Preparation method for diisononyl cyclohexane-1,2-dicarboxylate

A technology of diisononyl dicarboxylate and cyclohexane, which is applied in the field of fine chemicals, can solve the problems of shortening the reaction time, increasing the burden on enterprises, and high product color, so as to shorten the reaction time, improve production efficiency and yield, good catalytic activity

Active Publication Date: 2017-04-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The domestic device borrows from the single-step high-temperature esterification method of CN1962736, which greatly shortens the reaction time, but first neutralizes and then dealcoholizes, which consumes a lot and the ester and water are eas...

Method used

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  • Preparation method for diisononyl cyclohexane-1,2-dicarboxylate
  • Preparation method for diisononyl cyclohexane-1,2-dicarboxylate
  • Preparation method for diisononyl cyclohexane-1,2-dicarboxylate

Examples

Experimental program
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Embodiment 1

[0034] Add hexahydrophthalic anhydride, isononanol, and catalyst acetic anhydride in proportion to the reactor, wherein: the molar ratio of hexahydrophthalic anhydride to isononanol is 1:2.3, and the amount of acetic anhydride added is 1 / 2 of the quality of hexahydrophthalic anhydride 5%, heated and stirred under normal pressure, raised the temperature to 180°C and refluxed to start timing, continued to heat up the reaction, and kept at 230°C for 3 hours to obtain material 1, which was crude diisononyl cyclohexane-1,2-dicarboxylate ; The material 1 is passed through the falling film evaporator, and the excessive alcohol is flashed off under the negative pressure of -0.06MPa, and the residence time is 0.002 h to obtain the material 2, which enters the stripping tank; in the stripping tank, feed water vapor and Nitrogen gas is bubbled, and the low molecular weight impurities in the material 2 are evaporated to obtain the material 3, which is put into the decolorization kettle. T...

Embodiment 2

[0041] Add hexahydrophthalic anhydride, isononanol, and catalyst acetic anhydride in proportion to the reactor, wherein the molar ratio of hexahydrophthalic anhydride to isononanol is 1:2.1, and the amount of acetic anhydride added is 1 / 2 of the quality of hexahydrophthalic anhydride 2%, heated and stirred under normal pressure, raised the temperature to 180°C and refluxed to start timing, continued to heat up the reaction, and obtained material 1 after maintaining at 220°C for 3 hours, material 1 was crude diisononyl cyclohexane-1,2-dicarboxylate ; The material 1 is passed through the falling film evaporator, and the excess alcohol is flashed off under the negative pressure of -0.08MPa, and the residence time is 0.001 h to obtain the material 2, which enters the stripping tank; in the stripping tank, feed water vapor and Nitrogen gas is bubbled, and the low molecular weight impurities in the material 2 are evaporated to obtain the material 3, which is put into the decolorizati...

Embodiment 3

[0043] Put hexahydrophthalic anhydride, isononanol, and catalyst acetic anhydride into the reaction kettle in proportion, wherein: the molar ratio of hexahydrophthalic anhydride to isononanol is 1:2.5, and the amount of acetic anhydride added is 1 / 2 of the quality of hexahydrophthalic anhydride 6%, heated and stirred under normal pressure, raised the temperature to 180°C and refluxed to start timing, continued to raise the temperature to react, and obtained material 1 after maintaining at 250°C for 5 hours, and material 1 was crude diisononyl cyclohexane-1,2-dicarboxylate ; The material 1 is passed through the falling film evaporator, and the excessive alcohol is flashed off under the negative pressure of -0.096MPa, and the residence time is 0.001 h to obtain the material 2, which enters the stripping tank; in the stripping tank, feed water vapor and Nitrogen gas is bubbled, and the low molecular weight impurities in the material 2 are evaporated to obtain the material 3, which...

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Abstract

The invention provides a preparation method for diisononyl cyclohexane-1,2-dicarboxylate. The preparation method comprises the following steps: 1) adding hexahydrophthalic anhydride, isononanol and acetic anhydride into a reaction vessel at the same time, carrying out heating to 180 to 300 DEG C and then carrying out stirring and dehydration for 2 to 5 h, wherein a mol ratio of hexahydrophthalic anhydride to isononanol is 1: (2-5), and the addition amount of acetic anhydride is 1 to 10% of the mass of hexahydrophthalic anhydride; 2) removing excess alcohol through flash evaporation by using a falling-film evaporator at a negative pressure of -0.02 MPa to 0.096 MPa, wherein retention time is 0.001 to 0.05 h; 3) introducing water vapor and nitrogen into a stripping tank for bubbling and removing low-molecular-weight impurities in a material 2 through evaporation; and 4) adding active carbon accounting for 1 to 10% of the mass of a material 3 into a decoloring kettle and carrying out decoloring and filtering so as to obtain the final product diisononyl cyclohexane-1,2-dicarboxylate, wherein yield reaches 98.5% and purity reaches 99.8%. According to the invention, a single-step high-temperature esterification process is employed, so reaction time is greatly shortened; excess alcohol is removed through pressure-reduced flash evaporation, so energy consumption is lowered, and the phenomenon of emulsification is avoided; and neutralization and washing are not needed, so alkaline waste water is not produced, and the preparation method is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and is a novel method for preparing a new environment-friendly plasticizer, diisononyl cyclohexane-1,2-dicarboxylate. Background technique [0002] Diisononyl cyclohexane-1,2-dicarboxylate (alias: diisononyl hexahydrophthalate, abbreviation: DINCH) is an emerging safe and environmentally friendly plasticizer, which has the same properties as diisophthalate Nonyl ester (DINP) and dioctyl phthalate (DOP) have similar structures and properties, and are mainly used in: medical drugs, food packaging, children's toys and child care products, and more importantly, their plasticized products are naturally It can be biodegraded in the environment by itself, does not cause environmental pollution, is beneficial to human health and safety, and is a good substitute for benzenecarboxylate plasticizers. Therefore, it has become a general trend to develop new products of high-efficiency, non-toxic and degradable ...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C67/52C07C67/54C07C69/75
CPCC07C67/08C07C67/52C07C67/54C07C69/75
Inventor 王天慧黄伟付春韦志强孙阿沁史乐萌
Owner CHINA PETROLEUM & CHEM CORP
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