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Method and device for synthesizing plasticizer by regulating pressure

A technology for adjusting pressure and plasticizers, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of short reaction time, long time-consuming synthesis process, high energy consumption, etc., achieve color improvement and save energy Effects that consume and increase the reaction rate

Inactive Publication Date: 2013-09-25
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Technical problem to be solved: In order to solve the shortcomings of long time-consuming and high energy consumption of the synthesis process in the prior art, the present invention provides a method and device for quickly synthesizing DOTP by adjusting pressure, using a pressure vessel to synthesize DOTP under different pressures, and the reaction time Short, simple steps, no need to change other conditions such as the existing reaction ratio

Method used

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  • Method and device for synthesizing plasticizer by regulating pressure
  • Method and device for synthesizing plasticizer by regulating pressure

Examples

Experimental program
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Effect test

Embodiment 1

[0024] A device for adjusting pressure to synthesize a plasticizer, including a pressure-resistant kettle 1, a funnel line 2, a rectification tower 3, a pressure relief valve 4, a condenser 5 and a recovery tank 6, and the rectification tower 3 is located in the pressure-resistant kettle 1 The upper part of the funnel pipeline 2 is arranged in the pressure-resistant kettle 1, the outlet at the bottom of the rectification tower 3 is opposite to the upper inlet of the funnel pipeline 2, the upper part of the rectification tower 3 is connected with the recovery tank 6 through the condenser 5, and the pressure relief valve 4 It is arranged on the connecting pipeline between the rectification column 3 and the condenser 5. There is a gap between the bottom outlet of the rectification tower and the upper inlet of the funnel pipeline.

[0025] Raw materials: terephthalic acid, isooctyl alcohol, catalyst tetrabutyl titanate;

[0026] Put isooctyl alcohol and terephthalic acid with an ...

Embodiment 2

[0028] Raw materials: pool material PTA, isooctyl alcohol, catalyst isopropyl titanate, antioxidant sodium hypophosphite; the device is the same as in Example 1.

[0029] Put isooctyl alcohol with an alkyd molar ratio of 3.2:1 and pool material PTA into an autoclave, heat to 150°C for dehydration, then add 0.15%wt of isopropyl titanate and 0.1%wt of sodium hypophosphite to the reaction system Heating and stirring, pressurized reaction, when the temperature reaches 220°C and the pressure reaches 0.3MPa, the pressure control device will automatically exhaust the pressure and discharge the water generated in the reaction to the recovery tank, maintain the pressure at 0.25MPa, and release it after 1 hour of reaction Pressure to normal pressure reaction, the temperature rises again to 210°C within 2 to 3 hours, and gradually vacuums to -0.01MPa within 1 to 2 hours, and the pressure reaction can be stopped when the acid value is less than 1mgKOH / g. During the process, gaseous isooct...

Embodiment 3

[0031] Raw materials: ground material PTA, isooctyl alcohol, catalyst dibutyltin p-toluenesulfonate; the device is the same as in Example 1.

[0032] Put isooctyl alcohol with an alkyd molar ratio of 3:1 and the ground material terephthalic acid into an autoclave, heat to 160°C for dehydration, then add dibutyltin di-p-toluenesulfonate accounting for 0.3%wt of the reaction system, heat and stir, Pressurized reaction, when the temperature reaches 240°C and the pressure reaches 0.4MPa, the pressure control device automatically exhausts the pressure and discharges the water generated in the reaction to the recovery tank to maintain the pressure at 0.3MPa. After 1.5 hours of reaction, release the pressure to normal pressure for reaction, and the temperature rises to 200°C again within 2 to 3 hours, and gradually vacuum to -0.03MPa within 1 to 2 hours. When the acid value is less than 1mgKOH / g, the belt can be stopped. Pressure reaction, gaseous isooctyl alcohol is refluxed through...

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Abstract

The invention provides a method and a device for synthesizing a plasticizer by regulating pressure, using terephthalic acid, isooctyl alcohol and a catalyst as raw materials, wherein a mol ratio of isooctyl alcohol to terephthalic acid is 2.0-3.2:1, weight of the catalyst is 0.1-2% of that of a reaction system. The method comprises: adding the raw materials into a pressure resistant kettle, raising the temperature to 200-240 DEG C, maintaining the reaction pressure at 0-0.4MPa, discharging moisture generated in the reaction by a decompression valve when pressure is raised over 0.3-0.4MPa, and decompressing after 0.5-3h to normal pressure; and raising the temperature to 200-230 DEG C in 1-4h, then regulating negative pressure to -0.1-0MPa in 1-2h, and reaching a reaction endpoint until an acid value is less than 1mgKOH / g, wherein isooctyl alcohol in gaseous state flows back by a rectifying tower in the reaction process, and enters from a kettle bottom by a funnel tube. The method and the device provided in the invention can rapidly synthesize DOTP by regulating pressure, time is shortened, and energy consumption is reduced.

Description

technical field [0001] The invention belongs to the technical field of plasticizer synthesis, and in particular relates to a method and a device for synthesizing DOTP by using a pressure vessel. Background technique [0002] As we all know, plasticizer is a substance added to increase the plasticity, fluidity and flexibility of the finished product when processing high polymers such as rubber, plastics, and coatings. It is an indispensable additive in the plastics industry. And my country has become the world's largest producer and consumer. Among them, the proportion of phthalates and terephthalates accounts for more than 90%, but in recent years, studies have shown that phthalate plasticizers are potentially carcinogenic, and they are replaced by diisophthalic acid terephthalate. The rise of the octyl ester (DOTP) industry. However, the old-fashioned synthesis process with alcohol and water is mostly used, the reaction time is too long, the energy consumption is high, an...

Claims

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Application Information

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IPC IPC(8): C07C69/82C07C67/08
Inventor 蒋剑春李科许玉王奎陈水根许彬应浩陈洁
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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