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Method for improving conversion rate of aniline in synthesis of diphenylamine

A technology for the conversion rate of diphenylamine and aniline, which is applied in the fields of chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of low conversion rate of diphenylamine, achieve the improvement of conversion rate of aniline, increase conversion rate, experimental method simple effect

Active Publication Date: 2017-05-10
CHINA PETROLEUM & CHEM CORP +1
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  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0013] In order to solve the low conversion rate of diphenylamine from aniline in the prior art, the present invention provides a production method that couples the reaction of synthesizing diphenylamine from aniline and synthesizing isopropylamine from isopropanol, which not only improves the efficiency of synthesizing diphenylamine from aniline. The conversion rate of isopropanol is also used to synthesize isopropylamine, which eliminates the ammonia generated by the synthesis of diphenylamine from aniline and reduces environmental pollution.

Method used

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  • Method for improving conversion rate of aniline in synthesis of diphenylamine
  • Method for improving conversion rate of aniline in synthesis of diphenylamine
  • Method for improving conversion rate of aniline in synthesis of diphenylamine

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Embodiment 1

[0029] Catalyst preparation: The catalyst used in the experiment is a catalyst composed of beta zeolite, activated alumina and alkali metal. The specific preparation method is as follows:

[0030] (1) Take 200g Hβ zeolite (SiO 2 / Al 2 o 3 The molecular ratio is 28) and 1500mL (0.1mol / L) potassium chloride aqueous solution, placed in a 2000mL four-neck flask with a stirrer for ion exchange. The exchange reaction temperature is 75°C, the stirring speed is 200n / min, and the time is 5.0h. Afterwards, the above-mentioned exchanged zeolite and potassium aqueous solution are filtered, washed and dried; the washing process is: washing until no chlorine is present. The drying process is as follows: drying at 60° C. for 4.0 hours, and drying at 110° C. for 4.0 hours.

[0031] (2) Mix 70g of the above exchanged zeolite with 10g of aluminum hydroxide powder, add nitric acid and an appropriate amount of deionized water, wherein the amount of nitric acid added accounts for 0.5wt% of th...

Embodiment 2~4

[0033] A fixed bed reactor was adopted, and the catalyst prepared in Example 1 was used, and 200 mL of the catalyst was taken, and loaded into a stainless steel reactor with an inner diameter of 25 mm and a length of 1200 mm. The purity of the reaction raw material aniline is >99%, and the purity of isopropanol is >99%. Using the bottom feeding method, the aniline and isopropanol are fed into the reactor at the same time, and the synthesis reaction is carried out at different reaction temperatures, pressures and feed space velocities. The reaction products flow out from the top of the reactor and enter the separator after cooling. middle. The composition was analyzed by gas chromatography, and the specific reaction conditions and results are shown in Table 1.

[0034] The reaction conditions and the result of table 1. embodiment 2~4

[0035]

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Abstract

The invention discloses a method for improving the conversion rate of aniline in synthesis of diphenylamine. The method comprises the following steps: simultaneously introducing aniline and isopropanol into a reactor according to a ratio of 1: (0.4-0.6), and carrying out a reaction under catalysis of a beta zeolite molecular sieve, wherein the concrete reaction conditions are as follows: the reaction pressure is 1.5 to 6.0 MPa; the reaction temperature is 250 to 300 DEG C; and the volume space velocity of aniline is 0.1 h-1 to 0.5 h-1. According to the invention, through selecting a proper catalyst and optimizing reaction conditions, and on the basis of guaranteeing the reaction of synthesizing diphenylamine from aniline, the reaction of synthesizing isopropylamine from isopropanol can be performed in a certain extent, so two reactions are coupled, and the effects of improving the conversion rate of aniline and eliminating environmental pollution are achieved. Combined production of isopropylamine can be realized on an original device used for synthesizing diphenylamine from aniline, so the economy of the device is increased; and separation of an obtained product can be completed through conventional rectification, and industrial practical values are obtained.

Description

technical field [0001] The invention relates to a method for improving the conversion rate of diphenylamine synthesized from aniline, which belongs to the field of chemical synthesis technology. Background technique [0002] Diphenylamine (diphenylamine; N-phenylaniline), also known as N-phenylaniline, is a chemical raw material with a wide range of uses. In the rubber industry, it is mainly used for rubber anti-aging agents, or raw materials for rubber anti-aging agents, such as the production of anti-aging agents BLE, RT base (4-aminodiphenylamine), sulfide new blue BBF 1 and other raw materials, but also SO 3 And explosive stabilizers, raw materials for synthetic veterinary drugs, fruit preservatives, etc. [0003] At present, with the rapid development of economy after my country's entry into WTO, my country's tire industry has also experienced unprecedented rapid development. At present, more than 20 sets of radial tire production lines have been introduced, and many ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/55C07C209/02C07C211/06C07C209/16B01J29/70
CPCB01J29/7007C07C209/02C07C209/16C07C211/55C07C211/06
Inventor 祁文博艾抚宾徐彤袁毅乔凯
Owner CHINA PETROLEUM & CHEM CORP
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