Novel continuous production technique of phthalate plasticizer

A technology of ester plasticizers and phthalic acid, which is applied in the new process field of continuous production of phthalate plasticizers, can solve the problems of long time-consuming and high energy consumption in the esterification process, and achieve energy-enhancing Effects of utilization efficiency, reduction of production energy consumption, and improvement of esterification efficiency

Inactive Publication Date: 2015-12-02
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

During the reaction process, a large amount of raw material alcohol is evaporated, and then refluxed to the reac

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A mixture of 110 parts by mass of raw material phthalic anhydride, 300 parts by mass of raw material isooctyl alcohol, and 4 parts by mass of catalyst tetrabutyl titanate is continuously fed into the first-stage esterification tank at 50 g / min to 5000 g / min, and the raw materials are isooctanol Octanol is continuously fed into the 5-stage esterification kettle at 0.5-1000g / min, and nitrogen gas is continuously passed into the 5-stage esterification kettle at 0.1L / min-5L / min, and the residence time of the material in each stage of the esterification kettle is kept at 0.2 h ~ 1h, while ensuring that the liquid phase temperature in each level of esterification tank gradually rises from 180 ° C to 230 ° C; after 5 hours of reaction, the acid value of the crude product of dioctyl phthalate discharged from the fifth level esterification tank is 0.2 ~ 0.5 mgKOH / g, color number (Pt-Co) is 15~30.

Embodiment 2

[0019] A mixture of 300 parts by mass of raw material phthalic anhydride, 400 parts by mass of raw material butanol, and 2 parts by mass of catalyst 98% concentrated sulfuric acid is continuously fed into the primary esterification tank at 50 g / min to 5000 g / min, and the raw material butanol is 0.5-1000g / min is continuously fed into the 5-stage esterification kettle, and nitrogen gas is continuously passed into the 5-stage esterification kettle at 0.1L / min-5L / min, and the residence time of the material in each stage of the esterification kettle is kept at 0.2h-1h , and at the same time ensure that the liquid phase temperature in each level of esterification tank gradually rises from 130°C to 150°C; after 4 hours of reaction, the acid value of the crude product of dibutyl phthalate discharged from the 5th level esterification tank is 1.8~2.5mgKOH / g , the color number (Pt-Co) is 15~30.

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Abstract

The invention relates to a novel continuous production technique of a phthalate plasticizer. The technique comprises the following steps: raw materials phthalic anhydride and monobasic alcohol and a catalyst are continuously introduced into a first-stage esterification kettle, and a small amount of monobasic alcohol is continuously introduced into a fifth-stage esterification kettle; liquid-phase materials of all stages of esterification kettles gradually flow to the fifth-stage esterification kettle from the first-stage esterification kettle via a liquid-phase pipeline and flow out of the fifth-stage esterification kettle, thereby obtaining a reaction product; gas-phase materials of all stages of esterification kettles are gradually introduced into the first-stage esterification kettle from the fifth-stage esterification kettle via a gas-phase pipeline and enter a packing tower; and the temperatures of all stages of esterification kettles are kept at 130-230 DEG C, the gage pressures are kept at 0-2atm, and the retention time is kept at 0.2-2 hours. The acid number of the bottom discharge product of the fifth-stage esterification kettle is 0.2-2.5 mg KOH/g. The novel technique for continuously producing the phthalate plasticizer greatly reduces the esterification time and energy consumption, and enhances the economic benefit.

Description

technical field [0001] The invention relates to a new process for continuous production of phthalate plasticizers. Background technique [0002] Phthalate plasticizers are the plasticizers with the largest output, the largest amount, and the most widely used varieties. It is prepared by esterification reaction with phthalic anhydride and corresponding monoalcohol as raw material under the action of catalyst. [0003] The production methods of phthalate plasticizers in industry mainly include batch method, continuous method and semi-continuous method. For plasticizers with large output, continuous production is generally adopted, and multiple CSTR reactors are used in series to carry out multi-stage esterification while maintaining excess raw material alcohol. During the reaction process, a large amount of raw material alcohol is evaporated, and then condensed and refluxed to the reaction system. The entire esterification process takes a long time and consumes a lot of ener...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/80
CPCC07C67/08C07C69/80
Inventor 奚桢浩赵玲李双成
Owner EAST CHINA UNIV OF SCI & TECH
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