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A novel process for the manufacture of 5-nonyl salicylaldoxime

A technology of nonyl salicylaldoxime and catalyst, applied in the field of preparation of 5-nonylsalicylaldoxime, which can solve the problems of high cost and difficult sewage treatment

Inactive Publication Date: 2012-01-04
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

[0028] Place a 2-liter round-bottom 4-necked flask in a suitable heating mantle, equipped with a stirrer, reflux condenser, thermometer and dropping funnel, and fill it with 83g of toluene, 12.6g (0.525mol) of magnesium powder, 0.06 g iodine, 2.7 g anhydrous tin dichloride. In this way, under stirring conditions, 272 g of toluene methanol azeotrope was slowly added to the previously obtained mixture. The reaction mixture was heated to reflux temperature (approximately 64°C) for 60 minutes to ensure complete formation of magnesium alkoxide. Slowly add 220 g (1.0 mol) of nonylphenol and continue refluxing for another hour. 265 g of toluene was added, and the temperature rose to 80°C, at which temperature the toluene methanol azeotropic mixture began to distill. The distillation continues until all the azeotrope is distilled out.

[0029] Further, 0.9 g of tin dichloride was added to the above reaction amount, and 33 g (0.36 mol) of paraformaldehyde powder was added through the s...

example 2

[0036] Repeat the above experiment, replacing the previously added 2.7g and 0.9g with 4.05g and 1.35g tin dichloride. The purity of the product obtained by GC is about 90%. The percentage difference is due to the formation of more contaminants compared to Example 1.

example 3

[0038] Repeat Example 1, using 1.35g and 0.45g tin dichloride instead of the added 2.7g and 0.9g. The purity of the product obtained by GC is 92%, which is 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-nonylsalicylaldoxime. Background technique [0002] Aldase and its derivatives are used in many fields, such as cosmetics, pesticides, stabilizers, and as intermediates for many industrial compounds, including oximes used in hydrometallurgical extraction processes, such as nonyl, Aryl acetaldoxime with a long aliphatic chain such as dodecyl group provides hydrophobicity to acetaldoxime before it can be effectively used as a solvent extraction reagent. Aryl acetaldoxime or its derivatives are used for solvent extraction of metals such as copper, nickel, zinc, and cobalt. In the copper solvent extraction process, dilute sulfuric acid (H 2 SO 4 )deal with. Copper and other alkaline metals are dissolved as sulfates. The metal sulfate solution is treated with salicylaldoxime solution in kerosene. Copper selectively reacts with oximes and is transferred to the organic phase as a chelate. This reaction is best...

Claims

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Application Information

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Patent Type & Authority Patents(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