Method for preparing tert-butylamine by taking MTBE as raw material

A technology of tert-butylamine and raw materials, applied in the field of preparation of tert-butylamine, which can solve problems such as environmental pollution, harsh reaction conditions, and strong corrosiveness of catalysts

Active Publication Date: 2020-10-27
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, MTBE and HCN are used as raw materials to prepare tert-butylamine in the method that the catalyst is highly corrosive, pollutes the environment, the reaction conditions are harsh, and the conversion rate of MTBE is relatively low problem, the invention provides a method for preparing tert-butylamine

Method used

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  • Method for preparing tert-butylamine by taking MTBE as raw material
  • Method for preparing tert-butylamine by taking MTBE as raw material

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preparation example Construction

[0035] The preparation process of solid superacid catalyst: one, 50~100g ZrOCl2 Dissolved in ethanol to obtain ZrOCl with a mass concentration of 30% to 50% 2 Ethanol solution, titrated with 20% to 25% ammonia water until no white precipitate, washed several times with deionized water, 5 to 10 minutes each time, at a washing temperature of 40 to 50 ° C, until there was no chloride ion, and then washed at 80 Place it in a vacuum drying oven at ~90°C for 4-6 hours, extrude it, and then bake it at 500°C for 8 hours to obtain white solid particles for use. 2. Impregnate the white particles obtained in Step 1 with a silver nitrate sulfuric acid solution with a concentration of 2-4mol / L, the impregnation temperature is 55-60°C, and the impregnation time is 4-6h; the decompression vacuum degree is 15000-20000Pa; the ultrasonic vibration frequency is 50 ~60kHz, then dry the solid particles in a vacuum drying oven at 80-90°C for 4-6 hours, and then bake at 500°C for 8 hours to obtain P...

Embodiment 1

[0039] (1) Preparation of solid superacid catalyst: a: 50 grams of ZrOCl 2 Dissolved in ethanol to obtain a mass concentration of 30% ZrOCl 2 Ethanol solution, titrated with 20% ammonia water until there is no white precipitate, washed 5 times with deionized water, 10 minutes each time, washing temperature is 40 ° C, washed to no chloride ion, and then placed in vacuum drying at 90 ° C Dry in an oven for 6 hours, extrude and then bake at 500°C for 8 hours to obtain white solid particles for use. b: impregnate the white particles obtained in step a with a silver nitrate sulfuric acid solution with a concentration of 2mol / L, the impregnation temperature is 55°C, and the impregnation time is 6h; the decompression vacuum degree is 16000Pa; the ultrasonic vibration frequency is 56kHz, and then the solid particles are placed at 90°C Dry it in a vacuum oven for 6 hours under the condition of 500°C for 8 hours to obtain the particle I. c: Repeat the impregnation process of step b wi...

Embodiment 2

[0042] (1) Preparation of solid superacid catalyst: a: 50 grams of ZrOCl 2 Dissolved in ethanol to obtain a mass concentration of 30% ZrOCl 2 Ethanol solution, titrated with 20% ammonia water until there is no white precipitate, washed 5 times with deionized water, 10 minutes each time, washing temperature is 40 ° C, washed to no chloride ion, and then placed in vacuum drying at 90 ° C Dry in an oven for 6 hours, extrude and then bake at 500°C for 8 hours to obtain white solid particles for use. b: impregnate the white particles obtained in step a with a silver nitrate sulfuric acid solution with a concentration of 2mol / L, the impregnation temperature is 55°C, and the impregnation time is 6h; the decompression vacuum degree is 17000Pa; the ultrasonic vibration frequency is 57kHz, and then the solid particles are heated at 90°C Dry it in a vacuum oven for 6 hours under the condition of 500°C for 8 hours to obtain the particle I. c: Repeat the impregnation process of step b wi...

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Abstract

The invention discloses a method for preparing tert-butylamine by taking MTBE as a raw material. A Tubular reactor is used, and the MTBE and HCN are used as a feeding material I and enter from the topof the reactor; the MTBE is used as a feeding material II and enters from the bottom of the reactor; a plurality of catalyst bed layers which are arranged in a staggered manner are arranged in the reactor from top to bottom; the catalyst bed layers comprise bed plates and catalysts distributed on the bed plates, one end of each bed plate is hermetically connected with the reactor wall, the otherend of each bed plate horizontally extends to the reactor wall on the opposite side and keeps a certain distance with the reactor wall, vertical baffles are arranged at the tail ends of the bed plates, and two vertically adjacent bed plates are connected to the reactor walls on different sides; a plurality of open holes are formed in the bed plates, the feeding material I penetrates through the catalyst bed layers from top to bottom and reacts, and the feeding material II is in reverse contact with the feeding material I from bottom to top and further reacts with unreacted HCN in the feeding material I. According to the reactor and the feeding mode, the reaction process has the advantages of a trickle bed and catalytic rectification at the same time, and the reaction conversion rate is increased.

Description

technical field [0001] The invention relates to a method for preparing tert-butylamine, especially a method for preparing tert-butylamine by using MTBE (methyl tert-butyl ether) and HCN (hydrocyanic acid) as raw materials. Background technique [0002] Tert-Butylamine is a colorless, flammable liquid, miscible with water and ethanol. It is mainly used as an intermediate in organic synthesis such as rubber additives, insecticides, fungicides, dyes, and medicines. In recent years, with the enhancement of global environmental protection awareness and the improvement of environmental protection requirements in various countries, many green and environmentally friendly chemical product production technologies and production processes have emerged, and the subsequent product technology development and application of tert-butylamine have also been further developed. Such as the synthesis of Folipine, the synthesis of desulfurization and decarburization agent hindered amine and Ⅳ-t...

Claims

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Application Information

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IPC IPC(8): C07C211/03C07C209/00B01J23/89B01J37/02B01J8/04
CPCC07C209/00B01J23/892B01J37/0205B01J8/0446B01J8/0492B01J2208/00902C07C211/03Y02P20/10
Inventor 刘野赵亮王岩于庆志党雷
Owner CHINA PETROLEUM & CHEM CORP
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