyol component, the mass ratio of the isocyanate component to the polyol component is (100-:
the 3-functionality modified isocyanate had a P content of 4.7%, an N content of 12.7%, and an NCO% content of 19%.
The polyol component includes: polyether glycol taking sorbitol with the functionality of 6 as an initiator, 4' -bis-sec-butylaminodiphenylmethane, a chemical foaming agent, a reactive auxiliary agent and a physical foaming agent. Wherein the polyether polyol having sorbitol as an initiator with a functionality of 6 is present in an amount of 45 to 55% by weight based on the total weight of the polyol component; 4,4' -bis-sec-butylaminodiphenylmethane accounts for 25-35% of the total weight of the polyol component; the chemical foaming agent accounts for 0.2 to 1 percent of the total weight of the polyol component; the reaction type auxiliary agent accounts for 4.5-6.5% of the total weight of the polyol component, and the physical foaming agent accounts for 10-20% of the total weight of the polyol component.
Wherein, the polyether glycol taking sorbitol with the functionality of 6 as an initiator is high-activity polyether taking sorbitol as the initiator and propylene oxide as a polymerization monomer. The polyether polyol taking sorbitol with functionality of 6 as an initiator adopts YD6482 of the chemical group of northeast Asia east of Hebei province or NJ-6207 of the new material development company of Tanshun.
4,4' -bis-sec-butylaminodiphenylmethane is a liquid secondary diamine; the chemical foaming agent is mainly water, can effectively participate in the reaction of isocyanate, and improves the hard chain component in the foam.
The auxiliary agent comprises a foam surfactant and a reaction type catalyst, wherein the surfactant accounts for 1-3% of the total weight of the polyhydric alcohol, and the reaction type catalyst accounts for 3-5% of the total weight of the polyhydric alcohol;
the foam surfactant is silicone oil, the silicone oil is polydimethylsiloxane, and the silicone oil can adopt L6950 of Megashi material group. The catalyst is a non-emission amine catalyst and a potassium metal catalyst, and the non-emission amine catalyst is mainly Dabco T and the like which win special chemistry (Shanghai) Limited company;
the physical blowing agent is monofluorodichloroethane.
The synthesis method of the structural flame-retardant freezer terrace polyurethane thermal insulation foam material of the embodiment is formed by polymerizing an isocyanate component and a polyol component, wherein the isocyanate component is obtained by polymerizing trihydroxymethyl phosphine oxide and TDI, and the reaction equation is as follows:
the synthesis process of the 3-functionality modified isocyanate comprises the following steps:
1) heating the reaction kettle to 48-52 ℃;
2) according to the following tris (hydroxymethyl) phosphine oxide (available from Hubei Xingsheng chemical group Ltd.): adding all TDI with the molar ratio of (4-8) first, and then adding all the tris (hydroxymethyl) phosphine oxide at a constant speed;
3) heating the reaction kettle to 78-82 ℃, and then reacting for 1.9-2.2 h;
4) removing unreacted excessive TDI by using a thin film evaporator;
5) then cooling the reaction kettle to 48-52 ℃, taking out of the kettle and packaging to obtain a product with the P content of 4.7%, the N content of 12.7% and the NCO% content of 19%.
Test examples 1 to 5
The combined polyether polyol formulations of test examples 1-5 were as follows:
using 100 parts of the above-mentioned combination polyether polyol and the total parts of the isocyanate component and the physical flame retardant component of each test example in the following table, a foamed article was produced by mixing and stirring.
The isocyanate component and the additive-type flame retardant component of each test example were:
the flame retardant and environmental protection performance of each test example is tested as follows:
odor rating test criteria: the VDA270:1992,
and (3) fog testing: Q/ZK JS 364-.
In the case of no addition of physical flame retardant, the oxygen index is increased from 19.5% of the flame retardance to 28.2% of the flame retardance, the odor grade (80 ℃) is 3.5 and 3.5 respectively, the change is not large, the pressure resistance is 516kPa and 505kPa respectively, and the purpose of improving the flame retardance of polyurethane foam and avoiding the reduction of the environmental protection index of the flame retardant is achieved by the 3-functionality modified isocyanate.
Compared with the test example 4, the oxygen index is reduced from 28.2% to 27.0%, the odor grade (80 ℃) is increased from 3.5 to 4.5, the fog test is increased from 4.61mg to 59.83mg, and the compressive strength is reduced from 516kPa to 468kPa, thereby illustrating a technical route for improving flame retardance by using 3-functionality modified isocyanate, avoiding the problems brought by using a physical flame retardant TCPP in the aspects of environmental protection and plasticity, and solving the problem that environmental protection indexes such as high flame retardance, low odor and the like are mutually opposite.
In the test examples 2 and 4, under the condition that the weight of the material components is not changed, the oxygen index is reduced from 30.1 percent of flame retardance to 27.0 percent, the odor grade (80 ℃) is increased from 3.5 to 4.5, the fog test is increased from 4.88mg to 59.83mg, and the compressive strength is reduced from 512kPa to 468kPa, further, the technical route of improving the flame retardance by using 3-functionality modified isocyanate is further illustrated, the problem brought by using a physical flame retardant TCPP in the aspects of environmental protection and plasticity is solved, and the problem that environmental protection indexes such as high flame retardance, low odor and the like are mutually opposite is solved.
Experimental example 4 on the basis of the experimental example 3, the physical flame retardant component TCPP is added, all the others are unchanged, the odor grade (80 ℃) is increased to 4.5 from 3.5, the fog test is increased to 59.83mg from 4.45mg, and the compressive strength is reduced to 468kPa from 505kPa, so that the physical flame retardant component TCPP increases the foam flame retardance, seriously influences the environmental protection performance of the material, and has a plasticizing effect on the material.
Test examples 5 to 6
The formulation of the combined polyether polyol of this test example is as follows:
100 parts of the above-mentioned combined polyether polyol and 100 parts of 3-functionality-modified isocyanate component were mixed and stirred to prepare a foamed article.
The flame retardant and environmental performance of each test example is tested and compared with that of test example 1 as follows:
test examples 5 and 6, the ratio of YD6482 to 4,4' -bis-sec-butylaminodiphenylmethane in the white material formulation was changed from 5:3 to 3:5 and 7:1, respectively, with the isocyanate component unchanged, and the compressive strengths thereof were 458kPa and 472kPa, respectively, which were significantly reduced. The reason for this analysis may be due to: when YD6482:4,4' -bis-sec-butylaminodiphenylmethane is about 5:3, the strength of the foam reaches the maximum value, at the ratio, the hard segments in the foam are in a net-shaped crossed continuous phase, the soft segments are converted into a dispersed phase and dispersed in a hard segment network, and the material has reasonable microphase separation degree and hard segment micro-area size, so that the material has higher compressive strength. In the test example 7, the proportion of 4,4' -bis-sec-butylaminodiphenylmethane is too small, the soft segment is a reticular cross continuous phase, the hard segment is converted into a dispersed phase and is dispersed in the soft segment network, and the compressive strength of the foam is not ideal; in test example 6, the proportion of 4,4' -bis-sec-butylaminodiphenylmethane was too large, the average functionality in the combined polyether polyol was low, the foam crosslink density was insufficient, and the foam compressive strength was not satisfactory.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or equivalents thereof. Although the present invention has been described with reference to the specific embodiments, it should be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (9)
1. The structural flame-retardant freezer terrace polyurethane heat preservation foam material is formed by polymerizing an isocyanate component and a polyol component, and is characterized in that the mass ratio of the isocyanate component to the polyol component is (100-:
the polyol component includes: polyether glycol taking sorbitol with the functionality of 6 as an initiator, 4' -bis-sec-butylaminodiphenylmethane, a chemical foaming agent, a reactive auxiliary agent and a physical foaming agent. Wherein the polyether polyol having sorbitol as an initiator with a functionality of 6 is present in an amount of 45 to 55% by weight based on the total weight of the polyol component; 4,4' -bis-sec-butylaminodiphenylmethane accounts for 25-35% of the total weight of the polyol component; the chemical foaming agent accounts for 0.2 to 1 percent of the total weight of the polyol component; the reaction type auxiliary agent accounts for 4.5-6.5% of the total weight of the polyol component, and the physical foaming agent accounts for 10-20% of the total weight of the polyol component.
2. The structural flame retardant freezer floor polyurethane insulation foam material of claim 1, characterized in that the 3 functionality modified isocyanate has a P content of 4.7%, an N content of 12.7%, and an NCO% content of 19%.
3. The structural flame retardant freezer floor polyurethane insulation foam material of claim 1, characterized in that the polyether polyol with sorbitol with functionality of 6 as initiator is a high activity polyether with sorbitol as initiator and propylene oxide as polymerization monomer.
4. The structural flame retardant freezer terrace polyurethane insulation foam material of claim 1, characterized in that the chemical foaming agent is water and the physical foaming agent is monofluorodichloroethane.
5. The structural flame-retardant freezer floor polyurethane thermal insulation foam material as claimed in claim 1, characterized in that the auxiliary agent comprises foam surfactant and reaction type catalyst, the surfactant accounts for 1-3% of the total weight of the polyol, and the reaction type catalyst accounts for 3-5% of the total weight of the polyol.
6. The structural flame retardant freezer floor polyurethane insulation foam material of claim 5, characterized in that the foam surfactant is silicone oil, the silicone oil is polydimethylsiloxane, the silicone oil is L6950 of Michigan advanced materials group.
7. The structural flame retardant freezer terrace polyurethane insulation foam material of claim 5, characterized in that the catalyst is a non-emission amine catalyst; the non-emission amine catalyst is Dabco T which wins special chemistry (Shanghai) limited company.
8. The structural flame-retardant freezer floor polyurethane insulation foam material according to any one of claims 1-7, characterized in that a structural flame-retardant freezer floor polyurethane insulation foam material synthesis method, by isocyanate component and polyol component polymerization to form, isocyanate component is 3 functionality modified isocyanate, its characterized in that the 3 functionality modified isocyanate adopts trihydroxymethyl phosphine oxide and TDI polymerization to obtain, the reaction equation is as follows:
9. the structural flame retardant freezer terrace polyurethane insulation foam material of claim 8, characterized in that the synthesis process of the 3-functionality modified isocyanate is:
1) heating the reaction kettle to 48-52 ℃;
2) according to the following tris (hydroxymethyl) phosphine oxide: adding all TDI with the molar ratio of (4-8) first, and then adding all the tris (hydroxymethyl) phosphine oxide at a constant speed;
3) heating the reaction kettle to 78-82 ℃, and then reacting for 1.9-2.2 h;
4) removing unreacted excessive TDI by using a thin film evaporator;
5) then cooling the reaction kettle to 48-52 ℃, taking out of the kettle and packaging to obtain a product with the P content of 4.7%, the N content of 12.7% and the NCO% content of 19%.
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| SU572465A1 (en) * | 1973-03-19 | 1977-09-15 | Казанский Химико-Технологический Институт Имени С.М.Кирова | Method of preparing tris-(toluilen-2-izocianato-4-carbamoiloxymethyl) of phosphine or its oxide |
| CN102050836A (en) * | 2010-12-20 | 2011-05-11 | 武汉金磷化工科技有限责任公司 | Phosphorus-containing polyisocyanate and preparation method thereof |
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