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Hydroxylamine-oximation circulatoing system

A circulatory system and hydroxylamine technology, applied in the preparation of hydroxylamine and oxime, organic chemistry, etc., can solve problems such as unfavorable overall reaction, difficult removal of organic pollutants, corrosion of contact materials, etc.

Active Publication Date: 2008-07-23
CHINA PETROCHEM DEVMENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the exhaust gas emitted during this heat treatment is likely to cause corrosion of contact materials.
Furthermore, if the temperature of heat treatment is to be increased to further reduce the total organic carbon content in the inorganic treatment liquid, the condensation reaction of the organic matter may cause the color of the inorganic treatment liquid to turn yellow, making the remaining organic pollutants more difficult to remove, which is not conducive to overall response

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0047] The phosphate inorganic treatment solution is continuously fed to the hydroxylamine reactor per unit time, and the inorganic treatment solution contains 2.88 mol / kg of hydrogen ions, 2.68 mol / kg of phosphate, and 0.20 mol / kg of free nitric acid. Hydroxylamine phosphate was synthesized at a temperature of 53° C. and a hydrogen partial pressure of 55%, using 10% palladium / activated carbon catalyst (manufactured by Japan Degussa Company) for catalysis. In the phosphate inorganic treatment liquid at the outlet of the hydroxylamine reactor, the concentration of the synthesized hydroxylamine phosphate is 1.14 mol / kg.

[0048] The hydroxylamine phosphate inorganic treatment solution and the toluene solution containing cyclohexanone are continuously fed into the oximation tower from the top and bottom of the oximation tower for oximation reaction (the operating temperature of the oximation tower is 51° C.). The molar ratio is 0.90. In the organic phase overflowing from the top...

Embodiment 2

[0053] The phosphate inorganic treatment solution is continuously fed to the hydroxylamine reactor per unit time, and the inorganic treatment solution contains 3.45 mol / kg of hydrogen ions, 3.05 mol / kg of phosphate, and 0.58 mol / kg of free nitric acid. Hydroxylamine phosphate was synthesized at a temperature of 53° C. and a hydrogen partial pressure of 55%, using 10% palladium / activated carbon catalyst (manufactured by Japan Degussa Company) for catalysis. In the phosphate inorganic treatment liquid at the outlet of the hydroxylamine reactor, the concentration of the synthesized hydroxylamine phosphate is 1.41 mol / kg.

[0054] The inorganic treatment solution of hydroxylamine phosphate is firstly fed into the premixing reactor in the same direction as part of the toluene solution of cyclohexanone, and premixed at a temperature of 37° C. and a pressure of one atmosphere. In the mixed reaction liquid discharged from the premixing reactor, the concentration ratio of hydroxylamine...

Embodiment 3

[0060] The phosphate inorganic treatment solution is continuously fed to the hydroxylamine reactor per unit time, and the inorganic treatment solution contains 4.00 mol / kg of hydrogen ions, 3.27 mol / kg of phosphate, and 0.72 mol / kg of free nitric acid. Hydroxylamine phosphate was synthesized at a temperature of 53° C. and a hydrogen partial pressure of 55%, using 10% palladium / activated carbon catalyst (manufactured by Japan Degussa Company) for catalysis. In the phosphate inorganic treatment liquid at the outlet of the hydroxylamine reactor, the concentration of the synthesized hydroxylamine phosphate is 1.64 mol / kg.

[0061] The inorganic treatment solution of hydroxylamine phosphate is firstly fed into the premixing reactor in the same direction as part of the toluene solution of cyclohexanone, and premixed at a temperature of 37° C. and a pressure of one atmosphere. In the mixed reaction liquid discharged from the premixed reactor, the concentration ratio of hydroxylamine ...

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Abstract

The invention provides a hydroxylamine-oximation circulating system, which includes: (a)a hydroxylamine reaction zone; (b) an oximation reaction zone; (c) a decontamination area; and (d) a regulation area with a nitric acid absorber; only part of the inorganic treatment fluid used by the reaction system enters the nitric acid absorber in the regulation area to supplement the nitrate ion, and is mixed with the residual inorganic treatment fluid after the composition is adjusted, so the loss proportion of the hydroxylamine by the decomposition in the inorganic treatment fluid can be reduced. Furthermore, the decontamination area of this system can effectively remove the high boiling point organic pollutant in the inorganic treatment fluid, thus avoiding the catalyst needed by the hydroxylamine reaction from being poisoned, reducing the activity of the catalyst and the selectivity of the hydroxylamine reaction, and being more beneficial to the production of high concentration hydroxylamine.

Description

technical field [0001] The invention relates to a hydroxylamine-oximation circulation system, in particular to a hydroxylamine-oximation circulation system for producing high-concentration hydroxylamine phosphate. Background technique [0002] The production of hydroxylamine in the industry is usually combined with other treatment methods for recycling, such as the hydroxylamine-oximation cycle system, which uses phosphate as the inorganic treatment liquid, and uses nitric acid and hydrogen as raw materials to reduce nitrate ions to Hydroxylamine, the formed hydroxylamine is then oximated with cyclohexanone to form cyclohexanone oxime. Add nitric acid or absorb nitrous gas to the phosphate inorganic treatment solution after the oximation reaction to form nitric acid to increase the content of the required nitrate ion, and then enter the hydroxylamine reactor to prepare hydroxylamine. The reaction is shown in the following formula: [0003] Hydroxylamine reaction to produce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/14C07C249/08C07C251/44
Inventor 黄志达郑秀丽罗守礼
Owner CHINA PETROCHEM DEVMENT
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