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A novel process for the manufacture of 5-nonyl salicylaldoxime

A kind of technology of nonyl salicyl aldoxime and nonyl salicyl aldehyde is applied in the field of preparing 5-nonyl salicyl aldoxime, and can solve the problems of high cost, difficult sewage treatment and the like

Inactive Publication Date: 2008-12-17
氰特印度特种化学制品与材料私人有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The selectivity and yield of the treatment process seems to depend on the use of about 10 mole % tin chloride and nearly 40 mole % amine on the basis of phenol, making the commercial production too expensive and resulting in the treatment of sewage the puzzle

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0021] Place a 2-liter round-bottomed 4-neck flask in a suitable heating mantle, and be equipped with a stirrer, a reflux condenser, a thermometer and a dropping funnel, and charge 83 g of toluene, 12.6 g (0.525 mol) of magnesium powder, 0.06 g iodine, 2.7g anhydrous tin dichloride. Thus, 272 g of toluene-methanol azeotrope was slowly added to the previously obtained mixture under stirring conditions. The reaction mixture was heated to reflux temperature (approximately 64° C.) for 60 minutes to ensure complete formation of the magnesium alkoxide. 220 g (1.0 mol) of nonylphenol were added slowly and reflux was continued for another hour. 265 g of toluene were added and the temperature was raised to 80° C. at which point the toluene methanol azeotrope began to distill. This distillation is continued until all the azeotrope has distilled off.

[0022] Further, 0.9 g of tin dichloride was added to the above reaction volume, and 33 g (0.36 mol) of paraformaldehyde powder was add...

example 2

[0029] The above experiment was repeated, replacing the previously added 2.7 g and 0.9 g with 4.05 g and 1.35 g of tin dichloride. The product was about 90% pure by GC. The different percentages are due to the formation of more impurities compared to Example 1.

example 3

[0031]Example 1 was repeated, substituting 1.35 g and 0.45 g of tin dichloride for the 2.7 g and 0.9 g added. The product was 92% pure by GC due to the presence of unreacted nonylphenol.

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PUM

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Abstract

The invention relates to a process for producing 5-nonyl salicylaldoxime that comprises of converting nonyl phenol to a 5-nonyl aldehyde in a two-step reaction using a novel catalyst mixture, followed by the oximation of the said aldehyde using hydroxylamine sulphate, and that the said catalytic process of aldehyde production is the main invention, in that the effective use of the catalyst mixture helps the reaction proceed at a faster and controlled rate which leads to a higher yield of aldehyde, as a result of complete conversion of all the reactants to the final products.

Description

technical field [0001] The invention relates to a method for preparing 5-nonyl salicylaldoxime. Background technique [0002] Aldolase and its derivatives are used in many fields, such as cosmetics, pesticides, stabilizers, and as intermediates for the preparation of many industrial compounds, including oximes used in hydrometallurgical extraction processes, such as nonyl, Aryl acetaldoximes with long aliphatic chains such as dodecyl, which impart hydrophobicity to acetaldoxime, can then be effective as solvent extraction reagents. Aryl acetaldoxime or its derivatives are used for solvent extraction of copper, nickel, zinc, cobalt and other metals. In the copper solvent extraction process, dilute sulfuric acid (H 2 SO 4 )deal with. Copper and other alkaline metals dissolve as sulfates. Metal sulfate solutions were treated with salicylaldoxime solutions in kerosene. Copper selectively reacts with the oxime and transfers into the organic phase as a chelate. This reactio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/00C07C45/00
CPCC07C249/08C07C251/48
Inventor 萨雷什·巴希库莱尔·帕利沃尔维杰伊·巴汉格旺斯沃拉普·马瑟巴希库莱尔·纳西德斯·米兰尼
Owner 氰特印度特种化学制品与材料私人有限公司
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