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Cleaning production method of phthalic acid di-(2-ethyl) ethyl ester

A technology for the clean production of phthalic acid di- and phthalic acid, which is applied in the field of synthesis process in the chemical industry, can solve the problems of large amount of waste water, etc., and achieve the effect of reducing water consumption and reducing the amount of waste water generated

Active Publication Date: 2010-08-18
江苏雷蒙新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] From the above process, it can be seen that there are many links in the DOTP production process that produce wastewater, and the amount of wastewater is relatively large.

Method used

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  • Cleaning production method of phthalic acid di-(2-ethyl) ethyl ester

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Example 1, a clean production method of di(2-ethyl)hexyl phthalate, put purified terephthalic acid and octanol into a reaction kettle, carry out esterification under the action of a catalyst, neutralize with alkaline water, Vacuum dealcoholization and filtration to obtain finished products, and the esterification water generated during production is recycled:

[0023] (1) Collect and pretreat the esterification water generated by the esterification reaction. The pretreatment method is: heat the esterification water to boiling, evaporate 3-5% of the total weight of the esterification water to the sewage collection pool, The remaining water is the treated esterified water for subsequent use;

[0024] (2) Prepare a part of the treated esterification water and solid sodium hydroxide to prepare high-concentration alkaline water for neutralization of the subsequent esterification reaction solution. The concentration of alkaline water can be adjusted to a mass percentage conce...

Embodiment 2

[0027] Example 2, add 350g of PTA, 825g of octanol, and 2g of activated carbon into a 1500ml flask with a stirrer and a distillation device, stir and rapidly heat the mixture in the flask to 185°C, and add 0.9g of titanate catalyst to carry out esterification reaction , when the temperature of the mixture in the flask was raised to 215°C, 0.6g of the same catalyst as above was added, and the esterification time was 6 hours, and about 77ml of esterified water generated by the reaction was distilled off, and the temperature of the mixture in the flask rose to about 225°C, and the material When the acid value is 0.08mgKOH / g, turn off the heat source, vacuum dealcohol, lower the temperature of the mixture in the flask to 170°C±3°C, add 1.0ml of 25% NaOH lye and stir for 30min, continue vacuuming and slowly introduce 50ml of The treated esterified water was dealcoholized for 2 hours, and the temperature of the material in the flask was kept above 150°C. After the completion, the vac...

Embodiment 3

[0029] Example 3, 4.4 tons of PTA, 10.3 tons of octanol, and 20 kg of active carbon were added to 20 m 3 Stirrer in the reaction kettle, and heat the material to 185 ° C, add 5.3 kg of titanate catalyst for esterification, when the esterification reaction reaches the temperature of the kettle to 215 ° C, then add the same catalyst 3.5 kg, the esterification time is 7 hours, distill Remove about 951kg of esterified water generated by the reaction. When the temperature of the reactor rises to about 225°C and the acid value of the material in the reactor is ≤0.08mgKOH / g, the esterification reaction ends. Lower to 170°C±3°C, add 13kg of 25% NaOH lye, stir for another 30min, continue vacuuming and slowly introduce 500kg of treated esterified water for vacuum stripping and dealcoholization for 1.5 hours, and keep the temperature of the reactor at 160°C. After testing that the octanol content of the material is <500ppm, continue vacuuming until the moisture content of the material is...

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Abstract

The invention provides a cleaning production method of phthalic acid di-(2-ethyl) ethyl ester, which comprises the following steps of: putting purified phthalic acid and octanol into a reaction kettle; esterifying under the function of catalytic agent; neutralizing with alkaline water; performing dealcholization in vacuum; and filtering to obtain the finished product. The recycle of the esterified water in the production method comprises the step of collecting and pretreating the esterified water which is generated by esterification, wherein some treated esterified water is used for preparing the high-concentration alkaline water for neutralizing the follow-on esterification solution, and the residual treated esterified water is used for dealcholization in vacuum. with the recycle, the cleaning production method does not use the process water, thereby greatly reducing the production quality of waste water, and archiving the effect of cleaning production.

Description

technical field [0001] The invention belongs to the synthesis process in the field of chemical industry, in particular to a clean production method of di(2-ethyl)hexyl phthalate, and specifically relates to a clean production method that reduces waste water, saves water resources, and is beneficial to environmental protection. Background technique [0002] Di(2-ethyl)hexyl terephthalate, also known as dioctyl terephthalate, or DOTP for short, is mainly used as a plasticizer for PVC. With the further improvement of human's toxicological understanding of chemicals and environmental awareness, the proportion of traditional o-phthalic plasticizers is greatly reduced year by year, and they are replaced by environmentally friendly plasticizers such as DOTP, ATBC, and DINCH. As an environmentally friendly plasticizer with excellent performance and moderate cost performance, DOTP is being rapidly recognized by the market and has grown significantly. [0003] There are three main pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/82C07C67/08
Inventor 周永芳陈平曹立军
Owner 江苏雷蒙新材料有限公司