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Method for separating potassium chloride/ammonium chloride mixture by organic amine and ammonium chloride conversion

A technology of potassium ammonium chloride and organic amine, applied in the direction of ammonium halide, alkali metal halide purification, etc., can solve problems such as difficult separation of potassium chloride and ammonium chloride, and achieve excellent separation effect, high reaction conversion rate, economical obvious effect

Active Publication Date: 2012-09-19
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The object of the present invention is to solve the problem of co-precipitation of solid solutions in the crystallization of potassium chloride and ammonium chloride mixed solution, and to provide a production process for ammonium chloride and organic amines to react, convert and separate potassium chloride and ammonium chloride, in order to Solve the problem of difficult separation of potassium chloride and ammonium chloride

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Prepare 2mol / L ammonium chloride solution, take 50ml, the concentration of potassium ion and ammonium ion is 2mol / L, take 25ml (about 0.13mol) of tributylamine, and take 150ml of n-butanol and add it to the reactor, keep the temperature at 95°C Circulate water, pass condensed water (14°C), start stirring, set the stirring rate to 300 rpm, and give 4 hours to react. The substances produced by the reaction are tributylamine hydrochloride and ammonia gas, and the ammonia gas is introduced into 80 ml of water. After the reaction, the liquid was separated with a separating funnel for 30 minutes, and the volume of the organic phase was recorded as 208.5 ml, and the volume of the inorganic phase was 6.9 ml. Tributylamine hydrochloride exists in the diluent of the organic phase, and the inorganic phase is an ammonium chloride solution with an extremely low concentration that has not completely reacted. After analyzing the inorganic phase by chemical method, the conversion rate...

Embodiment 2

[0026] Prepare a mixed solution of potassium chloride and ammonium chloride. The concentration of potassium ions and ammonium ions is 2mol / L. Take 20ml, 20ml of triethylamine, and 20ml of isoamyl alcohol and add them to the reactor. Water (15°C), start stirring and set the stirring rate to 300 rpm, given 3 hours of reaction, the reaction products are triethylamine hydrochloride and ammonia gas, ammonia gas is introduced into 80ml of water. After the reaction, the reaction liquid was separated with a separating funnel for 30 minutes, and the volume of the organic phase was recorded as 42.8ml, and the volume of the inorganic phase was 23.5ml. After chemical analysis of the inorganic phase, the conversion rate of ammonium chloride obtained was 87.1% (calculated as ammonium ions). The organic phase was recovered with ammonia water for 4 h, separated again with a separatory funnel, and 38 ml of the upper organic phase was recovered, where the organic phase was triethylamine and iso...

Embodiment 3

[0028] Prepare a mixed solution of potassium chloride and ammonium chloride, the concentration of potassium ion and ammonium ion is 2mol / L, take 20ml, take 20ml of tripropylamine, and 40ml of isoamyl alcohol and add it to the reactor, control the constant temperature circulating water at 50°C, and pass the condensed water (15°C), turn on the stirring and set the stirring rate to 500 rpm, and react for 3 hours. The reaction product is tripropylamine hydrochloride and ammonia gas, and the ammonia gas is introduced into 80ml of water. After completion of the reaction, use a separatory funnel to stand still for 30 minutes to separate the liquid, record the volume of the organic phase as 57.4ml, and the volume of the inorganic phase as 15ml. The organic phase was recovered with ammonia water for 4 h, separated again with a separatory funnel, and 51 ml of the upper organic phase was recovered, where the organic phase was tripropylamine and isoamyl alcohol. The conversion of ammonium...

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PUM

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Abstract

The invention relates to a method for separating a potassium chloride / ammonium chloride mixture by organic amine and ammonium chloride conversion, which comprises the following steps: mixing organic amine, diluter and potassium chloride / ammonium chloride mixed solution, and stirring to react for 2-4 hours at 50-110 DEG C, wherein the mol ratio of the organic amine to the ammonium chloride is (1-2):1, the volume ratio of the diluter to the organic amine is (2-8):1, and the volume ratio of the sum of organic amine and diluter to the potassium chloride / ammonium chloride mixed solution is (2-5):1; leading out ammonia gas generated by the reaction to form ammonia water; after the reaction finishes, transferring the reaction liquid, and standing to stratify, wherein the organic amine hydrochloride exists in the supernatant organic phase diluter, and the understratum is mainly the potassium chloride solution; secondarily transferring the solution, and standing to stratify, wherein the supernatant is the recyclable organic phase, and the understratum is the ammonium chloride solution; and respectively crystallizing to separate potassium chloride / ammonium chloride. The invention has a far-reaching meaning for the potassium chloride / ammonium chloride mixed solution, prevents the ammonia gas from environmental pollution, and has the advantages of low temperature, energy saving and environmental protection.

Description

technical field [0001] The invention relates to a method for reacting organic amines and ammonium chloride and using the method to separate potassium chloride and ammonium chloride. Background technique [0002] my country is a large agricultural country, and the amount of potash fertilizer is in the forefront of the world. However, due to the shortage of land potash resources and the low self-sufficiency rate of potash fertilizer, most potash fertilizers depend on imports every year, which costs a lot. However, the total reserve of potassium in seawater reaches 550 trillion tons, which is 30,000 times that of the global total reserve of terrestrial potassium ore, and it is an inexhaustible potassium ore resource. Over the past century, many coastal countries in the world have invested a lot of manpower and material resources in researching the utilization technology of seawater potassium resources, and put forward hundreds of methods, but all failed to realize industrial pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D3/14C01C1/16
Inventor 陈建新袁俊生韩健李银辉卢爱党孙权
Owner HEBEI UNIV OF TECH