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Preparation method of hydroxylamine sulphate and devices used in preparation method

A technology of hydroxylamine sulfate and equipment is applied in the fields of pollution control and resource recovery and utilization, and can solve the problems of high raw material cost, complex process route and high cost of sulfur dioxide

Active Publication Date: 2016-07-06
BEIJING GUODIAN LONGYUAN ENVIRONMENTAL ENG +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese Patent Application No. 201010115879.6 discloses a method and system for recovering sulfur dioxide from flue gas and producing hydroxylamine sulfate. The method uses ammonia water to recover sulfur dioxide in flue gas to generate ammonium bisulfite, and then synthesizes hydroxylamine sulfate by Rashing oxidation method. The sulfur dioxide in the flue gas reduces the production cost of hydroxylamine, but the cost of recovering sulfur dioxide in the flue gas with ammonia water is

Method used

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  • Preparation method of hydroxylamine sulphate and devices used in preparation method
  • Preparation method of hydroxylamine sulphate and devices used in preparation method

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Embodiment 1

[0088] Step 1) Calcium salt conditioning: at 0°C, with a concentration of 30m% sulfuric acid solution, the pH value is 5, and the concentration sum of calcium bisulfite+calcium sulfite+sulfurous acid is 28m% calcium salt suspension The pH value was adjusted to 1.5.

[0089] Step 2) solution cooling: the temperature of the conditioned calcium salt suspension with a pH value of 1.5 is reduced to -5°C, and the temperature of the sodium nitrite solution with a concentration of 15m% is reduced to -5°C.

[0090] Step 3) solution mixing: the calcium salt suspension is added in the sodium nitrite solution, the mixing process is carried out under stirring, and the material ratio of the mixed solution is S in the calcium salt 4+ The molar ratio of (+4-valent sulfur) to nitrite is 2, the continuous heat exchange during the mixing process ensures that the temperature of the mixed solution is ≤0°C, and the solution temperature of the mixed solution after mixing is 0°C before adjusting the ...

Embodiment 2

[0095] Step 1) Calcium salt conditioning: at 0°C, with a concentration of 30m% sulfuric acid solution, the pH value is 5, and the concentration sum of calcium bisulfite+calcium sulfite+sulfurous acid is 28m% calcium salt suspension The pH value was adjusted to 1.5.

[0096]Step 2) Solution cooling: the temperature of the conditioned calcium salt suspension with a pH value of 1.5 is lowered to 0°C, and the temperature of the sodium nitrite solution with a concentration of 15m% is lowered to 0°C.

[0097] Step 3) solution mixing: the calcium salt suspension is added in the sodium nitrite solution, the mixing process is carried out under stirring, and the material ratio of the mixed solution is S in the calcium salt 4+ The molar ratio of (+4-valent sulfur) to nitrite is 2, and the heat exchange during the mixing process ensures that the temperature of the mixed solution is ≤0°C, and the solution temperature of the mixed solution after mixing is -2°C before the pH value is adjuste...

Embodiment 3

[0102] Step 1) Calcium salt conditioning: at 0°C, with a concentration of 30m% sulfuric acid solution, the pH value is 5, and the concentration sum of calcium bisulfite+calcium sulfite+sulfurous acid is 28m% calcium salt suspension The pH value was adjusted to 1.7.

[0103] Step 2) solution cooling: the temperature of the conditioned calcium salt suspension with a pH value of 1.7 is reduced to -1°C, and the temperature of the sodium nitrite solution with a concentration of 15m% is reduced to -1°C.

[0104] Step 3) solution mixing: the calcium salt suspension is added in the sodium nitrite solution, the mixing process is carried out under stirring, and the material ratio of the mixed solution is S in the calcium salt 4+ The molar ratio of (+4-valent sulfur) to nitrite is 2, and the heat exchange during the mixing process ensures that the temperature of the mixed solution is ≤0°C, and the solution temperature of the mixed solution after mixing is -1°C before the pH value is adju...

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Abstract

The invention provides a preparation method of hydroxylamine sulphate and devices used in the preparation method.The method includes the steps of calcium salt quenching and tempering, solution cooling, solution mixing, mixed solution PH value regulation and solution hydrolysis.Firstly, the PH value of a calcium salt solution or turbid liquid is regulated to 0.1-3.5 through acid; then, the calcium salt solution or the turbid liquid subjected to quenching and tempering and a solution containing nitrite are cooled to 10 DEG C or below respectively; the cooled calcium salt solution or the turbid liquid is mixed with the solution containing nitrite at the temperature of 10 DEG C or below; acid is added to the mixed solution to regulate the PH value of the solution to 0.1-3.5; finally, the solution or the turbid liquid is heated by 0.2-3 hours at a temperature smaller than 150 DEG C to obtain a solution containing hydroxylamine sulphate.The devices mainly include a calcium salt quenching and tempering cooling kettle, a disulfonate preparation reaction kettle and a hydrolysis reactor.The method is simple in process, mild in reaction condition and high in yield, and by-product resources obtained through coal-fired flue gas limestone wet desulphurization can be recycled and converted into hydroxylamine sulphate high in added value and wide in application range.

Description

technical field [0001] The invention belongs to the fields of pollution control and resource recycling, and in particular relates to a preparation method of hydroxylamine sulfate and equipment used therein. Background technique [0002] Hydroxylamine sulfate can be used for polymer synthesis, such as an important raw material for the synthesis of caprolactam, and can also be used for the synthesis of medicines and pesticides, such as for the production of isoxazole derivatives, sulfa drugs, vitamin B5, vitamin B12, acetone oxime, etc. It can be used as reducing agent, developer, rubber vulcanizing agent and building material adhesive, etc. The market price is more than 10,000 yuan / ton. It can be seen that hydroxylamine sulfate is a chemical raw material with wide application and high added value. [0003] The synthesis route of hydroxylamine sulfate mainly includes: Rashing oxidation method; nitric oxide reduction method; nitroalkane hydrolysis method; ketoxime hydrolysis me...

Claims

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Application Information

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IPC IPC(8): C01B21/14B01J19/26B01J19/18
CPCB01J19/0013B01J19/18B01J19/26B01J2219/00081C01B21/1427
Inventor 庄烨王洪亮刘科伟唐坚陈振宇
Owner BEIJING GUODIAN LONGYUAN ENVIRONMENTAL ENG
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