45 results about "O-Nitroanisole" patented technology

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.

The invention relates to a method for preparing o-nitroanisole and p-nitroanisole from mixed nitrochlorobenzene. According to the invention, mixed nitrochlorobenzene consisting of a product obtained after nitration of chlorobenzene, o-nitrochlorobenzene, m-nitrochlorobenzene and p-nitrochlorobenzene is used as a raw material, and in a methanol system, 30% of alkali lye and a phase-transfer catalyst are added for a reaction to prepare products of o-nitroanisole and p-nitroanisole, wherein m-nitrochlorobenzene does not participate in the reaction. The method provided by the invention overcomes the problems of great investment for rectifying tower equipment, great energy consumption in rectification, high cost, long process flow, harsh operation conditions, poor operational safety performances and generation of waste residues hardly to treat in rectification-crystallization separation of mixed nitrochlorobenzene in conventional production processes for o-nitroanisole and p-nitroanisole and overcomes the technical problems of generation of considerable alkaline waste water containing sodium hyposulfite and production of a poor-quality product in a sodium sulfide reduction process.

The invention discloses a preparation method of anhydrous system o-nitroanisole, which comprises the following steps: mixing and stirring o-nitro benzene chloride, methanol, and an alkalization deacidification agent, heating the mixture with a heating speed of 30 DEG C/h for reflux reaction, controlling the temperature at 40-80 DEG C, performing the reflux reaction for 2-10 h, filtering, recovering methanol, performing reduced-pressure distillation to obtain the product of o-nitroanisole. The invention obtains the product by directly heating o-nitro benzene chloride, methanol, and an alkali; after the reaction, the reaction solution is directly pressed into a storage groove for precipitation; methanol is recovered (by direct recycle); the obtained product and unreacted o-nitro benzene chloride (for recycle) are treated by rectification; the utilization rate of o-nitro benzene chloride reaches above 98%, and the yield of o-nitroanisole reaches 93%-95%; the utilization rate of methanol is greatly increased; the process steps are reduced; the distillation is reduced; the energy consumption is saved; and waste water generated during a traditional process is converted into solid wastes. Compared with the traditional processes, the invention has the advantages of short process, low energy consumption, high utilization rate of o-nitro benzene chloride, and less pollution.

The invention relates to a method of preparing o-anisidine and p-anisidine through hydrogenation reduction of a mixture of o-nitroanisole and p-nitroanisole. According to the method, o-nitroanisole and p-nitroanisole are used as raw materials, and o-anisidine and p-anisidine are prepared in a methanol system through hydrogenation reduction with Pt/C as a catalyst. With the method provided by the invention, the disadvantages of high energy consumption and high cost in conventional production process of o-anisidine and p-anisidine are overcome, and the technical problems of severe environmental pollution and loss of materials caused by considerable process waste water generated in the process of pretreatment in conventional production process are overcome; the method provided by the invention has the advantages of easiness, a high conversion rate, clean, green and environment-friendly process and a small amount of pollution by three wastes.

The present invention provides a new method for preparing o-nitro anisole by using a micro-channel reactor, particularly application of a micro-channel reactor with an enhanced mass transfer unit structure to carry out a continuous flow o-nitro chloro benzene etherification reaction. According to the present invention, the mass transfer and the heat transfer can be completed dependent on the kinetic energy of the fluid without the mechanical stirring process under the reactor operation condition higher than the normal temperature, the space time reaction rate of the micro-channel reactor can be substantially improved, the temperature fluctuation and the concentration fluctuation during the reaction process can be avoided, the phenomena such as temperature runaway and overheating do not exist, and the reaction process is safe.

The invention discloses a method for preparing o-nitroanisole. The method comprises the following steps: performing a methoxylation reaction in organic solvent and basic state; and collecting the o-nitroanisole from a reactant by adopting a conventional method, wherein the molar yield of the finished product reaches over 90 percent. The method has reasonable process route; and the finished productprepared by adopting the method has higher yield and purity, thus has larger industrial prospect.

The invention discloses electrolyte used for an electrolysis capacitor, and a preparation method thereof, and relates to the technical field of electrolyte. The electrolyte used for the electrolysis capacitor consists of the following raw materials in parts by weight: 20-60 parts of ethylene glycol, 5-9 parts of ammonium metatungstate, 2-10 parts of glycerol, 5-13 parts of ammonium sebate, 1-5 parts of polyvinyl alcohol succinate, 1-5 parts of sodium hypophosphite, 2-6 parts of o-nitroanisole, 2-14 parts of maleic anhydride, 0.5-3 parts of maleic anhydride, 3-11 parts of sodium tetraborate decahydrate, 0.3-0.7 part of nitrophenol and 1-9 parts of fire retardant. After the above technical scheme is adopted, the electrolyte has the beneficial effects that the electrolyte has an excellent flame retardant property while the electrolyte has good high-temperature-resistant performance, potential safety hazards are unlikely to happen, and therefore, the electrolyte is worth being popularizedand used.

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.

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.

The invention relates to anhydrous ultralow-temperature wide temperature working electrolyte which comprises, according to the parts by weight, 55-70 parts of gamma-butyrolactone, 10-20 parts of ortho-nitroanisole, 0.3-0.5 part of additive, 3-8 parts of gluconic acid delta lactone, 10-15 parts of ammonium succinate and 2-8 parts of passivant. The preparation method comprises the steps that firstly the gamma-butyrolactone, the ortho-nitroanisole and the gluconic acid delta lactone are mixed and the system is heated and the heat is preserved; then the ammonium succinate is added and the system is heated and the heat is preserved; and finally the additive and the passivant are added and the system is heated and the heat is preserved, then the temperature decreases to 80-90 DEG C within 5-10min and the heat is preserved, and finally the system is heated to 120-140 DEG C within 20-30min and the heat is preserved and then the system is naturally cooled. The anhydrous ultralow-temperature wide temperature working electrolyte has great electrochemical property.

The invention discloses an electrolyte suitable for a high-voltage aluminum electrolytic capacitor and a preparation method thereof and belongs to the technical field of high-voltage aluminum electrolytic capacitors. The electrolyte solution suitable for the high-voltage aluminum electrolytic capacitor comprises the following raw materials including, by weight, 40 to 60 parts of 4-hydroxybutyrolactone, 60 to 80 parts of polyethylene glycol, 50 to 70 parts of ethylene glycol, 30 to 50 parts of ethylene carbonate, 40 to 60 parts of propylene carbonate, 30 to 40 parts of diethyl carbonate, 20 to30 parts of dimethyl carbonate, 10 to 20 parts of ethyl methyl carbonate, 20 to 40 parts of ammonium azelate, 30 to 50 parts of ammonium dodecanedioate, 10 to 30 parts of benzoic acid, 40 to 60 partsof ammonium formate, 40 to 50 parts of diammonium hydrogen phosphate, 30 to 40 parts of phthalic acid, 10 to 20 parts of boric acid, 10 to 20 parts of p-nitrophenol, 5 to 10 parts of sodium hypophosphite, 10 to 20 parts of o-nitroanisole, and 20 to 30 parts of monobutyl phosphate. The preparation method of the invention has a simple preparation method and has a broad application prospect.

The invention discloses a preparation method of o-aminoanisole. The preparation method comprises the following steps: adding 4000L of o-nitroanisole into a reduction reaction kettle by using a feeding pump; closing all valves of a reduction reactor; entirely replacing oxygen in the reaction kettle by nitrogen; turning on a stirring device of the reduction reactor after replacing; adding 15kg of a catalyst, heating to 60 DEG C and introducing 600m<3> of hydrogen; heating through reaction heat; keeping the temperature at 130 DEG C by using a jacket and a coiler to cool; controlling a reaction temperature at 60-150 DEG C and a reaction pressure within a range of 0.8-3.0MPa in a reaction process; reducing a temperature inside the kettle to 40 DEG C after the reaction; stopping stirring to settle the catalyst; filtering out the catalyst; sending o-aminoanisole to a layering device; standing for layering; and finally, rectifying to obtain refined o-aminoanisole. The preparation method disclosed by the invention has no need of distillation; the energy consumption of steam is reduced by more than 80%; the yield can be doubled.

The invention discloses a capacitor electrolytic solution, a preparation method and application thereof. The capacitor electrolytic solution comprises the following components in parts by weight: 40-70 parts of ethylene glycol, 2-5 parts of polyethylene glycol, 10-20 parts of dimethylformamide-2, 15-45 parts of a long-carbon-chain hydroxyl mixture, 5-10 parts of a synthesis compound of polyvinyl alcohol and a high-temperature-resistant material thereof, 1-2 parts of mannitol, 2-4 parts of ammonium sebacate, 8-12 parts of ammonium adipate, 3-5 parts of ammonium benzoate, 0.5-1.0 part of m-nitroacetylbenzene, 0.2-0.8 part of o-nitroanisole, 0.5-1.0 part of ammonium dihydrogen phosphate and 8-10 parts of 1,2-ethylene glycol. According to the EG series electrolytic solution provided by the invention, the cost of the liquid chip capacitor is controlled; and an aluminum electrolytic capacitor produced by the EG series electrolytic solution provided by the invention can meet the electrical performance of a product, and is better than a GBL series in high temperature resistance, wherein the upper limit temperature is increased by at least 5 DEG C.

The invention discloses a battery composite electrolyte and a preparation method thereof. The composite electrolyte comprises, by weight, 10-20 parts of ethylene carbonate, 5-15 parts of lithium tetrafluoroborate, 4-12 parts of fluoroethylene carbonate, 8-18 parts of sodium silicate, 6-14 parts of magnesium carbonate, 2-6 parts of corrosion inhibitor, 2-8 parts of 2-phenylimidazoline quaternary ammonium salt, 3-9 parts of fatty alcohol polyoxyethylene ether, 4-10 parts of 2,3-dimethyl sebacic acid, 2-6 parts of o-nitroanisole and 1-4 parts of flame retardant. The preparation method is simple,the prepared composite electrolyte is environmentally friendly and non-toxic and is beneficial for improving the thermal stability of an electrolyte system, the high temperature cycle and high temperature storage performance of a battery can be improved, and the safety is high.

A crystallizing process for separation of nitro phenylmether mixture includes such steps as thermal dissolving of said mixture in methanol, decoloring, removing impurities, filtering to obtain refined liquid, cooling step by step for crystallizing, filtering to obtain p-nitro phenylmether and o-nitro phenylmether, respectively recrystallizing in methol, separation and refining to obtain refined two products.

The invention discloses a capacitor electrolytic blending liquid and a preparation method thereof. The capacitor electrolytic blending liquid comprises the following components in parts by weight: 35-50 parts of ethylene glycol, 1-2 parts of o-nitroanisole, 10-20 parts of a long-carbon-chain hydroxyl mixture, 10-20 parts of polyvinyl alcohol and a composition of a high-temperature-resistant material of the polyvinyl alcohol, 2-6 parts of ammonium sebacate, 0.5-0.8 part of ammonium hypophosphite and 10-20 parts of 1,2-ethylenediol. The capacitor electrolysis blending liquid can be used for blending electrolyte scrapped due to the performance of the electrolyte, so that the electrolyte can be reutilized, and the cost is reduced. In an electrolyte blended by the capacitance electrolysis blending liquid, the performance is tested by a conductivity tester, a PH tester, a sparking voltage tester, a silver nitrate titration method for detecting the content of chloride ions and the like, and the following parameters are obtained by testing at 30 DEG C: the sparking voltage, the conductivity, the PH value and the content of chloride ions are all normal, and the electrolyte is not abnormal after silver nitrate titration; and the requirement of electrolyte performance blending can be met.