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Method of simultaneously producing dimethyl succinate and 1,4-butyl glycol

A technology of dimethyl succinate and dimethyl maleate, which is applied in the field of simultaneous production of dimethyl succinate and 1, can solve problems such as increased cost, increased operating expenses, and increased operating energy consumption, and achieves a regular Effect of pore distribution, less by-products, and high selectivity

Active Publication Date: 2014-06-18
SHANGHAI HUAYI ENERGY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, when the pre-reaction zone is gas-phase hydrogenation, several problems will be caused: First, the reaction pressure in the pre-reactor and the main reactor is the same, both of which are relatively high at 30-70 bar, so that the hydrogenation can be performed at a lower pressure The operating cost of the pre-reaction zone under operation increases; the second is that the two catalysts in the pre-reaction zone and the main reaction zone, at least one catalyst does not operate under better reaction conditions, which indirectly leads to an increase in cost; The hydrogen-ester ratio in the main reaction zone is the same, but the reaction in the main reaction zone needs to be carried out at a higher hydrogen-ester ratio (preferably about 258), so that the amount of circulating hydrogen in the pre-reaction zone is much higher than the theoretically required amount , resulting in increased operating energy consumption

Method used

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  • Method of simultaneously producing dimethyl succinate and 1,4-butyl glycol
  • Method of simultaneously producing dimethyl succinate and 1,4-butyl glycol
  • Method of simultaneously producing dimethyl succinate and 1,4-butyl glycol

Examples

Experimental program
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Embodiment 1

[0047] Such as figure 2 The schematic diagram of the process flow shown (other equipment needed in industrial production, such as pumps, heat exchangers, compressors, cycle compressors, safety valves, control valves, storage tanks, etc., are not listed in the accompanying drawings, these Auxiliary equipment can be added according to chemical engineering equipment requirements, etc.). The raw material dimethyl maleate (DMM) of 115.2kg / h enters the low-pressure preheater 2 through pipeline 1, and the circulating hydrogen from the low-pressure cycle compressor merges with the fresh hydrogen from pipeline 8 through pipeline 7, and then passes through pipeline 9 Also enter the low-pressure preheater 2, dimethyl maleate is vaporized under the stripping action of hydrogen, the mol ratio of hydrogen and dimethyl maleate in the mixed steam is 80: 1, and the mixed steam flow enters through pipeline 3 Low-pressure reactor 4, catalyst is housed in the low-pressure reactor 4, under 140 ℃...

Embodiment 2

[0051] Technological process is identical with embodiment 1, and difference is dimethyl maleate feed amount, low-pressure reaction zone hydrogen-ester ratio and medium-pressure reaction temperature, and correspondingly, the output of each product is also different, and wherein, output The purity of the dimethyl succinate product is 99.75% (analyzed by gas chromatography), specifically as shown in table 1.

[0052] In the present embodiment, the catalyst packed in the low-pressure reactor 4 is Cu / ZnO / Al 2 o 3 Three-way catalyst, the preparation process and activation process of the catalyst are as shown in Example 1, except that the molar ratio of Cu, Zn, and Al is 1:0.85:0.25. The loading capacity of the catalyst is about 76kg, the bulk density of the catalyst is about 1.52kg / L, and the specific surface area is 89m 2 / g, the average pore diameter is 19.3nm.

Embodiment 3

[0054] Process flow is identical with embodiment 1, and difference is dimethyl maleate feed amount, low pressure reaction zone hydrogen ester ratio, temperature of reaction and pressure, and the hydrogen ester ratio, temperature and pressure of middle pressure reaction zone, correspondingly , The extraction amount of each product is also different, and wherein, the purity of the dimethyl succinate product of extraction is 99.5% (analyzes with gas chromatography), specifically as shown in table 1.

[0055] In the present embodiment, the catalyst packed in the low-pressure reactor 4 is Cu / ZnO / Al 2 o 3 Three-way catalyst, the preparation process and activation process of the catalyst are as shown in Example 1, except that the molar ratio of Cu, Zn, and Al is 1:0.80:0.25. The loading capacity of the catalyst is about 74kg, the bulk density of the catalyst is about 1.48kg / L, and the specific surface area is 100m 2 / g, the average pore diameter is 20nm.

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Abstract

The invention relates to a method of simultaneously producing dimethyl succinate (DMS) and 1, 4-butyl glycol. The method can also be used to simultaneously produce at least one of Tetrahydro furan (THF) and gamma-irradiation butyl lactone (GBL). In the invention, dimethyl maleate (DMM) is used as raw materials and contacts with hydrogen under the condition of gas phase in a low pressure reaction district and a middle pressure reaction district respectively. A low-pressure reactor and a middle-pressure reactor are equipped with a catalyst. DMS products are produced in the low pressure reaction district and 1, 4-butyl glycol products are produced in the middle pressure reaction district. Simultaneously, at least one of the GBL and THF can be produced in the middle pressure reaction district. Purity of DMS can reach over 99.5% without refining through using a gas-liquid separator. In the invention, the method is used in mild condition; heavier component does not need to be circulated; operation is simple; transesterification type polymerization and other side reactions are greatly reduced in a system.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for simultaneously producing dimethyl succinate and 1,4-butanediol. Background technique [0002] Dimethyl succinate (DMS) is mainly used in the synthesis of spices and food additives, and it is also an important chemical intermediate, widely used in the preparation of various chemicals, such as further hydrogenation to produce 1,4-butane Diol, γ-butyrolactone (GBL), tetrahydrofuran (THF), etc., or transesterification polymerization with 1,4-butanediol to produce a promising biodegradable material polybutylene succinate (PBS ). [0003] At present, dimethyl succinate is mainly obtained from succinic acid and methanol through esterification reaction under the catalysis of concentrated sulfuric acid catalyst. This process of using concentrated sulfuric acid to catalyze esterification has many side reactions, low yield, complex post-treatment, and se...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/40C07C67/303C07C31/20C07C29/149
Inventor 赵正康刘文艳何明康杨菊群郭平均张旭红程井动
Owner SHANGHAI HUAYI ENERGY CHEM
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