Process of preparing 4-nitro phthalic acid from the reaction mother liquor of nitrating phthalic anhydride to prepare 3-nitro phthalic acid
A nitrophthalic acid and reaction technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve problems such as cumbersome methods, difficult to apply in industrial production, etc., and achieve environmental protection and resource utilization. Effect
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[0012] Example 1
[0013] A. Nitrification
[0014] Add 237.5g of concentrated sulfuric acid to a dry 500ml three-necked flask, start the stirrer, add 112.5g of fuming nitric acid, heat to 55°C, stop heating, and start slowly adding 125g of phthalic anhydride in batches (addition in 4 times). Control the reaction temperature at 70-80°C and complete the addition in about 1.5 hours. Then react at 75-80°C for 3 hours, and then at 80-85°C for 1 hour. After the reaction, it was cooled to room temperature.
[0015] B. Filter separation
[0016] The reaction liquid in step A was suction filtered, and the crystals were filtered out to obtain 96.5g of the filter cake as 3-nitrophthalic acid (I); 200ml (345.6g) of the filtrate mainly contained 4-nitrophthalic acid (II) )
[0017] C. Preparation of 3-nitrophthalic acid
[0018] Add (I) to 2.5 times the mass of water and heat to dissolve it, cool to room temperature, precipitate crystals, filter with suction, and dry the filter cake to obtain...
Example Embodiment
[0021] Example 2
[0022] A. Nitrification
[0023] Add 237.5g of concentrated sulfuric acid to a dry 500ml three-necked flask, start the stirrer, add 112.5g of fuming nitric acid, heat to 55°C, stop heating, and start slowly adding 125g of phthalic anhydride in batches (addition in 4 times). Control the reaction temperature at 70-80°C and complete the addition in about 1.5 hours. Then react at 75-80°C for 3 hours, and then at 80-85°C for 1 hour. After the reaction, it was cooled to room temperature.
[0024] B. Filter separation
[0025] The reaction liquid in step A is suction filtered, and the crystals are filtered out, and 96.5 g of the filter cake is obtained as 3-nitrophthalic acid
[0026] (I); 200ml (345.6g) filtrate mainly contains 4-nitrophthalic acid (II)
[0027] C. Preparation of 3-nitrophthalic acid
[0028] Add (I) to 3 times the mass of water and heat to dissolve it, cool to room temperature, precipitate crystals, filter with suction, and dry the filter cake to obt...
Example Embodiment
[0031] Example 3
[0032] A. Nitrification
[0033] Add 237.5g of concentrated sulfuric acid to a dry 500ml three-necked flask, start the stirrer, add 112.5g of fuming nitric acid, heat to 55°C, stop heating, and start slowly adding 125g of phthalic anhydride in batches (addition in 4 times). Control the reaction temperature at 70-80°C and complete the addition in about 1.5 hours. Then react at 75-80°C for 3 hours, and then at 80-85°C for 1 hour. After the reaction, it was cooled to room temperature.
[0034] B. Filter separation
[0035] The reaction liquid in step A was suction filtered, and the crystals were filtered out to obtain 96.5g of the filter cake as 3-nitrophthalic acid (I); 200ml (345.6g) of the filtrate mainly contained 4-nitrophthalic acid (II) )
[0036] C. Preparation of 3-nitrophthalic acid
[0037] Add (I) to 3.5 times the mass of water and heat to dissolve it, cool to room temperature, precipitate crystals, filter with suction, and dry the filter cake to obtain...
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