33 results about "Tert-butylhydrazine" patented technology

The invention provides a pymetrozine-containing ultralow volume liquid agent, and belongs to the field of pesticides. The ultralow volume liquid agent consists of pymetrozine or active ingredient compounded by using the pymetrozine and an active ingredient II, and the balance of aids and solvent; and the active ingredient II is any one of bifenthrin, beta-cypermethrin, lambda-cyhalothrin, cyfluthrin, fenpropathrin, deltamethrin, etofenprox, triazamate, tolfenpyrad, chlorantraniliprole, flubendiamide, ethiprole, abamectin, emamectin benzoate, ivermectin, sec-butyl phenyl-N-methyl carbamate, buprofezin, hexaflumuron, flufenoxuron, chlorbenzuron, diafenthiuron, indoxacarb, 1,2-Dibenzoyl-1-tert-butylhydrazine and tebufenozide. The ultralow volume liquid agent is used for preventing and controlling multiple pests on paddy, wheat, corn, vegetables, tobacco, tea trees, fruit trees and sugarcane by ultralow volume spraying, low volume spraying or ultralow volume electrostatic spraying. The ultralow volume liquid agent has the advantages of low water consumption, high effect, long acting time, synergy and the like.

The invention discloses ultralow volume liquid containing spirotetramat, which is prepared by using spirotetramat or a compound of the spirotetramat and an activated ingredient II as an activated ingredient and adding adjuvant and solvent. An activated ingredient B is optional one of etofenprox, efficient cypermethrin, deltamethrin, tolfenpyrad, chlorantraniliprole, flubendiamide, ivermectin, indoxacarb, RH-5849 (1, 2-dibenzoyl-1-tert-butylhydrazine) and tebufenozide. The ultralow volume liquid containing spirotetramat has the advantages of convenience in processing, long-term effect, a target being not easy to resist the pesticide, low environmental pollution, pesticide and water economization, increase of pesticide utilization rate, and can be used for controlling various pests on rice, wheat, vegetables, tobacco plants, tea plants, fruit trees and sugarcanes by means of ultralow volume spray, low volume spray or ultralow volume static spray.

The invention discloses a method for measuring tert-butyl hydrazine hydrochloride by use of pre-column derivatization-high performance liquid chromatography. The method comprises the following steps: by taking benzaldehyde as a derivatization reagent, reacting under the PH of 5.0 and at 30 DEG C for 90 minutes; employing an Elitehplc 1201 high performance liquid chromatograph and an ultraviolet variable detector; adopting a Hypersil BDS C18 (5mu m, 4.6*250mm) chromatographic column; measuring under the conditions of a column temperature within the range of 25-35 DEG C, a mobile phase being 70%-100%(v/v) methanol aqueous solution, a flow velocity within the range of 0.8-1.2mL/min, a detection wavelength of 298nm and a sample size of 20mu L, and recording a peak area; drawing a tert-butyl hydrazine hydrochloride concentration-tert-butyl hydrazine hydrochloride derivative peak area standard curve by use of an external standard method and obtaining a standard curve regression equation; next, calculating the content of the tert-butyl hydrazine hydrochloride. The method is capable of eliminating the interference of hydrazine hydrochloride in the content measurement process and accurately quantitating the tert-butyl hydrazine hydrochloride. The method is complete in derivatization reaction, simple and easy to operate, convenient and reliable, and easy to popularize, and has relatively high accuracy and precision.

The invention discloses a method for continuously preparing tert-butylhydrazine hydrochloride by using a micro-channel reactor. The method comprises the steps of 1, carrying out primary reaction mixing on hydrazine hydrate with the mass concentration of 40-80% and hydrochloric acid with the concentration of 25-36% in the micro-channel reactor to obtain a hydrazine hydrochloride solution; 2, mixingthe hydrazine hydrochloride solution with a tert-butyl alcohol solution in the micro-channel reactor for later use; and 3, carrying out a secondary reaction on the material mixed in the step 2 to obtain a product aqueous solution, continuously concentrating the product aqueous solution to achieve a certain concentration, carrying out cooling crystallization, filtering, and drying to obtain the tert-butylhydrazine hydrochloride. According to the method, the reaction rate and the raw material utilization rate are increased, the side reaction for producing the olefin compounds through tert-butylalcohol dehydration is avoided, the reaction is easy to control, the production period is short, emission of three wastes is little, the total yield can reach 85% or above, and the automation degreeof the reaction process is high.

The invention discloses a preparation process of methoxyfenozide. The process comprises steps as follows: (1) a condensation reaction: tert-butylhydrazine hydrochloride and dichloroethane are added to a condensation kettle at the room temperature, a jacket is cooled to subzero 6 DEG C to subzero 5 DEG C with brine freezing water, a caustic soda liquid is dropwise added, the mixture is left to stand for layering, a water layer is separated out for wastewater treatment, an organic layer is kept at the temperature, 3-methoxy-2-methoxybenzoyl chloride is dropwise added, and the dropwise adding speed is controlled, so that the temperature of the kettle does not exceed 0 DEG C; after a reaction is performed for 7-9 h, if sampling analysis proves qualification, water is added for stirring again, the mixture is left to stand for layering, the water layer is sent for wastewater treatment, dichloroethane is separated out from the organic layer at 75-85 DEG C under the normal pressure condition, toluene is added for dissolution after the mixture is cooled to the room temperature, and a toluene solution of a condensation compound is obtained.

The invention discloses a preparation method of tert-butylhydrazine hydrochloride. According to the preparation method, tert-butyl alcohol and hydrazine hydrate are used as initial raw materials, andan organic acid buffering solution system is used for preparing a tert-butylhydrazine-organic acid solution; then hydrogen chloride is used for carrying out acidification reaction to prepare the tert-butylhydrazine hydrochloride. Compared with the prior art, the method abolishes a step of carrying out acidification by directly utilizing hydrochloric acid or hydrogen chloride gas in a process of synthesizing tert-butylhydrazine and side reactions including tert-butyl alcohol dehydration and the like are reduced; the reaction is mild and easy to control. The total yield of the reaction can reach85 percent or more, and the wastewater amount and the VOC (Volatile Organic Compound) emission amount are greatly reduced; the preparation method meets the requirements of green chemical industry andis suitable for industrial production.

The invention provides a preparation method of a microencapsulated pesticide for controlling sugarcane borers. The method specifically comprises following steps: a neonicotinoid pesticide, a feeding suppressant and an organic solvent are fed into a reaction barrel and heated, an ester compound is added to the stirring barrel after the neonicotinoid pesticide and the feeding suppressant are dissolved, a surfactant is added for emulsification after uniform stirring, and an emulsion is prepared; an aqueous solution of a microcapsule wall material is added to the emulsion and stirred for a capsule forming reaction, and the microencapsulated pesticide is prepared, wherein the neonicotinoid pesticide is one of imidacloprid, thiacloprid, acetamiprid, clothianidin and dinotefuran; the feeding suppressant is one of 1,2-dibenzoyl-tert-butylhydrazine, tebufenozide and nitenpyram. The microencapsulated pesticide prepared with the method has a sustained release function and is convenient to apply.

A composite pesticide containing a nicotine type compound is disclosed. Effective components of the composite pesticide comprise the nicotine type compound and dibenzoyl-1-tert-butylhydrazine. The nicotine type compound comprises one and/or a mixture of more selected from clothianidin, imidacloprid, pymetrozine, dinotefuran, thiachloprid, thiamethoxam, and other nicotine type pesticide compounds. The composite pesticide has good control effects for mixed damage of a plurality of pests such as sesamia inferens, chilo suppressalis, tryporyza incertulas, cnaphalocrocis medinalis guenee, nilaparvata lugens, laodelphax striatellus, and sogatella furcifera in rice fields, can effectively control damage of a plurality of snout moth's larvae, plant hoppers, aphid, vegetable diamondback moth, spodoptera litura, and the like for rice and sugarcane, avoids error and waste when a farmer temporarily mixes and uses a plurality of agents at an edge of a field, and enhances control effects.

The invention discloses a preparation method of methoxyfenozide and relates to the field of insecticide, and particularly relates to the preparation method of methoxyfenozide. The preparation method includes steps of preparation of 3, 5-dimethylbenzoyl chloride: adding 3, 5-mesitylenic acid and methylbenzene in a reaction bottle; raising temperature to 60 DEG C, and dropwise adding thionyl chloride within 2 hours; preserving temperature for 3 hours, depressurizing and removing solvent to obtain 3, 5-dimethylbenzoyl chloride; synthesis of midbody: adding tert-butylhydrazine, sodium hydroxide and methylbenzene in the reaction bottle, and cooling to 0 DEG C; adding di-tert-butyl dicarbonate ester and reacting for 10 hours at 0-5 DEG C; removing a water layer, adding 3, 5-dimethylbenzoyl chloride and sodium hydroxide solution in an organic layer; reacting for 4 hours at 0-5 DEG C, filtering a product and adding the filter cake in methanol; adding hydrochloric acid in the reaction mixture;reacting for 20 hours at 35 DEG C; filtering the product, washing and drying to obtain the midbody. The preparation method is simple in operation, safe and reliable in reaction; the production efficiency is greatly improved, and the production cost is reduced; moreover, the product is high-efficient, low-toxic and environment-friendly.

A primary coat, which consists of a V- or Ti-containing film, is formed on the surface of a subject on which holes or the like have been formed, according to the CVD technique, while using, for instance, a tetravalent amide-type vanadium-containing organometal compound as a raw gas and using, for instance, tertiary butyl hydrazine as a reducing gas, and a copper-containing film is then formed on the primary coat, according to the CVD technique, to thus fill the holes or the like with the copper-containing film and to thus form copper distributing wire, which is excellent in the hole-filling properties and excellent in the adhesion to a primary coat, this process can be applied to the field of copper distributing wires used in the semiconductor industries.

The invention discloses a pesticide composition containing pyrazosulfuron-ethyl and difenoconazole and belongs to the technical field of pesticide. The pesticide composition is compounded and prepared from the following effective ingredients: abamectin, pyrazosulfuron-ethyl, fluorine silicon iodine, sodium humate, 1,2-dibenzoyl-1-tert-butylhydrazine, trifloxysulfuron sodium, ethirimol, coumaphos, merida, a benzenesulfonic acid emulsifier and a benzene solvent. When a finished product of the pesticide composition is prepared, following auxiliary agents of the pesticide composition containing the pyrazosulfuron-ethyl and the difenoconazole, a dispersing agent, an additive, simethicone and water are needed, and a weight ratio of the abamectin to the pyrazosulfuron-ethyl to the 1,2-dibenzoyl-1-tert-butylhydrazine is 10 to 4 to 1. According to the pesticide composition, the two kinds of pesticides with completely different action mechanisms are mixed to achieve combined action on pests from multiple aspects to achieve the purpose of effectively preventing the pests; meanwhile, a use amount of the pesticides in fields is reduced, economical cost is saved, pollution of the pesticides to environment is reduced, and risk that the pests generate resistance to the pesticides is also reduced.

The invention discloses a purifying method of N-(3-methoxy-2-methyl benzoyl)-N'-tert-butylhydrazine. The purifying method comprises the steps as follows: adding water and acid to reaction product obtained by reaction of 3-methoxy-2-methyl benzoyl chloride and tert-butylhydrazine to carry out acidizing until pH is less than 3; keeping the hydrolysis temperature of 40 to 105 DEG C, and hydrolyzing for 0.5 to 5 hours for hydrolyzing the byproduct; filtering to remove 3-methoxy-2-methyl benzoic acid; adding alkali to the obtained mother liquor to carry out alkalizing; adjusting pH to 7 to 12; and filtering to obtain the high-purity product N-(3-methoxy-2-methyl benzoyl)-N'-tert-butylhydrazine. The purifying method disclosed by the invention is simple in production, and greatly improves the purity of the product; and moreover, the expensive intermediate 3-methoxy-2-methyl benzoic acid can be recycled, so that the producing cost is reduced; and little three wastes are produced during the processing; and the purifying method is beneficial to environmental protection, and is suitable for industrial production.

The invention discloses a pesticide mixture containing abamectin and pyrazosulfuron-ethyl and belongs to the technical field of pesticides. The pesticide mixture is compounded from the following active ingredients: abamectin, pyrazosulfuron-ethyl, iodine silicon fluoride, sodium humate, dibenzoyl-1-tert-butylhydrazine, trifloxysulfuron sodium, ethirimol, coumaphos, Merida, a benzene sulfonate emulsifier and a benzene solvent. When the finished pesticide mixture is prepared, the following adjuvants are needed: the pesticide mixture containing abamectin and pyrazosulfuron-ethyl, a dispersing agent, aids, dimethicone and water. The pesticide mixture is capable of co-acting on injurious insects from multiple aspects, and the aim of effectively controlling the injurious insects is achieved. Meanwhile, the dosage of pesticides in the field is reduced, the economic cost is saved, the pollution of the agent on the environment is reduced, and risk of the injurious insects producing resistance to the drug is reduced.

The invention relates to an insecticidal composition containing Polygonum hydropiper. The effective components include metaflumizone, 1,2-dibenzoyl-1-tert-butylhydrazine and a Polygonum hydropiper extractive solution at a weight ratio of 1:1:1. The insecticidal composition of the invention has a synergic effect, and has an excellent control effect on Lepidoptera pests in fruit trees, vegetables, cotton and rice.

The invention provides a method for synthesizing tert-butylhydrazine. According to the method, an alkylation reaction is carried out on tertiary butanol and hydrazine hydrate under the effect of a catalyst at a certain temperature under the protection of inert gases to generate tert-butylhydrazine, a reaction solution is refined after the reaction is finished so as to obtain a tert-butylhydrazinefinished product, and the catalyst used for the reaction is D72 porous strong acidity cation exchange resin. Compared with the prior art, the tert-butylhydrazine is synthesized from tertiary butanol and hydrazine hydrate as raw materials in a one-step method, and the method is simple in processing steps, not high in equipment requirement, low in equipment investment, high in production yield, lowin production cost and little in waste emission and is a green and environmentally-friendly production technology.

The invention relates to the technical field of methods for manufacturing a simple substance palladium thin film, and discloses a method for preparing the simple substance palladium thin film throughan atomic layer deposition technology. The method involves a palladium precursor and a hydrazine reductive precursor, wherein the palladium precursor can adopt palladium hexafluoroacetylacetonate Pd(hfac)2, the hydrazine reductive precursor can adopt C1-C5 hydrocarbon chain reductive precursors such as anhydrous hydrazine, methylhydrazine, ethylhydrazine, propyl hydrazine and tert-butyl hydrazine,and the structural formula of a hydrazine reductive agent is R1R2N-NR3R4, wherein R1, R2, R3 and R4 comprise hydrogen atoms and C1-C5 hydrocarbon chains, and R1, R2, R3 and R4 can be the same or different. The method has the advantages that the hydrazine reductive agent is selected as the reductive precursor, and the simple substance palladium thin film can be deposited by directly utilizing a thermal atomic layer deposition technology; and the thermal atomic layer deposition technology is superior to gases such as plasma hydrogen, oxygen and ozone adopted in the prior art, the more convenience, the more safety and the easier operation are achieved, the inconvenience in operation of plasma hydrogen, plasma ammonia gas and the like can be avoided, the preparation process of the simple substance palladium thin film can be simplified, and the cost is saved.

The invention provides a synthesis method of tert-butylhydrazine. The method is characterized in that under the protection of inert gas, tertiary butanol and hydrazine hydrate take alkylation reactionat certain temperature under the effect of catalysts to generate tert-butylhydrazine; after the reaction is finished, reaction liquid is rectified to obtain a finished product of the tert-butylhydrazine; the catalyst used for reaction is D002 macropore strong-acidity cation exchange resin. Compared with the prior art, the synthesis method has the advantages that the tert-butylhydrazine is synthesized by using the tertiary butanol and the hydrazine hydrate as raw materials by a one-step method; the process steps are simple; the requirements on equipment are low; the equipment investment is low; the reaction yield is high; the production cost is low; the discharged wastes are few; the synthesis method belongs to a green and environment-friendly production process.

The invention belongs to the field of pesticide intermediate, and discloses a method used for removing hydrazine hydrochloride in tert-butylhydrazine hydrochloride. The method comprises following steps: ethanol, and tert-butylhydrazine hydrochloride are introduced into a reaction container provided with a stirring device and a backflow device, 60 to 80 DEG C water bath stirring is carried out fordissolving, an obtained product is cooled to room temperature, ammonium bicarbonate is added, reaction is carried out for 1 to 3 at room temperature, after reaction, filtering is carried out, an obtained filter cake is washed with a small amount of ethanol and is dried, and an obtained filtrate is recycled for 1 to 3 times. The method is simple in operation, is capable of removing all hydrazine hydrochloride in tert-butylhydrazine hydrochloride; generation of waste gas, waste water, and solid waste in production process is little, it is beneficial for environment protection, and is suitable for industrialized production.

The invention belongs to the field of pesticides and pesticide intermediates and discloses a process for purifying tert-butylhydrazine hydrochloride. The process disclosed by the invention comprises the following operating steps: respectively adding ethanol and tert-butylhydrazine hydrochloride into a reaction container filled with a stirring device, stirring for 10-30 minutes, cooling to the temperature of 0-4 DEG C, and adding ferric trichloride; reacting at the temperature of 0-4 DEG C for 1-3 hours, immediately filtering after the reaction is ended, washing the filter cake with a small amount of cold ethanol, and drying, namely obtaining the product. The process disclosed by the invention is simple, and the purity of the tert-butylhydrazine hydrochloride is greatly improved. Moreover,less three wastes are produced in the production process, the environmental protection is facilitated, and the process is suitable for industrial production.

The invention provides a synthetic method for tert-butylhydrazine. The method comprises the following steps: subjecting tert-butyl alcohol and hydrazine hydrate to an alkylation reaction under the protection of inert gas and the action of a catalyst at a certain temperature so as to generate the tert-butylhydrazine, and after completion of the reaction, rectifying a reaction solution so as to obtain a finished tert-butylhydrazine product, wherein the catalyst used in the reaction is a ZnO/Al2O3 composite catalyst. Compared with the prior art, the synthetic method synthesizes the tert-butylhydrazine with the tert-butyl alcohol and the hydrazine hydrate as raw materials through a one-step process, has the advantages of simple process steps, low requirements on equipment, small equipment investment, high reaction yield, low production cost and less waste discharge, and is a green and environment-friendly production process.