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Method for directly synthesizing aniline from benzene and ammonia by one step

A benzene one-step, direct technology, applied in chemical instruments and methods, preparation of amino-substituted hydrogen atoms, molecular sieve catalysts, etc., can solve the problems of complex catalyst preparation process, unsatisfactory yield and other problems, and achieve short catalytic reaction time, low price, high yield effect

Inactive Publication Date: 2010-12-08
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process conditions are mild and the raw materials are cheap, but the yield is not ideal, and the catalyst preparation process is complicated, and the catalyst needs to be reduced by hydrogen before the reaction

Method used

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  • Method for directly synthesizing aniline from benzene and ammonia by one step
  • Method for directly synthesizing aniline from benzene and ammonia by one step
  • Method for directly synthesizing aniline from benzene and ammonia by one step

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1 weighs 0.1143g NiSO 4 , 0.1007g CuSO 4 ·5H 2 O, 0.0795g CeN 5 o 9 ·6H 2 O, 0.1004g VOSO 4 ·nH 2 O, 0.5127g TiCl 3 ·nH 2 O (35%) was dissolved in 2 mL of deionized water, heated and stirred until completely dissolved, and set aside. Weigh 5 parts of 1g TS-1 powder and place them in 5 branch test tubes respectively, and vacuumize at 25°C for 0.5 hours, the vacuum degree is 0.9×10 2 KPa, while maintaining the vacuum, pour 5 parts of metal salt solutions that have been prepared into the carriers in 5 branched test tubes while hot, and leave to age for 24 hours; °C until completely dry, then move the dried catalyst into a crucible and bake at 500 °C for 4 hours. Catalysts are marked as Ni / TS-1, Cu / TS-1, Ce / TS-1, V / TS-1, Ti / TS-1, and the weight percentage of the metal loading of the above five catalysts is 2.5%, and they are stored dry for later use .

Embodiment 2

[0019] Embodiment 2 weighed 0.2286g, 0.3429g, 0.4572g NiSO 4 According to the method of Example 1, Ni / TS-1 catalysts were prepared, wherein the nickel loading mass percentages were 5.0%, 7.5%, and 10.0%, respectively.

Embodiment 3

[0020] Example 3 Weigh TS-1, Ni / TS-1, V / TS-1, Cu / TS-1, Ce / TS-1, Ti / TS-1 respectively (wherein the metal loading mass percent is 2.5%) 0.3g into six 50mL two-necked bottles, add 5mL of benzene and 10mL of 25% ammonia water, stir and heat to 70°C, add 2mL of 30% H 2 o 2 , after which 2 mL of 30% H was added every 24 min 2 o 2 , adding a total of 10 mL of 30% H 2 o 2 , the reaction time was 2 hours, and the effects of different metal-loaded catalysts on the aniline yield and aniline selectivity were obtained. The results are shown in Table 1.

[0021] Table 1 Effect of different metal-loaded catalysts on the yield and selectivity of aniline

[0022]

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Abstract

The invention discloses a method for directly synthesizing aniline from benzene and ammonia by one step, which takes benzene as a raw material, ammonia as an aminating agent, hydrogen peroxide as an oxidizer, acetonitrile as a solvent and TS-1 loaded by metal as a catalyst. The method for synthesizing aniline by one step has the characteristics of high yield of aniline, mild reaction condition, simple catalyst preparing process and easily obtained cheap raw materials, thus being a green synthesis method which has low cost and high yield and is simple and practicable.

Description

technical field [0001] The invention relates to a method for directly synthesizing aniline from benzene and ammonia water. Background technique [0002] Aniline is an important organic chemical raw material and fine chemical intermediate, widely used in industrial fields such as polyurethane, rubber additives, dyes, pigments, pesticides, medicines, and special fibers. [0003] The existing aniline production route is obtained by subjecting nitrobenzene to catalytic hydrogenation or reduction under other conditions, or replacing it with phenol, halogenated benzene and amino group. These methods have disadvantages such as harsh operating conditions (high temperature and high pressure), poor atom economy, etc., and cause environmental hazards to a certain extent, so they do not meet the needs of sustainable green chemical industry development and low-carbon economy. The new method is used to directly introduce the amino group into the benzene ring, realize the synthesis of ani...

Claims

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Application Information

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IPC IPC(8): C07C211/46C07C209/02B01J29/89
Inventor 胡常伟郭滨张倩祝良芳李桂英
Owner SICHUAN UNIV
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