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Technique for synthesizing tert-butylamine

A synthetic process, the technology of tert-butylamine, applied in the field of fine chemical intermediate production, can solve problems such as difficult industrial production, and achieve the effects of less environmental pollution, loose reaction conditions and high yield

Active Publication Date: 2008-01-23
ZIBO LUHUA HONGJIN NEW MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It is difficult to form large-scale industrial production in our country

Method used

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  • Technique for synthesizing tert-butylamine
  • Technique for synthesizing tert-butylamine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] (1) The catalytic reaction product is hydrolyzed at 65°C.

[0074] (2) The acid produced by hydrolysis and the alcohol produced by the catalytic reaction undergo esterification reaction to form an ester, and the distillation temperature is controlled at 105° C. to collect corresponding fractions. Simultaneously, incompletely reacted methanol was distilled off.

[0075] (3) Carry out acid-base reaction, adopt the calcium hydroxide solution that mass concentration is 13% to neutralize tert-butylamine sulfate, control distillation temperature 30-100 ℃, then collect the cut of 43 ℃ through rectification and obtain product tert-butylamine. The yield of tert-butylamine is: 90%, and the purity is: >99.5%

[0076] The molar proportion of above each raw material, according to following setting:

[0077] MTBE:hydrocyanic acid=1:1

[0078] MTBE: concentrated sulfuric acid = 1:1

[0079] MTBE:Water=1:3

[0080] MTBE: Calcium Hydroxide = 1: 1.5

[0081] Below is the embodiment...

Embodiment 2

[0084] When methyl tert-butyl ether:concentrated sulfuric acid=1:0.5, the yield of tert-butylamine is 45%, and the purity is 80%.

Embodiment 3

[0086] When methyl tert-butyl ether:concentrated sulfuric acid=1:1, the yield of tert-butylamine is 90%, and the purity is 99.5%.

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Abstract

The invention belongs to the fine chemical field, which is mainly used for the synthesis of rubber accelerator NS and the intermediate raw material of the rifampicin-tert-butylamine. The invention is characterized in that: the methyl tert-butyl ether-hydrocyanic acid method is adopted to produce tert-butylamine; under normal pressure, the methyl tert-butyl ether is added with hydrocyanic acid and is added with concentrated sulphuric acid to carry out fully catalytic reaction; the methanol produced in the catalytic reaction is fully adopted and is added with water to perform hydrolysis, deep hydrolysis and esterification, and methyl formate and methanol without react completely are distilled; sulphates in calcium hydroxide solution and the butylamine to replace the butylamine to gain the butylamine through rectification and produce the byproduct calcium sulfate. The invention adopts the water instead of the methanol to carry out the hydrolysis and esterification and neutralizes the raw materials and adopts the calcium hydroxide to produce butylamine, which has the advantages of simple process, short production period, high yield, stable product quality, low production cost and small environment pollution.

Description

technical field [0001] The invention belongs to the technical field of production of fine chemical intermediates, and is mainly used for the synthesis process of tert-butylamine, an intermediate raw material of synthetic rubber accelerator NS and drug rifampicin. Background technique [0002] Product features and physical and chemical properties of tert-butylamine: [0003] Molecular formula: C 4 h 11 N [0004] Structural formula: [0005] [0006] Molecular weight: 73.14 [0007] Name: tert-butylamine, also known as tert-butylamine, 2-aminoisobutane [0008] Specific gravity: 0.6958 (20°C) [0009] Melting point: -67.5°C [0010] Boiling point: 43.6°C [0011] Refractive index (18°C): 1.3794 [0012] Flash point: 10°C. [0013] At room temperature, tert-butylamine is a colorless transparent liquid with an ammonia odor, miscible with water and ethanol, and soluble in common organic solvents. It is an intermediate in organic synthesis and can be used as a drug (...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/03C07C209/00
Inventor 卢国强浦为民王荣军郑福国
Owner ZIBO LUHUA HONGJIN NEW MATERIAL CO LTD
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