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Continuous preparation process for environment-friendly plasticizer and device used in process

A preparation process and technology for plasticizers, applied in the field of plasticizers, can solve the problems of high energy consumption, long time-consuming synthesis process, etc.

Inactive Publication Date: 2015-07-15
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 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 novel method for continuously synthesizing DOTP in a fluidized bed. The raw materials are first slurried and then reacted. The reaction is sufficient, the time is short, and the energy is high. Low consumption and continuous production

Method used

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  • Continuous preparation process for environment-friendly plasticizer and device used in process
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  • Continuous preparation process for environment-friendly plasticizer and device used in process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Raw materials: terephthalic acid, isooctyl alcohol, tetrabutyl titanate;

[0029] After refining the isooctyl alcohol and terephthalic acid with a molar ratio of 2.2:1 to reach a particle size of 10 microns, pour into the raw material tank and start stirring to prevent sedimentation, fill the reaction tank with a feed pump, and add 1% ester catalyst For tetrabutyl titanate, turn on the condensed water, raise the temperature and turn on the circulating pump to make the material circulate and react, keep the pressure at 0.3MPa to 230°C to release the pressure; when there is a fraction distilled out, after the water is automatically separated, turn on the reflux pump and the preheater to reflux The isooctyl alcohol reaches 190°C and is re-injected into the reactor from the bottom of the reactor; when the acid value of the material in the reactor drops to 2mgKOH / g, the feed pump and outlet can be turned on to realize continuous reaction.

Embodiment 2

[0031] Raw materials: terephthalic acid, isooctyl alcohol, isopropyl titanate, sodium hypophosphite;

[0032] Refining isooctyl alcohol and terephthalic acid with a molar ratio of 2.4:1 are injected into the raw material tank and started to stir to prevent sedimentation. Fill the reactor with a feed pump and add 0.5% catalyst isopropyl titanate and antioxidant Sodium hypophosphite, turn on the condensate, heat up and turn on the circulation pump to make the material circulate and react, keep the pressure at 0.2MPa to 230°C, release the pressure and gradually vacuum to -0.005MPa; when there is a distillate, automatically divide the water, turn on the return pump And the preheater will reflow the isooctyl alcohol to 180°C and re-inject the reaction kettle from the bottom of the kettle; when the acid value of the material in the kettle drops to 2mgKOH / g, the feed pump and outlet can be turned on to realize continuous reaction.

Embodiment 3

[0034] Raw materials: terephthalic acid, isooctyl alcohol, tetrabutyl titanate, isopropyl titanate;

[0035] Refining isooctyl alcohol and terephthalic acid with a molar ratio of 2.1:1 are poured into the raw material tank and started to stir to prevent sedimentation, fill the reactor with a feed pump, and add a total of 1% catalyst tetrabutyl titanate and isopropyl titanate, turn on the condensate, heat up and turn on the circulation pump to circulate the material; when there is a fraction distilled out, the water will be separated automatically, turn on the reflux pump and preheater to bring the refluxed isooctyl alcohol to 220°C from the The bottom of the kettle is injected into the reaction kettle; when the acid value of the material in the kettle drops to 1mgKOH / g, the feed pump and outlet can be turned on to realize continuous reaction.

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Abstract

The invention relates to a continuous preparation process for an environment-friendly plasticizer and a device used in the process. The process comprises the following steps of: enabling solid terephthalic acid and isooctyl alcohol which serve as raw materials to react in the existence of an esterification catalyst and an antioxidant for continuously preparing dioctyl terephthalate (DOTP); pulpifying the solid terephthalic acid in the isooctyl alcohol until the particle size of the solid terephthalic acid reaches 5 to 20 mu m; adding the isooctyl alcohol so as to adjust the mole ratio of alcohol to acid in pulp liquid as 2:1 to 4:1; adding into a slurry tank, preheating, and entering a reaction kettle from the bottom; reacting with the preheated isooctyl alcohol which enters from the bottom of the reaction kettle in the reaction kettle in the existence of the esterification catalyst and / or the antioxidant; reacting until an acid value decreases to be below 2, and continuously feeding the raw materials namely the solid terephthalic acid and the isooctyl alcohol; and adding the DOTP which is generated in reaction from the upper part of the reaction kettle to a product tank, condensing the isooctyl alcohol which does not completely reacts and the generated steam through a condenser on the top of the reaction kettle, separating through an oil water separator, and entering an octyl alcohol tank for recirculation.

Description

technical field [0001] The invention relates to a method for continuously synthesizing DOTP (dioctyl terephthalate) using a novel fluidized bed, and belongs to the technical field of plasticizers. In particular, it involves the slurrying of raw materials, the design of reaction bed and the synthesis process of DOTP. 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. my country's annual production capacity has reached 2800kt, has become the world's largest producer and consumer, and continues to show growth momentum. Among them, the proportion of phthalates and terephthalates accounted for more than 90%. However, studies have shown that phthalic plasticizers are potentially carcinogenic, and the production of green plasticizers such as epoxy gre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/82C07C67/08
CPCC07C67/08
Inventor 蒋剑春李科陈洁许玉徐俊明陈水根
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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