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Process for preparing benzoic ether plasticizer by using slurry method

A technology for preparing benzoic acid esters and plasticizers, which is applied in the field of pulping technology in the preparation of synthetic benzoic acid plasticizers, can solve the problems of high energy consumption and long time-consuming synthesis process, so as to improve the reaction contact surface and save Effects of energy consumption and efficiency improvement

Inactive Publication Date: 2011-08-17
JIANGSU QIANGLIN BIO ENERGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 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 for preparing benzoate plasticizers in a slurry state. The raw materials are first slurried and then reacted. The reaction is sufficient and the time is short. short

Method used

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  • Process for preparing benzoic ether plasticizer by using slurry method
  • Process for preparing benzoic ether plasticizer by using slurry method
  • Process for preparing benzoic ether plasticizer by using slurry method

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Raw materials: terephthalic acid, isooctyl alcohol, catalyst;

[0021] 300g of terephthalic acid and 480g of isooctyl alcohol were added into a refiner and pulped for 50 minutes to make a mixed slurry. Take out 130g of slurry and add it to a three-necked bottle equipped with an oil-water separator, add 14g of isooctyl alcohol, add 0.2g of tetrabutyl titanate when the temperature is raised to 160°C, gradually stir and raise the temperature to 220°C, and keep the temperature for 2 hours until the acid value is lower than 1 to end the reaction. Then dealcoholized to get plasticizers.

Embodiment 2

[0023] Raw materials: terephthalic acid, isooctyl alcohol, catalyst;

[0024] 300g of terephthalic acid and 610g of isooctyl alcohol were added into a disc refiner and slurried for 60 minutes to prepare a mixed slurry. Take out 150g of slurry and add it to a three-necked flask equipped with an oil-water separator, raise the temperature to 160°C, add 0.2g of tetrabutyl titanate, gradually stir and raise the temperature to 220°C, keep the reaction for 1 hour until the acid value is lower than 1 to complete the reaction. Then dealcoholized to get plasticizers.

Embodiment 3

[0026] Raw materials: terephthalic acid, isooctyl alcohol, catalyst;

[0027] Add 300g of terephthalic acid and 565g of isooctyl alcohol into the colloid mill for slurrying for 60 minutes to make a mixed slurry. Take out 145g of slurry and add it to a three-necked flask equipped with an oil-water separator, raise the temperature to 160°C, add 0.4g of tetrabutyl titanate, gradually stir and raise the temperature to 230°C, keep the reaction for 2 hours until the acid value is lower than 1 to complete the reaction. Then dealcoholized to get plasticizers.

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Abstract

The invention relates to a process for preparing a benzoic ether plasticizer by using a slurry method. In the process, benzoic acid and alcohol react in the presence of a catalyst to produce a benzoic ether plasticizer. The process is characterized by comprising the following steps of: slurrying solid granular, powdery or blocky raw material benzoic acid in alcohol; after the slurrying is finished, adjusting the mole ratio of the alcohol to the benzoic acid to be (1-4):1; then mixing with a conventional catalyst which accounts for 0.1-0.2% of the mass of the raw material benzoic acid, raisingthe temperature to 210-240 DEG C gradually while stirring in a reactor with an oil-water separator, reacting for 1-4h under heat insulation and ending the reaction till the acid value is lower than 1; and then performing conventional dealcoholization and purification treatment to obtain the benzoic ether plasticizer. The invention has the advantages that the original solid benzoic acid raw material is slurried under the condition that original equipment is not necessary to change completely, therefore, the reaction contact area of two phases is increased, the reaction speed is increased greatly, the efficiency is increased and the energy is saved.

Description

technical field [0001] The invention relates to a preparation method for synthesizing benzoic acid plasticizers by pulping technology, in particular to a method for preparing plasticizers by using mechanical grinding equipment to pulp solid raw materials and then performing a synthesis reaction. Background technique [0002] As we all know, plasticizers are substances added to increase plasticity, fluidity and flexibility of finished products when processing high polymers such as rubber, plastics, coatings, etc., and are essential additives in the plastics industry. my country's annual production capacity has reached 2,800 kt, and it has become the world's largest production and consumption country, 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 grease and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/82C07C69/80C08K5/12C09D7/12
Inventor 蒋剑春周永红李科冯国东聂小安陈洁许彬陈玉湘
Owner JIANGSU QIANGLIN BIO ENERGY
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