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Method for recovering ammonium chloride by preparing complex salt of magnesium ammonium chloride hexahydrate

A technology of ammonium chloride hexahydrate and ammonium chloride, which is applied in the direction of ammonium halide and chloride preparation, etc., to achieve the effects of low energy consumption, reduced environmental impact, and simple methods

Inactive Publication Date: 2013-01-09
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to overcome the deficiencies of the prior art, in order to solve the problem of reclaiming ammonium chloride in the by-product ammonium chloride aqueous solution in the production process of fine magnesium products, and in order to save energy, reduce costs and increase economic benefits; thereby providing A kind of ammonium chloride aqueous solution and magnesium chloride (magnesium chloride brine, hydrated magnesium chloride or anhydrous magnesium chloride) with ammonium bicarbonate method or ammonium method or ammonium method precipitation magnesium process by-product are raw materials to prepare hexahydrate ammonium chloride magnesium, and the obtained hexahydrate chlorination Ammonium magnesium is decomposed at low temperature to obtain ammonium chloride and a magnesium-rich aqueous solution for ammonium bicarbonate method or ammonia method for magnesium precipitation. This method adopts the mother liquor circulation method, no waste liquid discharge and reduced environmental pollution

Method used

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  • Method for recovering ammonium chloride by preparing complex salt of magnesium ammonium chloride hexahydrate
  • Method for recovering ammonium chloride by preparing complex salt of magnesium ammonium chloride hexahydrate
  • Method for recovering ammonium chloride by preparing complex salt of magnesium ammonium chloride hexahydrate

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Embodiment 1

[0029] For the specific process flow of this embodiment, please refer to figure 1 .

[0030] The raw material ammonium chloride solution selected in this embodiment is a by-product in the magnesium precipitation process. Concentration is 6mol / L; Add 400ml of ammonium chloride solution into the crystallization kettle, adjust the pH=4 of ammonium chloride solution in the crystallization kettle with hydrochloric acid (15wt%), then add saturated magnesium chloride brine until the concentration of magnesium chloride in the crystallization kettle reaches 3mol / L ; Under the condition of controlling the temperature of the crystallization tank at 10° C., continue stirring for 120 minutes; after filtering, the solid obtained is dried to obtain 109 g of magnesium ammonium chloride hexahydrate. According to the ratio of 0.7:1 in the mass ratio of tap water to magnesium ammonium chloride hexahydrate, the obtained 109g of magnesium chloride ammonium chloride hexahydrate is added to a react...

Embodiment 2

[0032] For the specific process flow of this embodiment, please refer to figure 1 .

[0033] Add 800ml of magnesium chloride by-product ammonium chloride solution in the ammonium bicarbonate method or ammonia magnesium precipitation process into the crystallization tank, wherein the ammonium chloride solution concentration is 1mol / L, adjust the ammonium chloride solution with hydrochloric acid (5wt%) pH = 6, then add anhydrous magnesium chloride until the concentration of magnesium chloride in the crystallization tank reaches 5mol / L; under the condition of controlling the temperature of the crystallization tank at 80°C, continue stirring for 30 minutes; the filtered solid is dried to obtain 395g of magnesium ammonium chloride hexahydrate . According to the mass ratio of the ammonium chloride solution and magnesium ammonium chloride hexahydrate by-product of heavy magnesium chloride, the 395g magnesium chloride ammonium chloride hexahydrate obtained will be added into a contai...

Embodiment 3

[0035] For the specific process flow of this embodiment, please refer to figure 1 .

[0036]400ml of by-product ammonium chloride solution by the ammonium bicarbonate method or the ammonia method of magnesium precipitation and 200ml of the filtrate obtained after the decomposition of ammonium chloride magnesium hexahydrate and recovery of ammonium chloride in Example 2 are added to the crystallization kettle together, wherein the ammonium chloride Solution concentration is 3mol / L, then ammonium chloride solution is adjusted ammonium chloride solution pH=4.5 with hydrochloric acid (36wt%), then adds magnesium chloride hexahydrate until magnesium chloride concentration reaches 3.5mol / L in the crystallization kettle; Stirring was continued for 100 minutes under the condition of 40° C.; the solid obtained after filtration was dried to obtain 256 g of magnesium ammonium chloride hexahydrate. According to the mass ratio of ammonium chloride solution and ammonium chloride magnesium ...

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Abstract

The invention relates to a method for recovering ammonium chloride by preparing complex salt of magnesium ammonium chloride hexahydrate (HH4MgC13 6H2O). The method comprises the following steps of: placing aqueous solution of ammonium chloride into a crystallizing kettle; regulating the pH of the solution to 4 to 6 by hydrochloric acid; controlling the temperature of the crystallizing kettle in the range of 10 to 80 DEG C; adding magnesium chloride into the crystallizing kettle under the stirring condition, stopping adding the magnesium chloride when the concentration of the magnesium chloride in the solution reaches 3 to 5mol / L and then continuously stirring for 30 to 120 minutes; drying filtered solid to obtain magnesium ammonium chloride hexahydrate; and decomposing the magnesium ammonium chloride hexahydrate at a lower temperature of 0 to 50 DEG C to obtain solid of ammonium chloride. With the adoption of the method, no waste liquid is discharged in the whole process, and an ammonium chloride recovery process and a magnesium precipitating process are well integrated. The method has strong operability and is easy to realize industrialization.

Description

technical field [0001] The present invention relates to the preparation method of ammonium chloride, particularly a kind of ammonium chloride aqueous solution and magnesium chloride (magnesium chloride brine, hydrated magnesium chloride or anhydrous magnesium chloride) which are by-products of ammonium bicarbonate method or ammonia magnesium precipitation process are used as raw materials, prepared by crystallization Magnesium ammonium chloride hexahydrate double salt, and the method of decomposing the double salt at low temperature to obtain ammonium chloride and a magnesium-rich aqueous solution for magnesium precipitation. Background technique [0002] my country is rich in brine magnesium resources, and a large amount of magnesium mainly exists in seawater, salt lake water and well brine in the form of chloride. After the brine is extracted with sodium and potassium, a saturated aqueous solution rich in magnesium chloride or magnesium chloride hydrate can be obtained. I...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B9/02C01C1/16
Inventor 李志宝王道广
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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