Recycling process of methyl sulcotrione solvent
A technology of mesotrione and solvent is applied in the field of solvent recovery technology in the synthesis of mesotrione, which can solve the problems of high cost and high energy consumption of rectification, and achieve the effects of low cost, low equipment investment and simple operation.
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example 1
[0013] Add 300ml of mesotrione dichloroethane solution containing 55ml of triethylamine after condensation and rearrangement of mesotrione, add 300ml of water, start stirring, add 32g of 91% sulfuric acid dropwise, measure pH=1.3, stir for 15 minutes, Leave to stand for stratification, the lower layer of mesotrione dichloroethane solution recovers water-containing dichloroethane, the upper layer of triethylamine sulfate solution 395g, pour it into the dropping funnel, add 25g of caustic soda to the triethylamine recovery kettle, and start stirring , drop triethylamine sulfate aqueous solution, pH = 10.6, atmospheric pressure distillation to recover aqueous triethylamine, temperature to 90 degrees, receive aqueous triethylamine 67ml, lower the temperature and pour the waste water into the acyl chloride tail gas absorption device. Water-containing triethylamine, separate the lower layer of water, and the upper layer is introduced into a triethylamine drying kettle, add 25g of cau...
example 2
[0015] Add 300ml of dichloroethane containing water into the sulfuric acid dehydration tank, start stirring, slowly add 30ml of 98% sulfuric acid dropwise, after the dropwise addition is completed, stir for 3 hours, let stand for stratification, separate out 32g of dilute sulfuric acid in the lower layer, the measured content is 91%, and set aside. Atmospheric distillation recovers dichloroethane, and the measured water content is 0.03%. The dilute sulfuric acid obtained in this embodiment can be introduced in embodiment 1 and used.
example 3
[0017] Put 900L triethylamine with 6% water content into the recovery drying kettle, add 370kg caustic soda, start stirring, stir for 3 hours, let it stand for stratification, and extract the upper triethylamine from the triethylamine high level tank with a vacuum device , Measured moisture 0.2%, can be recycled directly. The lower layer is left in the kettle for later use.
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