Method for generating hydroxylamine by cyclohexanone-oxime through hydrolyzing

A technology of cyclohexanone oxime and hydroxylamine, which is applied in the field of preparation of hydroxylamine by the hydrolysis of cyclohexanone oxime catalyzed by solid acid, can solve the problems of difficult separation of catalyst and product, difficult recycling of waste acid liquid, difficulty of continuous production, etc., and achieves environmental protection Friendly process, avoid equipment corrosion, mild condition effect

Active Publication Date: 2017-10-20
HEBEI UNIV OF TECH
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  • Claims
  • Application Information

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Problems solved by technology

[0008] Aiming at the difficulties in the continuous production of the above-mentioned liquid acids, the corrosion of equipment, the difficulty in recycling waste acid, the pollution of the environment by discharge, and the difficulty in separating catalysts from products, the present invention provides a method for preparing hydroxylamine by hydrolysis of cyclohexanone oxime. method
The invention solves the problems o

Method used

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  • Method for generating hydroxylamine by cyclohexanone-oxime through hydrolyzing
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  • Method for generating hydroxylamine by cyclohexanone-oxime through hydrolyzing

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Embodiment 1

[0020] Put 1g (0.0088mol) of cyclohexanone oxime, 20mL (1.111mol) of deionized water, and HZSM-5 catalyst (2g) with a silicon-aluminum ratio of 25 into a 100mL three-necked bottle, stir, reflux and condense, and react at 60°C The reaction was stopped after 1 h. At the reaction temperature, toluene is added for extraction, and the organic phase in the reaction liquid is separated to obtain cyclohexanone; the raffinate aqueous phase is centrifuged to obtain the product hydroxylamine aqueous solution and catalyst respectively.

[0021] Hydroxylamine in the aqueous phase was analyzed by potassium permanganate redox titration; the organic phase was qualitatively analyzed by the retention value method of pure substances and chromatographic-mass spectrometry, and the cyclohexanone in the organic phase was quantitatively analyzed by gas chromatography oxime conversion. The experimental results are shown in Table 1.

Embodiment 2

[0023] Step is with embodiment 1, and difference is that the catalyst that adds is silicotungstic acid (H 4 SiW 12 o 40 ). The experimental results are shown in Table 1.

Embodiment 3

[0025] Step is with embodiment 1, and difference is that the catalyst that adds is phosphotungstic acid (H 3 o 40 PW 12 ). The experimental results are shown in Table 1.

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Abstract

The invention relates to a method for generating hydroxylamine by cyclohexanone-oxime through hydrolyzing. The method comprises the following steps of adding cyclohexanone-oxime, a catalyst and deionized water into a reactor, stirring, refluxing, condensing, and reacting for 0.5 to 2h at the temperature of 15 to 25 DEG C, so as to obtain the hydroxylamine; adding an methylbenzene extracting agent into the reactor, extracting at the reaction temperature, extracting an organic phase from a reaction liquid, and extracting a water phase, so as to obtain a product, namely a hydroxylamine water solution, wherein the catalyst is HZSM-5, silicotungstic acid, phosphotungstic acid or phosphomolybdic acid with a ratio of silicon to aluminum (silicon dioxide/aluminum oxide)) is 25 to 50. The method has the advantages that the reaction conditions are moderate, the operation is simple, the energy consumption is decreased, the environment-friendly and economical meanings are realized, and the environment-friendly catalyzing reaction process is performed.

Description

technical field [0001] The invention relates to a method for producing hydroxylamine (aqueous solution), in particular to a process for preparing hydroxylamine (aqueous solution) through hydrolysis of cyclohexanone oxime catalyzed by a solid acid. Background technique [0002] Hydroxylamine is a reducing agent in organic synthesis, which condenses with carbonyl compounds to form oximes. The molecular formula for hydroxylamine is NH 2 OH, can be seen as NH 3 A derivative formed by replacing one of the protons with a hydroxyl group is an unstable white crystal at room temperature, easy to deliquescence, and often exists in the form of aqueous solution. Hydroxylamine has two isomers, cis and trans. It is trans in the solid state, and may be a mixture of cis and trans in the gaseous state (Chinese patent, 201310082379.0). Hydroxylamine is an important chemical intermediate, which is widely used in the manufacture of nylon 66, ink, pigment, drug, pesticide, etc. At present, t...

Claims

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Application Information

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IPC IPC(8): C01B21/14
CPCC01B21/1409C01P2006/80
Inventor 张东升王晓曼王延吉李志会徐元媛赵新强薛伟
Owner HEBEI UNIV OF TECH
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