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Method for preparing terephthalic acid ester plasticizer with pressurization method

A technology for terephthalate and terephthalic acid, applied in the field of synthesizing terephthalate plasticizers, can solve the problems of unsuitability for industrial production, long process cycle, long reaction time, etc., and achieve product separation Simple and efficient purification, promotion of diffusion, and stable product performance

Inactive Publication Date: 2012-12-05
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007]1. The traditional atmospheric pressure esterification process is adopted, the reaction time is longer, usually longer than 6 hours, and the reaction temperature is mostly 180-250°C, the process cycle is long and energy consumption bigger
[0008]2. Although other processes (such as microwave method) can greatly increase the reaction time, they consume a lot of energy and are not suitable for industrial production

Method used

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  • Method for preparing terephthalic acid ester plasticizer with pressurization method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] In the first step, according to the mass ratio, mix 100 parts of purified terephthalic acid, 160 parts of isooctyl alcohol, and 0.5 parts of tetrabutyl titanate into the high-pressure reactor, set the pressure threshold to 0.10 MPa, raise the temperature and pressurize, when When the temperature rises to 180 °C, start stirring, control the stirring speed at 1000 r / min, maintain the reaction temperature at 180 °C, and react for 3 h under the threshold pressure, and the acid value of the product is ≤1. During the reaction process, when the reaction pressure exceeds the set threshold, the pressure reducing valve will automatically open, exhaust and adjust the pressure, and the exhausted gas will be recovered after being condensed.

[0038] In the second step, after the reaction is completed, cooling water is passed through the kettle body. When the temperature is lower than 180 ° C, the gas outlet valve is opened to discharge the remaining gas, which is recovered after cond...

Embodiment 2

[0042] In the first step, according to the mass ratio, mix 100 parts of purified terephthalic acid, 240 parts of isooctyl alcohol, and 2.5 parts of tetrabutyl titanate into the high-pressure reactor, set the pressure threshold to 1.6 MPa, raise the temperature and pressurize, when When the temperature rises to 180°C, start the stirring, control the stirring speed at 1000 r / min, continue to raise the temperature to 250°C, and react at the threshold pressure for 1 hour, and the acid value of the product is ≤1. During the reaction process, when the reaction pressure exceeds the set threshold, the pressure reducing valve will automatically open, exhaust and adjust the pressure, and the exhausted gas will be recovered after being condensed.

[0043] In the second step, after the reaction is completed, the cooling water is passed through the kettle body. When the temperature is lower than 180°C, the gas outlet valve is opened to discharge the remaining gas, which is recovered after c...

Embodiment 3

[0047] In the first step, according to the mass ratio, mix 100 parts of purified terephthalic acid, 240 parts of isooctyl alcohol, and 2.5 parts of tetraisobutyl titanate into the high-pressure reactor, set the pressure threshold to 1.0 MPa, raise the temperature and pressurize, When the temperature rises to 180°C, start stirring, control the stirring speed at 1000 r / min, continue to raise the temperature to 220°C, and react for 2 hours under the threshold pressure, and the acid value of the product is ≤1. During the reaction process, when the reaction pressure exceeds the set threshold, the pressure reducing valve will automatically open, exhaust and adjust the pressure, and the exhausted gas will be recovered after being condensed.

[0048] In the second step, after the reaction is completed, the cooling water is passed through the kettle body. When the temperature is lower than 180°C, the gas outlet valve is opened to discharge the remaining gas, which is recovered after con...

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Abstract

The invention provides a method for preparing terephthalic acid ester plasticizer with a pressurization method. The method comprises the following steps that terephthalic acid, alcohol and a catalyst are mixed to be subjected to esterification reaction to obtain a terephthalic acid ester raw-product, and the terephthalic acid ester raw-product is subjected to neutralization washing and reduced pressure distillation to obtain a terephthalic acid ester finished-product; the esterification reaction is carried out in a high-pressure reactor under pressurization; in the reaction process, the pressure keeps at most 1.6MPa, and the reaction temperature is at most 250 DEG C; when the system pressure is beyond 1.6MPa in reaction, a reducing valve is turned on to exhaust and reduce pressure, and gas is recovered to be condensed; the reaction is carried out for 1-3 hours and then is finished until the acid value of a product is at most 1; and in the reaction, the alcohol is excessive, and the alcohol is C1-10. The method uses the terephthalic acid as a raw material to prepare the terephthalic acid ester plasticizer under the condition of pressurization. The variety of the raw material is not strictly restricted, the reaction time is short, the operation is simple and easy, the used solvents can be efficiently recovered, and the environment is friendly. The method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technique of synthesizing terephthalate plasticizers, in particular to a method for preparing terephthalate plasticizers by pressurization. Background technique [0002] Terephthalate-based plasticizers mainly diisooctyl terephthalate (DOTP) are new polyolefin green plasticizers that have developed rapidly in recent years. Compared with traditional plasticizers such as: Dioctyl phthalate (DOP), DOTP has excellent insulation properties, low volatility, good thermodynamic properties and good compatibility with PVC resin, it has attracted the attention of the rubber and plastic industry at home and abroad, and has become a DOP in the market The leading alternative. The preparation of high value-added terephthalate plasticizers from industrial purified terephthalic acid rich in terephthalic acid (PTA) has important social value and market prospects. [0003] The existing DOTP production process mostly uses terephthalic acid a...

Claims

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Application Information

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IPC IPC(8): C07C69/82C07C67/08
Inventor 蒋剑春王奎周永红李科司展吴欢陈水根应浩
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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