Method for preparing catalyst for catalytic synthesis of dialkyl succinate

A catalyst and sulfate technology are applied in the field of catalyst preparation for catalytic synthesis of dialkyl succinate, can solve problems such as difficulty in reaction, and achieve the effects of easy product separation, good catalyst stability and high catalytic activity

Inactive Publication Date: 2013-06-26
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the sulfonation reaction is an electrophilic substitution reaction. When the electron cloud density on the benzene ring decreases, the reaction will be more difficult

Method used

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  • Method for preparing catalyst for catalytic synthesis of dialkyl succinate

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Experimental program
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Effect test

Embodiment 1

[0034] Add 100 g of macroporous styrene-based strong-acid cation exchange resin into a reactor equipped with a stirrer, a reflux condenser, a thermometer, and a dropping funnel, add 150 ml of concentrated HCl, and add concentrated H 2 SO 4 30ml, FeCl 3 ·6H 2 O 3g, slowly drop in 30mlH from the dropping funnel 2 o 2 Solution, reacted at 60°C for 3h. Filter the reaction product, wash it with acid and then wash it with water to neutrality, and dry it in vacuum at 80°C to obtain the chlorinated heat-resistant resin;

[0035] Put 100% succinic acid and n-butanol with a molar ratio of 1:3.4 into a reactor equipped with a water separator, agitator, thermometer and condenser, and add 3% of the total reactant mass obtained in the previous step The chlorinated heat-resistant resin catalyst was used, the reaction temperature was 115°C, and the reaction time was 60 minutes to obtain the esterified product. The esterification rate is listed in Table 1.

Embodiment 2

[0039] Add 100 g of macroporous styrene-based strong-acid cation exchange resin into a reactor equipped with a stirrer, a reflux condenser, a thermometer, and a dropping funnel, add 150 ml of concentrated HCl, and add concentrated H 2 SO 4 50ml, FeCl 3 ·6H 2 O 10g, slowly add 60mlH from the dropping funnel 2 o 2 Solution, reacted at 90°C for 6h. Filter the reaction product, wash it with acid and then wash it with water to neutrality, and dry it in vacuum at 80°C to obtain the chlorinated heat-resistant resin;

[0040] Put 80% succinic acid aqueous solution and n-butanol with a molar ratio of 1:3.4 into a reactor with a water separator, agitator, a thermometer and a condenser tube, and add 3% of the total reactant mass prepared in the previous step. The obtained chlorinated heat-resistant resin catalyst was filtered at a reaction temperature of 115°C and a reaction time of 60 minutes. The used chlorinated heat-resistant resin was washed several times with absolute ethanol...

Embodiment 3

[0044] Add 100 g of macroporous styrene-based strong-acid cation exchange resin into a reactor equipped with a stirrer, reflux condenser, thermometer, and dropping funnel, add 120 ml of concentrated HCl, and add 120 ml of concentrated HCl. 2 SO 4 30ml, FeCl 3 ·6H 2 O 5g, slowly add 45mlH from the dropping funnel 2 o 2 Solution, reacted at 80°C for 4h. Filter the reaction product, wash it with acid and then wash it with water to neutrality, and dry it in vacuum at 80°C to obtain the chlorinated heat-resistant resin;

[0045] Immerse the chlorinated heat-resistant resin prepared in the previous step in 1% CaSO 4 After immersing in the solution for 1 hour at room temperature, evaporate to dryness with a rotary evaporator at 80°C, take it out and dry it in vacuum at 80°C to obtain a chlorinated heat-resistant calcium sulfate-loaded modified resin catalyst;

[0046] Put 70% succinic acid aqueous solution and n-butanol with a molar ratio of 1:3.4 into a reactor with a water s...

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Abstract

The invention discloses a method for preparing a catalyst for catalytic synthesis of dialkyl succinate, and specifically relates to a modified ion exchange resin catalyst and a preparation method thereof. The preparation method comprises the following steps of: (1) enabling macroporous styrenic strongly-acidic cation exchange resin to have substitution reaction on styrene to generate chlorinated temperature-resistant resin; and (2) steeping the chlorinated temperature-resistant resin in alkaline earth metal sulfate solution at room temperature, thereby obtaining chlorinated temperature-resistant alkaline earth metal sulfate loaded modified resin catalyst. The preparation method of the catalyst avoids the problems of difficulty of sulfonation after halogenation and low exchange quantity through direct chlorination of the macroporous styrenic strongly-acidic cation exchange resin which is low in cost and easily available, and then the alkaline earth metal sulfate loaded modified resin catalyst is adopted and applied to catalytic esterification reaction of succinic acid and alcohol; and the catalyst shows excellent heat resistant stability and efficient catalytic activity.

Description

technical field [0001] The invention relates to a catalyst preparation method for catalyzing and synthesizing dialkyl succinate, in particular to a modified ion exchange resin catalyst and a preparation method thereof. Background technique [0002] Succinic acid is a common natural organic dibasic acid, which widely exists in human body, plants, animals and microorganisms in nature. Because it has two carboxylic acid groups in its molecular structure, it can react with some alcohols to produce mono- and di-ester compounds. These monoester and diester compounds can not only be directly applied in the fields of food, drug synthesis, functional synthetic materials, etc., but also can derive a series of new compounds through their own special molecular structure, which are widely used in drugs, organic pigments, etc. and other industries. With the development of modern chemical industry, succinate and its derivatives are playing an increasingly important role, and their applic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/26C07C69/40C07C67/08
Inventor 任晓乾梁金花刘艳秋武文良姜岷
Owner NANJING UNIV OF TECH
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