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Process for preparing butanone oxime

A technology for butanone oxime and butanone, which is applied in the field of preparation of organic compound butanone oxime, can solve the problems of increased energy consumption and separation cost, and achieves the effects of good environmental protection, simple process and cost reduction.

Inactive Publication Date: 2008-12-10
ZHEJIANG UNIV
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Problems solved by technology

[0005] The preparation method of butanone oxime mainly contains hydroxylamine method and TS-1 molecular sieve catalytic ammoxidation method, and the existing TS-1 molecular sieve catalytic ammoxidation method of literature has used organic solvent in the reaction process, and needs pressurization to carry out reaction (Chemical industry and engineering, 2005, Vol.22, NO.4, 279~281), which increases the energy consumption and separation cost of this process

Method used

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  • Process for preparing butanone oxime
  • Process for preparing butanone oxime

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Embodiment 1, a kind of preparation method of butanone oxime, take butanone, ammoniacal liquor, hydrogen peroxide as raw material, operation steps are:

[0020] In a kettle with a volume of 250 mL, add TS-1 molecular sieve (containing 1.0 g of Ti) as a catalyst, and the content of Ti in the TS-1 molecular sieve is 1.5%; then add 20 mL of water as a solvent. Feed 20mL butanone (0.22mol, 16.1g) and 40mL ammonia water (0.53mol) with a mass fraction of 25% at one time, after heating to a reaction temperature of 65°C, add hydrogen peroxide with a mass fraction of 25% at a rate of 30g / h 30 mL (0.24 mol), during which the reaction temperature was maintained at 65°C. Under the reaction temperature of 65° C. and the reaction pressure of normal pressure, the reaction was completed after 1.5 hours of reaction; the still liquid was analyzed by gas chromatography. Analysis showed that the conversion of cyclohexanone was 71.7%, and the yield was 70.3%.

Embodiment 2～5

[0022] Change the following reaction conditions among the embodiment 1: Ti content in TS-1 molecular sieve (abbreviation active component content), the weight of Ti (abbreviation m1), reaction temperature (abbreviation T), the volume consumption (abbreviation V1) of hydrogen peroxide, The mass concentration of hydrogen peroxide (abbreviated as w1), the volumetric dosage of ammonia (abbreviated as V2), the mass concentration of ammonia (abbreviated as w2), and the reaction time (abbreviated as t) are obtained from Examples 2 to 5, thereby obtaining the conversion rate of corresponding butanone (referred to as x), product yield (referred to as y). See Table 1 for details and data results.

[0023] Table 1

[0024] Example number

[0025] V2(mL)

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Abstract

The invention discloses a preparation method for methylethylketoxime. The method is as follows: under the action of catalyst, the methylethylketoxime is produced by reacting butanone with hydrogen peroxide and ammonia in water, according to a molar ratio of the butanone to the hydrogen peroxide to the mole of the ammonia of 1:0.8-1.5:1-3.5, which is carried out at a temperature of between 55 and 80 DEG C, under the atmospheric pressure for 1 to 3 hours. The method for preparing the methylethylketoxime is characterized by moderate reaction conditions and environment protection, no requirement of an organic solvent, etc.

Description

technical field [0001] The invention relates to a preparation method of an organic compound butanone oxime. Background technique [0002] Butanone oxime with the structural formula shown in formula 1 is a chemical synthesis intermediate, which is an important raw material for the synthesis of neutral crosslinking agents methyl tributylketoxime silane and vinyl tributylketoxime silane, and can also be used as Oxygen scavenger for boilers and anti-skinning agent for paints and coatings, etc. [0003] [0004] Formula 1 [0005] The preparation method of butanone oxime mainly contains hydroxylamine method and TS-1 molecular sieve catalytic ammoxidation method, and the existing TS-1 molecular sieve catalytic ammoxidation method of literature has used organic solvent in the reaction process, and needs pressurization to carry out reaction (Chemical industry and engineering, 2005, Vol.22, NO.4, 279-281), which increases the energy consumption and separation cost of this proces...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/38C07C249/04B01J29/89
Inventor 陈新志周少东
Owner ZHEJIANG UNIV
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