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A kind of preparation method of cyclohexane-1,2-dicarboxylate plasticizer

A technology of diformate and cyclohexane, which is applied in the field of preparation of environmentally friendly plasticizers, can solve the problems of troublesome post-processing, high yield per kettle, dark product color, etc., achieves low equipment requirements, and reduces energy consumption , the effect of easy industrial control

Active Publication Date: 2020-12-22
HENAN VOCATIONAL COLLEGE OF APPLIED TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional esterification method using sulfuric acid as a catalyst is a homogeneous reaction, and the single-pot yield of the reaction is high, but it is easy to produce waste acid, the product has a darker color, troublesome post-processing, and serious equipment corrosion

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Synthesis of dibutyl cyclohexane-1,2-dicarboxylate: the composite catalyst is sodium bisulfate-iron powder, wherein the mass ratio of sodium bisulfate to iron powder is 5:1, and the particle size of the iron powder is 80 mesh. The raw materials cyclohexane-1,2-dicarboxylic acid and n-butanol are added to the stainless steel esterification reactor according to the acid-alcohol molar ratio of 1:2.5, and the composite catalyst accounting for 0.1% of the total mass of the material is added to the stainless steel esterification reactor at normal pressure, 145 ℃ for 5 hours, the water in the water separator did not increase significantly, stop the reaction, lower the temperature, separate the solid and liquid, the reaction liquid is colorless, the ester yield is 79%, recover the excess alcohol, add acid alcohol to the required molar ratio, continue next cycle.

[0026] Synthesis of dioctyl cyclohexane-1,2-dicarboxylate: the composite catalyst is sodium bisulfate-iron powder, ...

Embodiment 2

[0028] Synthesis of dibutyl cyclohexane-1,2-dicarboxylate: The composite catalyst is potassium hydrogen sulfate-iron powder, wherein the mass ratio of potassium hydrogen sulfate to iron powder is 5:1, and the particle size of the iron powder is 80 mesh. The raw materials cyclohexane-1,2-dicarboxylic acid and n-butanol are added to the stainless steel esterification reactor according to the acid-alcohol molar ratio of 1:2.5, and the composite catalyst accounting for 0.1% of the total mass of the material is added to the stainless steel esterification reactor at normal pressure, 145 ℃ for 4 hours, the water in the water separator did not increase significantly, stop the reaction, lower the temperature, separate the solid and liquid, the reaction liquid is colorless, the ester yield is 81%, recover the excess alcohol, add acid alcohol to the required molar ratio, continue next cycle.

[0029] Synthesis of dioctyl cyclohexane-1,2-dicarboxylate: the composite catalyst is potassium ...

Embodiment 3

[0031] Synthesis of dibutyl cyclohexane-1,2-dicarboxylate: The composite catalyst is potassium bisulfate-aluminum powder, wherein the mass ratio of potassium bisulfate to aluminum powder is 5:2, and the particle size of the aluminum powder is 80 mesh. The raw material cyclohexane-1,2-dicarboxylic acid and n-butanol are added to the stainless steel esterification reactor according to the acid-alcohol molar ratio of 1:2.5, and the composite catalyst accounting for 0.3% of the total mass of the material is added to the stainless steel esterification reactor at normal pressure, 155 ℃ for 4 hours, the water in the water separator did not increase significantly, stop the reaction, lower the temperature, separate the solid and liquid, the reaction liquid is colorless, the ester yield is 81%, recover the excess alcohol, add acid alcohol to the required molar ratio, continue next cycle.

[0032] Synthesis of dioctyl cyclohexane-1,2-dicarboxylate: the composite catalyst is potassium hyd...

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Abstract

The invention discloses a production method of cyclohexane-1,2-dicarboxylate plasticizer, which proceeds through the following steps: 1. Preparation of composite catalyst: hydrogen sulfate and metal powder with a particle size of 40 to 100 mesh According to the mass ratio of 2~5:1, the composite catalyst is obtained; 2. Use the molar ratio of: cyclohexane-1,2-dicarboxylic acid:alcohol = 1:2~3 as the material, which will account for the total mass of the material Add 0.1% to 1% of the composite catalyst to the reactor, stir under normal pressure, react at 140 to 170°C for 3 to 5 hours, cool down, and separate to obtain cyclohexane-1,2-dicarboxylate plasticizer. The catalyst is environmentally friendly and economical, easy to prepare, does not produce waste acid, has a long service life, flexible mass composition ratio, moderate catalytic activity, pure product and easy separation; low equipment requirements; cyclohexane-1,2 of the invention -The synthesis method of diformate plasticizer is simple, no other by-products are produced, and no complex product separation device is required. It greatly reduces energy consumption and investment costs, is easy to operate, and is easy to industrialize control.

Description

technical field [0001] The invention relates to a preparation process of an environment-friendly plasticizer, in particular, the invention relates to a preparation method of an environment-friendly plasticizer cyclohexane-1,2-dicarboxylate plasticizer. Background technique [0002] For a long time, plasticizers are mainly based on phthalates. As early as 1982, the authoritative National Cancer Institute of the United States conducted a biological identification of the carcinogenicity of dioctyl phthalate (DOP), and concluded that DOP is a carcinogen for rats and mice, and can make rodents of liver cancer. According to the research results of the National Cancer Institute, the U.S. Environmental Protection Agency has stopped the industrial production of 6 new phthalate plasticizers. DOP is limited to food packaging with high water content, and meat packaging must be used Other non-toxic plasticizer products instead; the Swiss government has decided to ban the use of DOP in ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/75B01J27/053B01J27/055
CPCC07C67/08B01J21/02B01J23/06B01J23/14B01J23/745B01J27/053B01J27/055B01J35/19C07C69/75
Inventor 柴凤兰张帆郑河清阎梦婓郭红艳马梦晨赵开楼
Owner HENAN VOCATIONAL COLLEGE OF APPLIED TECH
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