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Method for preparing dibutyl itaconate

A technology of di-n-butyl itaconate and itaconic acid, which is applied in the field of preparing di-n-butyl itaconate, can solve the problems of insufficient production process of concentrated sulfuric acid, dark product color, multiple side reactions, etc., and achieve energy consumption The effect of less time, short time and low reaction temperature

Active Publication Date: 2010-06-16
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

[0026] Buy itaconic acid, n-butanol, strongly acidic ion exchange resin, hydroquinone, benzene, toluene and xylene from the market, weigh 100Kg itaconic acid, 140Kg n-butanol, 5Kg strongly acidic ion exchange resin, Add 1Kg of hydroquinone into the reaction kettle in turn. The reaction kettle is equipped with a stirrer and a thermometer. Start the stirrer to mix the raw materials in the reaction kettle evenly. After heating to 130°C, start timing and react for 6 hours to obtain itaconic acid. Di-n-butyl ester crude product; stop heating, cool to room temperature and then filter to obtain filtrate and filter cake, wash the filtrate with water, then distill under reduced pressure to remove water and unreacted n-butanol to obtain di-n-butyl itaconate Finished product, yield 85%. The filter cake is recovered and directly used for the next esterification reaction without any treatment.

Embodiment 2

[0028] The method of obtaining raw materials is the same as in Example 1. Weigh 100Kg itaconic acid, 300Kg n-butanol, 20Kg strongly acidic ion exchange resin, 0.5Kg hydroquinone and 10Kg xylene, and put them into the reactor, which is equipped with a stirrer , a thermometer and a water separator, start the agitator to mix the raw materials evenly, 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; p-itaconic acid The crude product of di-n-butyl ester is cooled, and it can be cooled naturally. Of course, tap water can also be used for cooling in order to save time. The purification method is the same as in Example 1 to obtain the finished product of di-n-butyl itaconate with a yield of 98.7%.

Embodiment 3

[0030] Raw material acquisition method is the same as embodiment 1, takes by weighing 80Kg itaconic acid, 160Kg n-butanol, 10Kg strongly acidic ion-exchange resin, 0.75Kg hydroquinone and 20Kg benzene, drops in the reactor, and the reactor is provided with agitator, Thermometer and water separator, start the agitator to mix the raw materials evenly, 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, and the cooled crude product of di-n-butyl itaconate is left to stand, and after layering, the upper product phase is directly poured out to obtain the finished product of di-n-butyl itaconate. The yield is 95.9%; the lower strong 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 also...

Claims

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Application Information

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Patent Type & Authority Applications(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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