366 results about "Nitroaniline" patented technology

The invention discloses a method for preparing o-phenylenediamine by catalytic hydrogenation of o-nitrophenylamine. The method is characterized in that: in the hydrogenation reaction of o-nitrophenylamine, alcohol is used as a solvent, nickel is used as a catalyst, reduction reaction is performed for 2 to 10 hours under the hydrogen pressure of 1.0 to 6 MPa at the temperature of between 40 and 80 DEG C, and the reaction product is rectified to form the while o-phenylenediamine. The method has the advantages that the alcohol is used as the solvent in the catalytic hydrogenation for producing o-phenylenediamine, the alcohol can be reclaimed and directly used for next reaction, and the waste residue produced by distillation can be used as an organic fuel, so that the problem that a large amount of waste water containing organic substances is produced in reduction of iron powder or sodium sulfide in the conventional process is solved; and thick acid and thick alkali used in the conventional process are avoided in the hydrogenation process, so that corrosion of equipment is greatly reduced, pollution is reduced, and almost zero pollution is realized. In addition, compared with the conventional iron powder or sodium sulfide reduction, the catalytic hydrogenation process has the advantages of low pollution, high yield, high quality, short production period and low energy consumption.

The invention provides a synthesis method of an important intermediate 4-(4-aminophenyl)-3-morpholone of a new anticoagulant rivaroxaban, belonging to the field of chemical synthesis. The method comprises the following steps: 1) cyclizing nitroaniline and di-halogen aether to obtain 4-(4-nitrophenyl)-morpholine; 2) reacting 4-(4-nitrophenyl)-morpholine and organic hydroperoxide under the action of a catalyst to generate 4-(4-nitrophenyl)-morpholone; and 3) reducing the 4-(4-nitrophenyl)-morpholone into the under the action of a catalyst, wherein the mol yield of the three steps is higher than 49% (on the basis of nitroaniline). The synthesis method provided by the invention has the characteristics of accessible raw materials, low price, simple operation steps, mild reaction environment and the like, and is suitable for industrialized mass production; and the three wastes are easy to process.

The invention discloses a method and a device for co-production of o-phenylenediamine and p-phenylenediamine. The method for co-production of o-phenylenediamine and p-phenylenediamine is characterized in that a raw material of mixed nitrochlorobenzene obtained by chlorobenzene nitration undergoes an ammonolysis reaction to produce mixed nitroaniline; the mixed nitroaniline undergoes a hydrogenation reduction to produce mixed phenylenediamine; and the mixed phenylenediamine is subjected to rectification separation so that o-phenylenediamine and p-phenylenediamine are obtained. The method and a device for co-production of o-phenylenediamine and p-phenylenediamine have the advantages that production efficiency is high; operation is simple; technological parameters are stable; and safety hidden troubles existing in nitro-compound rectification separation are eliminated.

The invention relates to a preparation method of paranitroaniline. The preparation method comprises the following steps that: (1) a high-pressure conveying pump is used for respectively pumping p-nitrochlorobenzene and stronger ammonia water with the concentration being 45 to 55 weight percent into a tubular mixer according to a weight ratio of 1:(3.0-4.0), and a mixed material is obtained through sufficient mixing; (2) the mixed material is continuously conveyed into a pipeline reactor for reaction, the reaction temperature is 235 DEG C to 245 DEG C, the pressure is 10.0 to 14.0MPa, the reaction time is 40 to 90 minutes, after the reaction is completed, the materials are discharged into a low-pressure reaction kettle by a pressure relief valve, and ammonia is recovered through ammonia release; and (3) after the ammonia recovery, the separation is carried out, the materials are centrifuged and washed after the separation completion, and the paranitroaniline is obtained after the materials are centrifuged to the dry state. The method provided by the invention belongs to a method for continuously producing the paranitroaniline, the production is safer, the production capability is higher, the appearance and the purity of the obtained products are respectively improved, the product quality is excellent, and in addition, the cost is reduced.

The invention provides a method for preparing o-phenylenediamine by utilizing catalytic reduction of ortho-nitroaniline. A bimetal loaded graphene oxide is taken as a catalyst for taking part in hydrogenation reduction in a reaction kettle with a polytetrafluoroethylene liner. According to the scheme, the problems of difficulty in realizing industrial production, difficulty in keeping long-term stable activity of catalyst and the like of the prior art can be solved. The method has a broad industrial application prospect.

The invention discloses a method for preparing a gelatin protein and gold nanoparticle composite thin film and an application of the gelatin protein and gold nanoparticle composite thin film. By the method for preparing the gelatin protein and gold nanoparticle composite thin film, the gelatin protein and gold nanoparticle composite thin film is prepared by depositing gelatin on a Cu(OH)2 nano wire serving as a filtering layer by a filtering method, performing glue-connection and removing the Cu(OH)2 nano wire and then adsorbing and reducing chloroauric acid radical ions according to a reducing characteristic of the gelatin under the action of charge adsorption of the gelatin. The sizes of gold nanoparticles in the gelatin protein thin film can be controlled by controlling the pH value of a chloroauric acid solution and the reaction time of the gelatin protein thin film in the chloroauric acid solution. The method is simple and feasible; the gelatin protein and gold nanoparticle composite thin film can be used as a catalyst and the catalytic conversion efficiency of ortho-nitroaniline is extremely high; and the gelatin protein and gold nanoparticle composite thin film has the advantages of high repetitiveness and convenience in operation.

The invention relates to a synthesis process of 2-cyano-4-nitro-6-bromaniline. The synthesis process comprises the following steps: (1) putting chlorobenzonitrile into a sulfuric acid medium, dropwise adding a mixed acid and carrying out nitration, diluting a nitrified product by adding water and then filtering, dissolving the nitrified material in chlorobenzene, carrying out an ammonolysis reaction on a mixed nitrate-chloride liquid and liquid ammonia and then distilling so as to recycle a solvent, carrying out suction filtration and washing the solvent with water until the solvent is neutral, thereby obtaining a wet product; and (2) putting 2-cyano-4-nitroaniline into the sulfuric acid medium, dropwise adding hydrogen bromide and an oxidizing agent and reacting until the reaction is completely finished, and then filtering so as to obtain a wet 2-cyano-4-nitro-6-bromaniline product. The synthesis process is simple in process procedures and easy to control; and the prepared 2-cyano-4-nitro-6-bromaniline is high in yield and purity, stable in quality, low in cost, less in sewage generation and low in energy consumption, and the environmental index of the prepared 2-cyano-4-nitro-6-bromaniline can meet market demands. Thus, the process provided by the invention is a production process with low energy consumption and pollution.

The invention relates to a pollution-free production technology of direct fast black G, comprising the following implementation steps: firstly, primary acid coupling is carried out on nitroaniline after diazotization and H-acid; after the full reaction of the H-acid is detected, sodium carbonate is added and pH is adjusted to 8 to 8.2 to carry out secondary basic coupling; the coupling product is added into a sodium sulfide solution for reduction, and the temperature gradually raises to t of 38 DEG C to 40 DEG C in the reaction process; after the sodium carbonate is added into the reduction product after acidification to adjust the pH of a medium to 7.5 to 8, the mixture is adsorbed by activated carbon and filtered, and ternary coupling is carried out on the obtained filter liquor after diazotization and lentine; and after the reaction is detected to be end point, the materials are directly delivered to a drying tower for spray drying. In the invention, the reduced reaction solution does not need the processes of salting out, acidification and filtration, activated carbon adsorption is adopted instead. In the process, no waste liquor is generated, and environment pollution caused in the production process of dye is greatly reduced. Simultaneously, wastewater processing is not needed, and the cost is saved. The optimized technology directly transfers the reaction solution after ternary coupling into the drying tower for spray drying; and the yield and the coloring intensity of the dye are effectively increased, energy is saved, the consumption is reduced, and the effect is obvious.

The invention relates the alcohol ether fuel and addition agent. The addition agent comprises methyl formate, methyl methacrylate, trimethyl phosphate, dimethyl carbonate or 10-50wt% diethyl carbonate, dimethyl ether, isopropyl ether, propyl ether, 15-40wt% ethyl ether, isoamyl alcohol, isobutyl alcohol or 15-50wt% isoheptyl alcohol, aminoethyl alcohol, diethyl ethanolamine, triethylamine, hexadecylamine, octadecyl ammonium, 0.5-5wt% nitroaniline, and 0.1-1wt% nufenoxole. The invention has the advantages of non emulsification, non three wastes, low energy consumption and high productivity.

The invention relates to a method for producing 2, 6-dichloro-p-nitroaniline and a special reaction kettle thereof. The method is as follows: nitroaniline and chlorine gas are subjected to substitution reaction in a medium of concentrated hydrochloric acid to generate the 2, 6-dichloro-p-nitroaniline, in particular, the substitution reaction is carried out in a large-volume reaction kettle connected with a tail gas absorption tower, the large-volume reaction kettle comprises a kettle body cast by cement and ceramic tiles lined on the inner surface of the kettle body, and the volume of the reaction kettle is more than or equal to 15m<3>. The adopted large-volume reaction kettle can improve yield, reduce production cost, and reduce environmental pollution.

The invention discloses a method for synthesizing benzimidazole compounds expressed by a formula (III) through a one-pot method. The method comprises the following step of: with ortho-nitroaniline compounds expressed by a formula (I) and fatty alcohol expressed by a formula (II) as raw materials as well as water as a reaction solvent, synthesizing the benzimidazole compounds expressed by the formula (III) through the one-pot method in a shielding gas atmosphere under the action of a supported metal solid catalyst, wherein the supported metal solid catalyst is a Cu-Zn-Pd/Al2O3 catalyst. The method disclosed by the invention has the advantages of being simple in synthesis route, high in product yield, low in production cost, liable to separate the selected solid catalyst, high in activity, good in stability and free of liquid acid and organic solvent, and the like, thereby being an environment-friendly synthesis route. FORMUAL (I), R1CH2OH (II), (III) are described in the specification.

The invention discloses a preparation method and application of cellulose hydrogel-based nano-silver/silver chloride. The method comprises the following steps: (1) under a stirring condition, dropwiseadding a tannic acid solution into a cellulose solution to form a reaction solution I, continuously stirring for 1-3 hours, adjusting the pH value of the reaction solution, heating, then adding glutaraldehyde, and continuously stirring to obtain a reaction solution II; and (2) dropwise adding an AgNO3 solution into the reaction solution II, continuously stirring to obtain a reaction solution III,dropwise adding the reaction solution III into violently stirred deionized water to obtain floccule turbid liquid, performing suction filtration, and washing to obtain a filter cake, namely the silver/silver chloride@cellulose nano composite material. The silver/silver chloride@cellulose nano composite material prepared by the method disclosed by the invention not only is uniform in nano silver and silver chloride distribution, less in agglomeration and smaller in average particle size, but also shows higher catalytic efficiency, and can reduce p-nitrophenol, o-nitrophenol, p-nitroaniline andvarious organic dyes in a short time.

The invention discloses a method of nitroaniline discoloration for measuring nitrogen concentration of nitrite in solution, relating to a method for measuring nitrogen concentration of nitrite in solution. The method works in the following steps: first, 1 to 10 ml tested sample solution is taken and put in a measuring flask of 25 to 100 ml, then 1 to 10 ml nitroaniline solution with concentration of 0.001 to 0.010 mol/L is added and mixed, and then 1 to 10 ml acid solution with concentration of 0.1 to 10.0 mol/L is added and the volume is fixed to the scale through water, then the solution is blended and placed for 1 to 30 min; water is taken as blank, a 10 to 50 mm colorimetric ware is used, a spectrophotometer is adopted to measure the blank absorption value of the reagent and the sample at the scale of 400 to 500 nm, and compared with the standard curve, the nitrogen concentration of nitrite in the sample can be calculated. The method has the advantages of simple operation, larger range of concentration measurement, batch measurement of nitrogen content in nitrite in short time, steady and reliable result as well as good repeatability.

The invention discloses a preparation method of a bromo-nitroaniline dye stuff intermediate, which comprises the following steps of: adding inorganic acid aqueous solution into bromide aqueous solution; stirring the mixture; adding a nitroaniline compound into the mixture; raising the temperature of the mixture to be between 35 and 55 DEG C; pulping and stirring the mixture; dropping chlorate aqueous solution into the mixture, wherein the dropping time is more than 2 hours; stirring the mixture, and raising the temperature of the mixture to between 65 and 75 DEG C; filtering the mixture after reaction; washing a filter cake until the pH value is 5 to 8; and drying the filter cake to obtain the bromo-nitroaniline dye stuff intermediate. The product obtained by adopting the method has high quality and yield, the production cost is greatly reduced, the process is simple, and simultaneously, the pollution, caused by waste gases containing hydrogen bromide and waste water containing bromide salts, to the environment is greatly cut down.

The invention relates to a chitin deacetylase, and an expression gene and an application thereof The amino acid sequence of chitin deacetylase BcCDA is represented by SEQ ID NO.2; and the nucleotide sequence of the BcCDA expression gene is represented by SEQ ID NO.1. An engineering strain constructed by using the gene can efficiently secrete and express the chitin deacetylase BcCDA. A recombinant protein with biological activity is obtained after affinity chromatography one-step purification, and the recombinant protein can degrade solid plate generated yellow green 4-nitroaniline with 4-nitroacetanilide as a substrate. Cloning of the chitin deacetylase gene and the successful preparation of the recombinant protein with biological activity are of great theoretic and practical significance to deep development and high value utilization of the chitin resource.

The invention discloses a synthesis method for a telmisartan intermediate, N-Methyl-o-phenylenediamine (salt), and isomeride thereof. According to the synthesis method, o (m or p)-nitroaniline is subjected to methylation under the action of a methylation reagent and a catalyst so as to obtain N-Methyl-o (m or p)-nitroaniline; and then under the action of a reducing agent, the N-Methyl-o (m or p)-nitroaniline is used to prepare the N-Methyl-o (m or p)-phenylenediamine. According to the synthesis method, the o (m or p)-nitroaniline is adopted as an initial material and is cheap and easy to get, the selectivity of actions of the methylation reagent is strong, and by-product of N, N-dimethyl is avoided. The reaction in the two steps are all subjected to conventional unit operation, the reaction is simple and convenient, and the yield and quality are high, so that the synthesis method is applicable to mass industrial production.

The invention relates to a preparation method for disperse orange 30. The preparation method comprises the following steps of: (1) undergoing a diazotization reaction: undergoing a diazotization reaction on 2,6-dichloroparanitroaniline and nitrosyl sulfuric acid in a sulfuric acid medium to obtain a diazonium product solution; and (2) undergoing a coupling reaction: undergoing a coupling reactionon the diazonium product solution obtained in the step (1) and N-cyanoethyl-N-acetoxyethyl to generate disperse orange 30. Particularly, the chromatograph content of 2,6-dichloro paranitroaniline serving as a raw material used in the step (1) is over 99.8 percent by weight, the content of polychlorinated biphenyl amine is lower than 5 ppm, and the diazotization reaction is undergone at the temperature of 0-5 DEG C in the step (1). A product prepared with the method does not contain any international forbidden byproduct, i.e., polychlorinated biphenyl amine, and a basis is laid for the development of the international market; and moreover, the product prepared with method has high yield, high purity and gorgeous chromatic light.

The invention relates to the technical field of organic synthesis, and discloses a method for synthesizing 4-methoxy-2-nitroaniline by using a continuous flow reactor. The method comprises the following steps: S1, respectively adding a 4-methoxyaniline solution and acetic anhydride into a continuous flow reactor I, and carrying out an acetylation reaction to obtain a reaction solution I containing4-methoxyacetanilide; S2, respectively adding a nitration reagent and the reaction solution I into a continuous flow reactor II, and carrying out a nitration reaction to obtain a reaction solution IIcontaining 4-methoxy-2-nitroacetanilide; S3, respectively adding hydrolysate and the reaction solution II into a continuous flow reactor III, and carrying out a hydrolysis reaction to obtain a reaction solution III containing 4-methoxy-2-nitroaniline; and S4, carrying out post-treatment on the reaction solution III to obtain 4-methoxy-2-nitroaniline. The method is high in reaction speed, small inamount of byproduct 4-methoxy-3-nitroaniline, high in heat and mass transfer efficiency, high in reaction safety, high in selectivity, high in yield and purity and convenient in after-treatment.

The present invention provides 3-substituted amino-1, 2, 4-substituted phentriazine-1, 4-dioxides in the general expression as shown. The compounds are prepared with substituted one-nitroaniline as main material and through acylation to produce urea, cyclization, chlorination, amino substitution, oxidation and other steps. The tests show that the compounds of the present invention have anticancer activity and hypoxia selectivity higher than those of TPZ and may be used in preparing hypoxia selective anticancer medicine.

The invention provides a method for synthesizing N-(4-chlorphenyl)-1,2-phenylenediamine as a key clofazimine intermediate. The method specifically comprises the following steps: 1) by taking o-fluoronitrobenzene and p-chloroaniline as raw materials and utilizing organic base as a catalyst for condensation reaction, reacting in an organic solvent and performing conventional treatment after ending the reaction, thereby acquiring a condensation intermediate N-(4-chlorphenyl)-2-nitryl-1-aniline; 2) by utilizing metallic nickel as the catalyst, performing catalytic hydrogenation reaction on the acquired condensation intermediate in the organic solvent and performing conventional treatment after reducing, thereby acquiring a rough product of N-(4-chlorphenyl)-1,2-phenylenediamine; and 3) re-crystallizing the acquired rough product with the organic solvent, thereby acquiring the end product.

The invention discloses an azabenzotriazol containing ultraviolet absorber the molecular structure of which comprises both a benzotriazole structure and an azacycle structure. Particularly, the invention also discloses the preparation method of the absorber, which comprises the following steps in sequence: 1) carrying out a diazotization reaction on o-nitroaniline derivatives and getting a diazotization solution; 2) carrying out coupling reaction on diazonium salt of the o-nitroaniline derivatives and derivatives of pyrazolone or pyridone and getting a coupling product; and 3) carrying out reduction reaction on the coupling product to finally obtain the azabenzotriazol containing ultraviolet absorber. The molar extinction coefficient of the ultraviolet absorber disclosed by the invention is evidently lower than that of other azabenzotriazol containing ultraviolet absorber with a similar structure.

The invention relates to a method for synthesizing gold nanoparticles by using pycnoporus sanguineus and an application of the method for synthesizing gold nanoparticles by using pycnoporus sanguineu organisms. The method comprises the following steps: (1) culturing pycnoporus sanguineus to the stationary stage, centrifugally collecting, washing by using sterilized deionized water, performing cell lysis by using a cell cracker to release intracellular organic matters, and centrifugally collecting the supernatant to obtain the intracellular extract; and (2) mixing the intracellular extract with a chloroauric acid aqueous solution to obtain a mixed solution which is subjected to shake culture to obtain a gold nanoparticle solution which has higher catalytic property. Experiments show that the gold nanoparticle solution can rapidly and effectively catalyze the degradation of nitroaniline. The method disclosed by the invention is simple and convenient to operate, and is economic, effective, safe and environment-friendly.