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Process for preparing caprylhydroxamic acid

A technology of n-octyl amide and preparation process, applied in the chemical industry, can solve the problems of large demand and no public technical report on the production of N-hydroxy n-octyl amide, and achieves reduction of production cost, resolution of decomposition and explosion danger, and mild reaction conditions. Effect

Active Publication Date: 2015-05-06
烟台东方化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

N-hydroxyn-octylamide is in high demand due to its wide range of uses, but there is no published technical report on the production of N-hydroxyn-octylamide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] In a 500L enamel reaction kettle, add 100 kg of hydroxylamine hydrochloride, add 120 kg of methanol aqueous solution with a content of 80% at room temperature, and stir at a rate of 70 rpm for 10 minutes at room temperature. Then add 130kg of n-octanoic acid methyl ester, stir and mix for 30 minutes. Then add 0.1kg of solid 4-dimethylaminopyridine, then control the temperature at about 5°C, slowly add 40kg of solid NaOH, adjust the pH to 5.0, control the temperature to 20°C, stir for 1 hour, then cool down to 0°C, and centrifuge Remove sodium chloride, then set the temperature to 50°C, concentrate the filtrate in vacuum until viscous, cool down to crystallize, and centrifuge to obtain a crude product with a content of 90%. Dissolve 100kg of the crude product in 150kg of methanol, recrystallize, centrifuge, and dry under reduced pressure at 50°C to obtain N-hydroxy n-octylamide with a content of 99.2%.

Embodiment 2

[0017] In a 1000L enamel reaction kettle, add 200 kg of hydroxylamine hydrochloride, add 250 kg of ethanol aqueous solution with a content of 85% at room temperature, and stir at a rate of 75 rpm for 10 minutes at room temperature. Then add 330kg n-octanoic acid ethyl ester, stir and mix for 40 minutes. Then add 0.6kg of solid 4-dimethylaminopyridine, then control the temperature at about 7°C, slowly add 95kg of solid KOH, adjust the pH to 5.5, control the temperature to 30°C, stir and react for 1.5 hours, then cool down to -3°C, Centrifuge to remove potassium chloride, then set the temperature to 55°C, concentrate the filtrate in vacuum until viscous, cool down to crystallize, and centrifuge to obtain a crude product with a content of 92%. Dissolve 100kg of the crude product in 160kg of ethanol, recrystallize, centrifuge, and dry under reduced pressure at 50°C to obtain N-hydroxy n-octylamide with a content of 99.1%.

Embodiment 3

[0019] In a 2000L enamel reaction kettle, add 400kg of hydroxylamine hydrochloride, add 500kg of 87% methanol water solution at room temperature, and stir at a rate of 85rpm for 10 minutes at room temperature. Then add 500kg n-octanoic acid methyl ester, stir and mix for 50 minutes. Then add 1.2 kg of solid 4-dimethylaminopyridine, then control the temperature at about 8°C, and slowly add solid Na 2 CO 3 310kg, adjust the pH to 6.0, control the temperature to 35 degrees, stir the reaction for 2 hours, then lower the temperature to -8 degrees, remove sodium chloride by centrifugation, then set the temperature to 65 degrees, concentrate the filtrate in vacuum until viscous, cool down and crystallize , centrifuged to obtain a crude product with a content of 91%. Dissolve 100kg of crude product in 170kg of ethylene glycol, recrystallize, centrifuge, and dry under reduced pressure at 50°C to obtain N-hydroxy n-octylamide with a content of 99.1%.

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PUM

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Abstract

The invention belongs to the field of chemical engineering and relates to a process for preparing caprylhydroxamic acid. The process comprises the steps sequentially: adding hydroxylamine hydrochloride into a reactor, adding an alcoholic solution, and stirring to dissolve; adding n-octoate into the reactor, and stirring and mixing uniformly; then, adding 4-dimethyl aminopyridine, adding a solid base, controlling the temperature to be 5-15 DEG C, and adjusting the pH value of the solution in the reactor to be 5.0-6.5; controlling the temperature of the solution to be 20-40 DEG C at normal pressure, reacting for 1-3 hours, cooling to the temperature of -10 DEG C to 0 DEG C after reacting ends, filtrating sodium chloride or potassium chloride, and carrying out vacuum concentration, cooling crystallization and centrifugal separation, so as to obtain a crude product; and recrystallizing the crude product in a solvent, and drying, thereby obtaining caprylhydroxamic acid, of which the content is over 99%. According to the process, the used raw materials are easily obtained; the reaction conditions are mild, so that the danger of decomposed explosion of hydroxylamine resulting from too-high temperature is excellently avoided; the reaction medium is an alcohol-water system, is safe and cheap and can be repeatedly applied mechanically, so that the production cost is reduced greatly, and industrial production and market promotion are facilitated.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a preparation process of N-hydroxy n-octylamide. technical background [0002] N-Hydroxy n-octylamide (Caprylhydroxamic Acid, CHA) is widely used in daily chemical, pharmaceutical, industrial, agricultural and other fields. In the field of daily chemicals, N-hydroxyn-octylamide, as a new type of preservative, solves the following problems of traditional preservatives: such as the potential carcinogenicity of formaldehyde and its release body, the potential carcinogenicity of nitrosamines produced by Broble, organic Potential sensitization of halogens, hormone stimulation of paraben esters and other issues. In the industrial field, N-hydroxy n-octylamide can be used as a high-efficiency collector for non-sulfide minerals, used for flotation extraction of tungsten ore, tin ore, etc.; in the field of agriculture and medicine, N-hydroxy n-octylamide can be used for urease inhibition a...

Claims

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Application Information

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IPC IPC(8): C07C259/06
Inventor 蔡建王家卫秦莉锦陈晓辉
Owner 烟台东方化学有限公司
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