Continuous synthesis method of cyclohexane polyacid ester

A polybasic acid ester and cyclohexane technology, which is applied in the field of synthesizing cyclohexane polybasic ester, can solve the problems of large energy consumption and cumbersome steps, and achieve the effects of energy saving, production cost reduction, time and energy saving

Active Publication Date: 2015-11-11
中山联成化学工业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The current technology must purify diisononyl phthalate and then hydrogenate it. The steps are cumbersome, energy consumption is large, and the conversion rate of diisononyl phthalate can only reach 99%.

Method used

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  • Continuous synthesis method of cyclohexane polyacid ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add phthalic anhydride and isononyl alcohol with a molar ratio of 1:2.5 into the stirred tank reactor, and the reactor uses an alcohol-water reflux layering device, and then adds an acid catalyst and heats to 220°C for esterification reaction, as shown in the formula Shown in I, react to the acid value of diisononyl phthalate crude product below 0.2mgKOH / g, gained diisononyl phthalate crude product contains excess isononyl alcohol (containing about 85% phthalate diisononyl formate and approximately 15% isononyl alcohol). Take 3.9g of X catalyst and fill it in a stainless steel continuous trickle bed reactor with a diameter of 3 / 8 inches as a fixed bed (filling 6mL), and then directly feed the crude product of the esterification reaction without purification To the trickle bed reactor for hydrogenation reaction, as shown in formula I, the hydrogen pressure is 50bar, the temperature is 70°C, the hydrogen flow rate is 100mL / min, the esterification reaction crude product fl...

Embodiment 2

[0038]Add phthalic anhydride and isononyl alcohol with a molar ratio of 1:2.5 into the stirred tank reactor. The reactor uses an alcohol-water reflux layering device, and then adds an acid catalyst and heats it to 220°C for esterification reaction. The acid value of the crude diisononyl phthalate is lower than 0.2 mgKOH / g, and the obtained crude diisononyl phthalate contains excess isononyl alcohol. Take 3.9g of X catalyst and fill it in a stainless steel continuous trickle bed reactor with a diameter of 3 / 8 inches as a fixed bed (filling 6mL), and then directly feed the crude product of the esterification reaction without purification To the trickle bed reactor for hydrogenation reaction, the hydrogen pressure is 50bar, the temperature is 100°C, the hydrogen flow rate is 100mL / min, the esterification reaction crude product flow rate is 4.5mL / h, the hydrogen and diisononyl phthalate The molar ratio is about 28:1. After the reaction, add alkali to neutralize and remove acid, d...

Embodiment 3

[0041] Add phthalic anhydride and isononyl alcohol with a molar ratio of 1:2.5 into the stirred tank reactor. The reactor uses an alcohol-water reflux layering device, and then adds an acid catalyst and heats it to 220°C for esterification reaction. The acid value of the crude diisononyl phthalate is lower than 0.2 mgKOH / g, and the obtained crude diisononyl phthalate contains excess isononyl alcohol. Take 3.9g of X catalyst and fill it in a stainless steel continuous trickle bed reactor with a diameter of 3 / 8 inches as a fixed bed (filling 6mL), and then directly feed the crude product of the esterification reaction without purification To the trickle bed reactor for hydrogenation reaction, the hydrogen pressure is 50bar, the temperature is 120°C, the hydrogen flow rate is 100mL / min, the crude product flow rate of the esterification reaction is 4.5mL / h, the hydrogen and diisononyl phthalate The molar ratio is about 28:1. After the reaction, add alkali to neutralize and remove...

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Abstract

The invention relates to a synthesis method of cyclohexane polyacid ester. The method specifically comprises the following steps of: adding benzene polycarboxylic acid or anhydride thereof and alcohol into a stirring tank reactor; adding in an acid catalyst and raising the temperature to 200-240 DEG C; carrying out some reaction until an acid value is less than 0.2 mg KOH/g; directly adding a crude product resulting from the esterification reaction into a trickle bed reactor for hydrogenation reaction, wherein the hydrogen pressure is 40-100 bar, the temperature is 70-250 DEG C, and a catalyst is a porous oxide loaded with VIII B group metal; and after the reaction, adding in alkali for neutralization and acid removal, performing distillation or evaporation to remove alcohol, removing by-products; and performing filtration and deliming to obtain cyclohexane polyacid ester. According to the method provided by the invention, after the esterification reaction generates the crude product, no purification step is not performed; excess alcohol is used as a solvent for subsequent hydrogenation reaction; and after the hydrogenation reaction, purification steps such as alcohol removing, acid removing and filtration are performed, thereby saving time and energy. Meanwhile, according to the method provided by the invention, the alumina-magnesia composite oxide is used as the catalyst carrier, and palladium or ruthenium is selected as the metal catalyst, enabling the phenyl ring hydrogenation rate to be greater than 99.9%.

Description

technical field [0001] The invention relates to a method for synthesizing cyclohexane polybasic acid ester, in particular to a method for continuously esterifying and reducing raw materials to obtain cyclohexane polybasic acid ester. Background technique [0002] In recent years, it has been discovered that phthalate plasticizers may be harmful to human health. They can enter the human body through drinking, eating, skin contact and breathing. Long-term exposure to such compounds can cause damage to the peripheral nervous system and cause multiple neuropathy Inflammation and dysesthesia, numbness and other symptoms. The World Health Organization also pointed out that the hydrolysis metabolites of phthalates (especially short-chain phthalates) in the human body are likely to affect the metabolism and reproductive functions in organs, so they belong to environmental hormones and have biological functions. Cumulative. Therefore, many countries and regions (including the Europ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/75C07C67/303
CPCC07C67/08C07C67/303C07C69/75C07C69/80C07C69/76
Inventor 郑晓娜蔡满富刘治河马潮轸王敏玲陈连展
Owner 中山联成化学工业有限公司
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