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A kind of phthalic anhydride polyester polyol and preparation method thereof

A technology of phthalic anhydride polyester polyol and polyol, which is applied in the field of preparation of phthalic anhydride polyester polyol, can solve the problems of low lactone content, influence on polyurethane application, structural limitation of phthalic anhydride polyester polyol, etc., and achieves low lactone content Effect

Active Publication Date: 2022-04-22
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, phthalides are mobile in polyurethane products and may have a plasticizing effect, which in turn affects the application of polyurethane in some fields
[0004] Patent US2014018458A1 discloses a synthesis method of phthalic anhydride polyester polyol with low lactone content, reacting phthalic anhydride with PEG-200 or PEG-400 can obtain phthalic anhydride polyester polyol with low lactone content, because PEG-200 and PEG-400 is an oligomer, and the number of atoms in its main chain is much more than that of organic diol compounds, so it is difficult to form a cyclic lactone with phthalic anhydride
However, the structure of the phthalic anhydride polyester polyol synthesized by this scheme is relatively limited, and it is difficult to meet the demand for differentiated structure products of phthalic anhydride polyester polyol in different application fields

Method used

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  • A kind of phthalic anhydride polyester polyol and preparation method thereof
  • A kind of phthalic anhydride polyester polyol and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1) Add 9.0kg of phthalic anhydride, 1.0kg of adipic acid and 9.4kg of diethylene glycol into the reactor, raise the temperature of the system to 140°C until the system becomes clear and transparent, then raise the temperature of the system from room temperature to 210°C, And carry out the first stage reaction at this temperature for 2.0h until the acid value in the system is 40mgKOH / g;

[0035] 2) Continue to heat up to 230°C, and carry out the second-stage reaction at this temperature. When the acid value in the reaction system is 15mgKOH / g, add 2.1g tetraisopropyl titanate to continue the reaction. When the acid value in the system is Turn on the vacuum device at 10mgKOH / g, and react for 2h under the vacuum of -0.095MPa until the acid value in the system is 0.98mgKOH / g, the hydroxyl value is 57.22mgKOH / g, the system is cooled to 160°C, and the material is packaged to obtain polyester multi-component Alcohol A.

[0036] It is determined that the polyester polyol A has...

Embodiment 2

[0038] 1) Add 10.0kg of phthalic anhydride and 10.2kg of diethylene glycol into the reactor, raise the temperature of the system from room temperature to 210°C, and carry out the first-stage reaction at this temperature for 2.0h until the acid value in the system is 30mgKOH / g ;

[0039]2) Continue to heat up to 230°C, and carry out the second-stage reaction at this temperature. When the acid value in the reaction system is 19mgKOH / g, add 2.1g tetraisopropyl titanate to continue the reaction. When the acid value in the system is Turn on the vacuum device at 10mgKOH / g, react for 3h under the vacuum of -0.095MPa until the acid value in the system is 0.98mgKOH / g, the hydroxyl value is 57.22mgKOH / g, the system is cooled to 160°C, and the material is packaged to obtain polyester multi-component Alcohol B.

[0040] It was determined that the polyester polyol B had a hydroxyl value of 57.22 mgKOH / g, an acid value of 0.98 mgKOH / g, and an average molecular weight of 2000.

Embodiment 3

[0042] 1) Add 10.0kg of phthalic anhydride and 11.6kg of diethylene glycol into the reactor, raise the temperature of the system from room temperature to 210°C, and carry out the first-stage reaction at this temperature for 2.0h until the acid value in the system is 20mgKOH / g ;

[0043] 2) Continue to heat up to 230°C, and carry out the second-stage reaction at this temperature. When the acid value in the reaction system is 12mgKOH / g, add 2.1g tetraisopropyl titanate to continue the reaction. When the acid value in the system is Turn on the vacuum device at 10mgKOH / g, react for 4.5h under the vacuum of -0.095MPa until the acid value in the system is 0.43mgKOH / g, the hydroxyl value is 55.60mgKOH / g, the system is cooled to 160°C, and the material is packaged to obtain polyester Polyol C.

[0044] It was determined that the polyester polyol C had a hydroxyl value of 55.60 mgKOH / g, an acid value of 0.43 mgKOH / g, and an average molecular weight of 2000.

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Abstract

The invention provides a preparation method of phthalic anhydride polyester polyol, comprising the following steps: 1) mixing the alcohol component and the anhydride component, raising the temperature to 180-220°C to carry out the first-stage reaction, and the first-stage reaction proceeds to the system The acid value in the system is M1; 2) The temperature of the system is raised to 220-250°C for the second-stage reaction. The second-stage reaction proceeds until the acid value in the system is M2, and then continues the reaction under vacuum until the acid value in the system is M3. Value is 10~600mgKOH / g, obtains phthalic anhydride polyester polyol, the molar ratio of alcohol component and anhydride component in step 1) is 1.3~7.0:1, 20mgKOH / g<M1≤80mgKOH / ; In step 2), 5.0mgKOH / g<M2≤20mgKOH / g, 0.01mgKOH / g<M3≤5.0mgKOH / g. The preparation method of the phthalic anhydride polyester polyol provided by the invention has the advantages of low phthalic anhydride cyclic lactone content and reduces the content of migratory monomers.

Description

technical field [0001] The invention belongs to the technical field of preparing polyester polyols, in particular to a preparation method of phthalic anhydride polyester polyols. Background technique [0002] Phthalic anhydride polyester polyol is an intermediate widely used in the field of rigid foam, which can partially replace polyether polyol. The existence of benzene ring in its structure can endow rigid foam with good flame retardancy, and has the characteristics that polyether polyol is difficult to Competitive advantage. In addition, phthalic anhydride polyester polyols are also widely used in polyurethane fields such as coatings, elastomers, adhesives and sealants. [0003] The synthesis of phthalic anhydride polyester polyols is usually accompanied by the formation of phthalic anhydride cyclic lactones. The structure of phthalides does not contain reactive functional groups capable of reacting with isocyanates. Therefore, phthalides are mobile in polyurethane pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/672C08G63/181C08G63/78
CPCC08G63/672C08G63/181C08G63/78
Inventor 张存玉孙令民黄岐善
Owner WANHUA CHEM GRP CO LTD