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Synthesis method of 2-hydroxy-5-nonylpropiophenone and application of 2-hydroxy-5-nonylpropiophenone in copper extraction agent

A synthesis method and technology of copper extractant, which are applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of carbonyl compounds by hydrolysis, etc., can solve the problems of low product yield and purity, unstable synthesis process, and low conversion rate of finished products, etc. problems, to achieve high conversion rate and product purity, low stability in use, high product yield and purity

Inactive Publication Date: 2020-08-04
福建紫金选矿药剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the conversion rate of the finished product is low, and the product purity is not high; and there are many side reactions, the synthesis process is unstable, the distance is long, and the product yield and purity are not high.

Method used

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  • Synthesis method of 2-hydroxy-5-nonylpropiophenone and application of 2-hydroxy-5-nonylpropiophenone in copper extraction agent
  • Synthesis method of 2-hydroxy-5-nonylpropiophenone and application of 2-hydroxy-5-nonylpropiophenone in copper extraction agent

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Embodiment 1

[0021] The present invention provides a kind of technical scheme: the synthetic method of 2-hydroxyl-5-nonylpropiophenone and the application in copper extractant, the synthetic method of 2-hydroxyl-5-nonylpropiophenone comprises the following steps:

[0022] S1, esterification reaction, in a 500ml three-neck flask equipped with magnetic stirring, reflux condenser and HCl absorption device, 4-nonylphenol: propionyl chloride: tetrachloroethylene according to the ratio of 1:1.1:1.5 (molar ratio), Add propionyl chloride dropwise to nonylphenol tetrachloroethylene at room temperature under stirring, and react at 50°C for 5 hours to generate nonylphenol ester;

[0023] S2, rearrangement reaction, nonylphenol ester: TiCl4 is heated to reflux (120°C) according to 1:1 (molar ratio) and kept for 10 hours for ortho rearrangement reaction;

[0024] S3, hydrolysis reaction, hydrolyze with 6N HCl and 2N HCl at 50°C-70°C for 1 hour in sequence, then wash with water until pH 6.0 and separate...

Embodiment 2

[0028] The present invention provides a kind of technical scheme: the synthetic method of 2-hydroxyl-5-nonylpropiophenone and the application in copper extractant, the synthetic method of 2-hydroxyl-5-nonylpropiophenone comprises the following steps:

[0029] S1, esterification reaction, in a 500ml three-neck flask equipped with magnetic stirring, reflux condenser and HCl absorption device, 4-nonylphenol: propionyl chloride: tetrachloroethylene according to the ratio of 1:1.1:1.5 (molar ratio), Add propionyl chloride dropwise to nonylphenol tetrachlorethylene at room temperature under stirring, and react at 53°C for 5 hours to generate nonylphenol ester;

[0030] S2, rearrangement reaction, nonylphenol ester: TiCl4 is heated to reflux (120°C) according to 1:1 (molar ratio) and kept for 11 hours for ortho rearrangement reaction;

[0031] S3, hydrolysis reaction, hydrolyze with 6N HCl and 2N HCl at 50°C-70°C for 1.3h in sequence, then wash with water until pH 6.0 and separate ph...

Embodiment 3

[0035] The present invention provides a kind of technical scheme: the synthetic method of 2-hydroxyl-5-nonylpropiophenone and the application in copper extractant, the synthetic method of 2-hydroxyl-5-nonylpropiophenone comprises the following steps:

[0036] S1, esterification reaction, in a 500ml three-neck flask equipped with magnetic stirring, reflux condenser and HCl absorption device, 4-nonylphenol: propionyl chloride: tetrachloroethylene according to the ratio of 1:1.1:1.5 (molar ratio), Add propionyl chloride dropwise to nonylphenol tetrachlorethylene at room temperature under stirring, and react at 55°C for 5 hours to generate nonylphenol ester;

[0037] S2, rearrangement reaction, nonylphenol ester: TiCl4 is heated to reflux (120°C) according to 1:1 (molar ratio) and kept for 12 hours for ortho rearrangement reaction;

[0038] S3, hydrolysis reaction, hydrolyze with 6N HCl and 2N HCl at 58°C for 2.3 hours in sequence, then wash with water until pH 6.0 and separate phas...

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Abstract

The invention provides a synthesis method of 2-hydroxy-5-nonylpropiophenone and an application of the 2-hydroxy-5-nonylpropiophenone in a copper extraction agent. The synthesis method of the 2-hydroxy-5-nonylpropiophenone comprises the following steps: esterification reaction, rearrangement reaction, hydrolysis reaction and distillation purification. The method has the beneficial effects that thebrand-new synthetic route of the 2-hydroxy-5-nonylpropiophenone has the advantages that TiCl4 is adopted as a Lewis acid catalyst to carry out the rearrangement reaction of 4-nonylphenol ester, side reactions are fewer, and higher conversion rate and product purity can be obtained; according to the application of the 2-hydroxy-5-nonylpropiophenone oxime in the efficient copper extraction agent, the efficient copper extraction agent can be obtained after the 2-hydroxy-5-nonylpropiophenone oxime and the 2-hydroxy-5-nonylbenzaldoxime are compounded according to the ratio of 1:1, the product performance exceeds that of a Lix984N product, and the use stability and the unit consumption are lower.

Description

technical field [0001] The invention relates to the technical field of copper extractant, in particular to a synthesis method of 2-hydroxy-5-nonylpropiophenone and its application in copper extractant. Background technique [0002] Copper is the most important strategic metal and one of the important resources of the national economy. The "leaching-extraction-electrodeposition" technology in the copper refining process has been greatly developed at home and abroad. At present, about 20% of copper metal in the world is produced by this wet process, which is especially suitable for the development and utilization of low-grade copper ore resources. . In fact, the successful development of hydroxime-based industrial copper extractants has led to the large-scale application of hydrometallurgy technology around the world. [0003] At present, the most widely used and most representative copper extractant in the world is the LIX series of BASF in Germany. This type is a compound ...

Claims

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Application Information

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IPC IPC(8): C07C45/42C07C45/54C07C45/82C07C49/825C07C67/14C07C69/157C22B3/26C22B15/00
CPCC07C45/42C07C45/54C07C45/82C07C67/14C22B15/0084C22B3/306C07C49/825C07C69/157
Inventor 邹刚罗忠岩余海城梅天胜
Owner 福建紫金选矿药剂有限公司
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