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Preparation method of ketoxime

A technology of ketoxime and oximating agent, applied in oxime preparation, organic chemistry, etc., can solve the problems of unsuitable industrial application, long process time consumption, inconvenient operation, etc., achieve continuous production, short process time, and improve production efficiency Effect

Active Publication Date: 2012-01-25
LINZIZHENGHUA ACCESSORY INGREDIENT ZIBO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above method records that relatively high acetone conversion rate and acetone oxime selectivity can be obtained, in the above method, hydrogen peroxide needs to be slowly added dropwise, and the drop time may even be as long as 12 hours, which leads to inconvenient operation and long time consumption of the whole process. long problem, not suitable for industrial application

Method used

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  • Preparation method of ketoxime
  • Preparation method of ketoxime
  • Preparation method of ketoxime

Examples

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Embodiment approach

[0025] According to one embodiment of the present invention, the method for preparing ketoxime provided by the present invention may comprise the following steps:

[0026] (1) Mix ketone, oxidant and solvent to form solution A, and send the above solution A and oximating agent or oximating agent solution B into the reactor equipped with catalyst at the same time, at 60-110°C and 0.2MPa-2MPa Continuous reaction under pressure for 30-50 minutes;

[0027] (II) introducing the reaction product into an external membrane tube for solid-liquid separation;

[0028] (III) The solid obtained by the solid-liquid separation is recycled back to the reactor to be used as part or all of the catalyst, and the liquid component containing ketoxime is sent to the product storage tank.

[0029] Described tensio-active agent can exist in solution A, in solution B or in reactor, or exist in above-mentioned three at the same time, as long as guarantee that the contact of ketone and oximating agent ...

Embodiment 1

[0036] This example is used to illustrate the method for preparing ketoxime provided by the present invention.

[0037] 58g acetone (1 mole), 124g hydrogen peroxide (H 2 o 2 Concentration is 27.5% by weight, 1 mole), surfactant and 51g tert-butyl alcohol are made into mixed solution A, and 87g ammoniacal liquor (concentration is 25% by weight, 1.3 mole) and surfactant are made into solution B, solution A and Solution B joins together in the reactor containing HTS titanium silicon molecular sieve catalyst (purchased from Hunan Jianchang Co., Ltd. trademark is HTS-3) and surfactant, wherein the consumption of catalyst is 5.00g catalyst / mol acetone, solution A, The surfactant in the solution B and the reactor is a mixture of sorbitol fatty acid ester and polyoxyethylene sorbitan fatty acid ester with a weight ratio of 0.8: 1, wherein the grade of sorbitol fatty acid value is SP-60, the total The dosage is 0.008g surfactant / mol acetone, the grade of polyoxyethylene sorbitan fatt...

Embodiment 2

[0044] This example is used to illustrate the method for preparing ketoxime provided by the present invention.

[0045] 58g acetone (1 mole), 173g hydrogen peroxide (H 2 o 2 Concentration is 27.5% by weight, 1.4 mole), tensio-active agent and 102g tert-butanol are made into mixed solution A, will contain 115g ammoniacal liquor (concentration is 25% by weight, 1.7 mole) and tensio-active agent are made into solution B, solution A Join together with solution B in the reactor that contains catalyst HTS molecular sieve (purchased from Hunan Jianchang Co., Ltd. trademark is HTS-3), wherein the consumption of catalyst is 25g catalyst / mol acetone, and surfactant is sorbitol fatty acid ester (the brand is SP-60, the total consumption 0.013g surfactant / mol acetone in solution A and solution B) and polyoxyethylene sorbitan fatty acid ester (the brand is TW-80, in solution A and solution B The total amount used in 0.010g surfactant / mol acetone), the reaction temperature is controlled a...

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Abstract

The invention provides a preparation method of ketoxime, which is characterized by comprising contact of ketone and oximation agent under oximation reaction conditions with solvents, oxidizing agents, surfactants and catalysts. The preparation method of the acetone oxime has the advantages that the reaction operation is simple, the process time is short and continuous production can be achieved. For example, by adopting the method, the acetone conversion rate, the hydrogen peroxide conversion rate and the acetone oxime selectivity can reach above 98 percent within 40 minutes. For comparison in Example 1, the acetone conversion rate, the hydrogen peroxide conversion rate and the acetone oxime selectivity can only reach about 96 percent within 600 minutes under the same condition except for surfactants. Therefore, the production efficiency can be greatly increased when the method is adopted.

Description

technical field [0001] The invention relates to a method for preparing ketoxime. Background technique [0002] At present, there are two main processes for the industrial production of ketoxime: one is the hydroxylamine method, and the other is the sodium nitrite method. In the production process of these two processes, it is necessary to use hydrogen to convert nitrate ions or nitrite ions into hydroxylamine, and then the hydroxylamine reacts with the free buffer acid and / or acid salt in the system to form the corresponding hydroxylamine and / or hydroxylamine Ammonium salts, and then hydroxylammonium salts react with ketones to form the corresponding oximes. Above-mentioned technological process has many shortcomings of reaction step, long reaction time, by-product; In addition, the catalyzer that is used to reduce nitrate ion is generally loaded on the palladium and / or platinum on the charcoal or the aluminum oxide carrier, like this in the process of reaction Catalysts a...

Claims

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Application Information

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IPC IPC(8): C07C249/04C07C251/38
Inventor 侯永正翟少华林民冯志杰史文明
Owner LINZIZHENGHUA ACCESSORY INGREDIENT ZIBO
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