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Method for continuously producing hydroxylammonium

A technology of hydroxylammonium and hydroxylammonium salts, which is applied in the field of continuous process preparation of hydroxylammonium, and can solve the problems of high cost, reduced selectivity of hydroxylammonium, complex equipment, etc.

Active Publication Date: 2013-10-23
CAP III
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The equipment is complex, expensive and energy consuming (e.g. energy, steam)
[0037] It is therefore an object of the present invention to provide a process for the preparation of hydroxylammonium in a continuous process which can replace the known processes to overcome the problem of reduced selectivity for hydroxylammonium

Method used

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  • Method for continuously producing hydroxylammonium
  • Method for continuously producing hydroxylammonium
  • Method for continuously producing hydroxylammonium

Examples

Experimental program
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Effect test

Embodiment 1

[0087] The production of hydroxylammonium is carried out in the equipment, which adopts DSM technology. In the hydrogenation reactor, the by-product ammonia, N 2 O and N 2 .

[0088] The conditions of the nitrate hydrogenation reactor are:

[0089] Average temperature: 35-60°C

[0090] Reactor pressure: 2.0-3.0MPa.

[0091] Activator Type: GeO2

[0092] Activator / catalyst ratio: 3-7gr GeO 2 / kg catalyst

[0093] The compression ratio of the gas cycle compressor is in the range of 1.05 to 1.2.

[0094] Table 1 for catalyst type, d) fresh hydrogen component, dried a) off-gas component, off-gas:recycle gas ratio and hydroxylammonium selectivity.

[0095] The ratio of a) exhaust gas and b) circulating gas is maintained at 10:90-1:99.5; and the concentration of hydrogen in the purified gas is guaranteed to be greater than 30% by volume and less than 75% by volume, so that the selectivity of hydroxylammonium greater than 75% can be maintained .

[0096] Table 1

[0097]...

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Abstract

The invention provides a method for preparing hydroxylammonium through a continuous process. The method comprises the following steps of: purifying gases; and separating the purified gases into a) waste gases and b) recycle gases, wherein i) the ratio of a) waste gases to b) recycle gases is (10:90)-(0.5:99.5); ii) the concentration of the hydrogen in the purified gases is more than 30% and less than 75% by volume; and iii) a gas recycle compressor exists in a recycle gas line and has a compression ratio of 1.01-1.4.

Description

technical field [0001] The present invention relates to a method for the preparation of hydroxylammonium in a hydroxylammonium salt synthesis zone in a continuous process with high hydroxylammonium selectivity, which comprises making the purified gas The hydrogen concentration is greater than 30% by volume. Background technique [0002] An important use of hydroxylammonium salts is for the preparation of oximes from ketones or aldehydes, especially cyclohexanone oxime from cyclohexanone. For the preparation of the oxime, in the known circulation process, an aqueous acidic buffered reaction medium is kept circulating in the hydroxylammonium salt synthesis zone and the oxime synthesis zone. The reaction medium is acidically buffered, for example with phosphoric and / or sulfuric acid and buffer salts derived from these acids, for example basic and / or ammonium salts. In the hydroxylammonium salt synthesis zone, hydrogen is used to convert nitrate ions or nitrogen oxides in the ...

Claims

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Application Information

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IPC IPC(8): C01B21/14
Inventor 约翰·托马斯·廷格鲁道夫·菲利普斯·玛丽亚·古伊特
Owner CAP III
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