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Preparation method of tert-octylamine

A technology of tert-octylamine and tert-octylacetamide, which is applied in the field of preparation of tert-octylamine, can solve the problems of sensitive acylase reaction conditions, complicated hydrolysis process of acetamide, and low total yield of tert-octylamine, and achieves raw material Easy to obtain, increase yield and reduce production cost

Active Publication Date: 2021-07-13
SHANDONG YUHUANG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantage of this technology is that the amidation reaction uses a large amount of glacial acetic acid as a solvent, and the recovery pressure is high; the hydrolysis process of acetamide is complicated, and the acylase is sensitive to reaction conditions and is easy to be inactivated; the total yield of t-octylamine is low

Method used

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  • Preparation method of tert-octylamine
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  • Preparation method of tert-octylamine

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Experimental program
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Effect test

Embodiment 1

[0028] The mixture was stirred, 56 g of diisobutylene, 31 g of acetonitrile, 55 g concentration of 90% aqueous sulfuric acid solution and 1 g of phase transfer catalyst were added to the round bottom flask, and an amidated reaction was carried out at 70 ° C for 8 h. The reaction liquid recovered the phase transfer catalyst and the unreacted acetonitrile, diisobutylene, after water, added to a certain amount of an alkaline solution, and adjusted the solution pH microbialism, filtered, washed to the filtrate, neutral N-coushanine Acetamide contains water filter cake. The filter cake is dried in a vacuum oven to a vacuum oven to a constant weight, and the reserved sealing storage is obtained.

[0029] Effect of Table 1 Different phase transfer catalysts on the production of acetamide

[0030]

Embodiment 2

[0032] The mixture was stirred, 56 g of diusbutene, 31 g of acetonitrile, 55 g of a 20% aqueous solution of sulfuric acid and a certain amount of tetrabutylammonium chloride were added to the round bottom flask, and an amidation reaction was carried out at 70 ° C for 8 h. The reaction solution recovered tetrabutylammonium chloride and unreacted acetonitrile, diisobutylene, water was added to a certain amount of an alkaline solution, and after adjusting the pH of the solution, filtered, washed to the filtrate, neutral N- Uttal acetamide contains water filter cake. The filter cake is dried in a vacuum oven to a vacuum oven to a constant weight, and the reserved sealing storage is obtained.

[0033] Effect of Table 2 Phase Transfer Catalyst Dosage on Acetamide Yield

[0034]

Embodiment 3

[0036] The mixture was stirred, 56 g of diisobutylene, acetonitrile, sulfuric acid solution, and 1 g of tetrabutylammonium chloride were added to the round bottom flask for an amidation reaction. At the end of the reaction, tetrabutylammonium chloride and an unreacted acetonitrile, diisobutylene, after water, the reaction solution was added to a certain amount of an alkaline solution, and the solution pH is subjected to the solution, filtered, washed to the filtrate. N-tertianedon-containing acetamide containing water filter cake. The filter cake is dried in a vacuum oven to a vacuum oven to a constant weight, and the reserved sealing storage is obtained.

[0037] Table 3 Optimization of acetamide reaction process parameters

[0038]

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Abstract

The invention relates to the field of chemistry and chemical engineering, and particularly discloses a preparation method of tert-octylamine. By taking acetonitrile and diisobutylene as raw materials, and N-tert-octyl acetamide is prepared through amidation reaction under the action line of concentrated sulfuric acid and a phase transfer catalyst by adopting a solvent-free method; and hydrolysis reaction is carried out on N, N-tert-octyl acetamide in a sodium hydroxide aqueous solution, and distilling an organic phase of a reaction product to obtain tert-octyl amine. The amidation reaction adopts the phase transfer catalyst, so that the amidation yield is improved, and the total yield of tert-octylamine can reach 95% or above; the amidation reaction adopts a solvent-free method, and the acetamide hydrolysis reaction takes water as a solvent, so that the solvent loss and the solvent recovery cost are reduced, and the pollution to the environment is reduced; and the comprehensive utilization of the materials in the production process also effectively reduces the environmental pollution and the production cost.

Description

Technical field [0001] The present invention relates to the field of chemical chemistry, and more particularly to a method of preparing tertiactine. Background technique [0002] Uttalctamine is an important organic synthetic intermediate, mainly used in the synthesis of light stabilizer 944, in the fields of rubber promoters, dyes, pesticides, emulsifiers, metal extraction, dispersant, etc. 944 is mainly suitable for polymerized light stabilizers that are particularly protruding in terms of polyethylene, polypropylene, ABS, and polystyrene. The large-scale application of 944 has brought a broad market prospect to tertiactine. [0003] Unstectamine existing synthesis technique is to prepare chuster octamines by amidate and acetamide hydrolyzate in two steps by diisutyate and acetonitrile (or sodium cyanide, or hydrocyanic acid). The amidation is more than acetate as a solvent, and the reaction is formed into n-tertianediecetamide in sulfuric acid; the acetamide is hydrolyzed, and...

Claims

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Application Information

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IPC IPC(8): C07C209/62C07C211/07C07C231/06C07C233/03
CPCC07C231/06C07C209/62C07C233/03C07C211/07Y02P20/584
Inventor 谢恒来杜宝磊李雪于玉夺宋松王金书
Owner SHANDONG YUHUANG CHEM CO LTD
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