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Preparation method of dicarboxylic dihydric alcohol ester plasticizer

A technology of glycol ester and dicarboxylic acid, applied in the fields of polymer materials and chemical industry, can solve the problems of equipment corrosion, many by-products, affecting the quality of plasticizers, etc., and achieves easy separation, high yield and good application. Foreground effect

Inactive Publication Date: 2016-11-23
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sulfuric acid catalyst not only causes serious equipment corrosion, but also has many by-products, and the target product is not easy to separate and purify, which affects the quality of the plasticizer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: with 10mmol ethylene glycol, 22mmol benzoic acid, 0.15mmol Sb 2 o 3 and 0.15mmolSb(OAc) 2 Added to a 50mL round bottom flask. Heated to 120°C; reacted at this temperature for 4h. Then carry out vacuum distillation to obtain ethylene glycol dibenzoate. Calculated according to the feeding amount of ethylene glycol, the isolated molar yield of the ester is 97%, and the purity is 99.9%.

Embodiment 2

[0017] Embodiment 2: with 10mmol diglycol alcohol, 21mmol cyclohexyl formic acid, 0.001mmolSb 2 (OCH 2 CH 2 O) 3 Added to a 50mL round bottom flask. Heated to 105°C; reacted at this temperature for 48h. Then carry out vacuum distillation to obtain diethylene glycol dicyclohexyl formate. Calculated according to the feeding amount of diglycol, the isolated molar yield of the ester is 99%, and the purity is 99.7%.

Embodiment 3

[0018] Embodiment 3: 10mmol 1,2-propanediol, 30mmol hexanoic acid, 0.025mmol Ti(t-OC 4 h 9 ) 4 Added to a 50mL round bottom flask. Heated to 220°C; reacted at this temperature for 3h. Then carry out vacuum distillation to obtain propylene glycol dicaproate. Calculated according to the feeding amount of 1,2-propanediol, the isolated molar yield of the ester is 96%, and the purity is 99.8%.

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Abstract

A preparation method of dicarboxylic dihydric alcohol ester plasticizer includes the steps of conducting esterification reaction for 0.5-48 h with monobasic acid and dihydric alcohol as the raw materials under the catalysis effect at a temperature of 100-250 DEG C, and conducting reduced pressure distillation to obtain the dicarboxylic dihydric alcohol ester product. Dicarboxylic dihydric alcohol ester is non-toxic plasticizer and can replace phthalic acid ester to be used for the field of plastic industry, rubber industry and the like. The product prepared through the method is high in yield, easy to separate and friendly to the environment and has good application prospects.

Description

technical field [0001] The invention relates to the fields of macromolecular materials and chemical engineering, in particular to a method for preparing dicarboxylic acid glycol esters through esterification of monobasic acids and dihydric alcohols under catalysis. Background technique [0002] Plasticizers, or plasticizers, plasticizers, are widely used in plastics, concrete, drywall materials, cement and gypsum, etc., and are additives that increase the flexibility of materials. Among them, phthalate plasticizers are the most widely used, such as dioctyl phthalate (DOP), di(2-ethyl)hexyl phthalate (DEHP), and the like. Since the American Cancer Institute suspected that DOP has carcinogenic effects, developed countries such as Europe and the United States have restricted the use of phthalate plasticizers, especially DOP, which is widely used as the main plasticizer. my country also stipulates that the use of phthalate plasticizers in food, medicine, children's toys and oth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/78C07C69/75C07C69/28C07D493/04C07D307/42C08K5/103
CPCC07C67/08C07C69/28C07C69/75C07C69/78C07D307/42C07D493/04C08K5/103
Inventor 马继平徐杰贾秀全王敏高进苗虹黄义争
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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