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Preparation method of diethyl succinate

A technology of succinic acid diester and maleic anhydride, which is applied in the field of preparation of succinic acid diester, can solve the problems of low yield of methyl succinate, reduced activity of ion exchange resin solid acid catalyst, etc., and achieve The effect of reducing production cost, facilitating separation and refining, and simplifying the production process

Active Publication Date: 2013-01-09
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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Problems solved by technology

However, in the disclosed method of this patent, esterification and hydrogenation are carried out step by step. In the esterification process, the presence of water reduces the activity of the ion exchange resin solid acid catalyst, and the ion exchange resin solid acid catalyst should not be provided in this method. Run for a long time under the reaction temperature of reaction temperature, make the productive rate of the methyl succinate obtained lower

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  • Preparation method of diethyl succinate
  • Preparation method of diethyl succinate
  • Preparation method of diethyl succinate

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preparation example Construction

[0025] The invention provides a kind of preparation method of succinic acid diester, comprises the following steps:

[0026] Mix maleic anhydride, alcohol compounds, carbon dioxide, hydrogen and a hydrogenation catalyst to carry out esterification and hydrogenation reaction to obtain succinic acid diester.

[0027] The invention provides a method for preparing succinic acid diester. The method provided by the invention uses maleic anhydride, alcohol compounds and hydrogen as raw materials, carbon dioxide as a solvent and an acid catalyst, and carries out esterification under the catalysis of a hydrogenation catalyst. hydrogenation reaction to obtain succinic acid diester. The method provided by the invention uses carbon dioxide as a solvent and an acid catalyst for the esterification hydrogenation reaction, which has higher catalytic activity and improves the reaction rate; and it can also form an acid with the water generated in the reaction process, thereby promoting the rea...

Embodiment 1

[0048] Place 0.1 g of palladium chloride in 0.2 mL of dilute hydrochloric acid aqueous solution with a molar concentration of 1 mol / L, stir for 2 h to fully disperse the palladium chloride to obtain an aqueous palladium chloride solution; into the palladium chloride aqueous solution, fully immersed at room temperature, overnight, then dried at 60°C, and finally reduced at 150°C under a hydrogen atmosphere to obtain a supported Pd / C catalyst.

Embodiment 2

[0050] Put 0.28 g of nickel nitrate in 1 mL of water and stir for 1 h to obtain an aqueous solution of nickel nitrate; impregnate 1 g of the calcined pretreated aluminum oxide carrier into the aqueous solution of nitric acid, fully impregnate at room temperature overnight, and then Dry at 60°C, and finally calcined at 450°C in a muffle furnace, and then reduce under hydrogen atmosphere to obtain supported Ni / Al 2 o 3 catalyst.

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Abstract

The invention provides a preparation method of dimethyl succinate. The method comprises the steps of mixing maleic anhydride, an alcohol compound, carbon dioxide, hydrogen and a hydrogenation catalyst and conducting esterification hydrogenation reaction to obtain the dimethyl succinate. According to the method, the maleic anhydride, the alcohol compound and hydrogen serve as raw materials, the carbon dioxide serves as a solvent and an acid catalyst, under catalysis of the hydrogenation catalyst, the esterification hydrogenation reaction is conducted, and the dimethyl succinate is obtained. The carbon dioxide serves as the solvent of the esterification hydrogenation reaction and the acid catalyst, high catalytic activity is achieved, and the reaction rate is improved; the carbon dioxide and water generated in the reaction process can form acid, and an obtained product has certain solubility in the carbon dioxide, so that the reaction can be conducted in a positive direction, and the conversion rate and the production rate of the dimethyl succinate are improved. Experimental results show that the yield rate of the obtained dimethyl succinate exceeds 99%.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of succinic acid diester. Background technique [0002] Succinic acid diester is the product of the esterification reaction of succinic acid and alcohol compounds, such as dimethyl succinate, dipropyl succinate, diisopropyl succinate and di-n-octyl succinate, etc. Among them, Dimethyl Succinate is the most widely used. Dimethyl succinate is also known as dimethyl succinate. The CAS number is 106-65-0 and the molecular formula is C 4 h 10 o 4 , has the structure shown in formula (I). Dimethyl succinate is a colorless to light yellow liquid at room temperature, it can solidify after cooling, showing wine and ether aroma, fruity and burnt aroma, boiling point 195°C~196°C, or 80°C (1466Pa), melting point 18°C ~19°C, flash point 90°C. Slightly soluble in water (1%), soluble in ethanol (3%), easily soluble in ether and acetone, miscible in oil. Di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/40C07C67/30C07C67/08
Inventor 赵凤玉于彦存
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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