CN116284665A - High-temperature-resistant polyurethane heat-insulating pipe and preparation method thereof - Google Patents
High-temperature-resistant polyurethane heat-insulating pipe and preparation method thereof Download PDFInfo
- Publication number
- CN116284665A CN116284665A CN202310352923.2A CN202310352923A CN116284665A CN 116284665 A CN116284665 A CN 116284665A CN 202310352923 A CN202310352923 A CN 202310352923A CN 116284665 A CN116284665 A CN 116284665A
- Authority
- CN
- China
- Prior art keywords
- temperature
- resistant polyurethane
- insulating pipe
- polyurethane heat
- stirring
- 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.)
- Granted
Links
- 239000004814 polyurethane Substances 0.000 title claims abstract description 31
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000003063 flame retardant Substances 0.000 claims abstract description 42
- 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 39
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000178 monomer Substances 0.000 claims abstract description 38
- 239000000463 material Substances 0.000 claims abstract description 28
- 238000005187 foaming Methods 0.000 claims abstract description 24
- 239000012763 reinforcing filler Substances 0.000 claims abstract description 24
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000005058 Isophorone diisocyanate Substances 0.000 claims abstract description 11
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 60
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 60
- 238000002156 mixing Methods 0.000 claims description 44
- 238000003756 stirring Methods 0.000 claims description 38
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000008367 deionised water Substances 0.000 claims description 29
- 229910021641 deionized water Inorganic materials 0.000 claims description 29
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 28
- 238000001914 filtration Methods 0.000 claims description 24
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 23
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 22
- 239000000706 filtrate Substances 0.000 claims description 21
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 239000004368 Modified starch Substances 0.000 claims description 18
- 229920000881 Modified starch Polymers 0.000 claims description 18
- 235000019426 modified starch Nutrition 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 17
- -1 polyethylene Polymers 0.000 claims description 17
- 239000011246 composite particle Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000000758 substrate Substances 0.000 claims description 14
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 14
- 229920002472 Starch Polymers 0.000 claims description 12
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 claims description 12
- 239000008107 starch Substances 0.000 claims description 12
- 235000019698 starch Nutrition 0.000 claims description 12
- 239000010455 vermiculite Substances 0.000 claims description 12
- 229910052902 vermiculite Inorganic materials 0.000 claims description 12
- 235000019354 vermiculite Nutrition 0.000 claims description 12
- VNIXZWLYQDIGNU-UHFFFAOYSA-N 5-nitrobenzene-1,3-diol Chemical compound OC1=CC(O)=CC([N+]([O-])=O)=C1 VNIXZWLYQDIGNU-UHFFFAOYSA-N 0.000 claims description 11
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 11
- 239000003054 catalyst Substances 0.000 claims description 11
- UHUUYVZLXJHWDV-UHFFFAOYSA-N trimethyl(methylsilyloxy)silane Chemical compound C[SiH2]O[Si](C)(C)C UHUUYVZLXJHWDV-UHFFFAOYSA-N 0.000 claims description 11
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 10
- ASOKPJOREAFHNY-UHFFFAOYSA-N 1-Hydroxybenzotriazole Chemical compound C1=CC=C2N(O)N=NC2=C1 ASOKPJOREAFHNY-UHFFFAOYSA-N 0.000 claims description 10
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- BHUIUXNAPJIDOG-UHFFFAOYSA-N Piperonol Chemical compound OCC1=CC=C2OCOC2=C1 BHUIUXNAPJIDOG-UHFFFAOYSA-N 0.000 claims description 10
- 239000004698 Polyethylene Substances 0.000 claims description 10
- 229910000831 Steel Inorganic materials 0.000 claims description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 10
- 239000011609 ammonium molybdate Substances 0.000 claims description 10
- 229940010552 ammonium molybdate Drugs 0.000 claims description 10
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 10
- 239000004202 carbamide Substances 0.000 claims description 10
- 229920000573 polyethylene Polymers 0.000 claims description 10
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 10
- 239000010959 steel Substances 0.000 claims description 10
- GODZNYBQGNSJJN-UHFFFAOYSA-N 1-aminoethane-1,2-diol Chemical compound NC(O)CO GODZNYBQGNSJJN-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 8
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 229960000583 acetic acid Drugs 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000008096 xylene Substances 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 239000011810 insulating material Substances 0.000 abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 3
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 abstract description 2
- 125000004432 carbon atom Chemical group C* 0.000 abstract description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 abstract description 2
- 125000004437 phosphorous atom Chemical group 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 238000004321 preservation Methods 0.000 description 9
- 239000004205 dimethyl polysiloxane Substances 0.000 description 8
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 8
- 238000002347 injection Methods 0.000 description 8
- 239000007924 injection Substances 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000012774 insulation material Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 4
- 238000009413 insulation Methods 0.000 description 3
- 239000000779 smoke Substances 0.000 description 3
- 238000007792 addition Methods 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
- 229960005235 piperonyl butoxide Drugs 0.000 description 2
- 125000004591 piperonyl group Chemical group C(C1=CC=2OCOC2C=C1)* 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
Classifications
-
- 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
- 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
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3878—Low-molecular-weight compounds having heteroatoms other than oxygen having phosphorus
- C08G18/3891—Low-molecular-weight compounds having heteroatoms other than oxygen having phosphorus having sulfur in addition to 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
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
-
- 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
- C08G18/4833—Polyethers containing oxyethylene units
-
- 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
- C08G18/61—Polysiloxanes
-
- 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
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2101/00—Manufacture of cellular products
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2255—Oxides; Hydroxides of metals of molybdenum
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a high-temperature-resistant polyurethane heat-insulating pipe and a preparation method thereof, wherein a foaming material is prepared in the process of preparing a multilayer heat-insulating pipe, a flame-retardant monomer, PEG2000, dihydroxypolydimethylsiloxane 2000, dimethylbenzene and a reinforcing filler are firstly mixed to obtain a mixture, the mixture is mixed with isophorone diisocyanate to prepare the foaming material, polyurethane molecular chains formed by the foaming material contain a large number of organosilicon chain segments, the high-temperature-resistant effect of polyurethane can be well improved, the flame-retardant monomer takes organophosphorus as a main structure, the monomer molecules contain a plurality of nitrogen atoms which can cooperate with phosphorus atoms to form a stable carbon layer, and simultaneously, silicon atoms in the molecules can generate a carbon silicon compound with carbon atoms to further densify the carbon layer, so that the preparation-treated heat-insulating material has a certain flame-retardant effect.
Description
Technical Field
The invention relates to the technical field of heat preservation pipe preparation, in particular to a high-temperature-resistant polyurethane heat preservation pipe and a preparation method thereof.
Background
The heat preservation pipe is short for heat insulation pipelines, is used for conveying liquid, gas and other mediums, and is used for heat preservation in heat insulation engineering of pipelines such as petroleum, chemical industry, aerospace, hot spring, military, central heating, central air conditioner, municipal administration and the like, and the heat preservation is realized by filling heat preservation materials between the outer pipe body and the inner pipe body, so that the heat dissipation speed is reduced. However, because the pipe fitting is circular structure, the thermal insulation material that fills finally is annular structure, and massive stereoplasm thermal insulation material compares with soft thermal insulation material, the structure is more stable, but the thermal conductivity is higher, and thermal insulation material is mostly foaming material, meet the phenomenon that open flame can appear quick burning, partial thermal insulation material can increase flame retardant efficiency through adding inorganic fire retardant, because the material is in high temperature state for a long time in the heat preservation process, moisture that contains in the inorganic fire retardant can volatilize in advance, can't normally fire-retardant when leading to burning, reduce thermal insulation factor of safety.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant polyurethane heat-insulating pipe and a preparation method thereof, which solve the problem that the polyurethane heat-insulating material is inflammable at the present stage, and simultaneously solve the problem that the flame-retardant effect of the polyurethane heat-insulating material is reduced in a high-temperature environment for a long time.
The aim of the invention can be achieved by the following technical scheme:
the preparation method of the high-temperature-resistant polyurethane heat-insulating pipe specifically comprises the following steps:
step S1: adding a flame-retardant monomer, PEG2000, dihydroxypolydimethylsiloxane 2000, dimethylbenzene and reinforcing filler into a stirring kettle, and stirring for 2-4 hours under the condition of 600-800 r/min to prepare a mixture;
step S2: adding isophorone diisocyanate into the mixture, and stirring for 10-15s under the condition that the rotating speed is 800-1000 r/min to prepare a foaming material;
step S3: and (3) sleeving a polyethylene outer sleeve outside the working steel pipe, injecting a foaming material into a gap between the working steel pipe and the polyethylene outer sleeve under the conditions of a material injection speed of 200L/min and a material injection pressure of 10-15MPa, foaming for 1-1.5h at 50-60 ℃, heating to 90-95 ℃, and preserving heat for 10-15h to obtain the high-temperature-resistant polyurethane heat-preserving pipe.
Further, the molar ratio of the flame retardant monomer to the PEG2000 to the dihydroxypolydimethylsiloxane 2000 in the step S1 is 3:1:1, and the consumption of the reinforcing filler is 10-15% of the sum of the mass of the flame retardant monomer to the mass of the PEG2000 to the mass of the dihydroxypolydimethylsiloxane 2000.
Further, the molar ratio of isophorone diisocyanate to the flame retardant monomer, PEG2000, and dihydroxy polydimethylsiloxane 2000 in step S2 is 6:3:1:1.
Further, the flame-retardant monomer is prepared by the following steps:
step A1: dissolving cyanuric chloride in acetone, adding sodium hydroxide and piperonyl alcohol, stirring at a rotating speed of 150-200 r/min and a temperature of 0-5 ℃ for reaction for 6-8 hours to obtain an intermediate 1, uniformly mixing the intermediate 1, a Kanst catalyst, dimethylbenzene and toluene, introducing nitrogen for protection, stirring at a rotating speed of 200-300 r/min and a temperature of 60-65 ℃ and adding tetramethyl disiloxane for reaction for 40-50 hours to obtain an intermediate 2;
the reaction process is as follows:
step A2: mixing phosphorus trichloride, 2-dimethylolpropionic acid and triethylamine, introducing nitrogen for protection, reacting for 1-1.5 hours at the rotation speed of 150-200 r/min and the temperature of 80-90 ℃, heating to 135-145 ℃, reacting for 7-9 hours, heating to 155-165 ℃, reacting for 1-1.5 hours to obtain an intermediate 3, uniformly mixing the intermediate 3, 5-nitro-1, 3-benzenediol, potassium carbonate and dimethylbenzene, and reacting for 6-8 hours at the rotation speed of 300-500 r/min and the temperature of 0-5 ℃ to obtain an intermediate 4;
the reaction process is as follows:
step A3: uniformly mixing the intermediate 4, tin and concentrated hydrochloric acid, reacting at the rotation speed of 150-200 r/min and the temperature of 80-85 ℃ for 50-60 min, adding concentrated ammonia water to adjust the pH value to 8-8.5, filtering to remove filter residues, adding glacial acetic acid to adjust the pH value to 4.5, and filtering again to remove the filtrate to obtain an intermediate 5;
the reaction process is as follows:
step A4: uniformly mixing the intermediate 2, the intermediate 5, triethylamine and tetrahydrofuran, reacting for 8-10 hours at the rotation speed of 200-300 r/min and the temperature of 80-90 ℃ to obtain an intermediate 6, uniformly mixing the intermediate 6, the glycol amine, the 1-hydroxybenzotriazole and the tetrahydrofuran, reacting for 3-5 hours at the rotation speed of 150-200 r/min and the temperature of 20-25 ℃, distilling to remove the tetrahydrofuran, dispersing a substrate in deionized water, and filtering to remove filtrate to obtain the modified monomer.
The reaction process is as follows:
further, the molar ratio of cyanuric chloride, sodium hydroxide and piperonyl alcohol in the step A1 is 1:1:1, and the dosage ratio of the intermediate 1, the Karster catalyst, the xylene, the toluene and the tetramethyl disiloxane is 100mmo l:0.39g:20mL:20mL:50mo l.
Further, the molar ratio of phosphorus trichloride, 2-dimethylolpropionic acid and triethylamine in the step A2 is 1:1:1.1, and the molar ratio of the intermediate 3, 5-nitro-1, 3-benzenediol and potassium carbonate is 2:1:2.1.
Further, the dosage ratio of the intermediate 4 to the tin to the concentrated hydrochloric acid in the step A3 is 4g:9g:19mL, and the mass fraction of the concentrated hydrochloric acid is 36%.
Further, the molar ratio of intermediate 2, intermediate 5 and triethylamine described in step A4 was 1:4:4.1, and the molar ratio of intermediate 6, glycol amine and 1-hydroxybenzotriazole was 1:4:4.2.
Further, the reinforcing filler is prepared by the following steps:
step B1: mixing vermiculite, zinc nitrate hexahydrate, aluminum nitrate nonahydrate, urea and deionized water, carrying out hydrothermal reaction for 10-15h at 145-155 ℃, filtering to remove filtrate, washing a substrate with deionized water and ethanol in sequence, calcining for 5-7h at 300-350 ℃ to obtain load particles, uniformly mixing starch, KH560, DMF and sodium hydroxide, stirring for 8-10h at 200-300 r/min and 60-70 ℃, adding acetone, filtering to remove filtrate, drying the substrate to obtain modified starch,
step B2: uniformly dispersing the load particles and modified starch in acetone, adding deionized water, stirring for 8-10 hours at the rotation speed of 150-200 r/min and the temperature of 50-60 ℃ and the pH value of 9-10 to obtain composite particles, uniformly mixing the composite particles, ammonium molybdate and deionized water, stirring and adding molybdenum trioxide at the rotation speed of 150-200 r/min and the temperature of 90-95 ℃, reacting for 2-3 hours, and drying at the high temperature of 110-115 ℃ for 10-15 hours to obtain the reinforcing filler.
Further, the dosage ratio of vermiculite, zinc nitrate hexahydrate, aluminum nitrate nonahydrate, urea and deionized water in step B1 was 10g:30mmo l:10mmo l:15mmo l:150mL, and the dosage ratio of starch, KH560, DMF and sodium hydroxide was 5.5g:7.3g:50mL:0.2g.
Further, the mass ratio of the supported particles to the modified starch in the step B2 is 1:5, and the mass ratio of the composite particles, ammonium molybdate and molybdenum trioxide is 3.12:6.09:5.16.
The invention has the beneficial effects that: the invention prepares a flame-retardant monomer and a reinforcing filler in the process of preparing a high-temperature-resistant polyurethane insulating pipe, the flame-retardant monomer takes cyanuric chloride and piperonyl as raw materials, one chlorine atom site on cyanuric chloride reacts with hydroxyl on piperonyl through temperature control to prepare an intermediate 1, then the intermediate 1 reacts with tetramethyl disiloxane under the action of a Kanster catalyst to prepare an intermediate 2, phosphorus trichloride reacts with 2, 2-dimethylolpropionic acid to prepare an intermediate 3, the intermediate 3 reacts with 5-nitro-1, 3-benzenediol to prepare an intermediate 4, tin is used for reducing the intermediate 4 to prepare an intermediate 5, the intermediate 2 reacts with the intermediate 5 to prepare an intermediate 6, finally the intermediate 6 is dehydrated and condensed with ethylene glycol amine to prepare the flame-retardant monomer, the foaming material takes the flame-retardant monomer, PEG2000, dihydroxy polydimethyl siloxane 2000 and isophorone diisocyanate as raw materials, the polyurethane molecular chain formed by the raw materials contains a large amount of organic silicon chain segments, the high temperature resistant effect of polyurethane can be well improved, the flame retardant monomer takes organic phosphorus as a main structure, the monomer molecule contains a plurality of nitrogen atoms which can cooperate with phosphorus atoms to form a stable carbon layer, meanwhile, silicon atoms in the molecule can generate carbon silicon compounds with carbon atoms, and further the carbon layer is densified, so that the prepared heat insulation material has a certain flame retardant effect, the reinforced filler takes vermiculite as the raw material, a layer of hydrotalcite is coated on the surface of the vermiculite, starch and KH560 react with epoxy groups on KH560 under alkaline conditions, siloxane is grafted on the starch to prepare modified starch, the modified starch is used for treating load particles, so that the siloxane on the modified starch is hydrolyzed, and then the surface of the load particles is coated, and then molybdenum trioxide is loaded on the surface of the composite particles, so that the reinforcing filler is prepared, when the heat-insulating material burns, the reinforcing filler can generate a large amount of water, so that the burning problem is reduced, the flame-retardant effect is further improved by matching with the flame-retardant monomer, the smoke generated during burning is reduced, and the flame-retardant effect cannot be reduced in a high-temperature environment.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments 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
The preparation method of the high-temperature-resistant polyurethane heat-insulating pipe specifically comprises the following steps:
step S1: adding a flame-retardant monomer, PEG2000, dihydroxypolydimethylsiloxane 2000, dimethylbenzene and reinforcing filler into a stirring kettle, and stirring for 2 hours under the condition of 600 r/min to prepare a mixture;
step S2: adding isophorone diisocyanate into the mixture, and stirring for 10s under the condition that the rotating speed is 800 r/min to prepare a foaming material;
step S3: and (3) sleeving a polyethylene outer sleeve outside the working steel pipe, injecting a foaming material into a gap between the working steel pipe and the polyethylene outer sleeve under the conditions of a material injection speed of 200L/min and a material injection pressure of 10MPa, foaming for 1h at 50 ℃, heating to 90 ℃, and preserving heat for 10h to obtain the high-temperature-resistant polyurethane heat-preserving pipe.
The mol ratio of the flame-retardant monomer to the PEG2000 to the dihydroxyl polydimethylsiloxane 2000 in the step S1 is 3:1:1, and the consumption of the reinforcing filler is 10-15% of the sum of the mass of the flame-retardant monomer to the mass of the PEG2000 to the mass of the dihydroxyl polydimethylsiloxane 2000.
The molar ratio of isophorone diisocyanate to the flame-retardant monomer, PEG2000 and dihydroxypolydimethylsiloxane 2000 in the step S2 is 6:3:1:1.
The flame-retardant monomer is prepared by the following steps:
step A1: dissolving cyanuric chloride in acetone, adding sodium hydroxide and piperonyl alcohol, stirring at a rotation speed of 150 r/min and a temperature of 0 ℃ for reaction for 6 hours to obtain an intermediate 1, uniformly mixing the intermediate 1, a Karster catalyst, dimethylbenzene and methylbenzene, introducing nitrogen for protection, stirring at a rotation speed of 200 r/min and a temperature of 60 ℃ and adding tetramethyl disiloxane for reaction for 40 hours to obtain an intermediate 2;
step A2: mixing phosphorus trichloride, 2-dimethylolpropionic acid and triethylamine, introducing nitrogen for protection, reacting for 1h under the conditions of the rotating speed of 150 r/min and the temperature of 80 ℃, heating to 135 ℃, reacting for 7h, heating to 155 ℃, reacting for 1h to obtain an intermediate 3, uniformly mixing the intermediate 3, 5-nitro-1, 3-benzenediol, potassium carbonate and dimethylbenzene, and reacting for 6h under the conditions of the rotating speed of 300 r/min and the temperature of 0 ℃ to obtain an intermediate 4;
step A3: uniformly mixing the intermediate 4, tin and concentrated hydrochloric acid, reacting for 50 min at the rotation speed of 150-200 r/min and the temperature of 80 ℃, adding concentrated ammonia water to adjust the pH value to 8, filtering to remove filter residues, adding glacial acetic acid to the filtrate to adjust the pH value to 4, and filtering again to remove the filtrate to obtain an intermediate 5;
step A4: uniformly mixing the intermediate 2, the intermediate 5, triethylamine and tetrahydrofuran, reacting for 8 hours at the rotation speed of 200 r/min and the temperature of 80 ℃ to obtain an intermediate 6, uniformly mixing the intermediate 6, the glycol amine, the 1-hydroxybenzotriazole and the tetrahydrofuran, reacting for 3 hours at the rotation speed of 150 r/min and the temperature of 20 ℃, distilling to remove the tetrahydrofuran, dispersing a substrate in deionized water, and filtering to remove filtrate to obtain the modified monomer.
The molar ratio of cyanuric chloride, sodium hydroxide and piperonyl alcohol in the step A1 is 1:1:1, and the dosage ratio of the intermediate 1, the Karster catalyst, the dimethylbenzene, the methylbenzene and the tetramethyl disiloxane is 100mmo l:0.39g:20mL:20mL:50mo l.
The mol ratio of the phosphorus oxychloride, the 2, 2-dimethylolpropionic acid and the triethylamine in the step A2 is 1:1:1.1, and the mol ratio of the intermediate 3, 5-nitro-1, 3-benzenediol and the potassium carbonate is 2:1:2.1.
The dosage ratio of the intermediate 4 to the tin to the concentrated hydrochloric acid in the step A3 is 4g:9g:19mL, and the mass fraction of the concentrated hydrochloric acid is 36%.
The molar ratio of the intermediate 2, the intermediate 5 and the triethylamine in the step A4 is 1:4:4.1, and the molar ratio of the intermediate 6, the glycol amine and the 1-hydroxybenzotriazole is 1:4:4.2.
The reinforcing filler is prepared by the following steps:
step B1: mixing vermiculite, zinc nitrate hexahydrate, aluminum nitrate nonahydrate, urea and deionized water, carrying out hydrothermal reaction for 10 hours at 145 ℃, filtering to remove filtrate, washing a substrate with deionized water and ethanol in sequence, calcining for 5 hours at 300 ℃ to obtain load particles, uniformly mixing starch, KH560, DMF and sodium hydroxide, stirring for 8 hours at 200 r/min and 60 ℃, adding acetone, filtering to remove filtrate, drying the substrate to obtain modified starch,
step B2: uniformly dispersing the load particles and modified starch in acetone, adding deionized water, stirring for 8 hours at the rotation speed of 150 r/min and the temperature of 50 ℃ and the pH value of 9 to obtain composite particles, uniformly mixing the composite particles, ammonium molybdate and deionized water, stirring and adding molybdenum trioxide at the rotation speed of 150 r/min and the temperature of 90 ℃, reacting for 2 hours, and drying at the high temperature of 110 ℃ for 10 hours to obtain the reinforcing filler.
The dosage ratio of vermiculite, zinc nitrate hexahydrate, aluminum nitrate nonahydrate, urea and deionized water in the step B1 is 10g:30mmo l:10mmo l:15mmo l:150mL, and the dosage ratio of starch, KH560, DMF and sodium hydroxide is 5.5g:7.3g:50mL:0.2g.
The mass ratio of the load particles to the modified starch in the step B2 is 1:5, and the mass ratio of the composite particles to the ammonium molybdate to the molybdenum trioxide is 3.12:6.09:5.16.
Example 2
The preparation method of the high-temperature-resistant polyurethane heat-insulating pipe specifically comprises the following steps:
step S1: adding a flame-retardant monomer, PEG2000, dihydroxypolydimethylsiloxane 2000, dimethylbenzene and reinforcing filler into a stirring kettle, and stirring for 3 hours under the condition of 600 r/min to prepare a mixture;
step S2: adding isophorone diisocyanate into the mixture, and stirring for 15s under the condition that the rotating speed is 1000 r/min to prepare a foaming material;
step S3: and (3) sleeving a polyethylene outer sleeve outside the working steel pipe, injecting a foaming material into a gap between the working steel pipe and the polyethylene outer sleeve under the conditions of a material injection speed of 200L/min and a material injection pressure of 10MPa, foaming for 1.5h at 55 ℃, heating to 90 ℃, and preserving heat for 15h to obtain the high-temperature-resistant polyurethane heat-preserving pipe.
The mol ratio of the flame-retardant monomer to the PEG2000 to the dihydroxyl polydimethylsiloxane 2000 in the step S1 is 3:1:1, and the consumption of the reinforcing filler is 10-15% of the sum of the mass of the flame-retardant monomer to the mass of the PEG2000 to the mass of the dihydroxyl polydimethylsiloxane 2000.
The molar ratio of isophorone diisocyanate to the flame-retardant monomer, PEG2000 and dihydroxypolydimethylsiloxane 2000 in the step S2 is 6:3:1:1.
The flame-retardant monomer is prepared by the following steps:
step A1: dissolving cyanuric chloride in acetone, adding sodium hydroxide and piperonyl alcohol, stirring at a rotation speed of 150 r/min and a temperature of 5 ℃ for reaction for 7 hours to obtain an intermediate 1, uniformly mixing the intermediate 1, a Karster catalyst, dimethylbenzene and methylbenzene, introducing nitrogen for protection, stirring at a rotation speed of 200 r/min and a temperature of 65 ℃ and adding tetramethyl disiloxane for reaction for 45 hours to obtain an intermediate 2;
step A2: mixing phosphorus trichloride, 2-dimethylolpropionic acid and triethylamine, introducing nitrogen for protection, reacting for 1.5 hours at the rotation speed of 150 r/min and the temperature of 85 ℃, heating to 140 ℃, reacting for 8 hours, heating to 160 ℃, reacting for 1.5 hours to obtain an intermediate 3, uniformly mixing the intermediate 3, 5-nitro-1, 3-benzenediol, potassium carbonate and dimethylbenzene, and reacting for 7 hours at the rotation speed of 300 r/min and the temperature of 3 ℃ to obtain an intermediate 4;
step A3: uniformly mixing the intermediate 4, tin and concentrated hydrochloric acid, reacting for 55 min at the rotation speed of 150 r/min and the temperature of 85 ℃, adding concentrated ammonia water to adjust the pH value to 8.5, filtering to remove filter residues, adding glacial acetic acid to adjust the pH value to 4, and filtering again to remove the filtrate to obtain an intermediate 5;
step A4: uniformly mixing the intermediate 2, the intermediate 5, triethylamine and tetrahydrofuran, reacting for 9 hours at the temperature of 85 ℃ at the rotation speed of 200 r/min to obtain an intermediate 6, uniformly mixing the intermediate 6, the glycol amine, the 1-hydroxybenzotriazole and the tetrahydrofuran, reacting for 4 hours at the temperature of 20 ℃ at the rotation speed of 200 r/min, distilling to remove the tetrahydrofuran, dispersing a substrate in deionized water, and filtering to remove filtrate to obtain the modified monomer.
The molar ratio of cyanuric chloride, sodium hydroxide and piperonyl alcohol in the step A1 is 1:1:1, and the dosage ratio of the intermediate 1, the Karster catalyst, the dimethylbenzene, the methylbenzene and the tetramethyl disiloxane is 100mmo l:0.39g:20mL:20mL:50mo l.
The mol ratio of the phosphorus oxychloride, the 2, 2-dimethylolpropionic acid and the triethylamine in the step A2 is 1:1:1.1, and the mol ratio of the intermediate 3, 5-nitro-1, 3-benzenediol and the potassium carbonate is 2:1:2.1.
The dosage ratio of the intermediate 4 to the tin to the concentrated hydrochloric acid in the step A3 is 4g:9g:19mL, and the mass fraction of the concentrated hydrochloric acid is 36%.
The molar ratio of the intermediate 2, the intermediate 5 and the triethylamine in the step A4 is 1:4:4.1, and the molar ratio of the intermediate 6, the glycol amine and the 1-hydroxybenzotriazole is 1:4:4.2.
The reinforcing filler is prepared by the following steps:
step B1: mixing vermiculite, zinc nitrate hexahydrate, aluminum nitrate nonahydrate, urea and deionized water, carrying out hydrothermal reaction for 15 hours at 150 ℃, filtering to remove filtrate, washing a substrate with deionized water and ethanol in sequence, calcining for 5 hours at 350 ℃ to obtain load particles, uniformly mixing starch, KH560, DMF and sodium hydroxide, stirring at 300 r/min and 65 ℃ for 9 hours, adding acetone, filtering to remove filtrate, drying the substrate to obtain modified starch,
step B2: uniformly dispersing the load particles and modified starch in acetone, adding deionized water, stirring for 9 hours at the rotation speed of 150 r/min and the temperature of 55 ℃ and the pH value of 10 to obtain composite particles, uniformly mixing the composite particles, ammonium molybdate and deionized water, stirring and adding molybdenum trioxide at the rotation speed of 150 r/min and the temperature of 95 ℃, reacting for 2 hours, and drying at the high temperature of 110 ℃ for 15 hours to obtain the reinforcing filler.
The dosage ratio of vermiculite, zinc nitrate hexahydrate, aluminum nitrate nonahydrate, urea and deionized water in the step B1 is 10g:30mmo l:10mmo l:15mmo l:150mL, and the dosage ratio of starch, KH560, DMF and sodium hydroxide is 5.5g:7.3g:50mL:0.2g.
The mass ratio of the load particles to the modified starch in the step B2 is 1:5, and the mass ratio of the composite particles to the ammonium molybdate to the molybdenum trioxide is 3.12:6.09:5.16.
Example 3
The preparation method of the high-temperature-resistant polyurethane heat-insulating pipe specifically comprises the following steps:
step S1: adding a flame-retardant monomer, PEG2000, dihydroxypolydimethylsiloxane 2000, dimethylbenzene and reinforcing filler into a stirring kettle, and stirring for 4 hours under the condition of 800 r/min to prepare a mixture;
step S2: adding isophorone diisocyanate into the mixture, and stirring for 15s under the condition that the rotating speed is 1000 r/min to prepare a foaming material;
step S3: and (3) sleeving a polyethylene outer sleeve outside the working steel pipe, injecting a foaming material into a gap between the working steel pipe and the polyethylene outer sleeve under the conditions of a material injection speed of 200L/min and a material injection pressure of 15MPa, foaming for 1.5h at 60 ℃, heating to 95 ℃, and preserving heat for 15h to obtain the high-temperature-resistant polyurethane heat-preserving pipe.
The mol ratio of the flame-retardant monomer to the PEG2000 to the dihydroxyl polydimethylsiloxane 2000 in the step S1 is 3:1:1, and the consumption of the reinforcing filler is 10-15% of the sum of the mass of the flame-retardant monomer to the mass of the PEG2000 to the mass of the dihydroxyl polydimethylsiloxane 2000.
The molar ratio of isophorone diisocyanate to the flame-retardant monomer, PEG2000 and dihydroxypolydimethylsiloxane 2000 in the step S2 is 6:3:1:1.
The flame-retardant monomer is prepared by the following steps:
step A1: dissolving cyanuric chloride in acetone, adding sodium hydroxide and piperonyl alcohol, stirring at the rotation speed of 200 r/min and the temperature of 5 ℃ for reaction for 8 hours to obtain an intermediate 1, uniformly mixing the intermediate 1, a Karster catalyst, dimethylbenzene and methylbenzene, introducing nitrogen for protection, stirring at the rotation speed of 300 r/min and the temperature of 65 ℃ and adding tetramethyl disiloxane for reaction for 50 hours to obtain an intermediate 2;
step A2: mixing phosphorus trichloride, 2-dimethylolpropionic acid and triethylamine, introducing nitrogen for protection, reacting for 1.5 hours at the rotation speed of 200 r/min and the temperature of 90 ℃, heating to 145 ℃, reacting for 9 hours, heating to 165 ℃, reacting for 1.5 hours to obtain an intermediate 3, uniformly mixing the intermediate 3, 5-nitro-1, 3-dihydroxybenzene, potassium carbonate and dimethylbenzene, and reacting for 8 hours at the rotation speed of 500 r/min and the temperature of 5 ℃ to obtain an intermediate 4;
step A3: uniformly mixing the intermediate 4, tin and concentrated hydrochloric acid, reacting for 60 min at the rotation speed of 200 r/min and the temperature of 85 ℃, adding concentrated ammonia water to adjust the pH value to 8.5, filtering to remove filter residues, adding glacial acetic acid to adjust the pH value to 4.5, and filtering again to remove the filtrate to obtain an intermediate 5;
step A4: uniformly mixing the intermediate 2, the intermediate 5, triethylamine and tetrahydrofuran, reacting for 10 hours at the rotation speed of 300 r/min and the temperature of 90 ℃ to obtain an intermediate 6, uniformly mixing the intermediate 6, the glycol amine, the 1-hydroxybenzotriazole and the tetrahydrofuran, reacting for 5 hours at the rotation speed of 200 r/min and the temperature of 25 ℃, distilling to remove the tetrahydrofuran, dispersing a substrate in deionized water, and filtering to remove filtrate to obtain the modified monomer.
The molar ratio of cyanuric chloride, sodium hydroxide and piperonyl alcohol in the step A1 is 1:1:1, and the dosage ratio of the intermediate 1, the Karster catalyst, the dimethylbenzene, the methylbenzene and the tetramethyl disiloxane is 100mmo l:0.39g:20mL:20mL:50mo l.
The mol ratio of the phosphorus oxychloride, the 2, 2-dimethylolpropionic acid and the triethylamine in the step A2 is 1:1:1.1, and the mol ratio of the intermediate 3, 5-nitro-1, 3-benzenediol and the potassium carbonate is 2:1:2.1.
The dosage ratio of the intermediate 4 to the tin to the concentrated hydrochloric acid in the step A3 is 4g:9g:19mL, and the mass fraction of the concentrated hydrochloric acid is 36%.
The molar ratio of the intermediate 2, the intermediate 5 and the triethylamine in the step A4 is 1:4:4.1, and the molar ratio of the intermediate 6, the glycol amine and the 1-hydroxybenzotriazole is 1:4:4.2.
The reinforcing filler is prepared by the following steps:
step B1: mixing vermiculite, zinc nitrate hexahydrate, aluminum nitrate nonahydrate, urea and deionized water, carrying out hydrothermal reaction for 15 hours at 155 ℃, filtering to remove filtrate, washing a substrate with deionized water and ethanol in sequence, calcining for 7 hours at 350 ℃ to obtain load particles, uniformly mixing starch, KH560, DMF and sodium hydroxide, stirring for 10 hours at 300 r/min and 70 ℃, adding acetone, filtering to remove filtrate, drying the substrate to obtain modified starch,
step B2: uniformly dispersing the load particles and modified starch in acetone, adding deionized water, stirring for 10 hours at the rotation speed of 200 r/min and the temperature of 60 ℃ and the pH value of 10 to obtain composite particles, uniformly mixing the composite particles, ammonium molybdate and deionized water, stirring and adding molybdenum trioxide at the rotation speed of 200 r/min and the temperature of 95 ℃, reacting for 3 hours, and drying at the high temperature of 115 ℃ for 15 hours to obtain the reinforcing filler.
The dosage ratio of vermiculite, zinc nitrate hexahydrate, aluminum nitrate nonahydrate, urea and deionized water in the step B1 is 10g:30mmo l:10mmo l:15mmo l:150mL, and the dosage ratio of starch, KH560, DMF and sodium hydroxide is 5.5g:7.3g:50mL:0.2g.
The mass ratio of the load particles to the modified starch in the step B2 is 1:5, and the mass ratio of the composite particles to the ammonium molybdate to the molybdenum trioxide is 3.12:6.09:5.16.
Comparative example 1
This comparative example uses talc instead of reinforcing filler as compared to example 1, the rest of the procedure being the same.
Comparative example 2
This comparative example was compared to example 1 without the addition of reinforcing filler, the remainder of the procedure being identical.
Comparative example 3
This comparative example uses 1, 4-butanediol instead of the flame retardant monomer as compared to example 1, the rest of the procedure being the same.
Foaming the foaming materials prepared in examples 1-3 and comparative examples 1-3, cutting the foaming materials into samples with the thickness of 130mm multiplied by 15mm multiplied by 3mm, detecting flame retardance according to the standard of GB/T2408-2008, detecting smoke density according to the standard of I SO5659, and after the foaming materials are subjected to heat preservation at 200 ℃ for 10 hours, detecting flame retardance and smoke density again, wherein the results are shown in the following table;
the table shows that the invention has good flame-retardant and smoke-suppressing effects, and the flame-retardant and smoke-suppressing effects are not greatly reduced after the heat preservation at high temperature.
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. A preparation method of a high-temperature-resistant polyurethane heat-insulating pipe is characterized by comprising the following steps of: the method specifically comprises the following steps:
step S1: mixing a flame-retardant monomer, PEG2000, dihydroxypolydimethylsiloxane 2000, dimethylbenzene and a reinforcing filler to prepare a mixture;
step S2: adding isophorone diisocyanate into the mixture, and stirring to obtain a foaming material;
step S3: and (3) sleeving a polyethylene outer sleeve outside the working steel pipe, injecting foaming materials into a gap between the working steel pipe and the polyethylene outer sleeve, and performing foaming treatment to obtain the high-temperature-resistant polyurethane heat-insulating pipe.
2. The method for preparing the high-temperature-resistant polyurethane heat-insulating pipe according to claim 1, which is characterized in that: the flame-retardant monomer is prepared by the following steps:
step A1: dissolving cyanuric chloride in acetone, adding sodium hydroxide and piperonyl alcohol, stirring for reaction to obtain an intermediate 1, mixing and stirring the intermediate 1, a Kanst catalyst, dimethylbenzene and methylbenzene, adding tetramethyl disiloxane, and reacting to obtain an intermediate 2;
step A2: mixing phosphorus trichloride, 2-dimethylolpropionic acid and triethylamine for reaction, heating for reaction to obtain an intermediate 3, and mixing intermediate 3, 5-nitro-1, 3-benzenediol, potassium carbonate and xylene for reaction to obtain an intermediate 4;
step A3: mixing intermediate 4, tin and concentrated hydrochloric acid for reaction, adding concentrated ammonia water, filtering to remove filter residues, adding glacial acetic acid into the filtrate, and filtering again to remove the filtrate to obtain intermediate 5;
step A4: intermediate 2, intermediate 5, triethylamine and tetrahydrofuran are mixed for reaction to obtain intermediate 6, and intermediate 6, ethylene glycol amine, 1-hydroxybenzotriazole and tetrahydrofuran are mixed for reaction to obtain the modified monomer.
3. The method for preparing the high-temperature-resistant polyurethane heat-insulating pipe according to claim 2, which is characterized in that: the molar ratio of cyanuric chloride, sodium hydroxide and piperonyl alcohol in the step A1 is 1:1:1, and the dosage ratio of the intermediate 1, the Karster catalyst, the xylene, the toluene and the tetramethyl disiloxane is 100mmol:0.39g:20mL:20mL:50mol.
4. The method for preparing the high-temperature-resistant polyurethane heat-insulating pipe according to claim 2, which is characterized in that: the mol ratio of the phosphorus oxychloride, the 2, 2-dimethylolpropionic acid and the triethylamine in the step A2 is 1:1:1.1, and the mol ratio of the intermediate 3, 5-nitro-1, 3-benzenediol and the potassium carbonate is 2:1:2.1.
5. The method for preparing the high-temperature-resistant polyurethane heat-insulating pipe according to claim 2, which is characterized in that: the dosage ratio of the intermediate 4, tin and concentrated hydrochloric acid in the step A3 is 4g:9g:19mL.
6. The method for preparing the high-temperature-resistant polyurethane heat-insulating pipe according to claim 2, which is characterized in that: the molar ratio of the intermediate 2, the intermediate 5 and the triethylamine in the step A4 is 1:4:4.1, and the molar ratio of the intermediate 6, the glycol amine and the 1-hydroxybenzotriazole is 1:4:4.2.
7. The method for preparing the high-temperature-resistant polyurethane heat-insulating pipe according to claim 1, which is characterized in that: the reinforcing filler is prepared by the following steps:
step B1: mixing vermiculite, zinc nitrate hexahydrate, aluminum nitrate nonahydrate, urea and deionized water, performing hydrothermal reaction, filtering to remove filtrate, washing a substrate with deionized water and ethanol in sequence, calcining to obtain load particles, mixing starch, KH560, DMF and sodium hydroxide, stirring, adding acetone, filtering to remove filtrate, drying the substrate to obtain modified starch,
step B2: uniformly dispersing the load particles and the modified starch in acetone, adding deionized water, stirring to obtain composite particles, mixing and stirring the composite particles, ammonium molybdate and deionized water, adding molybdenum trioxide, and reacting to obtain the reinforced filler.
8. The method for preparing the high-temperature-resistant polyurethane heat-insulating pipe according to claim 7, which is characterized in that: the dosage ratio of vermiculite, zinc nitrate hexahydrate, aluminum nitrate nonahydrate, urea and deionized water in the step B1 is 10g:30mmol:10mmol:15mmol:150mL, and the dosage ratio of starch, KH560, DMF and sodium hydroxide is 5.5g:7.3g:50mL:0.2g.
9. The method for preparing the high-temperature-resistant polyurethane heat-insulating pipe according to claim 7, which is characterized in that: the mass ratio of the load particles to the modified starch in the step B2 is 1:5, and the mass ratio of the composite particles to the ammonium molybdate to the molybdenum trioxide is 3.12:6.09:5.16.
10. The utility model provides a high temperature resistant polyurethane insulating tube which characterized in that: the process according to any one of claims 1-9.
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