8 results about "Hexazinone" patented technology

The invention discloses a hexazinone preparation and a preparation method thereof, and belongs to the technical field of pesticide chemistry. The preparation method comprises the following steps: S1, preparing BC: adding BC, mixing and grinding with copper sulfate pentahydrate, putting into a tubular furnace, calcining, and cooling to obtain Cu-BC; s2, adding a modified silane coupling agent into an ethanol water solution, then adding the Cu-BC obtained in S1, stirring for 6-8 hours at 25-35 DEG C, filtering, washing and drying to obtain modified Cu-BC; s3, hexazinone is dissolved in absolute ethyl alcohol, then the modified Cu-BC is added, ultrasonic dispersion is conducted for 6-8 h, filtering, centrifugal washing and freeze-drying are conducted, and the hexazinone preparation is obtained. According to the preparation method of the hexazinone preparation, the slow release capacity of the preparation can be improved, the hexazinone utilization rate is increased, meanwhile, the preparation can be endowed with the sterilization effect, and the hexazinone preparation has wide application prospects.

This invention belongs to the field of cycloazinone preparation technology, and provides a high-yield cycloazinone synthesis process, including the following steps: Step 1: N-ethoxycarbonyl-N,N,N-trimethylguanidine and a solid-phase catalyst are added to toluene and stirred evenly. Under nitrogen protection, the temperature is raised to 40-60°C, and a cyclohexyl isocyanate toluene solution is added dropwise. Stirring is continued for 2-4 hours. The solid-phase catalyst is recovered by filtration, and the mixture is concentrated under reduced pressure to obtain N-cyclohexylcarbamoyl-N-ethoxycarbonyl-N,N,N-trimethylguanidine; Step 2: Under nitrogen protection, the temperature is raised to 50-60°C, and the N-cyclohexylcarbamoyl-N-ethoxycarbonyl-N,N,N-trimethylguanidine toluene solution is added dropwise to a sodium methoxide toluene solution and stirred for 1-2 hours. The temperature is lowered to room temperature, and glacial acetic acid is added for neutralization. After washing, the mixture is concentrated under reduced pressure, and a crystallizing agent is added. The temperature is lowered to 0-5°C, and the mixture is stirred for crystallization for 2-4 hours. After filtration and washing, the mixture is dried under vacuum to obtain the finished cycloazinone.

The invention discloses a purification process of hexazinone production wastewater, and relates to the technical field of wastewater treatment. The process comprises the following steps: introducing wastewater of a hexazinone production process into an enamel microfiltration reactor for reaction, and filtering out pretreated wastewater; the pretreated wastewater is pumped into a graphite condensation type oxidation tower, a composite catalyst composed of a sodium methoxide methanol solution and methyl chloroformate is added for a reaction, and oxygenated wastewater is obtained; adjusting the pH value of the wastewater subjected to oxygen catalysis to 7.0-7.5, introducing the wastewater into a biological denitrification reaction tank, and adding a microbial agent compounded by nitrifying bacteria and denitrifying bacteria for reaction to obtain purified wastewater; refluxing 80% of the purified wastewater to a raw material preparation process for hexazinone production for reuse, and discharging the remaining 20% of the purified wastewater after being detected to be qualified; according to the invention, a grading process of pretreatment, catalytic oxidation, biological denitrification and reclaimed water reuse is designed, so that deep purification of high-ammonia-nitrogen COD wastewater is realized.

The invention discloses a hexazinone-containing herbicide and a preparation method thereof, and belongs to the technical field of pesticides. The preparation method comprises the following steps: S1, preparing PEI / CS; and S2, uniformly mixing Tween-80 with a PEI / CS solution, dispersing hexazinone in DMF for ultrasonic dissolution, slowly dropwise adding the hexazinone solution into the PEI / CS solution under a magnetic stirring condition, carrying out a reaction for 30 min to obtain PEI / CS / hexazinone, dropwise adding a 2-hydroxy-4-methoxybenzophenone-5-sodium sulfonate solution into the PEI / CS / hexazinone, carrying out a stirring reaction for 30 min, and carrying out centrifugation, washing and drying to obtain the hexazinone-containing herbicide. The final product obtained by the method has high load rate, slow release stability and photodegradation resistance, the preparation efficiency is high, and the process is simple and controllable.

The invention relates to the technical field of organic synthesis, and discloses a production process for synthesizing hexazinone. The process comprises the following steps: S1, mixing a dimethylamine solution with deionized water, dropwise adding a cyano formamide aqueous solution, carrying out heating reaction, and carrying out reduced pressure distillation and recrystallization to obtain an intermediate I; s2, dissolving the intermediate I in N-methyl pyrrolidone, dropwise adding cyclohexyl isocyanate for reaction, adding a solid-phase catalyst and potassium carbonate for cyclization reaction, and performing post-treatment on reaction liquid to obtain hexazinone; the solid-phase catalyst is prepared by bonding a quaternary ammonium salt reagent on a silanization modified mesoporous silica carrier, can be simply and conveniently recycled after reaction, and has good reusability. No side reaction is generated, high-purity hexazinone can be obtained, the reaction efficiency can be effectively improved, the process stability is excellent, and the method is suitable for industrial production.

The invention discloses a hexazinone-containing efficient forest weed killer and a preparation method thereof, and belongs to the technical field of pesticides. The preparation method of the hexazinone-containing efficient forest weed killer comprises the following steps: S1, preparing a modified metal organic framework; s2, in a nitrogen atmosphere, dissolving the modified metal organic framework in deionized water, heating to 40-80 DEG C, then adding sodium lignin sulfonate to react with acrylic acid for 10-20 minutes, then adding an initiator, heating to 80-100 DEG C, reacting for 1-2 hours, cooling to room temperature, washing and drying to obtain a modified carrier; s3, dissolving hexazinone technical and the modified carrier in DMF, stirring at room temperature, centrifuging, washing and drying to obtain the herbicide. The finally obtained herbicide can realize slow release of hexazinone by virtue of a carrier, and the weeding long-term effect and the environmental safety are improved.

The application belongs to the technical field of herbicides, and provides a preparation method of the herbicide cycloxaprid, which comprises the following steps: 1, mixing and stirring monocyanamide and ethyl chloroformate, cooling to 0-2 DEG C, adding liquid alkali dropwise, controlling pH and temperature, and carrying out incubation reaction to obtain a product GH520-1; 2, adding dimethyl sulfate and benzyl triethylammonium chloride to the product GH520-1, carrying out warming reaction, and after the reaction is completed, standing and layering to obtain a product GH520-2; 3, adding dimethylamine hydrochloride and liquid alkali to the product GH520-2, supplementing toluene, carrying out warming reaction, cooling to room temperature, standing and layering to obtain a product GH520-3; 4, dissolving the product GH520-3 in toluene, adding cyclohexyl isocyanate, and controlling the reaction temperature to obtain a product GH520-4; and 5, adding sodium methoxide and dimethylamine aqueous solution to the product GH520-4, controlling the reaction temperature, and obtaining a product GH520.

The invention relates to the technical field of organic synthesis, and discloses a production method for continuously synthesizing hexazinone. The method comprises the following steps: preparing dimethylamine, a catalyst and toluene into a solution A, and continuously introducing the solution A and a toluene solution of cyanoformamide into a first micro-channel reactor through a peristaltic pump for reaction; premixing the obtained reaction liquid with a toluene solution of cyclohexyl isocyanate by a static mixer, and then pumping the mixture and a methanol solution of sodium methoxide into a second micro-channel reactor together for a cyclization reaction; and washing and separating the reaction effluent, performing reduced pressure concentration on the organic phase through a falling film evaporator to recover the solvent, and performing post-treatment on the concentrate to obtain the high-purity hexazinone. The continuous microchannel reaction technology is adopted, the reaction efficiency is high, side reactions are few, the product purity is high, highly toxic phosgene does not need to be used in the production process, meanwhile, raw materials are low in price, easy to obtain and environmentally friendly, and the method is suitable for industrial production.