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81 results about "O-nitrochlorobenzene" patented technology

Method for producing o-chloroaniline

An o-chloroaniline production method takes o-nitrochlorobenzene as raw material and is characterized in that the o-nitrochlorobenzene is dissolved in alcohol solvent in the presence of catalyst and additive and reacted with hydrogen at 10-120 DEG C and under 0.3-4.0 MPa; the reaction process is continuous reaction; after the completion of the reaction, the o-chloroaniline is obtained through treatment, wherein, the catalyst can be selected from one of the following: Ni/Al2O3, Raney Ni, Pt/C and Pd/C; while the additive can be selected from one, or two, or three of the following compounds: cyclohexylamine, ethylenediamine, ethanolamine, diethanolamine, triethanolamine, pyridine, liquid ammonia, ammonium bicarbonate, ammonium carbonate, sodium carbonate, sodium bicarbonate, potassium bicarbonate, potassium carbonate, potassium hydrogen phosphate, potassium dihydrogen phosphate, sodium hydrogen phosphate and sodium dihydrogen phosphate; the dosage of the catalyst takes up 0.05% to 20% of the mass of the o-nitrochlorobenzene; the dosage of the additive takes up 0. 5% to 20% of the mass of the o-nitrochlorobenzene; the alcohol can be methanol or ethanol; the dosage of alcohol takes up 30% to 150% of the dosage of the o-nitrochlorobenzene; the continuous reaction is realized through 1 to 6 tank reactors which are connected in series.
Owner:淮安嘉诚高新化工股份有限公司

A kind of production method of anthranil

The invention provides a production method of oamino pheylmethyl ether, and the method comprises the following steps of: reacting ortho nitrochlorobenzene serving as a raw material with sodium methoxide for carrying out a methoxylation reaction to obtain orthonitroanisole; secondly, carrying out hydrogenation reduction on the orthonitroanisole by using methanol as a solvent in the presence of a catalyst to prepare the oamino pheylmethyl ether; and finally, carrying out dealcoholization, dehydrogenation and refining on reactants to obtain the oamino pheylmethyl ether as a finished product. The production process comprises the following steps of: preparing sodium methoxide, etherifying the ortho nitrochlorobenzene, distilling the methanol and nitroether for separation, hydrogenating the orthonitroanisole, distilling a hydrogenating solution for separating the oamino pheylmethyl ether and treating wastewater. The production method has the characteristics of simple process, short procedure, continuity in reaction, high production efficiency, good product quality, less energy consumption, concentrated purification of reaction wastewater and no emission, and is suitable for producing the oamino pheylmethyl ether by using the ortho nitrochlorobenzene as the raw material.
Owner:LIAONING SHIXING PHARMA & CHEM

Method for preparing o-chloroaniline by catalytic hydrogenation

The invention discloses a method for preparing o-chloroaniline by catalytic hydrogenation. O-nitrochlorobenzene, ethyl acetate solution, a dechlorination inhibitor and hydrogen are subjected to catalytic hydrogenation synthetic reaction under the effect of a catalyst at the temperature of 25-90 DEG C to obtain the o-chloroaniline. For better technical effects, the o-nitrochlorobenzene, ethyl acetate solution, dechlorination inhibitor are continuously delivered to a fixed bed reactor by a metering pump, inlet amount of hydrogen is controlled by a flow meter, and catalytic hydrogenation synthetic reaction is conducted in the fixed bed reactor. The fixed bed reactor which uses Ni alloy as the catalyst and a neutral carrier as a catalyst carrier is used for controlling the inlet amount of raw materials and hydrogen and the catalyst, thus reducing cost and improving efficiency. In the invention, dechlorination reaction can be effectively inhibited, subsequent processing steps of the principal product are simplified, coupling compounds generated in reaction are little, the selectivity of o-chloroaniline is above 99%, and the dechlorinating amount is below 0.3%. The invention has the advantages of mass industrial production and environment protection.
Owner:JIANGSU KANGHENG CHEM

Method for producing anisidine by mixed nitrochlorobenzene reacting in aqueous solvent

The invention relates to a method for producing anisidine by mixed nitrochlorobenzene (comprising o-nitrochlorobenzene, p-nitrochlorobenzene and m-nitrochlorobenzene) in an aqueous solvent through steps of etherification, hydrogenation, distillation separation, and the like. The method comprises the technical processes: (1) enabling the mixed nitrochlorobenzene and methanol to react, using water as a solvent and sodium hydroxide as a catalyst; (2) separating an aqueous phase; (3) catalyzing and hydrogenating etherified oil, and directly hydrogenating and reducing the etherified oil by using water as the solvent without washing to remove alkaline by water; (4) filtering the catalyst; (5) separating crude products, cooling and precipitating an organic phase, and separating and removing the water phrase; and (6) rectifying and separating an organic phase, and rectifying the organic phase obtained by separating water to obtain pure p-anisidine and pure o-anisidine with the purity over 99 percent. The method for producing anisidine by mixed nitrochlorobenzene reacting in an aqueous solvent has simple technology, low cost and energy consumption, high product purity, environmental protection and low toxicity.
Owner:扬州铭睿达化工科技有限公司 +1

Method for synthetizing 3,5-dichloroaniline

The invention discloses a method for synthetizing 3,5-dichloroaniline by using industrial production residues, namely meta-position oil, of p-nitrchlorobenzene and ortho-nitrochlorobenzene by two steps of chlorination and reductive dechlorination. The method adopts the following technical scheme: adding an organic solvent to nitrochlorobenzene meta-position oil as a raw material, directly producing a quintozene mixture by one-step chlorination under the effect of a catalyst, reacting for 0.5-10 hours under the condition of 10-180 DEG C, and then cooling to 30 DEG C; filtering out quintozene, and putting into an autoclave after washing into a neutral state by hot water; carrying out dechlorination reduction reaction under the effects of an organic solvent and the catalyst, wherein the reaction temperature is 60-200 DEG C, the reaction pressure is 1-20 MPa, and the reaction time is 1-20 hours; cooling to room temperature after the reaction is ended; leading in oxygen or air to stir after blowing off; filtering and distilling under reduced pressure to remove the solvent, so as to obtain the product 3,5-dichloroaniline, wherein the yield is 80-90%. Waste materials are changed into precious materials by a synthetic route adopted by the technology disclosed by the invention; the target of zero emission is achieved; the method has the advantages of sustainable development, energy conservation and consumption reduction, and small environmental pollution.
Owner:CHINA PETROLEUM & CHEM CORP +1

Pt-load catalyst taking mesoporous carbon as carrier, as well as preparation method and usage thereof

The invention relates to a Pt-load catalyst taking mesoporous carbon as a carrier, which is characterized in that the mesoporous carbon is pretreated before Pt is loaded; the pretreatment method comprises one in the following steps of: (1) adding the mesoporous carbon into a 10-30% hydrogen dioxide solution, soaking for 1-24hours, washing and removing hydrogen peroxide; (2) adding the mesoporous carbon into a 1-6M hydrochloric acid or nitric acid solution, soaking for 1-24hours, washing and removing hydrochloric acid or nitric acid; and (3) adding the mesoporous carbon into a 1-6M sodium hydroxide solution, soaking for 1-24hours, washing and removing alkali, wherein the load quantity of Pt is 0.5-5%. The invention also relates to the application of the Pt-load catalyst in preparation of 2, 2'-dichloro hydroazobenzene (DHB) from ortho-nitrochlorobenzene through hydrogenation. The catalyst uses the mesoporous carbon as the carrier, so that the internal diffusion resistance can be better reduced, and the reaction speed is accelerated. The Pt-load catalyst is high in reaction activity and selectivity, and can be repeatedly used for more than eight times, so that the using cost of the catalyst is lowered.
Owner:CHANGZHOU UNIV +1

Yellow peach planting method

The invention relates to a yellow peach planting method, and relates to the technical field of yellow peach planting. The yellow peach planting method includes the following steps of selecting soil; deeply digging a tree pit; treating a sapling, wherein a trunk is wrapped with a layer of gauze, the tightness degree is suitable when the thumb can be inserted into the portion between the gauze and the trunk, the outer side is wrapped by a plastic film, the gauze is soaked in a soaking solution first, the soaking solution is prepared from, by weight, 1-3 parts of water-soluble ammonium polyphosphate, 1-3 parts of fluosilicic acid, 5-8 parts of bentonite, 4-8 parts of gelatin, 1-3 parts of o-nitrochlorobenzene, 0.1-0.3 part of dimethyl sulfone, 0.2-0.5 part of dimethylformamide and 100-200 parts of water, the gauze and the root are soaked together for 4-6 h, and then the sapling is planted; management after planting, wherein the sapling is watered once at the interval of 15-20 days, and water is injected into the gauze from the upper side of the trunk wrapped by the gauze during each time of watering. The method is high in survival rate and growth speed, and the tree hardly suffers from diseases and insects, which is beneficial for increasing the planting yield.
Owner:全椒县管坝民族玉龙生态农业发展有限公司

Device and method for production of o-chloroaniline through continuous catalytic hydrogenation reduction of o-nitro chloro benzene

The invention discloses a device and method for production of o-chloroaniline through continuous catalytic hydrogenation reduction of o-nitro chloro benzene. The method comprises the following steps: o-nitro chloro benzene, a catalyst and a dechlorination inhibitor are put into a hydrogenation reactor, and bottom materials are distributed well; nitrogen and hydrogen are sequentially used for displacing a system completely; a feed valve is opened, the o-nitro chloro benzene and the dechlorination inhibitor are continuously fed into the hydrogenation reactor, wherein the mass ratio of the o-nitro chloro benzene to the catalyst to the dechlorination inhibitor is 1:(0.001-0.005):(0.001-0.005); hydrogen is fed into the hydrogenation reactor for hydrogenation reaction, wherein the reaction temperature is 60-100 DEG C and the pressure is 0.5-1.5 MPa; hydrogenated liquid enters a heat exchanger firstly through a circulating pump and then passes through a cross-flow filter; the catalyst and part of hydrogenated liquid as well as fresh raw materials together enter an ejector for circulation, and the other part of the hydrogenated liquid is extracted out continuously, and o-chloroaniline is obtained after treatment. The device and the method disclosed by the invention have advantages that the production cycle is short, the catalyst selectivity is high, the dechlorination rate is low, the yield is high, the quality is stable, the equipment efficiency is high and continuous production is realized.
Owner:淮安嘉诚高新化工股份有限公司

Method for synthesizing o-aminoanisole by hydrogenation method

The invention discloses a method for synthesizing o-aminoanisole by a hydrogenation method. The synthesis method specifically comprises the following steps: adding metallic sodium to excess methanol to prepare a methanol solution of sodium methoxide, and then spraying o-nitrochlorobenzene and the methanol solution of sodium methoxide into an etherification kettle; firstly, performing centrifugal separation, then transferring to a distillation kettle for distillation, and then crystallizing and filtering; firstly, introducing the hydrogen gas to exhaust the gas, atomizing o-nitroanisole, usinga catalyst for catalyzing the reaction, introducing nitrogen gas to the kettle to exhaust the gas after the reaction is completed, then cooling and crystallizing, centrifuging at low temperature for separation and filtering, and repeatedly operating for 2 to 3 times to obtain o-aminoanisole. The method for synthesizing o-aminoanisole by the hydrogenation method uses nitrogen-doped porous carbon asa carrier for the catalyst, and the catalyst is made into a lattice. Contact area of the reactant is large, and the reaction proceeds rapidly. A methoxy reagent is directly prepared from the metallicsodium and methanol, and the methoxy reagent is dissolved with methanol to prepare a solution for spraying, so as to accelerate the reaction and promote the reaction to proceed forward.
Owner:ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD

Continuous ammoniation method of aniline organic intermediates

The invention discloses a continuous ammoniation method of aniline organic intermediates. The continuous ammoniation method concretely comprises the following steps of feeding o-nitrochlorobenzene and concentrated ammonia liquid into a six-stage serially connected high-pressure autoclave in a continuous feeding and continuous discharging mode; performing reaction for 10 to 15 hours at the inside pressure of 5.3MPa and the reaction temperature being 170 DEG C; obtaining ortho-nitroaniline; then, transferring the reaction liquid into a secondary reaction kettle; adding caustic alkali for regulating the pH value to be 12 to 13; then, performing reaction for 10 to 30min; obtaining high-purity ortho-nitroaniline and byproducts of ammonium chloride. The continuous ammoniation method has advantages that useful substances can be effectively recovered from intermediates of ortho-nitroaniline produced from carbendazim after the primary reaction is completed; the content of the ortho-nitroaniline after the hydrogenation is 98 percent or higher; the synthesis cost is reduced; the economic benefits are improved; the ammoniation yield is improved; the continuous ammoniation method and process design of the aniline organic intermediates are optimized; the continuous ammoniation method and process design requirements of the aniline organic intermediates are met.
Owner:ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD

Synthesis method of o-amino pheylmethyl ether

The invention discloses a preparation method of o-amino pheylmethyl ether, and relates to the technical field of chemical industry. The method comprises the following steps: adding o-chloronitrobenzene, methanol and a 40-percent sodium hydroxide solution into a high-pressure reaction kettle in sequence, raising the temperature in the kettle to 40 DEG C, and stirring; raising the temperature to 85 DEG C, controlling the pressure at 0.28-0.32MPa, reacting for 8 hours, distilling, removing an internal methanol solution, adding hot water of 70 DEG C for washing, standing for delaminating, and performing liquid separation to obtain o-nitroanisole for later use; putting o-nitroanisole into the high-pressure reaction kettle, adding a sodium sulfide aqueous solution, controlling the pressure at 0.05MPa, controlling the temperature at 118-120 DEG C, pressurizing, refluxing, cooling to 50-60 DEG C, preserving heat for 5 hours, performing liquid separation, removing internal waste water, distilling, crystalizing, drying to obtain finished o-amino pheylmethyl ether, packaging and warehousing. The preparation method has the beneficial effects of convenience and easiness in preparation, environmental friendliness, pollution freeness, ready availability of raw materials, small equipment investment, high purity and convenience in operation. The prepared o-amino pheylmethyl ether has a good use effect, and is safe and reliable.
Owner:安徽佑骏商品混凝土有限公司

Industrial production method of o-nitrobenzenesulfonyl chloride

The invention discloses an industrial production method of o-nitrobenzenesulfonyl chloride. The method comprises the following steps that o-nitrochlorobenzene and sodium methyl mercaptide are subjected to an etherification reaction, filtering is conducted, an obtained filter cake is subjected to recrystallization, and through centrifugation separation and drying, a dry product of o-nitrobenzene dimethyl sulfide is obtained; the dry product of o-nitrobenzene dimethyl sulfide is subjected to a chlorination reaction in batches to obtain a wet crude product, an appropriate amount of hydrochloric acid is added in a chlorination reaction system, the chlorination reaction is carried out in a hydrophilic organic acid solvent, and the mole ratio of the o-nitrobenzene dimethyl sulfide to water during the chlorination reaction is 1:(5-15); a finished product of o-nitrobenzenesulfonyl chloride is obtained through refining and drying. Through HPLC detection, the content of the o-nitrobenzenesulfonyl chloride synthesized by means of the method is 98-98.5%; the yield is 0.72-0.75, the acquisition rate is 0.97 or above, the turbidity (ppm) is 1.5-2, and the melting point is 66-67 DEG C. By adopting the hydrophilic organic acid solvent, the problems about large-scale production discharging, yield and quality are solved, and meanwhile the purposes of mixed application and post-treatment separation of large-scale production water-soluble solvents are achieved.
Owner:苏州市泽宸贸易有限公司

Production method for improving purity of o-nitrochlorobenzene

The invention discloses a production method for improving the purity of o-nitrochlorobenzene. The production method comprises the following steps that anhydrous chlorobenzene, a sulfuric acid solutionand a nitric acid solution are added into a nitrating kettle for a reaction until the amounts of substances do not change anymore; an obtained nitrochlorobenzene mixture is neutralized, filtered andwashed to obtain a precipitant; the washed nitrochlorobenzene mixture and water are heated and then enter an evaporation chamber to achieve azeotropy of the mixture and water, an azeotrope enters a separation chamber, then cooling is conducted to 10-30 DEG C, and filtering is conduced to obtain a crude product of o-nitrochlorobenzene; the crude product is transferred into a washing kettle to be washed and then dried, and then the high-purity o-nitrochlorobenzene is obtained. According to the production method, the nitrochlorobenzene mixture and water are subjected to flashing evaporation in the evaporation chamber, and separation is conducted to obtain the high-purity o-nitrochlorobenzene. According to the production method, an azeotropy separation process is adopted for avoiding the crystallization and heating process, the energy consumption can be effectively lowered, the purity of the product is improved at the same time, complete separation of three kinds of nitrochlorobenzene is achieved, the content of the product o-nitrochlorobenzene reaches 99% or above, and the yield reaches 98% or above.
Owner:ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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