A kind of production technology that improves hexazinone yield
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A production process and cycloazinone technology, applied in the field of cycloazinone, can solve the problems of incomplete reaction of raw materials, low yield of cycloazinone raw materials, etc., achieve uncomplicated reaction principle, practical reaction process control, and reduce residues Effect
Active Publication Date: 2022-05-03
ANHUI GUANGXIN AGROCHEM
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[0005] The object of the present invention is to provide a kind of production technology that improves the yield of hexazinone, solves the problem that the reaction of raw materials in the production process existing in the technology is not complete, causes the yield of the raw material product of hexazinone to be low
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[0036] A production process that improves the yield of cyclazinone, including the following steps:
[0037] Step S1, Synthetic methyl: first add 1.1 part by weight of amino cyanide to the methylation kettle, add 64 parts of liquid alkali and 3 parts of ethyl chloroformate to the metering tank, and then open the freezing valve of the methylation kettle, reduce the temperature in the methylation kettle to 0 ° C, add liquid alkali and ethyl chloroformate to the methylation kettle dropwise, control the temperature in the kettle is 2 ° C, after the completion of the drip addition of ethyl chloroformate, measure the pH value in the methylation kettle, when the pH value is stable to 8, stop the drip addition of liquid alkali, and close the refrigeration valve of the methylation kettle; open the jacket water and steam inlet and outlet valves, heat the materials in the methylation kettle, heat up to 38 °C, keep warm for 4h During the insulation period, the pH value in the methylation kettl...
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Abstract
The invention discloses a production process for improving the yield of hexazinone, comprising the following steps: step S1, first using cyanamide and ethyl chloroformate to generate ethyl cyanocarbamate, and then combining ethyl cyanocarbamate with dimethyl sulfate The ester synthesizes a methyl product under the catalytic condition of a catalyst; step S2, synthesizes a guanidine derivative with a methyl product and dimethylamine; step S3, uses chloroform to perform multiple extractions on the guanidine derivative; step S4, performs precipitation on the guanidine derivative Processing: step S5, reacting guanidine derivatives with cyclohexyl isocyanate to synthesize a hexazinone intermediate under the condition of toluene as a solvent; step S6, performing a cyclization reaction between the hexazinone intermediate and sodium methoxide to prepare hexazinone and washing with water; Step S7, purifying and drying hexazinone to obtain the technical product of hexazinone; the production process of the present invention is easy for industrial production and has strong practicability, and solves the technical problem of low yield of the technical product of hexazinone in the prior art.
Description
Technical field [0001] The present invention belongs to the field of cyclazinone technology, specifically, relates to a production process that improves the yield of cyclazinone. Background [0002] Cyclazinone, also known as Wilbur, Lincaojing, Phenoxygen, Sentai, chemical name is 3-cyclohexyl-6-dimethylamino-1-methyl-1,3,5-triazine-2,4-dione, is a colorless, odorless crystalline solid, is an endository selective, post-bud touch pyrrobenzophenone herbicide. [0003] Cyclazinone is mainly used in maintaining and opening up forest fire lanes, raising young forests, forest stand transformation and weeding and irrigation on railways, highways, airports, warehouses, docks, etc., and has special effects on the prevention of "Canada's yellow flowers". The product has a strong lethality on forest weeds, shrubs, vines and other plants, it can be absorbed by the stems and leaves of the plant, and the xylem is used inside the plant for conduction, and by directly interfering with the phot...
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