Aromatic carboxylic acid decarboxylastion method
A technology for decarboxylation of aromatic carboxylic acids, applied in chemical instruments and methods, organic decomposition, hydrocarbons, etc., can solve the problems of difficult separation, recovery and regeneration of catalysts, narrow application range, etc., and achieve high value-added utilization, Wide application range and high yield
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Embodiment 1
[0026] The decarboxylation catalyst was placed in an electric heating tube with an inner diameter of 2.0 cm and a height of 1 m. The electric heating tube has three stages of temperature control, the upper two stages are used for the gasification of aromatic carboxylic acids, and the third stage is used for filling catalysts. The catalyst bed portion of the tube was filled with about 10 g of catalyst. This section is contained between two layers of glass beads, which are 20 cm below and 40 cm above the catalyst bed, respectively. The diameter of the glass beads is 20-30 mesh. The temperature measuring thermocouple is located in the center of the catalyst layer. The decarboxylation catalyst is Zn-Fe-Al (30wt.%ZnO, 4wt.%Fe 2 o 3 , 66wt.%Al 2 o 3 ).
[0027] Dissolve 40.0 g of terephthalic acid in 250 ml of pyridine to form a 0.08 g / ml solution and place it in a storage tank. Pump the terephthalic acid solution into the reaction tube at a rate of 1ml / min, the nitrogen flo...
Embodiment 2
[0033] The composition, consumption and filling method of embodiment 2 decarboxylation catalyst are the same as embodiment 1.
[0034] Dissolve 30.0 g of PTA oxidation residue in 250 ml of pyridine, filter to remove insoluble matter, and place the filtrate in a liquid storage tank. The content of each component of the PTA oxidation residue is shown in the table above. The PTA oxidation residue solution was pumped into the reaction tube at a rate of 1ml / min, the nitrogen flow rate was 600ml / min, the temperature of the three sections of the reaction tube was set at 550°C, and the reaction time was 1h. The PTA oxidation residue was converted into benzene and carbon dioxide. After the catalytic bed, the reaction product is cooled by circulating water and a gas-liquid separator, and the tail gas is washed with water and vented.
[0035]The analysis method is the same as in Example 1, the analysis results of the product: benzene: 37.36wt.%, toluene: 0.61wt.%, biphenyl: 0.72w...
Embodiment 3
[0038] Embodiment 3 decarboxylation catalyst consumption and packing method are identical with embodiment 1. Catalyst components are 60wt.%ZnO, 5wt.%CuO, 35wt.%Al 2 o 3 .
[0039] 15g of 2,3,4,5-tetrafluorobenzoic acid was dissolved in 35ml of deionized water, and the configured solution was placed in a liquid storage tank, and the solution was pumped into the reaction tube at a rate of 0.5ml / min, nitrogen gas The flow rate is 200ml / min, and the temperature of the three sections of the reaction tube is set to 450°C. 2,3,4,5-tetrafluorobenzoic acid is converted into 1,2,3,4-tetrafluorobenzene and carbon dioxide. The reaction product is cooled by circulating water and a gas-liquid separator, and the tail gas is washed with water and emptied. The collected liquid was extracted with dichloromethane, the organic phase was separated, dried over magnesium sulfate and filtered to obtain 10.7 g of crude 1,2,3,4-tetrafluorobenzene.
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