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Method for preparing dibutyl itaconate

A technology of di-n-butyl itaconate and itaconic acid, applied in the field of preparing di-n-butyl itaconate, achieving the effects of easy separation and post-treatment, high yield and low reaction temperature

Active Publication Date: 2014-03-19
QINGDAO LANGYATAI GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The easiest way to prepare di-n-butyl itaconate is to use concentrated sulfuric acid as the direct esterification method of catalyst, but due to the strong oxidizing characteristics of concentrated sulfuric acid and the imperfect production process, there are many side reactions, which lead to the production of the obtained product Problems such as dark color, low purity, and the production of three wastes (especially waste water) in the production process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Buy itaconic acid, n-butanol, strong acid ion exchange tree, hydroquinone, benzene, toluene and xylene from the market, weigh 100Kg itaconic acid, 140Kg n-butanol, 5Kg strong acid ion exchange resin, 1Kg of hydroquinone was added to the reactor in turn. The reactor was equipped with a stirrer and a thermometer. The stirrer was turned on to mix the raw materials in the reactor. After heating to 130°C, it started to count and reacted for 6 hours to obtain itaconic acid. The crude product of di-n-butyl ester; stop heating, cool to room temperature and then filter to obtain the filtrate and filter cake, wash the filtrate with water, and then remove water and unreacted n-butanol by distillation under reduced pressure to obtain di-n-butyl itaconic acid The finished product has a yield of 85%. The filter cake is recovered and used directly in the next esterification reaction without any treatment.

Embodiment 2

[0029] The raw materials were obtained in the same manner as in Example 1. Weigh 100Kg of itaconic acid, 300Kg of n-butanol, 20Kg of strong acid ion exchange resin, 0.5Kg of hydroquinone and 10Kg of xylene, and put them into the reactor. The reactor is equipped with a stirrer. , Thermometer and water separator, start the stirrer to mix the raw materials uniformly, heat the reactor while stirring, start timing when heated to 90°C, and react for 8 hours to obtain the crude product of di-n-butyl itaconate; The crude di-n-butyl ester product can be cooled by natural cooling. Of course, tap water cooling can be used to save time. The purification method is the same as that in Example 1, to obtain a finished product of di-n-butyl itaconic acid with a yield of 98.7%.

Embodiment 3

[0031] The raw materials were obtained in the same manner as in Example 1. Weigh 80Kg of itaconic acid, 160Kg of n-butanol, 10Kg of strong acid ion exchange resin, 0.75Kg of hydroquinone and 20Kg of benzene, and put them into the reactor. The reactor is equipped with a stirrer, Thermometer and water separator, start the stirrer to mix the raw materials uniformly, heat the reactor while stirring, start timing when heated to 120°C, and react for 6 hours to obtain the crude product of di-n-butyl itaconate; The crude product of n-butyl ester is naturally cooled, the cooled crude product of di-n-butyl itaconate is allowed to stand still, and the upper product phase is poured out directly after layering to obtain the finished product of di-n-butyl itaconate. The yield is 95.9%; the lower strongly acidic ion exchange resin can be used for the next esterification reaction without any treatment.

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Abstract

The invention discloses a method for preparing dibutyl itaconate. In particular, the method comprises the following steps of: adopting a novel high-efficiency catalysis-polymerization inhibition combined system to catalyze the reaction of itaconic acid and normal butyl alcohol at normal pressure and a temperature of between 90 and 130 DEG C for 2 to 8 hours to form the dibutyl itaconate, wherein the catalysis-polymerization inhibition combined system comprises a catalyst of strong acid ion exchange resin and a polymerization inhibitor of hydroquinone. Compared with the conventional acid catalytic method, the method of the invention has the characteristics that: 1, the reaction time is short, and the energy consumption is low; 2, in a process of esterification, polymers are hardly generated, and the selectivity is high; 3, the product of the dibutyl itaconate is automatically separated from the catalyst, and the separating process is easier; and 4, the used catalyst in the reaction can be directly reused without treatment.

Description

technical field [0001] The invention relates to a method for preparing di-n-butyl itaconate, in particular to a method for preparing di-n-butyl itaconate by catalyzing the esterification reaction of itaconic acid and n-butanol with a strongly acidic ion exchange resin. Background technique [0002] Di-n-butyl itaconate is a colorless and transparent oily liquid with low toxicity. It is an important active monomer, comonomer and intermediate in organic synthesis, and is also an internal plasticizer for various plastics; it can be used automatically Polymerization and copolymerization, the products obtained by copolymerization are widely used in molding materials, coating materials, fiber and film treatment agents, lubricating oil and its additives, binder ion exchange resins, etc. The copolymer containing di-n-butyl itaconate and vinyl acetate has good heat insulation effect; adding di-n-butyl itaconate to detergent can improve the washing effect; di-n-butyl itaconate is als...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/593C07C67/08
Inventor 李悦明张希铭徐建春孙慧彬
Owner QINGDAO LANGYATAI GRP
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