Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Process for preparing tert-butylamine in dynamic equilibrium of raw materials

A technology of dynamic balance and tert-butylamine, which is applied in the preparation of amino compounds, organic compounds, chemical instruments and methods, etc. It can solve the problems of enhanced alkalinity, harsh requirements for reaction devices, and large pressure fluctuations, and achieve stable performance and low price. , the effect of short reaction time

Active Publication Date: 2018-10-02
ZHEJIANG JIANYE CHEM +1
View PDF12 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the critical or supercritical conditions are reached, the pressure fluctuates greatly, and NH 3 The alkalinity is greatly strengthened, and the requirements for the reaction device will be very harsh

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Process for preparing tert-butylamine in dynamic equilibrium of raw materials
  • Process for preparing tert-butylamine in dynamic equilibrium of raw materials
  • Process for preparing tert-butylamine in dynamic equilibrium of raw materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1 (using non-molecular sieve type aluminosilicate catalyst)

[0043] Prepare tert-butylamine according to the following method, comprising the following steps:

[0044] (1) Put 29.2990g tert-butanol, liquid ammonia, self-made non-molecular sieve type aluminosilicate catalyst (prepared by the method described in CN106732496A) and isobutylene into the reactor, at a reaction temperature of 275°C and a reaction pressure of 23MPa Reaction 2h; Wherein, the feed molar ratio of tert-butanol and ammonia is 1:3.0, the mass ratio of tert-butanol and catalyst is 5.9:1, and the feed molar ratio of tert-butanol and isobutylene is 1:1.5;

[0045] (2) After the reaction is finished, cool down to room temperature, collect liquid phase substances, and measure and obtain various reaction performance parameters according to the above method.

[0046] In this reaction, the yield of t-butylamine was 2.58%.

Embodiment 2

[0047] Embodiment 2 (using molecular sieve type aluminosilicate catalyst, without isobutylene circulation)

[0048] Prepare tert-butylamine according to the following method, comprising the following steps:

[0049] (1) 39.4940g tert-butanol, liquid ammonia and ZSM-5 molecular sieve powder are put into the reactor, and react for 2h at a reaction temperature of 275°C and a reaction pressure of 23MPa; wherein, the feed molar ratio of tert-butanol and liquid ammonia is 1:3.0, the mass ratio of tert-butanol and ZSM-5 molecular sieve is 7.8:1, and the silicon-aluminum ratio of ZSM-5 molecular sieve is 27;

[0050] (2) After the reaction is finished, cool down to room temperature, collect liquid phase substances, and measure various reaction performance parameters.

[0051] In this reaction, the yield of tert-butylamine was 10.91%.

Embodiment 3

[0052] Embodiment 3 (using molecular sieve type aluminosilicate catalyst, isobutylene recycles)

[0053] Prepare tert-butylamine according to the following method, comprising the following steps:

[0054] (1) Put 18.2210g of tert-butanol, liquid ammonia, ZSM-5 molecular sieve particles and isobutene into the reactor, and react for 3.2h at a reaction temperature of 275°C and a reaction pressure of 17MPa; among them, the feed of tert-butanol and liquid ammonia The molar ratio is 1:3.4, the mass ratio of tert-butanol and ZSM-5 molecular sieve is 4.6:1, the feed molar ratio of tert-butanol and isobutene is 1:1.7, and the silicon-aluminum ratio of ZSM-5 molecular sieve is 25;

[0055] (2) After the reaction is finished, cool down to room temperature, collect liquid phase substances, and measure various reaction performance parameters.

[0056] In this reaction, the yield of tert-butylamine was 11.92%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a novel process for preparing tert-butylamine in dynamic equilibrium of raw materials, and tert-butylamine is obtained through catalytic amination reaction of tertiary butanoland ammonia in the presence of a catalyst, wherein the catalyst is an aluminosilicate catalyst, and the catalytic amination reaction is conducted in the presence of dynamic equilibrium of isobutene and tertiary butanol. The invention adopts low-cost aluminosilicate catalyst, and improves the reaction efficiency by introducing isobutene as a circular substance during reaction, wherein the conversion per pass of tertiary butanol is 60% to 99%, the yield of tert-butylamine is 4% to 35%, isobutene generated by raw materials ensures that tert-butylamine selectivity is close to 100% through the system or mature tertiary butanol hydration process, and compared with other production processes, the process is short in reaction time and low in raw material cost, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of fine organic synthesis, and relates to a new process for amination in a dynamic equilibrium reaction of tert-butanol and isobutene by using tert-butanol as a raw material and isobutene as a carrier gas. Dynamic balance is conducive to keeping the concentration of active raw materials stable, and inactive raw materials continue to develop in two directions: conversion to active raw materials and self-amination, thus greatly improving the selectivity and yield of amination. Using aluminosilicate catalyst, there is no complicated and expensive modification preparation process, and the great improvement of reaction yield only depends on the design of dynamic equilibrium of raw materials. The designed process obtains tert-butylamine with high yield and high selectivity under certain and relatively mild catalytic conditions. Meet the sustainable development of green environmental protection process requirements. Backgro...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07C209/16C07C211/07
CPCC07C209/16C07C211/07
Inventor 周新锐冯烈孔洋陈云斌王兆国刘尚文李杰李东张建明
Owner ZHEJIANG JIANYE CHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com