反应 #324365

反应方程式

hydrogen

pyromellitic acid

hydrogen

hydrogen

hydrogen

→

1,2,4,5-cyclohexanetetracarboxylic acid

收率 85.1%

溶剂

water

反应条件

后处理

1. 1
   过滤was filtered while it
2. 2
   其他to separate the catalyst
3. 3
   浓缩The filtrate was concentrated
4. 4
   其他by evaporating water under reduced pressure
5. 5
   其他a rotary evaporator
6. 6
   其他to precipitate crystals
7. 7
   其他The precipitated crystals were separated by solid-liquid separation at room temperature
8. 8
   其他dried

实验过程

A 5-L Hastelloy (HC22) autoclave was charged with 552 g of pyromellitic acid, 200 g of a catalyst, that is, rhodium carried on activated carbon, available from N.E. Chemcat Corporation, and 1,656 g of water. The inner atmosphere of the reactor was replaced with nitrogen gas under stirring. After replacing the inner atmosphere of the reactor with hydrogen gas, the hydrogen pressure in the reactor was adjusted to 5.0 MPa and the temperature was raised to 60° C. While maintaining the hydrogen pressure at 5.0 MPa, the reaction was allowed to proceed for 2 hours. Then, after replacing the hydrogen gas in the reactor with nitrogen gas, the reaction product solution taken out of the autoclave was filtered while it was still hot to separate the catalyst. The filtrate was concentrated by evaporating water under reduced pressure using a rotary evaporator to precipitate crystals. The precipitated crystals were separated by solid-liquid separation at room temperature and dried, thereby obtaining 481 g of 1,2,4,5-cyclohexanetetracarboxylic acid (yield: 85.0%).

来源