46 results about "P-aminodiphenylamine" patented technology

The invention relates to a method for preparing p-aminodiphenylamine, which comprises the following: (1) a step of condensation, in which, nitrobenzene and aniline produce condensation reaction in the presence of a catalyst to generate condensation solution including 4-nitrodiphenylamine and 4-nitrosodiphenylamine; (2) a step of extraction, in which, water phase and organic phase in the condensation solution are separated by an extracting method; (3) a step of reduction, in which, hydrogen and the organic phase of the condensation solution produce reduction reaction in the presence of the catalyst to generate reduction solution including the p-aminodiphenylamine; (4) a step of separation, in which, the p-aminodiphenylamine is separated from the reduction solution to form crude p-aminodiphenylamine feed liquid; and (5) a step of rectification, in which, the p-aminodiphenylamine is separated from the crude p-aminodiphenylamine feed liquid in a rectification mode to form a p-aminodiphenylamine product. The method is suitable for serialized industrialized production in large scale, and has the advantages of low reduction reaction temperature, mild reaction condition, few side products, high conversion rate and selection, low labor intensity and no corrosive liquid, thereby reducing pollution to environment.

The invention relates to a preparation method for p-aminodiphenylamine, and belongs to the technical field of industrial preparation for p-aminodiphenylamine. The technical problem to-be-solved is to provide a preparation method for p-aminodiphenylamine with a condensation reaction catalyst capable of being activated and reused and a reduction reaction solvent having no danger and being easily separated. The technical solution adopted includes: a first step of feeding nitrobenzene, aniline and a complex alkali catalyst into a reactor for a condensation reaction to generate a condensation liquid; a second step of adding alkali to form salt to get a qualified condensation liquid; a third step of adding soft water and composite nickel catalyst slurry, and feeding hydrogen to perform a reduction reaction to get a reduction liquid; a fourth step of extracting and distilling the reduction liquid to get a rectification raw material; and a fifth step of performing a multi-stage rectification for the rectification raw material to get the finished p-aminodiphenylamine. The method can be widely applied to the field of p-aminodiphenylamine preparation.

The invention belongs to the technical field of rubber materials, and relates to an anti-aging natural rubber synthesis method, which comprises: (1) synthesizing an anti-aging silane coupling agent: adding gamma-glycidyl ether propyltrimethoxysilane and p-aminodiphenylamine to a reaction kettle, introducing 0.2-0.6 MPa nitrogen, heating to a temperature of 120-150 DEG C, and stirring for 1-1.5 h at a stirring rotation speed of 100-120 r/min to obtain anti-aging silane coupling agent; and (2) preparing an in-situ modified filler: weighing carbon black, white carbon black and an anti-aging silane coupling agent, placing into the reaction kettle, introducing 0.1-0.2 MPa N2 gas, carrying out heating to a temperature of 50-60 DEG C, and stirring for 1-1.5 h at a stirring rotation speed of 100-120 r/min to prepare the in-situ modified filler. According to the present invention, with the preparation method, the anti-aging natural rubber is prepared by adding the anti-aging coupling agent modified filler, such that the aging resistance of the rubber is improved, and the operation is simple; and the prepared anti-aging rubber has advantages of high strength, strong aging resistance and thelike.

The invention discloses a method for recovering, treating and recycling quaternary ammonium base. According to the invention, the method overcomes disadvantages in conventional recovery and treatmentof quaternary ammonium base produced in preparation of p-aminodiphenylamine by using a nitrobenzene process; the method of the invention has an extra procedure of solvent extraction and recovery of p-aminodiphenylamine and macromolecular viscous organic substances in the quaternary ammonium base, thereby lowering the content of p-aminodiphenylamine and macromolecular viscous organic matters in theammonium base, reducing the viscosity of the recovered quaternary ammonium base, decreasing difficulties in desalting filtering of the recovered quaternary ammonium base, improving desalting effect on the recovered quaternary ammonium base and promoting normal implementation of subsequent condensation reactions and reduction reactions.

The invention provides a method for accumulating nitrite nitrogen by performing short-cut denitrification on p-aminodiphenyl amine production wastewater. The method comprises the following steps of: mixing formic acid-containing wastewater generated in the p-aminodiphenyl amine production process with nitrate-containing wastewater and homogenizing, regulating the C/N ratio and the pH value of the wastewater, adding N and P nutritive salts, carrying out such treatments as sedimentation and air floatation, and then removing high-concentration organic matters out of the wastewater through an oxygen-poor short-cut denitrification reaction, and generating yielding water containing the nitrite nitrogen, which is advantageous for the subsequent anaerobic ammonia oxidation reaction. The method provided by the invention is low in investment, high in income, simple and convenient to operate and stable in treatment effect; besides, the generated wastewater can be further treated and utilized; and as a result, the purpose of reducing wastewater emission is reached and the economic benefit is improved.

The invention discloses a method for separating, desalting and recycling recovered quaternary ammonium base. The method for separating, desalting and recycling the recovered quaternary ammonium base,disclosed by the invention, has the advantages that shortcomings in the prior art of recovering the quaternary ammonium base during using a nitrobenzene method to prepare p-aminodiphenyl amine are eliminated; a procedure of centrifugally separating p-aminodiphenyl amine and macromolecular viscous organic substances in the recovered quaternary ammonium base is increased to reduce the contents of the p-aminodiphenyl amine and macromolecular viscous organic substances in the recovered quaternary ammonium base, reduce the viscosity of the recovered quaternary ammonium base, reduce the desalting and filtering difficulty of the recovered quaternary ammonium base, improve the desalting effect of the recovered quaternary ammonium base and promote normal implementations of follow-up condensation reaction and reduction reaction.

The invention provides a treatment method of p-aminodiphenylamine production device wastewater, particularly a high-efficiency treatment method of process wastewater containing high-concentration formic acid. The method comprises the following steps: primary pH regulation of p-aminodiphenylamine production device wastewater, C/N ratio control in a homogenizing tank, secondary pH regulation, air floatation, N and P nutritive salt addition, influent water temperature regulation, biochemical denitrification treatment and the like. After the p-aminodiphenylamine production device wastewater is treated by the treatment procedure provided by the invention and corresponding conditions, the formic acid concentration in the wastewater can be lowered from 160000 mg/L or so to 0.1 mg/L below, and the removal ratio is up to higher than 90%. The method has the advantages of stable treatment effect and low treatment cost, is simple to operate, and can easily implement industrial application.

The invention discloses a preparation method of functionalized graphene oxide. The method includes: under an ice-water bath condition, adding cyanuric chloride into a mixed solution of acetone and water, stirring the substances evenly, adding ammonia water, carrying out reaction at 1-5DEG C for 30-50min, and then conducting filtering, washing and drying to obtain a material A; adding the materialA into 1, 4-dioxane, mixing the substances evenly, adding a 1, 4-dioxane solution of p-aminodiphenyl amine and sodium carbonate, conducting stirring at room temperature for 30-100min, and performing filtering, washing and drying to obtain a material B; adding the material B into 1, 4-dioxane, adding 1H, 1H-perfluorooctylamine, adjusting the pH to 7, carrying out reaction at 80-90DEG C for 3-4h, and conducting standing, filtering and drying to obtain a material C; subjecting graphene oxide to acylating chlorination, then adding the product into dimethylformamide, adding a material C, carrying out reaction at 80-90DEG C for 20-30h, conducting filtering and drying, mixing the obtained material with plant polyphenol and water evenly, carrying out reaction at 35-60DEG C for 30-48h, and performing drying.

The invention provides a treatment method of p-aminodiphenylamine production device wastewater, particularly a high-efficiency treatment method of process wastewater containing high-concentration formic acid. The method comprises the following steps: homogenizing the p-aminodiphenylamine production device wastewater, regulating the pH value, controlling the C/N ratio, precipitating, adding N and P nutritive salts, regulating the influent water temperature, carrying out biochemical denitrification treatment and the like. After the p-aminodiphenylamine production device wastewater is treated by the treatment procedure provided by the invention and corresponding conditions, the formic acid concentration in the wastewater can be lowered from 160000 mg/L or so to 0.1 mg/L below, and the removal ratio is up to higher than 90%. The method has the advantages of stable treatment effect and low treatment cost, is simple to operate, and can easily implement industrial application.

A process for the preparation of 4-oxo-4-((4-(phenylamino)phenyl)amino)-2-butenoic acid includes reacting p-aminodiphenyl amine and maleic anhydride in a reaction first mixture containing a volatile organic solvent under suitable reaction conditions to provide a second mixture containing 4-oxo-4-((4-(phenylamino)phenyl)amino)-2-butenoic acid product; subjecting the second mixture to vacuum distillation to remove the volatile organic solvent while simultaneously adding diluent oil to produce a dispersion of 4-oxo-4-((4-(phenylamino)phenyl)amino)-2-butenoic acid in the diluent oil.

The invention provides a method for preparing p-aminodiphenylamine through continuous catalysis. According to the method, 4-nitrodiphenylamine and 4-nitrosodiphenylamine are used as raw materials andsubjected to continuous reduction in the presence of an organic solvent under the catalysis of a supported catalyst so as to obtain p-aminodiphenylamine. The method of the invention solves the problems of environmental pollution, low catalyst activity, difficult catalyst recovery and high labor intensity in the prior art.

The invention discloses a method for preparing a tire antioxidant 3100, belongs to the field of fine chemical synthesis, and concretely relates to a production technology for the tire antioxidant 3100. The production technology comprises the following steps: p-aminodiphenylamine and a catalyst are placed in a reaction vessel, and are heated to 110-140 DEG C, the temperature is kept, vacuumizing iscarried out to -0.06 MPa, a mixture of phenol and o-cresol is added under a stirring condition, the obtained mixture is reacted until no water is evaporated, the temperature is reduced to 90-100 DEGC, and the catalyst is filtered out to obtain the tire antioxidant 3100. The technology has the advantages of easily available raw materials, simple reaction process, mild conditions, low and controlled energy consumption, few generated wastes, and suitableness for large-scale production.

The invention relates to a novel anti-aging agent and a preparation method and an application thereof, the novel anti-aging agent is a reaction product of p-aminodiphenylamine (PPDA) and an epoxy compound, the epoxy compound is a compound containing an epoxy group and double bonds, and the molar ratio of p-aminodiphenylamine to the epoxy compound is 1: (1-5), preferably 1: (2-4). The anti-aging agent can be used as the anti-aging agent for natural rubber or synthetic rubber. The novel anti-aging agent provided by the invention has lower migration performance and extraction resistance, and can prolong the service life of a rubber product and avoid environmental pollution; the migration rate of the novel anti-aging agent in rubber neutralization is lower than that of a traditional anti-aging agent, so that good stability, low migration rate and good later-stage anti-aging performance of the anti-aging agent can be better guaranteed.

The present invention is a method for separating p-aminodiphenylamine reducing liquid, which belongs to the field of crude product material separation, and the problem to be solved is to reduce the consumption of crude product material separation; the present invention mainly includes the following steps: solvent distillation, centrifugal separation, inorganic phase concentration, For processes such as organic phase distillation, by adding solvent distillation steps and using centrifugal separation to replace the extraction unit in production, the amount of extraction agent used in the system is greatly reduced, thereby greatly reducing energy consumption by more than 60%.

The invention relates to a preparation method of N-substituted carboxylic acid polyaniline covalently grafted graphene composite material. The preparation method of the N-substituted carboxylic acid polyaniline covalently grafted graphene composite material comprises the following steps: taking graphite powder, preparing graphene oxide (GO), and carrying out ultrasonic dispersion to form a uniform solution; then dissolving a certain amount of p-aminodiphenyl amine in a certain volume of mixed solution of concentrated hydrochloric acid and absolute ethyl alcohol, and carrying out ultrasonic dispersion; in ice-water bath, slowly dropwise adding a quantitative NaNO2 solution into the mixed solution, slowly dropwise adding the GO solution after the NaNO2 solution is dropwise added, reacting for a certain period of time, then treating the obtained functional GO, and then reducing by virtue of hydrazine hydrate and ammonia water; and finally dissolving a certain amount RGO and quantitative N-phenylglycin into an HCl solution with constant concentration, carrying out ultrasonic dispersion, adding a certain amount of initiator ammonium persulphate, and reacting for a certain period of time, so that an NPAN covalently grafted RGO composite material is obtained. Electrical conductivity of the prepared composite material can reach 5.0*10<-1>S/cm, and solubility and stability are obviously improved; and the obtained composite material can be applied to the fields of super capacitors, sensor, solar cells and the like.

The invention relates to the technical field of production of rubber antioxidant midbody, and particularly discloses a separation method of a hydrogenated mixture in the production process of p-aminodiphenylamine. The separation method is characterized in that hydrogenated mixed liquid is sent to a desolventizer tower to remove hydrogenation reaction solvent alcohol, and the rest mixed liquid is recovered from the tower bottom; the tower bottom mixed liquid is sent to an extraction separating tower, meanwhile an extraction solvent is melted in the tower, aniline and p-aminodiphenylamine in themixed liquid are extracted out to serve as an oil phase to be extracted from the tower top of the extraction tower, and a tetramethyl ammonium hydroxide water solution is extracted from the tower bottom; and the oil phase is sent to a distillation separation procedure, an extraction agent and aniline are steamed from the tower top respectively, and p-aminodiphenylamine is extracted out from the tower bottom. Compared with a traditional separation method, the separation method effectively improves the layering speed and the separation effect of the oil phase and a water phase, water consumption amount is small, the postprocessing difficult for recycling a condensation catalyst-tetramethyl ammonium hydroxide is reduced, consumption of the condensation catalyst is decreased, meanwhile the extraction agent is easy to recycle for cycle use, and the method is convenient and rapid, and economical and effective.

According to the invention, condensation is carried out at a temperature of 60-100 DEG C by using a platinum-loaded macroporous polystyrene strong base resin as a condensation catalyst and using aniline and nitrobenzene as raw materials to prepare 4-(nitroso)nitrodiphenylamine, and hydrogenation reduction is carried out on the obtained condensation liquid so as to prepare p-aminodiphenylamine; andwith the application of the method in preparation of p-aminodiphenylamine, the complex recovery processes such as liquid alkali concentration, desalination and the like are not needed so as to simplify the production process and reduce the energy consumption and the material consumption, tetramethylammonium hydroxide easily decomposed to generate trimethylamine is not adopted so as to achieve environmental protection, the conversion rate of nitrobenzene is greater than or equal to 95%, and the selectivity of 4-(nitroso)nitrodiphenylamine is greater than or equal to 93%.