Method for preparing benzylidene camphor sulfonic acid
A technology of camphorsulfonic acid and benzylidene, which is applied in the field of preparation of benzylidene camphorsulfonic acid, can solve the problems of large amount of waste water, cumbersome process operation, and high cost of raw materials, and achieve less waste water, low cost of raw materials, and high safety Effect
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Embodiment 1
[0022] Put 100g of camphorsulfonic acid and 100g of water into a 500ml four-necked bottle, stir and dissolve at 25-30°C. Add 58g of 30% sodium hydroxide to the four-necked flask under stirring, and adjust the pH to 7-8. If the system is not dissolved at this time, add an appropriate amount of water to ensure that the system is in a dissolved state. On the premise that the system is dissolved, add 5g PEG-400 to the four-necked bottle. The temperature was raised to 45°C with stirring.
[0023] Control the temperature at 45±2°C, slowly add 45g of benzaldehyde dropwise to the four-necked bottle, and drop it for about 5 hours. After dropping, control the temperature at 45±2°C and keep stirring for 2 hours.
[0024] Stir and heat up to 50°C, slowly adjust the pH to 1 with 50g of 50% sulfuric acid, then cool down to ≤10°C with stirring and keep the temperature under 10°C for 1 hour.
[0025] Suction filtration, the filter cake was washed with an appropriate amount of water to obt...
Embodiment 2
[0037] Put 100g of camphorsulfonic acid and 100g of water into a 500ml four-necked bottle, stir and dissolve at 25-30°C. Add 58g of 30% sodium hydroxide to the four-necked flask under stirring, and adjust the pH to 7-8. If the system is not dissolved at this time, add an appropriate amount of water to ensure that the system is in a dissolved state. On the premise that the system is dissolved, add 5g of 18 crown 6 to the four-necked bottle. The temperature was raised to 45°C with stirring.
[0038] Control the temperature at 45±2°C, slowly add 45g of benzaldehyde dropwise to the four-necked bottle, and drop it for about 5 hours. After dropping, control the temperature at 45±2°C and keep stirring for 2 hours.
[0039] Stir to raise the temperature to 50°C, slowly adjust the pH to 1 with 51g of 50% sulfuric acid, then stir to lower the temperature to ≤10°C and control the temperature to ≤10°C and keep stirring for 1h.
[0040] Suction filtration, the filter cake was washed wi...
Embodiment 3
[0052] Put 100g of camphorsulfonic acid and 100g of water into a 500ml four-necked bottle, stir and dissolve at 25-30°C. Add 58g of 30% sodium hydroxide to the four-necked flask under stirring, and adjust the pH to 7-8. If the system is not dissolved at this time, add an appropriate amount of water to ensure that the system is in a dissolved state. On the premise that the system is dissolved, add 5g PEG-400 to the four-necked bottle. The temperature was raised to 60°C with stirring.
[0053] Control the temperature at 60±2°C, slowly add 45g of benzaldehyde dropwise to the four-necked bottle, and drop it for about 5 hours. After dropping, control the temperature at 60±2°C and keep stirring for 2 hours.
[0054] Stir and cool down to 50°C, slowly adjust the pH to 1 with 50g of 50% sulfuric acid, then stir and cool down to ≤10°C and control the temperature to ≤10°C and keep stirring for 1h.
[0055] Suction filtration, the filter cake was washed with an appropriate amount of ...
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