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Method for preparing diisooctyl itaconate

A technology for diisooctyl itaconic acid and itaconic acid is applied in the field of preparing diisooctyl itaconic acid to achieve the effects of low reaction temperature, short time and low energy consumption

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-isooctyl itaconate is to use concentrated sulfuric acid as a direct esterification method as a 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

[0028] Buy itaconic acid, isooctyl alcohol, strong acid ion exchange resin, hydroquinone, benzene, toluene and xylene from the market, weigh 100Kg itaconic acid, 500Kg isooctyl alcohol, 5Kg strong acid 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 150°C, start timing and react for 8 hours to obtain itaconic acid. Diisooctyl crude product; stop heating, cool to room temperature and then filter to obtain filtrate and filter cake, wash the filtrate, and then distill under reduced pressure to remove water and unreacted isooctyl alcohol to obtain diisooctyl itaconate Finished product, the yield is 90%. The filter cake is recovered and directly used for the next esterification reaction without any treatment.

Embodiment 2

[0030] The raw material acquisition method is the same as in Example 1. Weigh 100Kg itaconic acid, 250Kg isooctyl alcohol, 20Kg strongly acidic ion exchange resin, 0.5Kg hydroquinone and 10Kg toluene, and put them into the reactor. The reactor is provided with a stirrer, Thermometer and water separator, start the agitator to mix the raw materials evenly, heat the reaction kettle while stirring, start timing when heated to 200°C, and react for 4 hours to obtain the crude product of diisooctyl itaconate; The crude product of isooctyl ester is cooled, it can be cooled naturally, of course, it can also be cooled with tap water in order to save time, the method of purification is the same as that of Example 1, and the finished product of diisooctyl itaconate is obtained with a yield of 98.4%.

Embodiment 3

[0032] The method of obtaining raw materials is the same as in Example 1. Weigh 100Kg itaconic acid, 400Kg isooctyl alcohol, 10Kg strongly acidic ion exchange resin, 0.75Kg hydroquinone and 20Kg 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 180°C, and react for 10 hours to obtain the crude product of diisooctyl itaconate; The crude product of di-isooctyl is naturally cooled, and the cooled crude product of di-iso-octyl itaconate is left to stand, and after layering, the upper product is directly poured out to obtain the finished product of di-iso-octyl itaconate. The rate is 97.9%; the strong acid ion exchange resin in the lower layer can be used for the next esterification reaction without any treatment.

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PUM

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Abstract

The invention discloses a method for preparing diisooctyl 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 isooctanol at normal pressure and a temperature of between 150 and 200 DEG C for 4 to 10 hours to form the diisooctyl 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 diisooctyl 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 diisooctyl itaconate, in particular to a method for preparing diisooctyl itaconate by catalyzing the esterification reaction of itaconic acid and isooctyl alcohol with a strongly acidic ion exchange resin. Background technique [0002] Diisooctyl itaconate is an intermediate for the synthesis of diisooctyl sodium itaconate, and diisooctyl sodium itaconate is one of the series of sodium succinate sulfonate products with excellent performance. anionic surfactant. Diisooctyl itaconate itself is a kind of comonomer, which is copolymerized with monomers such as polyvinyl chloride, vinyl acetate, styrene, acrylate, etc., and the obtained copolymer has excellent impact resistance, crack resistance, Electrical and chemical properties, can be used to prepare films, coatings, adhesives, rubber, pigment fixatives, petroleum additives, paper treatment agents, etc.; the copolymer of diisooctyl itaconate and vinyl ac...

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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