75 results about "4-aminodiphenylamine" patented technology

This invention relates to a process for preparing 4-nitrodiphenylamine and 4-nitrosodiphenylamine to be used for 4-aminodiphenylamine as an intermediate of antiozonant, wherein carbanilide is reacted with nitrobenzene in the presence of an appropriate base, while simultaneously adding aniline to the mixture so as to regenerate some amounts of carbanilide as a starting material. According to this invention, 4-nitrodiphenylamine and 4-nitrosodiphenylamine can be prepared in a higher selectivity and conversion rate via a continuous reaction by recycling carbanilide, a starting material, while adding a certain amount of aniline during the process. Further, the amount of waste water can be significantly reduced compared to the conventional method without any corrosive materials harmful to the environment.

A curing agent for epoxy agent having N-phenyl-p-phenylenediamine(4-aminodiphenylamine). An epoxy resin combination having a main agent and a curing agent. The main agent has an epoxy resin. The curing agent has a N-phenyl-p-phenylenediamine(4-aminodiphenylamine).

The present invention discloses a method for preparing 4-aminodiphenylamine by continuously hydronating condensate obtained from the reaction by using nitrobenzol and phenylamine as raw material and adopting compound powdered catalyst. i,e, adopts a catalyst and hydrogen gas circulation and solvent circulation combined new process to make the hydrogenation reaction be implemented under the condition of high-concentration, low-temp. and low pressure. The invented catalytic hydrogenation conversion rate can be up to 100%, and its selectivity is greater than 99%, and it is suitable for industrial production of 4-aminophenylamine.

A process for preparing 4-aminodiphenylamine using nitrobenzene and aniline as raw materials, a complex base catalyst as the condensation catalyst, and a powdery composite catalyst as the hydrogenation catalyst. The process has 5 process stages including condensation, hydrogenation, separation I, separation II, and refining.

The invention belongs to the technical field of catalysts, and discloses a modified condensation reduction alkylation catalyst used in preparation of a rubber anti-aging agent 4020 by undergoing a hydrogenated reduction alkylation reaction on 4-aminodiphenylamine and methyl isobutyl ketone and preparation of a rubber anti-aging agent 4010NA by undergoing a hydrogenated reduction alkylation reaction on 4-aminodiphenylamine and acetone. The catalyst is a copper-series catalyst, and is mainly characterized in that: the catalyst contains a silicon element; and the molar ratio of copper to silicon is (0.5-10):1. Due to the adoption of the catalyst, a side reaction of ketone hydrogenation for generating an alcohol in the reacting process is suppressed remarkably, raw materials are saved, products 4010NA and 4020 are not required to be passivated by using 4-amino diphenylamine produced by reducing alkali sulfide at an earlier using stage, and unqualified products are avoided; and the catalyst has high intensity and long service life, and is not pulverized easily in the using process.

The invention discloses a preparation method for tetra-alkyl ammonium hydroxide. The preparation method is implemented by the following technical scheme: performing a reaction on trialkylamine and alkyl halide in a single organic solvent to obtain tetra-alkyl ammonium halide; performing ion exchange on the tetra-alkyl ammonium halide and an oxide or a hydroxide of an alkali metal or an alkaline earth metal in the presence of an organic solvent; and obtaining the aqueous solution of the tetra-alkyl ammonium hydroxide by after-treatment. The method has the advantages of convenient raw material source, low cost, simple preparation process, high halide ion-exchange rate and the like. The tetra-alkyl ammonium hydroxide prepared by adopting the method is particularly suitable to be used as a base catalyst, which is used for the condensation of nitrobenzene and aniline for generating 4-nitrodiphenylamine and/or 4-nitrosodiphenylamine and the reduction for generating 4-aminodiphenylamine by hydrogenating. Therefore, the conversion rate of the nitrobenzene is greater than or equal to 99.5 percent and the selectivity is up to over 92 percent.

This invention provides a method for improving the yield of 4-aminodiphenylamine, comprising: use nitrobenzene and phenylamine as raw material to conduct condensation and hydrogenation reactions, where the nitrobenzene is added in to start the condensation reaction when the mole ratio of water and alkaline in the catalyst is 4-6:1, and stop the reaction when the mass percentage of the alcohol compounds in the reaction solution becomes less than 0.3%. This invention is characterized in that it can precisely control the water content by detecting the alcohol compounds during the condensation reaction, so as to efficiently prevent the decomposition of condensing catalyst, obtain a high production yield, and accomplish the repeated use of the catalyst.

The present invention discloses a process for preparing 4-aminodiphenylamine, which process uses nitrobenzene and aniline as raw materials, a complex base catalyst as condensation catalyst and a powdery composite catalyst as hydrogenation catalyst, and comprises five process stages: condensation; separation I; hydrogenation; separation II; and refining. The process can be continuously carried out. By selecting a complex base catalyst to catalyze the condensation reaction and separating it prior to the hydrogenation, the problem that the complex base catalysts thermally decompose in the hydrogenation reaction is avoided, the selectable range of hydrogenation catalysts is largely enlarged so that it is possible to select cheaper hydrogenation catalyst, and the selection of production process and equipment is easier and further industrialization is easier. The complex base catalysts used in the present invention are inexpensive and have higher catalytic activity. The process can be carried out at mild conditions and can adapt to broad range of water content, by-product is less and conversion and selectivity are higher. The operational strength is low, no corrosive liquid is produced, and environment pollution is reduced. The purity of 4-aminodiphenylamine prepared can exceed 99 wt.-%, and the yield in the industrial production process can be over 95%.

The invention discloses a production method of 4-aminodiphenylamine, which comprises the following steps of: (1) mixing phenylamine and alkaline water solution, distilling out phenylamine-water azeotrope; (2) adding nitrobenzene for reaction; (3) adding water, Ni-B amorphous alloy catalyst, and filling hydrogen; (4) carrying out solid-liquid separation, separating out Ni-B amorphous alloy catalyst and liquid phase, and returning the Ni-B amorphous alloy catalyst back into the step (3); separating the liquid phase to obtain organic phase and alkaline water solution, carrying out rectification on the organic phase to obtain the product 4-aminodiphenylamine, recovering phenylamine, and returning the phenylamine back into the step (1); and (5) returning the alkaline water solution which is separated out back into the step (1), or treating the alkaline water solution by activated carbon and then returning back in the step (1). The method is simple, improves the purity of circulating alkaline water solution, avoids using expensive electrolytic process, shortens the process flow, is low in equipment investment, has simple operation, and can remarkably reduce the operation cost.

A solid base catalyst having a carrier, an organic base, and an inorganic base. Both of the organic base and inorganic base are loaded on the carrier. The solid base catalyst is especially suitable for the synthesis of 4-Aminodiphenylamine (4-ADPA).

The invention provides a non-mobility graphene oxide grafted anti-aging agent and preparation method thereof. 4-aminodiphenylamine is used for carrying out grafting modification on graphene oxide by so as to enable a hydroxyl group in the carboxyl group of graphene oxide to be replaced with an R group, wherein the structural formula of the R group is described in the description; the grafting rateof the R group is 7-15wt%. The preparation method comprises the following steps: (1) dissolving graphene oxide into thionyl chloride, carrying out a refluxing reaction, separating out a reaction product, and washing to remove thionyl chloride so as to obtain thionyl chloride modified graphene oxide; (2) adding the thionyl chloride modified graphene oxide into dimethylformamide, carrying out ultrasonic treatment to enable the thionyl chloride modified graphene oxide to be fully dissolved, and dissolving 4-aminodiphenylamine into dimethylformamide; then, mixing the thionyl chloride modified graphene oxide solution with the 4-aminodiphenylamine solution, carrying out a refluxing reaction and solid-liquid separation, and fully soaking the obtained solid phase in absolute ethanol, separating out the soaked solid product, and drying to obtain the non-mobility graphene oxide grafted anti-aging agent.

The invention belongs to the technical field of rubber framework oil-sealing production, and relates to an environmentally friendly anti-high and low temperature rubber oil-sealing material and a preparation method thereof. The preparation method comprises the following steps: 1) weighing the following raw materials in parts by mass: nitrile rubber, carbon fiber powder, zinc oxide, iron oxide, cerium oxide, stearic acid, sulphur, carbon black, dibutyl phthalate, dicapryl phthalate, oxidized polyethylene, a carbon black dispersant, 4-aminodiphenylamine, 2,2-disulfbenzothiazole, tetraethylthiuram disulfide, tellurium diethyl dithiocarbamate, a silane coupling agent, and a mold lubricant, placing the raw materials in an open mill and uniformly mixing the raw materials, blanking and placing a mixture overnight; 2) placing an overnight rubber compound in the open mill and re-milling the material, and obtaining the sheets; 3) after the rubber compound is preformed, placing the preformed rubber compound and a metal framework coated with an adhesive at an edge part in a sulfuration die together for sulfuration; and 4) performing steps of trimming, examination, packaging and warehousing. The environmentally friendly anti-high and low temperature rubber oil-sealing material belongs to environment friendly-type sealing, and has excellent oil resistant performance and high/low temperature-resistant performance.

A method for refining an organic composition containing 4-aminodiphenylamine, aniline, azobenzene, and phenazine, having the steps of feeding the organic composition to a first rectification column, producing a first effluent composition containing aniline, azobenzene, phenazine, and a small amount of 4-aminodiphenylamine at the top of the first rectification column and a second effluent composition containing crude 4-aminodiphenylamine at the bottom of the first rectification column, feeding the second effluent composition to a second rectification column, and producing a 4-aminodiphenylamine composition at the top of the second rectification column and a residual composition at the bottom of the second rectification column.

The invention relates to a dye suitable for nylon dyeing, which is a compound shown by the following formula (I). The preparation method comprises the following steps: a. adding a para-beta-hydroxyethyl sulfonyl aniline solution into a cyanuric chloride solution to react to obtain a primary condensation solution, and adding J acid into the primary condensation solution to obtain a secondary condensation solution; b. adding a hydrochloric acid solution and a sodium nitrite solution into 4-aminodiphenylamine-2-sulfoacid to react under the condition that the PH is less than 2, and eliminating excessive nitrous acid by utilizing sulfamic acid to obtain a heavy nitrogen solution; c. dropwisely adding the heavy nitrogen solution obtained in step b into the secondary condensation solution obtained in step a to obtain a coupling reaction solution; d. heating the coupling reaction solution obtained in step c, and hydrolyzing under the condition that the pH is equal to 8-11; e. filtering the hydrolyzed reaction solution obtained in step d to remove waste residue, and collecting the filter liquor; f. regulating the colored light and intensity of the filter liquor in step e; and g. carrying out spray drying on the color solution in step f to obtain the final product in the formula (I).

The invention relates to a catalyst for preparing 4-aminodiphenylamine and a preparation method of the catalyst, and specifically provides a preparation method of a palladium/carbon catalyst for preparing the 4-aminodiphenylamine through hydrogenation. The catalyst is characterized in that activated carbon is used as a carrier, palladium is used as an active component, and a preparation process comprises the steps of pretreating the activated carbon, performing impregnation, performing reduction, performing washing, performing drying and the like. The prepared catalyst is used for a catalytic hydrogenation process of preparing the 4-aminodiphenylamine by a nitrobenzene method. Raw materials for preparing the catalyst disclosed by the invention are easy to obtain, the technology is simple, and the catalyst is used for preparing the 4-aminodiphenylamine through the hydrogenation, is high in activity and good in stability, and has good application prospects.

The present invention relates to a method for refining 4-aminodiphenylamine by adopting three-column continuous rectification and intermittent distillation. The crude product of 4-aminodiphenylamine can be obtained by rectification in the column No.1, and the substances of phenylamine, phenazine and azobenzene can be obtained at the top of column, said crude product can be purified in column No.2, in the column No.3 the phenylamine is separated, and the intermittent column can be used for making batch distillation of 4-aminophenylamine made up by using column bottoms of column No.2 and returning it into column No.2 for refining it. The yield rate of its whole process can be raised to 99% from 94%, and the content of 4-aminodiphenylamine in the finished product is greater than 99 wt%, at the same time the phenylamine can be recovered, and can be used.

The invention discloses a method for extracting high-purity phenazine from an RT base byproduct waste material, belonging to the technical field of refining of the phenazine. The technical problem to be solved is to provide a method for extracting the phenazine from the RT base byproduct waste material, wherein the product is high in purity and bright in color and gloss, the amount of used solvents is small and the recycle rate of the solvents is high. The method comprises the following steps: separation by heating, extraction, primary crystallization, secondary decoloration and crystallization, drying, primary distillation and crystallization and secondary solvent distillation, wherein due to the step of the separation by heating, the amount of the used solvents in the extraction step and the crystallization step is reduced, and an active carbon decoloration step is added, so the product purity is stable and not lower than 99.8% and the product is also brighter in color and gloss and totally meets the requirements of all markets including a pharmaceutical-grade market; due to the addition of the secondary distillation, the recycle rate of the solvents is as high as 99.5%, the consumption of purifying solvents is reduced, and the amount of the solvents introduced to an RT production system causes no burthen to an existing RT production system.

The invention relates to a preparation method of a rubber antioxidant, in particular to a rubber antioxidant 4030. The preparation method comprises the steps of mixing, synthesizing, separating and purifying. According to the preparation method, the rubber antioxidant 4030 is produced by adopting p-phenylenediamine as a raw material instead of a process route with scarce 4-aminodiphenylamine as the raw material, the material supply bottleneck is solved, and mass production of the rubber antioxidant 4030 can be realized.

The invention relates to a production technology of a precursor of 4-aminodiphenylamine. The technology comprises the following steps: respectively processing and degassing nitrobenzene and phenylamine through an alkali metal oxide or a hydroxide; continuously feeding the processed phenylamine and concentrated quaternary ammonium alkali catalyst to a tubular condensation reactor by flow measurement according to a certain ratio after concentrating the quaternary ammonium alkali catalyst in vacuum; firstly, reacting the phenylamine to form aniline anions; continuously adding the processed nitrobenzene at different positions of the tubular condensation reactor from a plurality of points and controlling the water yield, so that the anions generate 4-nitrosodiphenylamine and 4-nitrodiphenylamine condensed liquid by replacing hydrogen reaction on nitrobenzene by nucleophilic addition. The technology disclosed by the invention is reasonable in steps and composition and advanced in equipment, and is used raw material enters a continuous production device of a high-efficiency reactor pipeline after being pretreated under a totally-enclosed condition, so as to produce the 4-nitrosodiphenylamine and the 4-nitrodiphenylamine.