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Method for synthesizing aniline by directly oxidizing and aminating benzene by one step

A technology of amine oxide and aniline, applied in the fields of organic chemistry, amino-substituted hydrogen atom preparation, etc., can solve the problems of difficult reproducibility of catalysts, unfriendly environment, uneconomical cost, etc., and achieve the effects of high activity, simple preparation and strong stability

Inactive Publication Date: 2013-11-27
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above reaction conditions are mild, and the raw materials are cheap and easy to get. When 2.5%Ni / TS-1 is used as a catalyst, the yield and selectivity of aniline are high, but the preparation of the catalyst is difficult to repeat, and acetonitrile is used as a solvent, which is not only environmentally friendly Unfriendly and uneconomical in cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022]Example 1: Weigh 91 grams of tetraethyl orthosilicate and place it in a 1000 ml beaker, add 40 grams of isopropanol, 40 grams of water, 160 grams of tetrapropylammonium hydroxide (20% ), stirred for 10 minutes, heated up to 55°C and hydrolyzed for 1 hour, then heated up to 85°C and continued to hydrolyze for 6 hours. At the same time, the water evaporated during the hydrolysis process was compensated by dropwise addition, and the final volume of the solution was kept at about 300 ml. , after hydrolysis, put it at 25°C for 12 hours, adjust the pH value to 9 with hydrochloric acid, transfer it to a 500ml high-pressure reactor, add 1 atmosphere of nitrogen, crystallize at 175°C for 7 days, cool, and filter , washed with ultra-pure water until neutral, dried in an oven at 100°C for 12 hours, and finally transferred to a crucible, placed in a muffle furnace for temperature-programmed roasting (the first step, 20-100°C for 16 minutes; the second step , 100°C for 1 hour; the th...

Embodiment 2

[0023] Embodiment 2: Weigh 3 grams of sodium hydroxide and dissolve it in 270 milliliters of water, add 9 grams of cetyltrimethylammonium bromide, after fully dissolving, add 52 grams of ethyl orthosilicate dropwise, and use sodium hydroxide solution Adjust the pH to 11, stir at 25°C for 2 hours, transfer to a 500ml autoclave, add 1 atmosphere of nitrogen, crystallize at 110°C for 5 days, cool, filter, wash with ultrapure water until neutral, and place Dry in an oven at 100°C for 12 hours, and finally transfer to a crucible, place in a muffle furnace for temperature-programmed calcination (the calcination procedure is the same as in Example 1), and obtain silica with a mesoporous structure.

Embodiment 3

[0024] Example 3: Weigh 5 grams of microporous, mesoporous and macroporous silica samples respectively and place them in 3 branched test tubes, vacuumize to 2.7-5.3 kPa at 25°C and keep for 0.5 hours. At the same time, take 3 0.47 g Cu(NO 3 ) 2 ·3H 2 O was respectively dissolved in distilled water equal in volume to 3 parts of silicon dioxide, and the above-mentioned silicon dioxide was impregnated with 3 parts of solutions respectively. After the impregnated sample was placed at 25°C for 24 hours, the water was removed in a vacuum oven at 60°C, dried in an oven at 100°C for 12 hours, and finally transferred to a crucible, placed in a muffle furnace for temperature-programmed roasting ( Roasting procedure is the same as embodiment 1), finally obtains the CuO / SiO that copper loading mass percent is 2.5% 2 Catalysts are marked as 1#, 2# and 3# respectively.

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Abstract

The invention provides a method for synthesizing aniline by directly oxidizing and aminating benzene by one step. The method is characterized by taking benzene as a raw material, ammonia water as an aminating agent, hydrogen peroxide as an oxidizing agent, water as a solvent and CuO / SiO2 which is obtained after silicon dioxide with microporous, mesoporous and macroporous structures is modified with metallic copper as a catalyst. The method has the characteristics that the yield of aniline is higher; the reaction conditions are mild; the catalyst preparation process is simple; the raw material is cheap and accessible; and therefore, the method is environment-friendly and has the advantages of low cost, high yield, simplicity and practicability.

Description

technical field [0001] The invention relates to a method for synthesizing aniline in one step by direct oxidative amination of benzene. Background technique [0002] Aniline, the molecular formula is C 6 h 5 NH 2 , Colorless oily liquid, boiling point 184 ° C. Aniline is widely used in industrial fields such as polyurethane, rubber additives, pigments, dyes, pesticides, medicine and special fibers. It is an important organic chemical raw material and an intermediate of fine chemicals. [0003] The existing production method of aniline is to convert benzene into derivatives of benzene such as nitrobenzene, halogenated benzene and phenol, and then reduce the derivatives of benzene to amino groups or replace them with amino groups. These methods involve multi-step reactions, harsh operating conditions, many by-products, low atom utilization, are not environmentally friendly, and do not meet the needs of sustainable green chemical industry development and low-carbon economy....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/46C07C209/02
Inventor 胡常伟余天华李桂英
Owner SICHUAN UNIV
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