Method for continuously synthesizing diphenylamine by utilizing phenylamine

A technology of diphenylamine and aniline, which is applied in the field of liquid-phase continuous synthesis of diphenylamine, can solve the problems of catalyst activity cycle (shortening of regeneration cycle, insufficient independence of diphenylamine production equipment, decrease of reaction conversion rate and selectivity, etc., and achieve energy consumption The effect of reduction, scale reduction, and equipment investment reduction

Active Publication Date: 2013-04-17
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

This method has the following disadvantages: (1) The loss of hydrogen is relatively large. One is that there will be a loss of about 30% in the pressure swing adsorption process; The separation process should have a loss of about 10%
(2) Due to the use of large-displacement hydrogen compressors and circulating compressors, the energy consumption is high, which reduces the profit of the product
The method is to use non-hydrogenation reaction. After a period of operation, it is found that although the non-hydrogenation reaction process is relatively simple and the energy consumption is also reduced, the following disadvantages are also brought about by the reaction without hydrogenation: (1) Reaction The conversion rate and selectivity both decreased; (2) The separation difficulty was also increased due to the decrease in selectivity; (3) The activity period (regeneration period) of the catalyst was correspondingly s

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example

[0026] Comparative Example 1 ~ 3

[0027] This experiment is the original liquid phase hydrogen process, the liquid phase non-hydrogen process and the liquid phase 75% hydrogen (hydrogen volume purity) process, the catalyst activity evaluation experiment under these three process conditions.

[0028] The catalyst used in the experiment is a fixed-bed catalyst containing H-beta zeolite (the brand name is FD-20 catalyst developed by Fushun Petrochemical Research Institute), its diameter is Φ2mm strip, and its length is 2-3mm. 25mm, 1200mm long stainless steel reactor. The reaction raw material hydrogen is electrolytically purified hydrogen with a purity of >99%. The specific reaction conditions and results are listed in Table 1.

[0029] Table 1 Catalyst evaluation experiments under three process conditions

[0030] run number DPA-1-1 DPA-1-2 DPA-1-3 Process type Liquid phase hydrogenation process Liquid phase non-hydrogen process The liquid pha...

Example Embodiment

[0035] Example 1

[0036] This experiment is a catalyst evaluation experiment under the conditions of the dissolved hydrogen reaction process of the present invention.

[0037] The catalyst used in the experiment was FD-20, 400 ml of which was taken and put into a stainless steel reactor with an inner diameter of 25 mm and a length of 1200 mm. The reaction raw material hydrogen is electrolytically purified hydrogen, the purity is more than 99%. After the hydrogen and the raw material are fully contacted in the stirring mixer, the excess hydrogen is separated, and the liquid-phase raw material containing dissolved hydrogen enters the reactor for synthesis reaction. The reaction is the lower feed, the reaction material flows out from the top of the reactor, enters the separator after cooling, the gas phase ammonia is discharged from the top of the separator, the bottom liquid phase is sampled regularly, and the composition is analyzed by gas chromatography. The specific reacti...

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Abstract

The invention discloses a method for continuously synthesizing diphenylamine by utilizing phenylamine. Phenylamine raw material contacts with hydrogen before entering into a reactor, the hydrogen is dissolved into the phenylamine raw material, the phenylamine raw material with the dissolved hydrogen enters into a reactor used for continuously synthesizing diphenylamine by virtue of phenylamine, the phenylamine raw material with the dissolved hydrogen passes through a catalyst bed layer, and a diphenylamine synthesizing reaction by virtue of the phenylamine is carried out, wherein the catalyst bed layer contains no gas-phase hydrogen. Compared with the prior art, the method disclosed by the invention has the advantage that the dissolved hydrogen substitutes for massive gas-phase recycled hydrogen while conversion rate of the reaction, selectivity of a target product and service life of a catalyst are guaranteed, so that equipment investment and operation energy consumption are greatly reduced, and reduction of production cost can be facilitated.

Description

technical field [0001] The invention relates to a method for continuously synthesizing diphenylamine in liquid phase with aniline as raw material in the presence of hydrogen and a solid catalyst. Background technique [0002] The traditional production method for synthesizing diphenylamine from aniline is a batch-type liquid-phase catalytic synthesis method. Since aluminum trichloride is used as a catalyst, the production equipment is severely corroded, polluted the environment, the reaction selectivity is low, and the separation of the catalyst and the product is difficult. The production process route Long, the unit consumption of raw materials is high, and the product cost is high. [0003] In order to overcome the shortcoming of above-mentioned synthetic technique, literatures such as US3118944, US4454348 adopt the vapor phase synthesis process of diphenylamine from aniline, use the solid catalyst of activated alumina as the main component, the reaction temperature is mo...

Claims

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Application Information

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IPC IPC(8): C07C211/55C07C209/60
Inventor 艾抚宾乔凯宋丽芝徐彤袁毅黎元生
Owner CHINA PETROLEUM & CHEM CORP
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