Method for producing succinic acid
A technology of succinic acid and butyrolactone, which is applied in the preparation of carboxylic anhydrides and organic chemistry, can solve the problems of high reaction temperature and pressure, large waste liquid pollution, difficult reaction temperature, etc., achieve mild reaction conditions and enhance service life , the effect of reducing the requirement
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Embodiment 1
[0027] The internal diameter is 25mm, and the continuous fixed-bed reactor that is 1.2m is high is loaded with 20mlPd / Cu / C (the weight content of Pd in the catalyst is 5%, the weight content of Cu is 3%) catalyst, and the catalyst is diluted 3 times with quartz sand . A 15% mass concentration MA / GBL (maleic anhydride / γ-butyrolactone) solution was prepared and pumped into the reactor. The reaction conditions are: reaction temperature 75°C, hydrogen partial pressure 1.0MPa, hydrogen / maleic anhydride molar ratio 100, LHSV 2.0h -1 (Liquid hourly volume space velocity based on maleic anhydride γ-butyrolactone solution), continuous reaction for 300 hours, MA conversion rate of 100% through analysis, SA (succinic anhydride) selectivity of 96.6%, GBL selectivity of 3.4%. The product is hydrolyzed at 80°C by adding 30g of water, and then crystallized and separated at -10°C to obtain a white crystalline succinic acid product. The yield of succinic acid is 96.8%, and the purity is 97....
Embodiment 2
[0029] Inner diameter is 25mm, and high is 20mlPd / Cu / C (the weight content of Pd is 10%, the weight content of Cu is 1%) catalyst on the continuous fixed-bed reactor of 1.2m high, and catalyst is diluted 3 times with quartz sand. A 75% mass concentration MA / GBL solution was prepared and pumped into the reactor. The reaction conditions are: reaction temperature 90°C, hydrogen partial pressure 1.0MPa, hydrogen / maleic anhydride molar ratio 300, LHSV 1.0h -1 , continuous reaction for 300h, the analysis showed that the conversion rate of MA was 100%, the selectivity of SA was 97.6%, and the selectivity of GBL was 2.4%. The product is hydrolyzed at 80°C by adding 30g of water, and then crystallized and separated at -10°C to obtain a white crystalline succinic acid product. The yield of succinic acid is 96.2%, and the purity is 97.6%. GBL separates the water and recycles it.
Embodiment 3
[0031] Inner diameter is 25mm, and height is 20mlPd / Fe / C (the weight content of Pd is 4%, the weight content of Fe is 3%) catalyst on the continuous fixed-bed reactor of 1.2m high, and catalyst is diluted 3 times with quartz sand. A 50% mass concentration MA / GBL solution was prepared and pumped into the reactor. The reaction conditions are: reaction temperature 65°C, hydrogen partial pressure 1.5MPa, hydrogen / maleic anhydride molar ratio 400, LHSV 1.0h -1 , continuous reaction for 300h, the analysis showed that the conversion rate of MA was 100%, the selectivity of SA was 98.1%, and the selectivity of GBL was 1.9%. The product is hydrolyzed at 80°C by adding 30g of water, and then crystallized and separated at -10°C to obtain a white crystalline succinic acid product. The yield of succinic acid is 97.6%, and the purity is 98.8%. GBL separates the water and recycles it.
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