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Method for synthesizing phthalate compounds

A technology for ester compounds and phthalic acid, applied in the field of synthesis of phthalic acid ester compounds, can solve the problems of poor stability, difficult to realize industrialization, low catalytic activity, etc., and achieve a simplified separation process and a long time , Improve the conversion rate, the effect of less side reactions

Inactive Publication Date: 2015-05-06
NANJING COLLEGE OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For now, a variety of catalytic systems have been developed, including liquid acids, salts, heteropolyacids and their immobilization, solid (super) acids, etc. except concentrated sulfuric acid, but these catalysts generally have low catalytic activity ( Reaction temperature is generally at 200 ℃ or above), stability is not very good (such as various loaded solid acids, salts, etc.) and other obvious deficiencies, it is difficult to realize industrialization

Method used

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  • Method for synthesizing phthalate compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 50 grams of phthalic anhydride in the 250 milliliter three-necked flask with stirring, water separator and reflux condenser, the addition of n-butanol is 2.4 times of the molar number of phthalic anhydride, 0.25 grams of catalyst (by weight In percent, sodium bisulfate: tetrabutylammonium bromide: Polyethylene Glycol=10:1.0:0.1), after heating up to boiling reaction 1h, obtain the catalytic performance of this catalyst with chromatographic analysis: phthalic anhydride conversion ratio The yield of dibutyl phthalate was 99.1%, and the yield of dibutyl phthalate was 98.0%.

Embodiment 2

[0026] Add 50 grams of phthalic anhydride to a 250-milliliter three-neck flask with stirring, water separator and reflux condenser, the addition of n-butanol is 4.0 times the molar number of phthalic anhydride, and 2.0 grams of catalyst (by weight Percentage, potassium hydrogensulfate:polyethylene glycol=10:0.1), after heating up to boiling reaction 2h, obtain the catalytic performance of this catalyst with chromatographic analysis: phthalic anhydride conversion rate is 93.5%, phthalic acid di Butyl ester yield was 93.2%.

Embodiment 3

[0028] Add 50 grams of phthalic anhydride in a 250 ml three-necked flask with stirring, water separator and reflux condenser, the addition of n-butanol is 2.4 times the molar number of phthalic anhydride, 2.5 grams of catalyst (by weight Percentage, sodium bisulfate: tetrabutylammonium bromide=10:0.8), be warming up to boiling reaction after 0.5h, obtain the catalytic performance of this catalyst with chromatographic analysis: phthalic anhydride conversion rate is 94.6%, o-phthalic anhydride The yield of dibutyl dicarboxylate was 94.2%.

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Abstract

The invention provides a method for synthesizing phthalate compounds. By taking a weak acid as a main catalyst assisted by a composite catalyst formed by other co-catalysts, the phthalate compounds are synthesized. The method specifically comprises the following steps: adding phthalic anhydride, alcohol and the composite catalyst into a reactor, wherein the molar ratio of phthalic anhydride and alcohol is 1: (2.1-5.0) and the addition of the composite catalyst is 0.2-10wt% of phthalic anhydride; and sealing the reactor, raising the temperature till boiling, reacting for 0.5-2 hours and rectifying to obtain a product. The method not only can realize a catalytic effect of concentrated sulfuric acid, but also overcome the defects. Moreover, the used catalyst can be separated and reused by using a conventional method, so that the separating flow is greatly simplified and continuous production is facilitated.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and relates to a method for synthesizing phthalates. Background technique [0002] Phthalate, also known as phthalate, abbreviated as PAE, is a general term for esters formed by phthalic anhydride. Phthalates have excellent comprehensive processing properties, high plasticizing efficiency, low volatility, and good cold resistance, flexibility, and electrical properties. Phthalates, mainly used as plasticizers (plasticizers), are added to plastics to enhance elasticity, transparency, durability and longevity, and are widely used in a variety of products, such as pills and nutritional supplements casings, viscosity agents, gelling agents, membrane aids, stabilizers, dispersants, lubricants, binders, emulsifiers and suspending agents, etc. [0003] When phthalates are used as plastic plasticizers, they generally refer to esters formed between phthalic acid and alcohols containing 1 to 1...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/80C07C67/08B01J31/26B01J31/06
Inventor 吴永忠丁志平李亭亭李新月
Owner NANJING COLLEGE OF CHEM TECH
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