24 results about "Nitrochlorobenzene" patented technology

The invention discloses a 96-hole preassembled plate fat-soluble vitamin pretreatment kit, and belongs to the technical field of in-vitro diagnostic reagents. Comprising magnetic bead suspension liquid, equilibrium liquid, leacheate 1, leacheate 2 and eluent which are carried on a preassembled plate, and the magnetic bead suspension liquid comprises absolute ethyl alcohol and magnetic beads; the preparation process of the magnetic beads comprises the following steps: activating carboxyl of the carboxyl magnetic beads through EDC and NHS; then nitrochlorobenzene and triethylamine are added for a coupling reaction; mixing the coupling reaction product with pyrrolidone, ammonium persulfate and a pore-foaming agent to obtain target magnetic beads; the magnetic beads can be specifically combined with fat-soluble vitamins in human serum or plasma, efficient separation and release of an object to be detected are achieved through a magnetic separation technology, and the magnetic beads are suitable for follow-up mass spectrum quantitative analysis. The kit disclosed by the invention has the characteristics of simplicity and convenience in operation, high extraction efficiency and good stability, the pretreatment time can be remarkably shortened, the detection accuracy is improved, and an efficient solution is provided for clinical detection of fat-soluble vitamins.

This utility model discloses an apparatus for preparing 2,4,4'-trichloro-2'-nitrodiphenyl ether, relating to the technical field of 2,4,4'-trichloro-2'-nitrodiphenyl ether production apparatus. The inlet of the reaction vessel is connected via pipelines to a 2,4-dichlorophenol tank, a 2-nitro-4-chlorophenol tank, a sodium hydroxide tank, and an N,N-dimethylformamide tank. The outlet of the reaction vessel is connected via pipelines to an extraction tank. The inlet of the extraction tank is connected via pipelines to a deionized water tank and an ethyl acetate tank. The outlet of the extraction tank is connected via pipelines to an organic phase tank. The outlet of the organic phase tank is connected via pipelines to a drying tank. The inlet of the drying tank is connected via pipelines to an anhydrous sodium sulfate tank. The outlet of the drying tank is connected via pipelines to a vacuum distillation tank. The bottom outlet of the vacuum distillation tank is connected via pipelines to a product tank. The process is simple, and the product yield and purity are high.

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.

This invention discloses a tail gas recovery device for nitrochlorobenzene production, relating to the field of nitrochlorobenzene production technology. It includes a treatment chamber with an inlet pipe connected to one side of its bottom and an exhaust pipe connected to its top. A piston plate is installed inside the treatment chamber, and an electric telescopic rod is connected to one side of the chamber. A first lifting rod is connected to the telescopic end of the electric telescopic rod and is connected to the piston plate. Multiple atomizing nozzles are distributed laterally at equal intervals on the bottom of the piston plate. The tail gas generated during nitrochlorobenzene processing enters the treatment chamber through the inlet pipe. The atomizing nozzles on the piston plate spray the tail gas with a reaction liquid, facilitating the elimination of harmful substances in the tail gas. During this process, the piston plate also descends, compressing the tail gas and atomized liquid within the treatment chamber, ensuring sufficient contact and reaction within a smaller space, thereby improving the treatment effect.

The invention belongs to the technical field of organic synthesis and fine chemical engineering, and particularly relates to a method for continuously synthesizing 2, 5-dimethoxy-4-nitrochlorobenzene. A continuous flow reaction system is adopted, 2, 5-dimethoxychlorobenzene and 75%-78% nitric acid are pumped into the system respectively, mixed and then enter a silicon carbide microchannel reactor, an initial reaction is carried out at the temperature of 40-60 DEG C, then the mixture enters a coil delay microreactor at the temperature of 50-70 DEG C to complete nitration, and the total retention time is 20-80 seconds. According to the method disclosed by the invention, accurate temperature control on the strong exothermic nitration reaction is realized through enhanced mixing and heat transfer of the microreactor, concentrated sulfuric acid does not need to be added, the reaction can be completed within tens of seconds, the raw material conversion rate is high (the residue is less than or equal to 0.13%), the product selectivity is good (the content is more than or equal to 98.33%), and the production efficiency and the process safety are remarkably improved; the method is suitable for green, efficient and continuous production of the intermediate, realizes accurate monitoring, and is suitable for large-scale safe production.

The present application relates to the synthesis of pesticide compounds, in particular to a method for preparing a pyrasulfotole intermediate. The method comprises: (1) using p-chlorotoluene as a raw material, through nitration, chlorination, hydrolysis, or chlorination, hydrolysis, nitration, to obtain 3-nitro-4-chlorobenzaldehyde, (2) fluorination and reduction of 3-nitro-4-chlorobenzaldehyde to obtain 4-fluoro-3-amino benzaldehyde; (3) 4-fluoro-3-amino benzaldehyde is then contacted with chloroformate for reaction, and then chlorination to obtain compound IV; (4) compound IV is contacted with trifluorobutanamine ester under alkaline conditions for reaction to obtain compound I. The process for preparing compound I avoids using expensive raw material 2-chloro-4-fluorobenzoic acid, effectively reduces the cost of raw materials, reduces the three wastes generated in the process, and at the same time, the total yield of the reaction is high, and it is suitable for industrial mass production.

The application discloses a method for synthesizing 2,4-dinitroanisole based on a channel type continuous flow. The method uses a methanol solution of 2,4-dinitrochlorobenzene as a first mixed solution, an aqueous sodium hydroxide solution as a second mixed solution, then controls parameters of a micro-channel reactor, pumps the first mixed solution and the second mixed solution into the micro-channel reactor for mixing and reaction, finally cools and collects the mixed solution by using ice water, and filters and dries to obtain 2,4-dinitroanisole. In the method, the conversion rate of 2,4-dinitrochlorobenzene is high, the yield of 2,4-dinitroanisole is high, the quality of 2,4-dinitroanisole is high, the synthesis process is environmentally friendly, and safety is good.

The application discloses a wastewater treatment method for nitrochlorobenzene production and belongs to the technical field of organic chemical wastewater treatment. The treatment method comprises the following steps: wastewater is self-flowed into a pretreatment tank and is layered by standing, upper-layer wastewater is treated by using adsorption resin to obtain desorption liquid, catalyst and potassium persulfate are added into the desorption liquid, stirring and filtering are carried out, and treatment liquid is obtained, and the treatment liquid is discharged after being detected to be qualified. In the application, sulfate radicals are used as main active molecules to treat phenolic substances. In order to improve the treatment efficiency, the application prepares a catalyst. The catalyst prepared by the application is prepared by loading active substances on a carrier. The carrier is a diatomite-based carrier with high porosity and strong catalytic performance. The main component of the active substances is magnetic nano CoFe2O4 particles. The wastewater treatment method for nitrochlorobenzene production disclosed by the application can significantly reduce the content of nitrochlorobenzene and the total phenol content in wastewater.

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.

The invention discloses a photocatalytic oxidation combined treatment process and device for nitrochlorobenzene wastewater, and the process comprises the following steps: continuously feeding nitrochlorobenzene wastewater into a first-stage synergistic catalysis system, introducing ozone and hydrogen peroxide, and carrying out a synergistic oxidation reaction to obtain first-stage oxidized effluent; and continuously adding primary oxidation effluent into a secondary photocatalytic oxidation system, adding hydrogen peroxide, and carrying out an oxidation reaction under co-catalysis of ultraviolet light and a photocatalyst. The chromaticity of the wastewater is reduced to 500-1000 times by adopting ozone / hydrogen peroxide concerted catalysis, then the wastewater is connected with a subsequent improved secondary photocatalytic oxidation system for photocatalytic oxidation, and meanwhile, a thin wire is wound on an ultraviolet lamp sleeve with relatively high light intensity, so that turbulent flow near the sleeve can be enhanced, and more wastewater enters a strong ultraviolet light area; the photocatalyst is arranged on the reactor wall with relatively weak light intensity, so that the oxidation capacity of a weak ultraviolet region can be enhanced, the treatment capacity of the tubular reactor is improved, the treatment time is shortened, and the treatment cost is saved.

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 relates to the technical field of synthesis of organic compounds, and particularly discloses a synthesis process of paranitroaniline. The synthesis process comprises the following steps: (1) preparing strong ammonia water with the concentration of 38-42% by using an ammonia water preparation unit; (2) adding p-nitrochlorobenzene, stronger ammonia water and an auxiliary agent into the reaction kettle, and then carrying out heat preservation reaction for 14-16 hours under the conditions that the temperature is 150-170 DEG C and the pressure is 5.6-6.2 MPa; the auxiliary agent comprises modified cyclodextrin and trehalose; and (3) transferring the material in the reaction kettle into a water washing kettle after pressure relief, carrying out water washing stirring for 1-2 hours, and carrying out centrifugal separation on the material liquid after water washing to obtain p-nitroaniline. According to the synthesis process disclosed by the invention, the problem of balance between main reaction efficiency and side reaction inhibition is solved from a reaction mechanism level through compounding and synergy of the modified cyclodextrin and the trehalose, and finally, high yield and high purity in the paranitroaniline synthesis process are synchronously achieved.

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.

This utility model relates to the field of nitrochlorobenzene purification technology, and discloses a p-nitrochlorobenzene purification device, including a mounting plate, a heating plate fixedly mounted on the bottom of the mounting plate, a mixing box fixedly connected to one side of the mounting plate, a crushing barrel connected through the upper surface of the mixing box, a crystallization barrel connected through the upper surface of the crushing barrel, a first variable speed motor fixedly mounted on the upper surface of the crystallization barrel, and a crushing frame fixedly connected to the output end of the first variable speed motor. This utility model facilitates the filtration of crushed coarse materials, and the addition of springs not only enhances the elasticity of the filter plates, but also causes the filter plates to vibrate back and forth, effectively improving the filtration effect and helping to filter materials of different particle sizes more finely. Furthermore, by releasing the limiting block from obstructing the crystallization plate, the operator can easily pull the crystallization plate out from inside the limiting ring for necessary cleaning, replacement, or maintenance.

The application relates to the technical field of organic compound synthesis, and particularly discloses a synthesis process of p-nitroaniline. The synthesis process of p-nitroaniline comprises the following steps: (1) preparing concentrated ammonia water with a concentration of 38%-42% by using an ammonia water preparation unit; (2) adding p-nitrochlorobenzene, concentrated ammonia water and an additive into a reaction kettle, and then carrying out heat preservation reaction under the condition of 150-170 DEG C and 5.6-6.2 MPa for 14-16 h; the additive comprises modified cyclodextrin and trehalose; (3) after pressure relief, the materials in the reaction kettle are transferred into a water washing kettle to carry out water washing and stirring for 1-2 h, and the material liquid after water washing is subjected to centrifugal separation to obtain p-nitroaniline. According to the synthesis process, the modified cyclodextrin and the trehalose are compounded and synergized, the balance problem of the main reaction efficiency and the side reaction inhibition is solved from the reaction mechanism level, and finally the high yield and the high purity in the synthesis process of p-nitroaniline are simultaneously achieved.

The application discloses a preparation method of high-purity N,N'-bis(4-amino-2-chlorophenyl) terephthalamide with purity above 99.5% and application thereof. The high-purity N,N'-bis(4-amino-2-chlorophenyl) terephthalamide is prepared from 2-chloro-4-nitrophenylamine and terephthaloyl chloride as starting materials, and the preparation comprises the following steps: firstly, condensation reaction is carried out to obtain N,N'-bis(4-nitro-2-chlorophenyl) terephthalamide; and then, catalytic hydrogenation reaction is carried out to obtain N,N'-bis(4-amino-2-chlorophenyl) terephthalamide. The condensation reaction is carried out in a toluene solvent at a temperature of 90-100 DEG C; and the catalytic hydrogenation reaction is carried out in a tetrahydrofuran or N,N-dimethylformamide or n-butanol solvent at a temperature of 60-70 DEG C. The prepared N,N'-bis(4-amino-2-chlorophenyl) terephthalamide has purity above 99.5%, and can be applied to preparation of a liquid crystal alignment agent. The liquid crystal alignment agent prepared from the N,N'-bis(4-amino-2-chlorophenyl) terephthalamide has a high and stable pre-tilt angle, a high voltage holding ratio, a low residual direct current voltage, a low ion concentration and good rubbing resistance, and can be used in a high-generation TFT liquid crystal production line.

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 preparation method of dendrophenol-glycyrrhizic acid self-assembled gel spray as well as a product and application thereof, and belongs to the field of new medical application of active ingredients of traditional Chinese medicinal materials. The preparation method comprises the following steps: preparing dendrophenol-glycyrrhizic acid self-assembled nanoparticles by taking dendrophenol and glycyrrhizic acid as raw materials, mixing the nanoparticles with chitosan, adding a cross-linking agent, and further preparing into a gel spray dosage form. Experimental results show that the gel spray has good biocompatibility and remarkable antibacterial performance, inflammatory response and epidermis thickening of a mouse allergic skin disease model induced by 2, 4-dinitrochlorobenzene can be effectively inhibited, scratching behaviors are reduced, skin tissue inflammation and oxidative stress injury are relieved, and the gel spray has a good application prospect. The infiltration of eosinophilic granulocytes and mast cells at the affected part is reduced, and the immune balance is regulated. The product obtained by the invention has various effects of resisting allergic reaction, diminishing swelling, relieving itching and the like, and has a good application prospect in the aspect of treatment of allergic skin diseases.

The invention discloses a preparation method of m-(beta-hydroxyethyl sulfone) aniline, which comprises the following steps: (1) taking m-nitrochlorobenzene as an initial raw material, taking 2-mercaptoethanol as a sulfhydrylation condensing agent, and carrying out sulfhydrylation condensation reaction to obtain m-nitrophenyl-beta-hydroxyethyl sulfide; (2) carrying out oxidation reaction on the m-nitrophenyl-beta-hydroxyethyl sulfide obtained in the step (1) by taking hydrogen peroxide as an oxidizing agent to obtain m-nitrophenyl-beta-hydroxyethyl sulfone; and (3) carrying out hydrogenation reduction on the m-nitrophenyl-beta-hydroxyethyl sulfone obtained in the step (2) to obtain the m-(beta-hydroxyethyl sulfone) aniline. The method has the advantages of low cost, simple process flow, mild reaction conditions, cleanness, no pollution, high product yield and high product purity.

The invention provides a method for separating p-nitrochlorobenzene from o-nitrochlorobenzene and m-nitrochlorobenzene in a chlorobenzene nitration product. The separation method comprises the following steps: step 1, introducing a chlorobenzene nitration product into a moving bed filled with an adsorbent, and selectively adsorbing m-nitrochlorobenzene to obtain a raffinate phase without meta-isomers and an adsorption phase rich in m-nitrochlorobenzene; step 2, desorbing the adsorption phase by using a desorption agent to obtain a desorption solution, carrying out reduced pressure rectification on the desorption solution, collecting an m-nitrochlorobenzene product at a tower kettle, and obtaining a regenerated desorption agent at the tower top for recycling; step 3, carrying out melt crystallization on the raffinate phase, and separating to obtain a p-nitrochlorobenzene product and crystallization mother liquor; and step 4, rectifying the crystallization mother liquor to obtain an o-nitrochlorobenzene product at a tower kettle. By adopting the separation method disclosed by the invention, the purity of para-nitrochlorobenzene, ortho-nitrochlorobenzene and meta-nitrochlorobenzene is greater than 99.2%, the purity of meta-nitrochlorobenzene is not less than 75%, the energy consumption is remarkably reduced, and the benefit is improved.

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.

The embodiment of the invention provides a crude nitrochlorobenzene washing system and method, and relates to the technical field of chemical separation and purification. The crude nitrochlorobenzene washing system comprises a centrifugal machine shell and a bottom frame and is characterized in that one side of the centrifugal machine shell is communicated with a light phase outlet and a light phase inlet from top to bottom, the other side of the centrifugal machine shell is communicated with a heavy phase outlet and a heavy phase inlet from top to bottom, and the bottom of the centrifugal machine shell is communicated with a drain outlet externally connected with a sewage treatment plant pipeline; a washing assembly is arranged in the centrifugal machine shell, a shaking-up assembly is arranged in the bottom frame, and a drum pressing assembly is arranged at the outer end of the drain outlet. A centrifugal motor embedded in the top of the centrifugal machine shell provides driving force for the washing assembly, and a heavy phase collecting cavity and a light phase collecting cavity are formed in the upper-layer space of the centrifugal machine shell. The centrifugal extraction machine is adopted, mixed washing and centrifugal force field separation processes are completed in one device, the separation process is rapid and sufficient, and the problems that emulsification is prone to occurring and layering is slow in traditional stirring washing are fundamentally solved.

The invention relates to the field of biological medicine, in particular to a chlorzoxazone preparation process which comprises synthesis of 2-nitro-4-chlorophenol, synthesis of a 2-amino-4-chlorophenol methanol solution, preparation of a chlorzoxazone crude product and refining of chlorzoxazone, the 2-nitro-4-chlorophenol can be synthesized at normal temperature and normal pressure by adopting p-chlorophenol with lower cost as a starting material, and the 2-nitro-4-chlorophenol can be used for preparing chlorzoxazone. The addition rate of hydrochloric acid is strictly controlled in the preparation of the crude product, urea byproducts generated by urea digestion can be avoided, impurity wrapping of the product can be reduced through hot filtration and slow cooling crystallization, the purity of the product is further improved, and in the refining link, activated carbon decoloration can adsorb small molecular impurities, and the purity of the product is improved. High-content impurities and trace single impurities can be removed through two times of crystallization, high-purity purification of the product is achieved, and meanwhile salt slag pollution generated by traditional acid-base refining is avoided.