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A kind of method that glauberite prepares sodium bicarbonate by-product ammonium sulfate and calcium carbonate

A sodium bicarbonate and glauberite technology, applied in chemical instruments and methods, calcium carbonate/strontium/barium, ammonium sulfate, etc., can solve problems such as sales difficulties, low utilization rate of sodium ions and sulfate radicals, and complicated processes , achieving significant economic and environmental benefits, resource utilization, and simple processes

Active Publication Date: 2022-03-04
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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Problems solved by technology

However, due to the low conversion rate of sodium sulfate metathesis reaction, the utilization rate of sodium sulfate is less than 60%, and it is impossible to obtain ammonium sulfate with pure phase, the cost is high, so the technology of sodium sulfate to prepare soda ash is at a standstill
Some studies have added organic amines to the reaction system of sodium sulfate to prepare sodium carbonate to promote the metathesis reaction. This method can increase the conversion rate to more than 90%, but because the organic amine is easily soluble in water, it is extremely difficult to separate, and Due to the residue of organic matter in ammonium sulfate and sodium carbonate, the loss of organic amine is large, the cost is high, and the product quality is low
[0005] CN101544385A discloses a kind of method that takes sodium sulfate as raw material and supplements organic amine to prepare sodium carbonate to co-produce calcium sulfate, described method can realize the conversion rate of sodium reaches more than 90%, but organic amine has high boiling point, high viscosity, evaporation recovery energy The consumption is high, and the entrainment of organic amine in sodium bicarbonate and calcium sulfate is much, the recovery is difficult, the loss is large, and the production cost is high
[0006] CN104355326A, CN102198953A and CN202016881U all disclose a method for preparing sodium bicarbonate and co-producing ammonium sulfate by metathesis. Using sodium sulfate and ammonium bicarbonate as raw materials, sodium bicarbonate is obtained through metathesis, and the separated mother liquor is deaminated at high temperature. Evaporate and concentrate at 130°C to obtain sodium sulfate crystals. After separation, the mother liquor is cooled and crystallized to obtain the double salt of sodium sulfate and ammonium sulfate. The mother liquor is then evaporated and crystallized to obtain ammonium sulfate products. However, the process of the method is complicated and requires multiple high temperatures, cooling, etc. process, high energy consumption, low utilization rate of sodium ions and sulfate radicals, large evaporation depth, large material circulation, high production cost, and no industrialized precedent at present
[0007] CN105000579A and CN105712382A all disclose a kind of precipitation method, and this method prepares sodium bicarbonate by double decomposition reaction of ammonium bicarbonate and sodium sulfate, then adds lime in sodium bicarbonate mother liquor, reclaims wherein ammonia, but in this process ammonia The recovery rate is only about 50%, resulting in waste of resources and increased operating costs, and the by-product calcium sulfate has a large output, low value, and poor quality, which makes it difficult to sell and easily causes secondary pollution

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  • A kind of method that glauberite prepares sodium bicarbonate by-product ammonium sulfate and calcium carbonate

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Effect test

Embodiment 1

[0050] Present embodiment provides a kind of method that Glauber's salt prepares sodium bicarbonate by-product ammonium sulfate and calcium carbonate, as figure 1 As shown, the method includes the following steps:

[0051] (1) Introduce carbon dioxide with a concentration of 90vol% into the salting-out mother liquor, conduct a calcification reaction at 32°C for 75 minutes, and filter to obtain sodium bicarbonate and sodium bicarbonate mother liquor;

[0052] (2) Pass ammonia gas into the sodium bicarbonate mother liquor obtained in step (1), and carry out an ammoniation reaction at 50° C. for 45 minutes to obtain the ammoniated mother liquor;

[0053] (3) According to the mass ratio of 2.4:1:3.6, mix the Glauber's salt raw material, sodium sulfate and the ammoniated mother liquor obtained in step (2), conduct a salting-out reaction at 32°C for 90 minutes, and pass the solid slurry obtained from the salting-out reaction into The cyclone is separated, and the first double salt ...

Embodiment 2

[0060] Present embodiment provides a kind of method that Glauber's salt prepares sodium bicarbonate by-product ammonium sulfate and calcium carbonate, as figure 1 As shown, the method includes the following steps:

[0061] (1) Introduce carbon dioxide with a concentration of 80vol% into the salting-out mother liquor, perform a calcification reaction at 30°C for 90 minutes, and filter to obtain sodium bicarbonate and sodium bicarbonate mother liquor;

[0062] (2) Pass ammonia gas into the sodium bicarbonate mother liquor obtained in step (1), and perform an ammoniation reaction at 40° C. for 60 minutes to obtain the ammoniated mother liquor;

[0063] (3) According to the mass ratio of 2.2:1:3.5, mix the Glauber's salt raw material, sodium sulfate and the ammoniated mother liquor obtained in step (2), conduct a salting-out reaction at 30°C for 120 minutes, and pass the solid slurry obtained from the salting-out reaction into The cyclone is separated, and the first double salt t...

Embodiment 3

[0070] Present embodiment provides a kind of method that Glauber's salt prepares sodium bicarbonate by-product ammonium sulfate and calcium carbonate, as figure 1 As shown, the method includes the following steps:

[0071] (1) Introduce carbon dioxide with a concentration of 70vol% into the salting-out mother liquor, conduct a calcification reaction at 35°C for 60 minutes, and filter to obtain sodium bicarbonate and sodium bicarbonate mother liquor;

[0072] (2) Pass ammonia gas into the sodium bicarbonate mother liquor obtained in step (1), and carry out an ammoniation reaction at 60° C. for 30 minutes to obtain the ammoniated mother liquor;

[0073] (3) According to the mass ratio of 2.5:1:3.8, mix the Glauber's salt raw material, sodium sulfate and the ammoniated mother liquor obtained in step (2), conduct a salting-out reaction at 35°C for 60 minutes, and pass the solid slurry obtained from the salting-out reaction into The cyclone is separated, and the first double salt ...

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Abstract

The invention provides a method for preparing sodium bicarbonate by-product ammonium sulfate and calcium carbonate from glauberite, specifically: (1) introducing carbon dioxide into the salting-out mother liquor for calcification reaction, and separating solid and liquid to obtain sodium bicarbonate and bicarbonate Sodium mother liquor; (2) Ammonia gas is passed into the sodium bicarbonate mother liquor for ammoniation reaction to obtain ammoniated mother liquor; (3) Glauber’s salt raw material, sodium sulfate and ammoniated mother liquor are mixed for salting-out reaction, solid-liquid separation, and obtained The first double salt, calcium carbonate and salting-out mother liquor; (4) Mix double salt and water for reaction, solid-liquid separation to obtain sodium sulfate and separation mother liquor; (5) Mix ammonium sulfate mother liquor and separation mother liquor for cooling crystallization, solid-liquid Separation to obtain the second double salt and crystallization mother liquor; (6) Evaporation and crystallization of the crystallization mother liquor, solid-liquid separation to obtain ammonium sulfate and ammonium sulfate mother liquor. The method uses glauberite as a raw material to prepare sodium bicarbonate, realizes high-value conversion of sodium sulfate and calcium sulfate, and solves the problem of glauberite tailings stockpiling.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering and environmental protection, and relates to a method for preparing sodium bicarbonate, in particular to a method for preparing sodium bicarbonate by-product ammonium sulfate and calcium carbonate from glauberite. Background technique [0002] As a mineral resource rich in sodium sulfate and calcium sulfate, glauberite is an important raw material for the preparation of anhydrous sodium sulfate. China has abundant glauberite reserves. The traditional mining method is to extract sodium sulfate from it by dissolving it in water, and then produce sodium sulfate, but the calcium sulfate cannot be effectively utilized and is mainly stockpiled. In addition, due to the small application fields of anhydrous sodium sulfate, and the impact of industrial by-product sodium sulfate and the impact of reduced demand from downstream industries, the market demand has gradually shrunk. In order to rea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F11/18C01D7/00C01C1/24
CPCC01F11/18C01D7/00C01C1/24C01P2006/80
Inventor 张洋范兵强张贺东申长帅郑诗礼曹宏斌陈沛松
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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