Method for preparing gamma-butyrolactone through catalytic hydrogenation of dimethyl succinate

A dimethyl succinate, catalytic hydrogenation technology, applied in the chemical industry, can solve environmental pollution and other problems, achieve the effect of shortening the operation time, increasing the pH value, and continuous process

Inactive Publication Date: 2010-05-12
JIANGSU POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Patent CN 1687045A adopts sol-gel method to synthesize CuO-CrO 3 / SiO 2 As a catalyst, γ-butyrolactone is prepared by dehydrogenating 1,4-butanediol as a raw material. The catalytic effect is better, but Cr is used in the catalyst preparation and recovery process, which causes great pollution to the environment

Method used

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  • Method for preparing gamma-butyrolactone through catalytic hydrogenation of dimethyl succinate
  • Method for preparing gamma-butyrolactone through catalytic hydrogenation of dimethyl succinate
  • Method for preparing gamma-butyrolactone through catalytic hydrogenation of dimethyl succinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. Preparation and pretreatment of catalyst: 249.7g CuSO 4 ·5H 2 O, 16.8g ZnCl 2 And 73.6g Al(NO 3 ) 3 ·9H 2 O is dissolved in deionized water to form a 1mol / L solution. Then, under the condition of high-speed stirring and constant temperature water bath at 60℃, 2mol / L NaOH solution was added dropwise to a small amount of deionized water at the same time to generate precipitation. During the precipitation process, pH 7-8 was controlled. After the precipitation was complete, stirring was continued for 1h, and then at 80℃ Leave it to stand and age in a constant temperature water bath for 1 hour, overnight. The precipitate was filtered, washed, dried at 100°C for 24h, calcined at 300°C for 12h, and finally pressed into a tablet with a compressive strength of 5MPa. Take the 10 mesh catalyst precursor into a fixed-bed tubular reactor with an inner diameter of 8mm and a length of 800mm, with a packing rate of 3%, adjust the temperature to 150°C and pressure to 0.5MPa, and then...

Embodiment 2

[0031] 1. Preparation and pretreatment of the catalyst: 170.5g CuCl 2 ·2H 2 O, 94.7g ZnSO 4 ·7H 2 O and 11.0g Ba(NO 3 ) 2 Dissolve in deionized water to form a 1mol / L solution. Then, mix with 1mol / L of K under high-speed stirring 2 CO 3 The solution was added dropwise to 64.5g 31%(Wt, SiO 2 ) Precipitation is formed in the silica sol solution. The following steps are the same as in Example 1. Drying at 110°C for 16 hours and baking at 350°C for 10 hours. Take a 20-mesh catalyst precursor fixed-bed reactor with a pressure resistance of 10MPa, the filling rate is 5%, the temperature is adjusted to 200℃ and the pressure is 1.0MPa, and then hydrogen and nitrogen with a volume of 15% of hydrogen are introduced into the reactor. The activation time is 8h.

[0032] 2. Catalytic hydrogenation: The temperature of the reactor is raised to 350°C, the pressure is 2.0MPa, and the mixed solution of dimethyl succinate and methanol in a volume ratio of 1:3 is pumped into the fixed bed reactor t...

Embodiment 3

[0035] 1. The preparation and pretreatment of the catalyst: 241.6g Cu(NO 3 ) 2 ·3H 2 O, 146.9g Zn(NO 3 ) 2 ·6H 2 O, 13.2gBa(NO 3 ) 2 , 33.7g Ca(NO 3 ) 2 ·4H 2 O and 75.0g Al(NO 3 ) 3 ·9H 2 O is dissolved in deionized water to form a 1mol / L solution. Then, mix with 1mol / L Na 2 CO 3 The solution solution was added dropwise to 44.5g 31%(Wt, SiO 2 ) Precipitation is formed in the silica sol solution. The following steps are the same as in Example 1. Drying at 120°C for 12 hours and firing at 400°C for 8 hours. Take a 30-mesh catalyst precursor fixed-bed reactor with a pressure resistance of 20MPa, the filling rate is 10%, the temperature is adjusted to 250°C and the pressure is 2.0MPa, and then hydrogen and nitrogen with 30% of the hydrogen volume are introduced into the reactor. The activation time is 6h.

[0036] 2. Catalytic hydrogenation: The temperature of the reactor is raised to 300°C, the pressure is 3.00MPa, and the mixed solution of dimethyl succinate and methanol in a vol...

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Abstract

The invention relates to a method for preparing gamma-butyrolactone through catalytic hydrogenation of dimethyl succinate, which belongs to the field of chemical technology. Gamma-butyrolactone is prepared by utilizing the catalytic hydrogenation of multicomponent metallic oxide catalyst through a fixed bed tubular reactor by adopting dimethyl succinate as raw material and carbinol as solvent. The multicomponent metallic oxide catalyst is prepared through a coprecipitation method, the major catalyst comprises 15 to 80 percent (Wt) of copper oxide and 10 to 50 percent (Wt) of zinc oxide, the catalyst accelerator comprises 0 to 10 percent (Wt) of one or a plurality of the oxides of calcium, barium, magnesium, manganese, nickel, molybdenum or cobalt, and a carrier comprises 5 to 30 percent (Wt) of one or a plurality of aluminium oxide, zirconium dioxide and silicon dioxide. When the reaction temperature is 200 to 300 DEG C, the reaction pressure is 2 to 4 MPa, the mol ratio of hydrogen to ester is 100 to 250, and the liquid hourly space velocity is 0.2 to 0.5 h per hour, the conversion rate of dimethyl succinate is larger than 95 percent, and the selectivity of gamma-butyrolactone is larger than 90 percent. The multicomponent metallic oxide catalyst has higher activity and is inexpensive, and both preparation and recovery of the catalyst can not pollute the environment.

Description

Technical field [0001] The invention belongs to the technical field of chemical industry, and specifically relates to a method for preparing γ-butyrolactone by hydrogenating dimethyl succinate as a raw material. Background technique [0002] γ-butyrolactone is abbreviated as GBL, also known as 1,4-butyrolactone. It is an important fine chemical and pharmaceutical intermediate. It is mainly used to prepare pyrrolidone series products such as α-acetyl γ-butyrolactone and pharmaceutical intermediates. Cyclopropylamine is also used in agricultural chemistry and petrochemical fields. It is widely used in the fields of medicine, pesticides, synthetic resin additives, food and feed additives, dyes and pigments. [0003] At present, the industrialized methods for synthesizing γ-butyrolactone include 1,4-butanediol dehydrogenation method, maleic anhydride esterification hydrogenation method and maleic anhydride hydrogenation method. [0004] Patent CN 1687045A uses sol-gel method to synthes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33B01J23/80
Inventor 刘建武张跃严生虎沈介发
Owner JIANGSU POLYTECHNIC UNIVERSITY
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