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Preparation method for trimethylolpropane tricarboxylate

A technology of trimethylolpropane tricarboxylate and trimethylolpropane, which is applied in the field of preparation of trimethylolpropane tricarboxylate, can solve problems such as not being environmentally friendly and not suitable for industrial production, and achieve good purity , protect the environment or safe production, easy to separate the effect

Inactive Publication Date: 2014-12-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the defects that the preparation method of the prior art is not environmentally friendly and not suitable for industrial production, and provides a new preparation method of trimethylolpropane tricarboxylate

Method used

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  • Preparation method for trimethylolpropane tricarboxylate
  • Preparation method for trimethylolpropane tricarboxylate
  • Preparation method for trimethylolpropane tricarboxylate

Examples

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preparation example Construction

[0016] According to the preparation method of the present invention, when R 1 , R 2 , R 3 At the same time, carboxylate R 1 COOR, R 2 COOR, R 3 COOR means the same substance, hereinafter referred to as carboxylate R 1 COOR.

[0017] According to the preparation method of the present invention, only in the presence of a catalyst containing anhydrous potassium carbonate, the trimethylolpropane with the structural formula (II) and carboxylate R 1 The purpose of the present invention can be achieved when the transesterification reaction of COOR occurs, that is, it is beneficial to environmental protection, the product is easily separated from the reactant and the catalyst, and the yield is high and the purity is good. However, preferably, the transesterification reaction includes performing the reaction under distillation or rectification conditions (at this time, the distillation or rectification conditions are equivalent to the trimethylolpropane with the structural formul...

Embodiment 1

[0037] This embodiment is used to illustrate the preparation method of trimethylolpropane tripalate provided by the present invention.

[0038] Add 9.84g (0.075mol) trimethylolpropane (98%), 50.55g (0.44mol) methyl n-valerate, 2.01g (0.015 mol) anhydrous potassium carbonate, heat the oil bath in contact with the round bottom flask to 118°C, and react at 0.1MPa. During the reaction, distill the generated methanol to the liquid separator by distillation method and remove it. After reacting for 6 hours, transfer to Add toluene into the round-bottomed flask, add 6 times in total, the time interval between two adjacent additions is 1.5 hours, add 10mL each time, react for 1 hour after each addition of toluene, and distill toluene and azeotrope out of the round bottom at the same time The flask, after the reaction solution was cooled for about 30 minutes, added the next toluene. After the reaction, the mixture in the round bottom flask was cooled and filtered to remove anhydrous po...

Embodiment 2

[0040] This embodiment is used to illustrate the preparation method of trimethylolpropane tri-n-butyrate provided by the present invention.

[0041] Add 10.66g (0.08mol) trimethylolpropane (98%), 51.78g (0.50mol) methyl n-butyrate, 2.22g (0.016 mol) anhydrous potassium carbonate, heat the oil bath in contact with the round-bottomed flask to 98°C, and react at 0.1MPa. During the reaction, distill the generated alcohol to the liquid separator by distillation and remove it. After 6 hours of reaction, transfer to Add methyl n-butyrate into the round bottom flask, add 6 times in total, the time interval between two adjacent additions is 2 hours, add 10mL each time, add methyl n-butyrate each time and react in an oil bath at 100°C 1.5 hours and at the same time methyl n-butyrate and the azeotrope were distilled out of the round bottom flask, and the next methyl n-butyrate was added after the reaction liquid was cooled for about 30 minutes. After the reaction, the mixture in the rou...

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Abstract

The invention discloses a preparation method for trimethylolpropane tricarboxylate with a structural formula (I). The method comprises the steps of reacting 1,1,1-trimethylolpropane with a structural formula (II) with carboxylic ester R1COOR, R2COOR, R3COOR in presence of an anhydrous potassium carbonate-containing catalyst to generate products of trimethylolpropane tricarboxylate with the structural formula (I) and corresponding alcohol HOR, wherein R1, R2 and R3 are identical or different and are independently selected from one of a linear chain C2-C17 alkyl, a branch chain C3-C17 alkyl and C4-C8 cycloalkyl; and R is selected from C1-C5 alkayl. The method provided by the invention is beneficial to environment protection; and the product has high yield and good purity. The structural formula (I) and (II) are shown in the description.

Description

technical field [0001] The invention relates to a preparation method of ester plasticizer or lubricating oil, in particular to a preparation method of trimethylolpropane tricarboxylate. Background technique [0002] Plasticizers refer to plastic additives used in the molding process of polyvinyl chloride and other plastics. Adding them to the polymer system can reduce the glass transition temperature of the polymer and increase its plasticity, making it easy to process. Trimethylolpropane tricarboxylate is a class of plasticizers suitable for polyvinyl chloride (PVC) processing. Another use of trimethylolpropane tricarboxylate is as lubricating oil. [0003] US6673959B2 discloses a method for synthesizing carboxylic acid esters including trimethylolpropane tricarboxylate. The method uses alkylsulfonic acid as a catalyst to directly carry out 1,1,1-trimethylolpropane and carboxylic acid The esterification reaction produces trimethylolpropane tricarboxylate. The method uses...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/30C07C67/03
CPCC07C67/03B01J27/232C07C67/54C07C2601/12C07C69/30C07C69/608
Inventor 谢伦嘉梁健田宇赵思源冯再兴孙竹芳
Owner CHINA PETROLEUM & CHEM CORP
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