Method for efficiently and environmentally friendly preparing dibutyl itaconate on basis of heterogeneous catalysis

A technology of di-n-butyl itaconate and heterogeneous catalysis, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve problems affecting product color and performance, many reaction by-products, and product color To achieve the effects of high product yield, less discharge of three wastes, and light product color

Inactive Publication Date: 2019-03-19
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Itaconic acid di-n-butyl ester is usually obtained by the esterification reaction of itaconic acid and n-butanol under concentrated sulfuric acid as a catalyst, but due to the strong oxidation of concentrated sulfuric acid, there are many by-products of the reaction, And then cause the obtained product to have dark color and low purity. In addition, the concentrated sulfuric acid corrodes the equipment seriously, produces waste water, and pollutes the environment.
And in the existing process of preparing di-n-butyl itaconate, water-carrying agents such as benzene, toluene, xylene and cyclohexane will be added to promote the removal of water produced in the reaction process, thereby accelerating the forward reaction. To improve the conversion rate, but the commonly used water-carrying agents are toxic chemicals, which pollute the environment, and after post-treatment, some of them remain in the product, affecting the color and performance of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The purchased sodium type D001 type macroporous strongly acidic cation exchange resin was washed with absolute ethanol and deionized water, and then placed in a solution with a hydrochloric acid concentration of 4% for 6 hours of replacement.

[0033] Weigh 13.01g of itaconic acid and 29.648g of n-butanol, add it into a three-necked flask with a water separator and a thermometer, magnetically stir and heat up, and weigh 0.6505g of hydrogenated D001 type strongly acidic cation after itaconic acid is completely dissolved Put the exchange resin into the three-necked flask, start timing after heating to 110°C, and react for 4 hours to obtain the crude product of di-n-butyl itaconate; stop heating, cool to room temperature and filter, and the filtrate is washed with anhydrous sodium sulfate and dried. Pressure distillation, the unreacted n-butanol obtained in the first stage is used for the next esterification reaction, and the finished product of di-n-butyl itaconate is obta...

Embodiment 2

[0035] The purchased sodium type D001 macroporous strongly acidic cation exchange resin was washed with absolute ethanol and deionized water, and then placed in a solution of 5% hydrochloric acid for 8 hours of replacement.

[0036] Weigh 13.01g of itaconic acid and 25.942g of n-butanol, add it into a three-necked flask with a water separator and a thermometer, stir it magnetically and raise the temperature, and weigh 1.301g of hydrogenated D001 type strongly acidic cation after the itaconic acid is completely dissolved Put the exchange resin into the three-necked flask, heat it to 115°C, start timing, and react for 4 hours to obtain the crude product of di-n-butyl itaconate; the subsequent purification process is the same as in Example 1 to obtain the finished product of di-n-butanol itaconate. The rate is 97.8%.

Embodiment 3

[0038] The purchased sodium type D001 macroporous strongly acidic cation exchange resin was washed with absolute ethanol and deionized water, and then placed in a solution with a hydrochloric acid concentration of 6% for 8 hours of replacement.

[0039] Weigh 26.02g of itaconic acid and 59.296g of n-butanol, add it to a three-necked flask with a water separator and a thermometer, magnetically stir and heat up, and weigh 3.2525g of hydrogenated D001 type strongly acidic cation after the itaconic acid is completely dissolved Put the exchange resin into the three-necked flask, heat it to 120°C, start timing, and react for 5 hours to obtain the crude product of di-n-butyl itaconate; the subsequent purification process is the same as in Example 1 to obtain the finished product of di-n-butanol itaconate, The rate is 96.4%.

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Abstract

The invention discloses a method for efficiently preparing dibutyl itaconate on the basis of heterogeneous catalysis. Particularly, an efficient solid acid catalyst is adopted, itaconic acid and n-butanol are catalyzed heterogeneously to react without a water-carrying agent to generate the dibutyl itaconate under the conditions that the reaction temperature is 100-140 DEG C and the reaction time is 2-5 hours; and the solid acid catalyst hydrogenated macroporous strong acid type cation exchange resin. Compared with a traditional proton acid catalysis method, the method has the characteristics that 1, the catalytic efficiency is high, the reaction time is short, and the energy consumption is low; 2, heterogeneous catalysis is carried out, a reaction product and a catalyst are easily separated, and aftertreatment is simple; 3, esterification reaction are gentle, and side reactions are less; and 4, after the catalyst is separated, the repeated utilization rate of the catalyst is high.

Description

technical field [0001] The invention relates to the field of organic synthesis, and furthermore, relates to a method for preparing di-n-butyl itaconate in an efficient and environment-friendly way based on heterogeneous catalysis. Background technique [0002] With the depletion of petrochemical resources, bio-based products have attracted more and more attention. As an important chemical raw material in modern industrial production, itaconic acid is favored because it can be obtained from biomass resources through biological fermentation, and its molecular structure contains unsaturated double bonds and active carboxyl groups. At present, domestic enterprises producing itaconic acid mainly include Qingdao Langyatai Group and Zhejiang Guoguang Biochemical Co., Ltd. Among them, Langyatai Group is the largest domestic production enterprise with an annual output of 30,000 tons. [0003] As the product of itaconate esterification reaction, itaconate is an important intermediate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/593
CPCC07C67/08C07C69/593
Inventor 张立群吴浩杰王润国雷巍巍耿漪亭张奇男
Owner BEIJING UNIV OF CHEM TECH
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