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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.
Active Publication Date: 2014-10-08
ZHEJIANG ZHONGSHAN CHEM IND GRP
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Problems solved by technology
[0004] The technical problem to be solved by the present invention is to provide a new process for solvent recovery of mesotrione, which can overcome the problems of high energy consumption and high cost of rectification. Apply directly, reduce energy consumption, reduce waste water discharge, simplify operation and reduce cost
Method used
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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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Abstract
The invention discloses a recycling process of a methyl sulcotrione solvent. The recycling process comprises the following steps: transferring a methyl sulcotrione dichloroethane solution which is subjected to condensation and rearrangement and contains triethylamine into a triethylamine salifying kettle and adding water under the condition that the volume ratio of dichloroethane to the water is 1 to (1-5) (v/v) (Volume Per Volume), starting stirring, slowly dripping a 80% to 91% dilute sulphuric acid solution according to the condition that the molar ratio of the triethylamine to the dilute sulphuric acid is 1 to (0.5-0.8) (mol/mol), regulating pH within 1 to 1.5, stirring for 15 minutes, separating out a methyl sulcotrione dichloroethane solution at a lower layer, and carrying out reduced pressure distillation for recycling the dichloroethane containing the water; putting a triethylamine sulfate aqueous solution at an upper layer into a storage tank; and simultaneously treating the obtained dichloroethane containing the water and the triethylamine sulfate aqueous solution. According to the recycling process, an acid-base neutralization salifying theory is adopted; the performances of dehydration and water absorption of materials are utilized, so that the whole recycling process is low in energy consumption, low in cost, mutually complementary, less in equipment investment and simple to operate, and is used for completely solving the problems of high cost and high energy consumption of the solvent separated in a distillation recycling manner. Thus, the recycling process disclosed by the invention conforms to the ideals of energy conservation and emission reduction in China.
Description
technical field [0001] The invention belongs to the field of resource recycling and environmental protection, and in particular relates to a solvent recovery process in the synthesis of mesotrione. Background technique [0002] The full name of mesotrione is 2-(4-methylsulfonyl-2-nitro-benzoyl)cyclohexane-1,3-dione, which is a triketone herbicide developed by Syngenta, and is known as The trade name callisto (Mistone) was sold in Europe in 2001. It is a broad-leaf herbicide before and after buds in corn fields. It is not only safe for corn fields, but also safe for the environment and subsequent crops. It is a broad-spectrum herbicide that can control many weeds such as cocklebur, velvetleaf, Artemisia annua, lettuce, thorn, and tribulus. Urea herbicides are effective in developing resistant weeds. [0003] At present, the process of producing mesotrione at home and abroad mainly uses p-thiamphenicol toluene as the main raw material, which is nitrated and oxidized to synth...
Claims
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