One-step synthesis method of toluidine by catalytic distillation of toluene
A catalytic distillation, methylaniline technology, applied in the chemical industry, organic chemistry, amino-substituted hydrogen atom preparation and other directions, can solve the problems of low toluene conversion rate methylaniline yield, low utilization rate, etc., to achieve improved yield, Ease of handling, reduced possible effects of deep oxidation
Inactive Publication Date: 2014-07-23
SICHUAN UNIV
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Problems solved by technology
However, due to the high concentration of hydrogen peroxide in the tank reaction system, its self-decomposition leads to its low utilization rate, and the conversion rate of toluene and the yield of methylaniline are very low (the highest conversion rate of toluene is 1.4%)
Method used
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Embodiment 1
[0013] Example 1: Weigh 3g of TS-1 carriers respectively and place them in five 50mL beakers, add Cu(NO 3 ) 2 ·3H 2 The aqueous solution of 0.1798g, 0.2265g, 0.2831g, 0.3398g, 0.3964g, leave standstill 24h, evaporate to dryness in water bath, dry overnight in 100 DEG C of ovens, transfer to muffle furnace and roast 8h down at 550 DEG C, prepare Get Cu / TS-1 (respectively named 1#, 2#, 3#, 4#, 5#).
Embodiment 2
[0014] Example 2: Weigh 3g of TS-1 carrier and place it in a 50mL beaker, add VOSO 4 ·5H 2 O0.3721g of the aqueous solution was left to stand for 24h, evaporated to dryness in a water bath, dried overnight in a 100°C oven, transferred to a muffle furnace and roasted at 550°C for 8h to obtain a V / TS-1 (6#) catalyst.
Embodiment 3
[0015] Example 3: Weigh 3g of TS-1 carrier and place it in a 50mL beaker, add (CH 3 COO) 2 Ni·4H 2 O0.3165g, let it stand for 24h, evaporated to dryness in a water bath, dried overnight in an oven at 100°C, transferred to a muffle furnace and roasted at 550°C for 8h to obtain a Ni / TS-1 (7#) catalyst.
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Abstract
A one-step synthesis method of toluidine by catalytic distillation of toluene is disclosed, wherein a metal-modified Ti-Si molecular sieve M / TS-1 is taken as a catalyst, ammonia water is taken as an amination agent, hydrogen peroxide is taken as an oxidizing agent, and water is taken as a solvent. Ammonia water and hydrogen peroxide are diluted by water, and pressed into a reaction system by using a feeding pump under protection of an ice-water bath, and toluidine is synthesized by direct oxidation and amination of toluene. In the method, a catalytic distillation device is employed, the characteristic of a larger difference between boiling points of the raw material toluene and the product is utilized, a long time contact of the catalyst and the product in a conventional tank reaction is avoided, deep oxidation of the product is effectively inhibited, and forward movement of the chemical balance is promoted. The method is mild in reaction condition and simple in operation.
Description
technical field [0001] The invention relates to a method for synthesizing methylaniline in one step by catalytic distillation of toluene. Background technique [0002] Methylaniline, the molecular formula is C 7 h 7 NH 2 , There are ortho (o-), inter (m-), right (p-) isomers. Methylaniline is widely used in the fields of industry, agriculture, medicine and health, etc. It is mainly used to synthesize various dyes and drugs, and is an important chemical raw material. There is a huge demand for methylaniline all over the world. The traditional synthesis method of methylaniline is to nitrate toluene in the presence of concentrated nitric acid and concentrated sulfuric acid to obtain the corresponding nitrotoluene, and then reduce the nitrotoluene to obtain the corresponding methylaniline. This method can obtain a higher methylaniline yield, but it needs to be carried out in two steps, the process flow is cumbersome, the cost is high, the equipment is highly corrosive, and ...
Claims
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IPC IPC(8): C07C211/47C07C209/02
CPCY02P20/10
Inventor 胡常伟夏晟李桂英祝良芳
Owner SICHUAN UNIV