12 results about "P-nitrochlorobenzene" patented technology

The present application relates to the technical field of chemical production, and discloses a method and device system for continuously producing nitrochlorobenzene and application thereof. In the method, mixing of reaction raw materials and reaction are completed in steps, so that the defect of too severe heat release, too high temperature, side reaction and safety problem caused by direct reaction is avoided. Meanwhile, by controlling the volume flow ratio of nitric acid and chlorobenzene feed, the raw material conversion rate and the yield of the target product are improved, and the proportion of p-nitrochlorobenzene in the product is also increased, so that the economic benefit is improved. In addition, the method provided by the present application does not need concentrated sulfuric acid as a catalyst, so that the problem of difficult treatment of waste sulfuric acid is solved, and the environmental protection of nitrochlorobenzene production is improved.

The invention discloses a nitrochlorobenzene isomer separation method, which belongs to the technical field of nitrochlorobenzene production, and comprises the following steps: carrying out rectification treatment on meta-position oil at the rectification temperature of 243-245 DEG C, and separating to obtain o-nitrochlorobenzene and meta-position low oil; enabling the meta-position low oil to flow into a membrane separation system, and separating a p-nitrochlorobenzene crude product and an m-nitrochlorobenzene crude product through a ceramic nanofiltration membrane; and finally, respectively introducing the p-nitrochlorobenzene crude product and the m-nitrochlorobenzene crude product into a reduced-pressure rectifying tower for reduced-pressure rectification treatment to obtain p-nitrochlorobenzene and m-nitrochlorobenzene with the purity of 99.9% or above. The separation method provided by the invention not only can effectively separate three isomers of nitrochlorobenzene, but also has low energy consumption in the separation process.

The present invention provides a method for recovering and treating a 4,4-dinitrodiphenyl ether by-product, and belongs to the technical field of organic synthesis. The present invention adjusts the pH value to 3-4 to remove substances that can react with acid in the by-product salt, and the functions of ferrous sulfate and the first activated carbon are to decolorize and remove the color of the 4,4-dinitrodiphenyl ether material. The pH value is then adjusted to 6-8 to remove ferrous sulfate, and then a second decolorization is performed to obtain a white solid salt. The function of hydrogen peroxide is to remove organic matter in the reaction, and the resin column elution ensures that p-chloronitrobenzene, sodium p-nitrophenolate, and DNP organic matter are completely removed. Finally, a solid salt having a sodium chloride content of ≥99.1g / 100g and a TOC (total organic carbon) of less than 50mg / kg is obtained. The obtained solid salt does not have the odor of p-nitrochlorobenzene, meets the industrial salt standard, and realizes the recovery and use of the 4,4-dinitrodiphenyl ether by-product, thereby reducing costs.

The invention relates to the technical field of chemical products, in particular to preparation and application of polysubstituted phenol intermediates, and discloses a green preparation method of polysubstituted phenol intermediates (such as p-nitrophenol and 2, 4-dinitrophenol), the core is that a chitosan-montmorillonite composite carrier is used for loading a nano zero-valent iron catalyst, and the nano zero-valent iron catalyst is used for preparing the polysubstituted phenol intermediates (such as p-nitrophenol and 2, 4-dinitrophenol). Efficient synthesis is realized through a normal-temperature and normal-pressure hydrolysis-reduction one-step method. The cost of the catalyst is reduced by 60% compared with that of the traditional supported catalyst, and the yield is still kept at 88.8% after the catalyst is repeatedly used for five times; by adding the dispersing agent, the substrate-catalyst contact area is increased, and the p-nitrochlorobenzene is high in conversion rate, high in yield and high in purity; by adopting a normal-temperature and normal-pressure process, the energy consumption is reduced by 40% compared with that of a high-temperature hydrogenation method, and the COD (Chemical Oxygen Demand) The method is suitable for the fields of medicines, pesticides, materials and the like, solves the problems of expensive catalyst, harsh conditions and heavy pollution in the prior art, and has a wide industrial prospect.

The application discloses a treatment process of p-nitrochlorobenzene wastewater and belongs to the technical field of wastewater treatment. The treatment process comprises the following steps: in the first step, the p-nitrochlorobenzene wastewater is introduced into a composite oxidation tank, the pH of the p-nitrochlorobenzene wastewater is adjusted to 5-6, a functional additive and a persulfate salt are added into the composite oxidation tank, and stirring is carried out for 3-4 hours to obtain oxidation wastewater; and in the second step, the oxidation wastewater is filtered, the filtrate is discharged after detection, and the filtrate that does not reach the qualified standard is introduced into the composite oxidation tank for cyclic treatment. The functional additive is a (3-carboxylpropyl) triphenylphosphonium bromide modified zeolite loaded with Pd / Fe. In view of the problem that the p-nitrochlorobenzene is difficult to be directly oxidized and degraded, the p-nitrochlorobenzene is reduced into an amine intermediate product that is easy to be degraded by introducing the functional additive, and then the amine intermediate product is oxidized and degraded by using the persulfate salt, so that the content of the p-nitrochlorobenzene in the wastewater is effectively reduced.

The invention discloses a preparation method of high-purity p-nitrochlorobenzene, and belongs to the technical field of chemical raw materials. The preparation method comprises the following steps: S1, adding chlorobenzene, nitric acid and a catalyst into a synthesis kettle for reaction, and obtaining a mixed product after the reaction is completed; s2, the mixed product is cooled and pumped into a plate-and-frame filter press for solid-liquid separation, a nitrate oil phase is separated out, the nitrate oil phase is neutralized, washed with water, dried and crystallized, and high-purity p-nitrochlorobenzene is obtained. According to the method, the target of efficiently preparing the high-purity p-nitrochlorobenzene is achieved through functional adaptation and process synergy of all the steps, the solid catalyst is adopted, catalytic sites are concentrated, and high catalytic efficiency can be achieved by adding a small amount of the solid catalyst.

This invention provides a method for treating nitrochlorobenzene tar by catalytic hydrogenation to obtain aniline compounds containing chloroaniline and chlorodiphenylamine. This invention utilizes low-value production wastewater to produce chloroaniline and chlorodiphenylamine, which have higher economic value, thus solving the problems of high safety risks and low recovery rates in existing nitrochlorobenzene tar disposal methods.

The invention discloses a method for solvent-free synthesis of 4, 4 '-dinitrodiphenyl ether, and belongs to the field of organic synthesis. The synthesis method comprises the working procedures of feeding dehydration, condensation reaction, reduced pressure distillation, steam distillation, water washing, reduced pressure suction filtration and drying, and the 4, 4 '-dinitrodiphenyl ether is synthesized by taking sodium p-nitrophenolate and p-nitrochlorobenzene as raw materials through solvent-free condensation reaction under the catalysis of potassium chloride. The method provided by the invention has the advantages of direct contact of reactants, short reaction time, high efficiency, energy saving, environmental protection, low production cost, high product yield and good product quality, also avoids the use of organic solvent nitrobenzene, reduces the environmental pollution problem, and realizes green production.

The invention relates to a preparation method of 3, 4 '-diaminodiphenyl ether (3, 4'-ODA). A first aspect of the present application relates to a method for preparing 3-amino-4 '-nitrodiphenyl ether, comprising: (1) synthesizing 3-amino-4'-nitrodiphenyl ether from p-nitrochlorobenzene, m-aminophenol in a first solvent in the presence of a condensing agent wherein the first solvent is selected from sulfones, sulfoxides, amides, phosphamides, and step (1) is carried out under reduced pressure, and step (2) is carried out under reduced pressure; and removing the generated water during the proceeding of the step (1). The invention relates to a method for preparing 3, 4 '-ODA in the second aspect, and the method comprises the steps of (a) preparing 3-amino-4'-nitrodiphenyl ether through the method in the first aspect, and (b) reducing the 3-amino-4 '-nitrodiphenyl ether obtained in the step (a) in the presence of a reducing agent to obtain the 3, 4'-ODA. The invention further relates to the 3, 4 '-ODA obtained through the method in the second aspect.

The invention discloses a preparation method of a medical intermediate 2-(4-nitrophenyl) butyric acid, and belongs to the technical field of medical fine chemical engineering. According to the method, p-nitrochlorobenzene and alkyl cyanoacetate are used as raw materials to react to prepare an intermediate 2-cyano-2-(4-nitrophenyl) acetoacetate, and then the intermediate 2-cyano-2-(4-nitrophenyl) acetoacetate reacts with diethyl sulfate under the alkaline condition to obtain the 2-cyano-2-(4-nitrophenyl) butyric acid alkyl ester. And finally, hydrolyzing through a concentrated sulfuric acid and acetic acid mixed system to obtain the 2-cyano-2-(4-nitrophenyl) butyric acid. The raw materials and reagents used in the method are cheap and easy to obtain, the process is simple and easy to implement, and the cost advantage is remarkable. Meanwhile, the adopted reaction route does not generate isomeride impurities such as 2-(2-nitrophenyl) butyric acid and the like, the yield is high, and the quality of the obtained product is good.

The invention discloses a p-nitrochlorobenzene production wastewater treatment process, and relates to the technical field of wastewater treatment, the p-nitrochlorobenzene production wastewater treatment process comprises the following steps: S1, filtering p-nitrochlorobenzene production wastewater, and removing suspended solid particles to obtain a preliminary purification liquid; s2, adjusting the pH value of the primary purified liquid to 5-6 in an adjusting tank, then adding a humus / montmorillonite / zinc oxide composite material and persulfate, carrying out ultraviolet irradiation, and stirring for 1-2 hours to obtain oxidized wastewater; and S3, carrying out solid-liquid separation on the oxidized wastewater, and discharging the separated liquid after the separated liquid reaches the qualified standard. By using the humus / montmorillonite / zinc oxide composite material, not only can p-nitrochlorobenzene molecules be specifically adsorbed and enriched, but also p-nitrochlorobenzene can be degraded under the action of zinc oxide and persulfate, so that the degradation rate and the total treatment efficiency are remarkably improved.

The utility model discloses a p - nitrochlorobenzene nitration reactor, specifically relates to the technical field of nitration reactor, including the reaction kettle shell, the bottom fixedly connected with support leg of reaction kettle shell, the bottom fixedly connected with the bottom plate of support leg, the top fixedly connected with the cover of reaction kettle shell, the top of cover is provided with the feeding opening, the inside of reaction kettle shell is provided with the inner bag, the inside of inner bag is provided with the stirring rod, and the top of cover is installed the motor of drive stirring rod rotation. The utility model discloses through setting up the multilayer type shock pad of assemblable clamping structure, can effectively when the reactor use to the vibration that produces plays good shock attenuation effect, reduces the vibration influence to the placement surface, and convenient in use to the heat release of p - nitrochlorobenzene nitration reaction process carries out the circulating heat exchange cooling treatment, avoids the problem that the air pressure change caused by the big temperature difference inside and outside causes the inner bag or the reaction kettle shell to take place the bulge of the air pressure change.