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Method for preparing calcium carbonate and hydrogen chloride gas by mineralizing alkali-making distilled ammonia waste liquid

A technology of hydrogen chloride gas and ammonia distillation waste liquid, applied in the directions of chlorine/hydrogen chloride, calcium carbonate/strontium/barium, etc., can solve the problems of wasting resources and harming the environment, and achieves the realization of recycling, reliable and stable operation, and simple process flow. Effect

Inactive Publication Date: 2021-07-13
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the ammonia distillation waste liquid is discharged as waste after dilution, which not only wastes resources, but also seriously endangers the environment

Method used

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  • Method for preparing calcium carbonate and hydrogen chloride gas by mineralizing alkali-making distilled ammonia waste liquid
  • Method for preparing calcium carbonate and hydrogen chloride gas by mineralizing alkali-making distilled ammonia waste liquid
  • Method for preparing calcium carbonate and hydrogen chloride gas by mineralizing alkali-making distilled ammonia waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Calcium carbonate and hydrogen chloride gas are prepared by comprehensively utilizing the ammonia distillation waste liquid and carbon dioxide in the above method. Specifically:

[0044] Get 250ml containing 1mol / L Calcium Chloride Ammonia distillation waste liquid, 80ml industrial tertiary amine N235 as extraction agent, 120ml isoamyl alcohol as diluent in jacketed reactor, control stirring speed to be 200r / min, the The reactants were mixed evenly. The reaction temperature was controlled at 25° C., and carbon dioxide gas was introduced into the reaction system.

[0045] Depending on the progress of the reaction, different intake rates are controlled. Within 1 hour of the reaction, the intake rate is controlled to 50ml / min; The air intake rate was 5ml / min, and the reaction was stopped after 3.5 hours. The calcium carbonate powder was obtained by filtering solid-liquid separation, washed alternately with deionized water to remove entrained organic impurities and water...

Embodiment 2

[0048]Calcium carbonate and hydrogen chloride gas are prepared by comprehensively utilizing the ammonia distillation waste liquid and carbon dioxide in the above method. Specifically:

[0049] Take 150ml of alkali-making ammonia distillation waste liquid containing 1.5mol / L calcium chloride, 250ml of primary amine N1923 as extractant, 125ml of isopropanol, and 250ml of isoamyl alcohol as diluent in a jacketed reactor, and control the stirring speed to 300r / min to mix the reactants evenly. The reaction temperature was controlled at 30° C., and carbon dioxide gas was introduced into the reaction system.

[0050] According to the different progress of the reaction, different intake rates are controlled. Within 1 hour of the reaction, the intake rate is controlled to 55ml / min; The gas rate was 5ml / min, and the reaction was stopped after 3 hours. Through solid-liquid separation by filtration, calcium carbonate powder was obtained, washed alternately with deionized water to remo...

Embodiment 3

[0053] Calcium carbonate and hydrogen chloride gas are prepared by comprehensively utilizing the ammonia distillation waste liquid and carbon dioxide in the above method. Specifically:

[0054] Get 150ml containing 2mol / L Calcium Chloride Ammonia distillation waste liquid, 125ml industrial tertiary amine N235 as extractant and 125ml methyl isobutyl ketone as diluent in jacketed reactor, control stirring speed is 200r / min, The reactants were mixed well. The reaction temperature was controlled at 10° C., and carbon dioxide gas was introduced into the reaction system.

[0055] According to the different progress of the reaction, different intake rates are controlled. Within 1 hour of the reaction, the intake rate is controlled to 80ml / min; The gas rate was 6ml / min, and the reaction was stopped after 3 hours. Through solid-liquid separation by filtration, calcium carbonate powder was obtained, washed alternately with deionized water to remove entrained organic impurities and wa...

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Abstract

The invention provides a method for preparing calcium carbonate and hydrogen chloride gas by mineralizing alkali-making distilled ammonia waste liquid. The method comprises the following steps: (1) weighing the alkali-making distilled ammonia waste liquid, an extracting agent and a diluent, mixing in a reactor, and uniformly stirring; (2) introducing carbon dioxide in a bubbling form, controlling the reaction temperature to be 10-45 DEG C, and reacting for 3-5 hours; (3) after the reaction is finished, carrying out solid-liquid separation on a reaction system, and washing and drying a solid phase to obtain a calcium carbonate product; and standing and separating the liquid phase into a water phase and an organic phase; and (4) carrying out thermal decomposition reaction on the organic phase in the step (3) to obtain hydrogen chloride gas. According to the method, two wastes are coupled and cooperatively treated, and calcium carbonate and hydrogen chloride gas are prepared through mineralization reaction extraction crystallization coupling, so that the process is green and environment-friendly, and resource utilization is realized; and the whole technological process is simple, low in energy consumption, reliable and stable in operation, mild in technological condition and beneficial to industrial application.

Description

technical field [0001] The invention belongs to the technical field of resource utilization of soda-making waste liquid and carbon dioxide mineralization, and in particular relates to a method for preparing calcium carbonate and hydrogen chloride gas by mineralizing soda-making ammonia distillation waste liquid. Background technique [0002] my country is the world's largest soda ash-making country. In 2019, my country's soda ash production capacity reached 32.47 million tons, and the actual output was 28.87 million tons. It is estimated that by 2022, the production capacity of my country's soda ash industry will reach 34.47 million tons, of which the ammonia-soda production process accounts for about 49%. %. The ammonia-soda method has the characteristics of large production scale, and it needs to discharge a large amount of waste liquid, which is called ammonia distillation waste liquid. For every ton of soda ash produced, 8-11 cubic meters of ammonia distillation waste liq...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F11/18C01B7/01
CPCC01B7/01C01F11/18C01P2004/03C01P2004/60
Inventor 宋兴福刘程琳杨颖代超燕于建国
Owner EAST CHINA UNIV OF SCI & TECH
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