CN111995740A - Method for preparing aromatic polyester polyol with good pentane compatibility - Google Patents
Method for preparing aromatic polyester polyol with good pentane compatibility Download PDFInfo
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- CN111995740A CN111995740A CN202010868127.0A CN202010868127A CN111995740A CN 111995740 A CN111995740 A CN 111995740A CN 202010868127 A CN202010868127 A CN 202010868127A CN 111995740 A CN111995740 A CN 111995740A
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- Prior art keywords
- polyester polyol
- aromatic polyester
- preparing
- pentane compatibility
- good
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- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229920005906 polyester polyol Polymers 0.000 title claims abstract description 46
- 125000003118 aryl group Chemical group 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000005886 esterification reaction Methods 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000007599 discharging Methods 0.000 claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 26
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 14
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 9
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 9
- 238000005086 pumping Methods 0.000 claims description 9
- 230000032050 esterification Effects 0.000 claims description 8
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 6
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 239000005642 Oleic acid Substances 0.000 claims description 6
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 6
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 6
- 235000021313 oleic acid Nutrition 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 5
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- -1 carbon chain monocarboxylic acid Chemical class 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 150000002762 monocarboxylic acid derivatives Chemical class 0.000 claims description 4
- 235000021314 Palmitic acid Nutrition 0.000 claims description 3
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 3
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 3
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 3
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 claims description 2
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims 1
- ACCCMOQWYVYDOT-UHFFFAOYSA-N hexane-1,1-diol Chemical compound CCCCCC(O)O ACCCMOQWYVYDOT-UHFFFAOYSA-N 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 4
- 239000006260 foam Substances 0.000 abstract description 4
- 229920002635 polyurethane Polymers 0.000 abstract description 4
- 239000004814 polyurethane Substances 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000004088 foaming agent Substances 0.000 description 6
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 2
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 description 1
- 229940051250 hexylene glycol Drugs 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/672—Dicarboxylic acids and dihydroxy compounds
-
- 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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4205—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups
- C08G18/4208—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups
- C08G18/4211—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups derived from aromatic dicarboxylic acids and dialcohols
- C08G18/4219—Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups derived from aromatic dicarboxylic acids and dialcohols from aromatic dicarboxylic acids and dialcohols in combination with polycarboxylic acids and/or polyhydroxy compounds which are at least trifunctional
-
- 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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4244—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups
- C08G18/4247—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups derived from polyols containing at least one ether group and polycarboxylic acids
- C08G18/425—Polycondensates having carboxylic or carbonic ester groups in the main chain containing oxygen in the form of ether groups derived from polyols containing at least one ether group and polycarboxylic acids the polyols containing one or two ether 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
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/68—Unsaturated polyesters
- C08G18/683—Unsaturated polyesters containing cyclic 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/20—Polyesters having been prepared in the presence of compounds having one reactive group or more than two reactive groups
- C08G63/21—Polyesters having been prepared in the presence of compounds having one reactive group or more than two reactive groups in the presence of unsaturated monocarboxylic acids or unsaturated monohydric alcohols or reactive derivatives thereof
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
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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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/141—Hydrocarbons
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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
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
- C08J2375/06—Polyurethanes from polyesters
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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
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
- C08J2375/14—Polyurethanes having carbon-to-carbon unsaturated bonds
Abstract
The invention discloses a method for preparing aromatic polyester polyol with good pentane compatibility, which comprises the following steps: placing raw materials for synthesizing aromatic polyester polyol into reaction equipment for nitrogen replacement; heating the reaction equipment to perform esterification reaction on the aromatic polyester polyol raw material; and vacuumizing the reaction equipment, cooling and discharging to obtain the aromatic polyester polyol. According to the method for preparing the aromatic polyester polyol with good pentane compatibility, the prepared aromatic polyester polyol has good pentane compatibility, can be used for the combined polyester polyol of a premixed pentane system and a polyurethane rigid foam system with high requirements on flame retardance, and the whole method for preparing the aromatic polyester polyol with good pentane compatibility is simple, has a better using effect compared with a traditional mode, is low in cost, can facilitate large-scale production of people, and brings a better using prospect.
Description
Technical Field
The invention relates to the field of foaming agents, in particular to a method for preparing aromatic polyester polyol with good pentane compatibility.
Background
Polyurethane rigid foam is widely applied to heat insulation materials, aromatic polyester polyol is widely used in application scenes needing high flame retardance, a traditional foaming agent is 141B, a pentane foaming agent is used for replacing the foaming agent such as 141B due to the pressure of environmental protection, but the compatibility of the pentane foaming agent and the aromatic polyester polyol is very poor, the common aromatic polyester polyol cannot be used in a system for premixing pentane and can only be applied to scenes of on-line mixing, but a considerable part of manufacturers need products with premixed foaming agents due to equipment limitation, so that the existing aromatic polyester polyol cannot meet the use requirements of people, and therefore, a method for preparing the aromatic polyester polyol with good pentane compatibility is provided.
Disclosure of Invention
The main object of the present invention is to provide a method for preparing aromatic polyester polyol having good pentane compatibility, which can effectively solve the problems of the background art.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for preparing an aromatic polyester polyol having good pentane compatibility, comprising the steps of:
(1) placing the raw materials for synthesizing the aromatic polyester polyol into reaction equipment for nitrogen replacement;
(2) heating the reaction equipment to perform esterification reaction on the aromatic polyester polyol raw material;
(3) and vacuumizing the reaction equipment, and then cooling and discharging to obtain the aromatic polyester polyol.
Preferably, the raw materials for synthesizing the aromatic polyester polyol in the step (1) comprise dihydric alcohol, trihydric alcohol, long-carbon-chain monocarboxylic acid and phthalic anhydride or terephthalic acid, and the content of the long-carbon-chain monocarboxylic acid accounts for 5-25% of the weight of the aromatic polyester polyol.
Preferably, the triol is one or two of glycerol or trimethylolpropane, the diol is one or more of ethylene glycol, propylene glycol, diethylene glycol, dipropylene glycol, hexylene glycol and neopentyl glycol, and the long carbon chain monocarboxylic acid is one or more of oleic acid, linoleic acid, stearic acid and palmitic acid.
Preferably, the temperature of the reaction equipment in the step (2) is raised to 100-180 ℃, and the esterification reaction time is 3-8 h.
Preferably, in step (2): the esterification reaction needs an esterification catalyst, the esterification catalyst is one of T9, T12, T120 and phthalate ester, and the esterification catalyst is 0.01-0.2% of the raw materials for synthesizing the aromatic polyester polyol.
Preferably, the temperature of the evacuation in the step (3) is 125-.
Pentane refers to cyclopentane, n-pentane, and isopentane.
Compared with the prior art, the invention has the following beneficial effects: according to the method for preparing the aromatic polyester polyol with good pentane compatibility, the prepared aromatic polyester polyol has good pentane compatibility, can be used for the combined polyester polyol of a premixed pentane system and a polyurethane rigid foam system with high requirements on flame retardance, and the whole method for preparing the aromatic polyester polyol with good pentane compatibility is simple, convenient to operate, better in using effect compared with a traditional mode, lower in cost and capable of facilitating mass production of people.
Drawings
FIG. 1 is a flow chart showing the overall structure of a process for preparing an aromatic polyester polyol having good pentane compatibility according to the present invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
Connecting a water separator, a stirrer, a condenser, a thermometer and an electric heater in a 1.5L 4-mouth flask, adding 70g of glycerol, 450g of dipropylene glycol, 150g of stearic acid, 350g of phthalic anhydride and 0.2g of T9, heating to 150 ℃ for esterification after nitrogen replacement, cooling to 130 ℃ after 5h, vacuumizing for 3h, cooling and discharging to obtain a brown yellow transparent product, and detecting the brown yellow transparent product, wherein the hydroxyl value test result is 220mgKOH/g, and the viscosity is 9000cps (25 ℃).
Example 2
A water separator, a stirrer, a condenser, a thermometer and an electric heater are connected to a 1.5L 4-mouth flask, 70g of glycerol, 450g of dipropylene glycol, 100g of palmitic acid, 350g of phthalic anhydride and 0.2g of T9 are added, the temperature is raised to 150 ℃ for esterification after nitrogen replacement, the temperature is reduced to 130 ℃ after 5h, vacuum pumping is carried out for 3h, the temperature is reduced and discharging is carried out, and a brown yellow transparent product is obtained, wherein the hydroxyl value test result is 250mgKOH/g, and the viscosity is 12000cps (25 ℃).
Example 3
A water separator, a stirrer, a condenser, a thermometer and an electric heater are connected to a 1.5L 4-mouth flask, 70g of glycerol, 400g of dipropylene glycol, 200g of oleic acid, 350g of phthalic anhydride and 0.2g of T9 are added, the temperature is raised to 150 ℃ for esterification reaction after nitrogen replacement, the temperature is lowered to 130 ℃ after 5 hours, vacuum pumping is carried out for 3 hours, the temperature is lowered for discharging, and a brown yellow transparent product is obtained, wherein the hydroxyl value test result is 170mgKOH/g, and the viscosity is 13000cps (25 ℃).
Example 4
A water separator, a stirrer, a condenser, a thermometer and an electric heater are connected to a 1.5L 4-mouth flask, 100g of glycerol, 400g of dipropylene glycol, 100g of stearic acid, 450g of terephthalic acid and 0.2g of T9 are added, the temperature is raised to 150 ℃ for esterification reaction after nitrogen replacement, the temperature is lowered to 130 ℃ after 5h, vacuum pumping is carried out for 3h, the temperature is lowered and discharging is carried out, and a brown yellow transparent product is obtained, wherein the hydroxyl value test result is 210mgKOH/g, and the viscosity is 12000cps (25 ℃).
Example 5
A water separator, a stirrer, a condenser, a thermometer and an electric heater are connected to a 1.5L 4-mouth flask, 100g of glycerol, 400g of diethylene glycol, 150g of oleic acid, 500g of terephthalic acid and 0.2g of T9 are added, the temperature is raised to 150 ℃ for esterification reaction after nitrogen replacement, the temperature is lowered to 130 ℃ after 5 hours, vacuum pumping is carried out for 3 hours, the temperature is lowered, discharging is carried out, and a brown yellow transparent product is obtained, wherein the hydroxyl value test result is 230mgKOH/g, and the viscosity is 10000cps (25 ℃).
Example 6
A water separator, a stirrer, a condenser, a thermometer and an electric heater are connected to a 1.5L 4-mouth flask, 60g of glycerol, 400g of propylene glycol, 150g of stearic acid, 500g of terephthalic acid and 0.2g of phthalate are added, the temperature is raised to 140 ℃ for esterification reaction after nitrogen replacement, the temperature is lowered to 130 ℃ after 5 hours, vacuum pumping is carried out for 3 hours, the temperature is lowered and discharging is carried out, and a brown yellow transparent product is obtained, wherein the hydroxyl value test result is 330mgKOH/g, and the viscosity is 7000cps (25 ℃).
Example 7
A water separator, a stirrer, a condenser, a thermometer and an electric heater are connected to a 1.5L 4-mouth flask, 50g of glycerol, 450g of neopentyl glycol, 150g of oleic acid, 400g of terephthalic acid and 0.2g of T9 are added, the temperature is raised to 150 ℃ for esterification reaction after nitrogen replacement, the temperature is lowered to 130 ℃ after 5 hours, vacuum pumping is carried out for 3 hours, the temperature is lowered for discharging, and a brown yellow transparent product is obtained, wherein the hydroxyl value test result is 280mgKOH/g, and the viscosity is 8000cps (25 ℃).
Example 8
A water separator, a stirrer, a condenser, a thermometer and an electric heater are connected to a 1.5L 4-mouth flask, 70g of trimethylolpropane, 500g of dipropylene glycol, 200g of oleic acid, 350g of terephthalic acid and 0.1g of T12 are added, after nitrogen replacement, the temperature is raised to 160 ℃ for esterification reaction, after 5 hours, the temperature is lowered to 130 ℃, vacuum pumping is carried out for 3 hours, the temperature is lowered and discharging is carried out, and a brown yellow transparent product is obtained, wherein the hydroxyl value test result is 230mgKOH/g, and the viscosity is 9000cps (25 ℃).
The formulations were based on the polyester polyols of examples 1, 2, 3 and 4 (the reaction equipment in the examples could also be replaced by other equipment with the same function), and PS 3152 was used as a reference to observe the comparative solubility.
The method for preparing the aromatic polyester polyol with good pentane compatibility has the advantages that the aromatic polyester polyol prepared by the method has good pentane compatibility, can be used for combined polyester polyol of a premixed pentane system and a polyurethane rigid foam system with high requirements on flame retardance, is simple in whole preparation method, convenient to operate, better in using effect compared with a traditional mode, lower in cost and capable of facilitating mass production of people.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A method for preparing aromatic polyester polyol with good pentane compatibility is characterized in that: the method comprises the following steps:
(1) placing the raw materials for synthesizing the aromatic polyester polyol into reaction equipment for nitrogen replacement;
(2) heating the reaction equipment to perform esterification reaction on the aromatic polyester polyol raw material;
(3) and vacuumizing the reaction equipment, and then cooling and discharging to obtain the aromatic polyester polyol.
2. The process according to claim 1 for preparing an aromatic polyester polyol having good pentane compatibility, wherein: the raw materials for synthesizing the aromatic polyester polyol in the step (1) comprise dihydric alcohol, trihydric alcohol, long-carbon-chain monocarboxylic acid and phthalic anhydride or terephthalic acid, wherein the content of the long-carbon-chain monocarboxylic acid accounts for 5-25% of the weight of the aromatic polyester polyol.
3. The process for preparing an aromatic polyester polyol having good pentane compatibility according to claim 2, wherein: the triol is one or two of glycerin or trimethylolpropane, the dihydric alcohol is one or more of ethylene glycol, propylene glycol, diethylene glycol, dipropylene glycol, hexanediol and neopentyl glycol, and the long carbon chain monocarboxylic acid is one or more of oleic acid, linoleic acid, stearic acid and palmitic acid.
4. The process according to claim 1 for preparing an aromatic polyester polyol having good pentane compatibility, wherein: in the step (2), the temperature of the reaction equipment is raised to 100-180 ℃, and the esterification reaction time is 3-8 h.
5. The process according to claim 1 for preparing an aromatic polyester polyol having good pentane compatibility, wherein: in the step (2): the esterification reaction needs an esterification catalyst, the esterification catalyst is one of T9, T12, T120 and phthalate ester, and the esterification catalyst is 0.01-0.2% of the raw materials for synthesizing the aromatic polyester polyol.
6. The process according to claim 1 for preparing an aromatic polyester polyol having good pentane compatibility, wherein: the temperature during the vacuum pumping in the step (3) is 125-135 ℃, the vacuum pumping time is 2.5-3.5h, and the hydroxyl value of the obtained aromatic polyester polyol is 150-350 mgKOH/g.
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