Method for preparing polyester polyol

Patent metadata

Field	Value
Publication number	US-12091501-B2
Application number	US-201817293899-A
Country	US
Kind code	B2
Filing date	Nov 15, 2018
Priority date	Nov 15, 2018
Publication date	Sep 17, 2024
Grant date	Sep 17, 2024

Abstract

The present application discloses a method for preparing polyester polyol comprising performing transesterification of raw materials containing inorganic oxyacid ester and polyhydric alcohol to obtain the polyester polyol. The polyester polyol obtained by the method described in the present application has higher heat resistance.

First claim

The invention claimed is:

1. A method for preparing a polyester polyol comprising performing transesterification of an inorganic oxyacid ester and a polyhydric alcohol as raw materials to obtain the polyester polyol;
wherein the method comprises the following steps:
a) mixing the inorganic oxyacid ester, the polyhydric alcohol and a transesterification catalyst, and then performing a transesterification reaction under stirring conditions and in an inert atmosphere, wherein the reaction temperature ranges from 80 to 180° C., and the reaction time ranges from 2 to 10 hours;
b) after the reaction in step a), performing vacuum distillation during which the vacuum degree ranges from 0.01 to 5 kPa, the reaction temperature ranges from 170 to 230° C., and the reaction time ranges from 0.5 to 5 hours;
wherein a molar ratio of inorganic oxyacid ester, polyhydric alcohol and transesterification catalyst satisfies: inorganic oxyacid ester:polyhydric alcohol=(0.8˜1.2)n 3 /x,
wherein x is the number of moles of alkoxyl groups contained in each mole of inorganic oxyacid ester, and n 3 is the number of moles of hydroxyl groups contained in each mole of polyhydric alcohol.

2. The method according to claim 1 , wherein the inorganic oxyacid ester is at least one of compounds having a chemical formula shown in Formula I and Formula II,
M(OR 1 ) n 1   Formula I

O═P(OR 2 ) n 2   Formula II

wherein, M is a metal element or a non-metal element that does not include P, R 1 and R 2 are independently selected from at least one of C 1 to C 8 alkyl groups, n 1 =2˜8, n 2 =2˜8.

3. The method according to claim 2 , wherein M is B, Si, Ge, Al, Ti, Fe, Sn, V, Ga, Zr, Cr, Sb or W.

4. The method according to claim 1 , wherein the inorganic oxyacid ester comprises at least one of trimethyl borate, triethyl borate, tripropyl borate, tributyl borate, tri-n-hexyl borate, triisooctyl borate, trioctyl borate, tetramethoxysilane, tetraethyl orthosilicate, tetrapropyl silicate, tetrabutyl silicate, ethyl orthogermanate, triethyl phosphate, tripropyl phosphate, tributyl phosphate, tri-n-pentyl phosphate, trihexyl phosphate, aluminium ethoxide, aluminum isopropoxide, aluminum n-butoxide, aluminum tert-butoxide, tetraethyl titanate, tetraisopropyl titanate, tetrabutyl titanate, tetrahexyl titanate, tetraisooctyl titanate, tetrabutyl ferrite, tetrabutyl stannate, butyl orthovanadate, gallium ethoxide, tetra-n-propyl zirconate, tetrabutyl zirconate, tert-butyl chromate, ethyl antimonite, butyl antimonate, tungsten ethoxide and tungsten isopropoxide.

5. The method according to claim 1 , wherein the number of hydroxyl groups in the polyhydric alcohol is not less than two.

6. The method according to claim 1 , wherein the polyhydric alcohol comprises at least one of ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, 1,2-propanediol, 1,3-propanediol, 1,4-butylene glycol, 1,6-hexanediol, polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600, polyethylene glycol 800, 1,4-cyclohexanediol, 1,4-cyclohexane dimethanol, terephthalyl alcohol, glycerin, trimethylolpropane, pentaerythritol, xylitol and sorbitol.

7. The method according to claim 1 , wherein an amount of the transesterification catalyst is in a range from 0.1 wt % to 5 wt % of the inorganic oxyacid ester.

8. The method according to claim 1 , wherein the transesterification catalyst is at least one of acidic catalyst and basic catalyst.

9. The method according to claim 8 , wherein the acidic catalyst comprises at least one of alcohol-soluble acid, solid acid, aluminum alkoxide, aluminum phenoxide, tetrabutyl stannate, titanium alkoxide, zirconium alkoxide, ethyl antimonite and butyl antimonite; and the basic catalyst comprises at least one of alcohol-soluble base and solid base.

10. The method according to claim 1 , wherein an initial decomposition temperature of the polyester polyol is higher than 300° C.

11. The method according to claim 10 , wherein an initial decomposition temperature of the polyester polyol reaches 500° C.

Assignees

• Dalian Inst Chem & Physics Cas

Inventors

• Yuan Danhua
• Xing Jiacheng
• Xu Yunpeng
• Liu Zhongmin

Classifications

• C08G63/87

  Non-metals or inter-compounds thereof (boron C08G63/84) · CPC title

• C08G63/866

  Antimony or compounds thereof · CPC title

• C08G63/85

  Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof {(C08G63/823 takes precedence)} · CPC title

• C08G63/84 Primary

  Boron, aluminium, gallium, indium, thallium, rare-earth metals, or compounds thereof {(C08G63/823 takes precedence)} · CPC title

• C08G63/83

  Alkali metals, alkaline earth metals, beryllium, magnesium, copper, silver, gold, zinc, cadmium, mercury, manganese, or compounds thereof {(C08G63/823 takes precedence)} · CPC title