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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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The process conditions are mild and the raw materials are cheap, but the yield is not ideal, and the cataly

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
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Effect test

Example Embodiment

[0018] Example 1 Weigh 0.1143g NiSO respectively 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 heated and stirred in 2 mL of deionized water until all was dissolved, and set aside. Weigh 5 parts of 1g TS-1 powder and place them in 5 test tubes respectively, and vacuumize at 25℃ for 0.5 hours, the vacuum degree is 0.9×10 2 KPa, while maintaining the vacuum, respectively pour the prepared 5 parts of the metal salt solution into the carrier in the 5 test tubes while it is hot, and let stand for 24 hours; move the test tube into the drying box, Dry it at a temperature of ℃ to completely dry, transfer the dried catalyst into a crucible, and calcinate at 500℃ for 4 hours. The catalysts are labeled as Ni / TS-1, Cu / TS-1, Ce / TS-1, V / TS-1, Ti / TS-1, and the metal loading percentages of the above 5 catalysts are all 2.5%. Store them dry for later use .

Example Embodiment

[0019] Example 2 Weigh 0.2286g, 0.3429g, 0.4572g NiSO respectively 4 According to the method of Example 1, a Ni / TS-1 catalyst was prepared, in which the mass percentages of nickel loading were 5.0%, 7.5%, and 10.0% respectively.

Example Embodiment

[0020] Example 3 Weigh TS-1, Ni / TS-1, V / TS-1, Cu / TS-1, Ce / TS-1, Ti / TS-1 (the metal loading percentages are all 2.5%) 0.3g in six 50mL two-necked flasks, add 5mL benzene and 10mL 25% ammonia water, stir and heat to 70℃, add 2mL30%H 2 O 2 , Then add 2mL 30% H every 24 minutes 2 O 2 , Add a total of 10mL 30% H 2 O 2 , The reaction time is 2 hours, and the effects of different metal-supported catalysts on the yield of aniline and the selectivity of aniline are obtained. The results are shown in Table 1.

[0021] Table 1 The influence of different metal supported 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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