Process for preparing 4-amino diphenylamine

A technology of aminodiphenylamine and aniline, which is applied to the preparation of amino compounds from amines, the preparation of amino compounds through condensation/addition reactions, and chemical recovery. It can solve the problems of difficult operation, prolonged reaction time, and increased production costs. Reduce the difficulty of manipulation, reduce the amount of aniline, and avoid the effect of loss

Active Publication Date: 2006-01-18
JIANGSU SINORGCHEM TECH CO LTD
View PDF3 Cites 16 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are some common disadvantages in these methods: one is that the selected catalyst is expensive, and the application to industrial scale production will cause the production cost to be too high, and there is no advantage compared with the current production process
In this patent, it is necessary to have a solvent and control the content of the proton material in the solution. The introduction of the solvent brings increased energy consumption and difficulty in separation. Controlling the proton material brings difficulty to the...

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Process for preparing 4-amino diphenylamine
  • Process for preparing 4-amino diphenylamine
  • Process for preparing 4-amino diphenylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] Preparation of composite base catalyst:

[0076] In a 1000 ml three-necked flask equipped with a condenser and a stirrer, add 227.5 grams of 20% (by weight) tetramethylammonium hydroxide aqueous solution (0.50 moles), 10 grams of sodium hydroxide (0.25 moles), 346 grams of 30% tetramethylammonium carbonate aqueous solution (0.5 mol), stirred evenly at 72-77 ℃, promptly made composite base catalyst, concentration 27.3% (weight).

Embodiment 2

[0078] Preparation of composite powder catalyst:

[0079]Take 46 grams of nickel powder, 51 grams of aluminum powder, and 3 grams of iron powder, mix them evenly, and melt them into an alloy in an induction furnace. The molten alloy is sprayed on the high-speed rotating copper drum through the nozzle by the pressure of the gas, and it is rapidly quenched. (The cooling rate can reach 10 5 -10 6 K / S). The cooled alloy is rolled into powder by a ball mill, and sieved to obtain 99.7 grams of 40-300 mesh powder. In a three-necked flask equipped with a thermometer and a stirrer with a capacity of 500 milliliters, 375 grams of a concentration of 20% (weight) of NaOH aqueous solution was added slowly, and the powder prepared above was slowly added, stirred at 60° C. for 4 hours, and then The solid was washed with deionized water until neutral to obtain a composite powder catalyst.

Embodiment 3

[0081] Open the composite base catalyst, aniline and nitrobenzene transfer pump simultaneously under vacuum, adjust the flow rate to 150 kg / hour of aniline, 30 kg / hour of nitrobenzene, and 200 kg / hour of composite base catalyst, the above components Nitrobenzene, aniline and composite base catalysts are continuously fed into the falling film reactor for heating to carry out condensation reaction; the condensation liquid in the falling film reactor is discharged from the lower part into the primary reactor to continue the condensation reaction; part one The condensate at the bottom of the first-stage reactor is returned to the falling film reactor through the circulation pump to form a partial circulation system. The heat medium of the falling film reactor is alcohol vapor at 78-90°C. Control the reaction temperature to 75°C, the pressure to 0.008MPa (absolute pressure), and the flow rate of the circulating fluid to be 1 meter 3 / Hour. The material from the primary reactor ov...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The present invention discloses production process of 4-amino diphenylamine with nitrobenzene and phenylamine as materials. The production process includes five steps of condensation; hydrogenation; separating, recovering and reusing composite alkali catalyst, and separating, recovering and reusing at least partial regenerated composite powdered catalyst; separating, recovering and reusing phenylamine and hydrogenation solvent; and refining. For the condensation and hydrogenation, composite alkali catalyst and composite powdered catalyst are adopted separately. The production process has mild reaction condition and less side products, may be completed continuously, and is suitable for industrial production. The production process has 4-amino diphenylamine yield industrial scale over 95 % and 4-amino diphenylamine purity over 99 wt%.

Description

technical field [0001] The invention relates to a method for preparing 4-aminodiphenylamine, in particular to a method for continuously preparing 4-aminodiphenylamine by using nitrobenzene and aniline as raw materials, using two composite catalysts and a cyclic operation process flow. Background technique [0002] 4-Aminodiphenylamine is an important antioxidant and stabilizer intermediate, and an important chemical product in the rubber industry and polymer industry. According to the different raw materials used, the current methods of producing 4-aminodiphenylamine are: (1) the aniline method, using p-nitrochlorobenzene and aniline as raw materials, reacting under the action of a catalyst to generate 4-nitrodiphenylamine, and then using vulcanization Alkali reduction to 4-aminodiphenylamine; (2) formanilide method, using formic acid and aniline as raw materials to prepare formanilide, and then reacting with p-nitrochlorobenzene in the presence of an acid-binding agent (suc...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07C211/55C07C209/60C07C209/68
CPCY02P20/584
Inventor 冯晓根王农跃茅晓晖余瑞标程千文
Owner JIANGSU SINORGCHEM TECH CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap