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Process for the production of hydroxylamine by reduction of nitrate or nitrogen monoxide

A technology for producing hydroxylamine and nitric oxide, applied in chemical instruments and methods, preparation of hydroxylamine and lactam, etc., can solve the problems of increasing the variable cost of hydroxylamine, consuming ion exchange resin, increasing the required input, etc. The effect of energy consumption, reduction of raw material consumption, and reduction of energy consumption

Active Publication Date: 2014-01-22
CAP III
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The implementation of this technology resulted in an increase in the inputs required for the production of hydroxylamine, which had a negative impact on the fixed costs for the production of hydroxylamine and the products produced therefrom
In addition, ion exchange resin is also consumed, and its alkaline regeneration complicates the entire process
Increased variable costs for producing hydroxylamine and products produced therefrom due to the expense of ion exchange resins and bases

Method used

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  • Process for the production of hydroxylamine by reduction of nitrate or nitrogen monoxide
  • Process for the production of hydroxylamine by reduction of nitrate or nitrogen monoxide
  • Process for the production of hydroxylamine by reduction of nitrate or nitrogen monoxide

Examples

Experimental program
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Embodiment Construction

[0064] The invention is illustrated, but not limited, by the following examples.

[0065] This experiment was carried out in a commercial cyclohexanone oxime facility according to The process operates. Continuous and selective reduction of nitrates with hydrogen to hydroxylamine. The prepared hydroxylamine is converted to cyclohexanone oxime by reaction with cyclohexanone in the oximation zone. The structure is mainly as figure 1 shown.

[0066] The device includes a hydroxylamine formation zone where nitrate is reduced in an aqueous phosphate buffered saline solution. Using heterogeneous catalyst Pd / C and adding accelerator GeO 2. The part of the phosphate-containing acidic aqueous solution that also contains hydroxylamine is continued to be exported and fed to the oximation zone after removal of the catalyst by filtration. In the oximation zone the aqueous hydroxylamine solution is contacted with cyclohexanone dissolved in toluene. The oximation zone was operated ...

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Abstract

The present invention provides a process for the continuous production of hydroxylamine, comprising i) feeding to a hydroxylamine formation zone: a) hydrogen-containing gas; b) phosphate-containing acidic aqueous solution; and c) nitrate or nitrogen monoxide dissolved in said phosphate-containing acidic aqueous solution; ii) reducing, in said hydroxylamine formation zone, nitrate or nitrogen monoxide with hydrogen to form hydroxylamine; iii) removing hydroxylamine from said phosphate-containing acidic aqueous solution, in a hydroxylamine removal zone; iv) adding to said phosphate-containing acidic aqueous solution nitrous gases and / or nitrate; and v) returning to said hydroxylamine formation zone said phosphate-containing acidic aqueous solution; characterized in that a portion of said phosphate-containing acidic aqueous solution is removed; and phosphoric acid is added to the remaining phosphate-containing acidic aqueous solution; a process for preparing oximes therefrom; a process for preparing lactams therefrom; and a fertilizer product produced therefrom.

Description

technical field [0001] The present invention relates to a method for producing hydroxylamine by reducing nitrate or nitric oxide; a method for preparing oxime thereby; a method for preparing lactam thereby; and a fertilizer product prepared thereby. Background technique [0002] Hydroxylamine is a common reagent in most organic and inorganic reactions. It is particularly useful for the preparation of oximes, especially cyclohexanone oxime, which is converted to caprolactam by a Beckmann rearrangement reaction. The Beckmann rearrangement reaction to prepare caprolactam in general is well known in the art, eg from Ullmann's encyclopedia of Industrial Chemistry, eg 7th edition (2005), chapter on caprolactam (DOI: 10.1002 / 14356007.a05.031 (Retrieved Feb. 18, 2011) Other oximes prepared from hydroxylamine include cyclododecanone oxime (eg EP‐A1329448) and butanone oxime. [0003] Methods of preparing hydroxylamine are also well known in the art. Further, various patent rights ...

Claims

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Application Information

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IPC IPC(8): C01B21/14C07C249/08C07C251/44C07D201/04C07D223/10C05G1/00
CPCC05D9/02C07C249/08C05B7/00C01B21/1418C07C2601/14C07C2601/20C07C251/44C07C251/38C01B21/14C05F11/00
Inventor 约翰·托马斯·廷格丹尼尔·朱丽斯·玛利亚·奥兹哲姆
Owner CAP III
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