Novel process for producing 1,4-dihydroxy anthraquinone
A technology of dihydroxyanthraquinone and new process is applied in the field of p-chlorophenol production, which can solve the problems of high labor intensity, long process time, unstable product quality, etc. The effect of production cost and labor intensity
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Embodiment 1
[0010] Example 1: Add 200ml of oleum and 35g of boric acid into a three-necked flask equipped with a stirring blade and a thermometer, slowly raise the temperature to 110°C, keep it warm for 30-60 minutes, then add 95g of phthalic anhydride, and the temperature will be reduced by the heat released by the reaction. When the temperature rises to about 130°C, start to add 75 grams of p-chlorophenol several times in batches, and complete the addition within 4 hours. The temperature of the whole feeding process is controlled at 130-150°C. After adding p-chlorophenol, the temperature was raised to 200-205°C and kept for 5 hours. Pour the reaction product into 8 times the volume of water for hydrolysis, control the temperature above 100°C and stir for 30 minutes, add 200ml of toluene to the hydrolyzate, drain the lower layer of waste acid after standing, add 100ml of 90°C to the upper layer extract Wash with hot water, drain the washing wastewater after standing still, heat and steam...
example 2
[0011] Example 2: Add 200ml of oleum and 45 grams of boric acid into a three-necked flask equipped with a stirring blade and a thermometer, slowly heat up to 110°C, keep warm for 30 to 60 minutes, then add 95 grams of phthalic anhydride, and raise the temperature by the heat released by the reaction. When the temperature reaches about 130°C, start to add 75 grams of p-chlorophenol several times in batches, and complete the addition within 4 hours. The temperature of the whole feeding process is controlled at 130-150°C. After the addition, the temperature was raised to 200-205°C for 5 hours. Pour the reaction product into 8 times the volume of water for hydrolysis, control the temperature above 100°C and stir for 30 minutes, add 200ml of toluene to the hydrolyzate, drain the lower layer of waste acid after standing, add 100ml of 90°C to the upper layer extract Wash with hot water, drain the washing wastewater after standing still, heat and steam the toluene, the residue in the ...
example 3
[0012] Example 3: Add 4000kg of fuming sulfuric acid and 350kg of boric acid into a 5000L reactor, slowly raise the temperature to 110°C, keep it warm for 30-60 minutes, then add 950kg of phthalic anhydride, and the temperature will rise to about 130°C by the heat released by the reaction. Begin to add 750kg of p-chlorophenol in batches several times, and finish adding within 4 hours. The temperature of the whole addition process is controlled at 130-150°C. After adding p-chlorophenol, the temperature was raised to 200-205°C and kept for 5 hours. Put the reaction product into a hydrolysis kettle pre-added with 12000kg of water, control the temperature above 100°C and stir for 30 minutes, add 2000 L of toluene to the hydrolysis kettle, drain the lower layer of waste acid after standing still, and then add 1000 L Wash with hot water above 90°C, drain the washing wastewater after standing still, pump the extract into the toluene still, and recycle the evaporated toluene. After t...
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