CN109437248B - Method for joint production of soda ash and ammonium sulfate by using mirabilite and ammonium bicarbonate as raw materials - Google Patents
Method for joint production of soda ash and ammonium sulfate by using mirabilite and ammonium bicarbonate as raw materials Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/12—Preparation of carbonates from bicarbonates or bicarbonate-containing product
- C01D7/126—Multi-step processes, e.g. from trona to soda ash
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- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
- C01C1/244—Preparation by double decomposition of ammonium salts with sulfates
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/02—Preparation by double decomposition
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Abstract
The invention belongs to the technical field of chemical processes, and particularly relates to a method for jointly producing sodium carbonate and ammonium sulfate by using mirabilite and ammonium bicarbonate as raw materials. The method comprises the steps of simultaneously adding ammonium bicarbonate, sodium sulfate and water into a reactor for mixing reaction, namely generating sodium bicarbonate crystals, carrying out vacuum filtration, washing and centrifugal dehydration on the sodium bicarbonate crystals to obtain a filter cake which is a wet sodium bicarbonate material, delivering the wet sodium bicarbonate material to a calcination working section for calcination to obtain a soda product, and delivering filtered mother liquor to a subsequent working section for treatment. The conversion rate of sodium sulfate in the method reaches more than 75 percent, the average particle size of the obtained wet material of sodium bicarbonate is 100-230 mu m, the moisture content is lower than 5 percent, the energy consumption of subsequent working sections is reduced, and the salt content of the obtained soda ash is less than 0.1 percent.
Description
Technical Field
The invention belongs to the technical field of chemical processes, and particularly relates to a method for jointly producing sodium carbonate and ammonium sulfate by using mirabilite and ammonium bicarbonate as raw materials.
Background
The soda ash is a basic raw material of a plurality of industries, is widely applied to daily life of people and industrial departments of chemical industry, light industry, metallurgy, textile, building materials and the like, and plays an important role in the development and construction process of national economy.
Before 18 th century, the alkali needed by people was obtained from trona because of the absence of alkali-making industry in the world, and in 1791, the French doctor Rubus was successful in researching "Rubus by calcining sodium sulfate, coal and limestone. In 1863, belgian engineers solvay improved based on comprehensive predecessor work, and realized that soda ash (namely ammonia-soda process) was produced by the "solvay process". The ammonia-soda process has the advantages of low price of raw materials, generally easy obtaining, high product purity, suitability for large-scale production and the like compared with the Loulan process, so the Loulan process is replaced and widely adopted up to now, production enterprises are generally distributed in coastal areas because the ammonia-soda process generates a large amount of calcium chloride-containing waste water, and the conversion rate of sodium chloride in the ammonia-soda process can only reach 72-76 percent, and 24-28 percent of sodium ions and almost all chloride ions are abandoned. In 1943, Houdenbang in China developed a combined soda process by developing soda test research, two products of soda and ammonium chloride can be produced simultaneously, raw materials are fully utilized, production cost is reduced, and the superiority of large-scale combined production is reflected.
At present, the total production capacity of soda production devices in China is nearly 3000 ten thousand tons, except for trona, the main production methods are an ammonia-soda method and a combined soda method, and all raw materials are sodium chloride. The total reserve volume of mirabilite which is proved in China at present is about 200 hundred million tons (calculated by anhydrous sodium sulfate) and is the first in the world, the output and sale volume of the mirabilite in China is the first in the world and accounts for about 70 percent, and the mirabilite is mainly used in the industries of detergents and sodium sulfide and is used in the industries of paper pulp, artificial fiber and glass. At present, the mirabilite production capacity reaches 1200 ten thousand tons and the output is 980 ten thousand tons in China, while the domestic demand is only about 800 ten thousand tons, and the excess production capacity is serious. In a word, mirabilite resources in China are very rich, and the market capacity of sodium sulfate is limited, so that the research significance of strengthening comprehensive utilization of mirabilite resources in China is great and promising.
Researchers at home and abroad have been exploring new ways for preparing alkali from mirabilite for many years. A series of experimental researches on sodium sulfate alkali preparation are successively carried out in China, but various problems of high byproduct yield, complex process, high energy consumption, low sodium sulfate conversion rate and the like exist, so that no industrial achievement exists all the time.
Disclosure of Invention
The invention aims to solve the technical problems and provides a method for jointly producing sodium carbonate and ammonium sulfate by taking mirabilite and ammonium bicarbonate as raw materials. The method improves the conversion rate of sodium sulfate by designing a reasonable process flow, obtains the sodium bicarbonate product with large granularity, high purity and low salt content, ensures that the sodium sulfate is used as the raw material to prepare the sodium carbonate, has excellent economic benefit, provides a new raw material source for the production of the sodium carbonate, and provides a new way for the comprehensive utilization of the sodium sulfate.
In order to achieve the above purpose, the specific technical scheme of the invention is as follows:
a method for jointly producing sodium carbonate and ammonium sulfate by taking mirabilite and ammonium bicarbonate as raw materials comprises the following steps:
(1) adding ammonium bicarbonate, sodium sulfate and water into a premixing tank with a stirrer at the same time, and carrying out primary reaction on the materials in the premixing tank to generate sodium bicarbonate crystals, wherein the mass ratio of the water to the ammonium bicarbonate, the water to the sodium sulfate is 1: 0.6-1.5: 0.6 to 1.5, the retention time of the materials in the premixing tank is 0.5 to 2 hours, and the temperature of the premixing tank is 20 to 40 ℃.
(2) And (2) feeding the mixed material in the step (1) into a reaction crystallizer, further reacting the material to grow sodium bicarbonate crystals, wherein the temperature of the reaction crystallizer is 30-60 ℃, the pressure is 0.1-0.6MPa, and the reaction time is 0.5-2 h.
(3) And (3) conveying the mixed material in the step (2) to a vacuum belt filter for vacuum dehydration, washing for multiple times in a subarea manner, and washing off the salt on the surface of the sodium bicarbonate. When the vacuum belt filter is used for filtering the sodium bicarbonate slurry, the solid materials are washed in different areas, the washing water in the five areas is desalted water, the washing water in the four areas is the filtrate of the centrifuge in the rear working section, the washing water in the three areas is the filtrate in the five areas, and the filtrate in the three areas and the filtrate in the four areas are mixed and then washed with the materials in the two areas.
(4) And (4) conveying the sodium bicarbonate slurry obtained in the step (3) to a centrifugal machine for centrifugal dehydration, wherein a filter cake is a sodium bicarbonate wet material, and filtering mother liquor is returned to a vacuum belt filter to be used as washing water for washing the sodium bicarbonate wet material.
(5) And (4) sending the wet sodium bicarbonate material in the step (4) to a drying section to prepare baking soda or sending the wet sodium bicarbonate material to a calcining section to prepare sodium carbonate.
(6) And (5) sending the filtered mother liquor in the step (5) to a subsequent working section for treatment.
The positive effects of the invention are as follows:
the method for jointly producing the soda ash and the ammonium sulfate by taking the mirabilite and the ammonium bicarbonate as the raw materials has the advantages that the conversion rate of the sodium sulfate reaches over 75 percent, the highest conversion rate of the sodium sulfate in the traditional method is only 65 percent, and the method has short flow, less equipment and easy operation.
The invention relates to a method for jointly producing sodium carbonate and ammonium sulfate by taking mirabilite and ammonium bicarbonate as raw materials, a crystallization reactor is used in the reaction process, the average particle size of the obtained wet sodium bicarbonate material can reach 230 mu m, the particle structure is compact, the surface is smooth, the wet sodium bicarbonate material does not contain wrapping mother liquor, the product purity is high, and the wet sodium bicarbonate material can be calcined into sodium carbonate or directly dried into baking soda.
The method for jointly producing the soda ash and the ammonium sulfate by taking the mirabilite and the ammonium bicarbonate as the raw materials has the advantages that the moisture content of the obtained wet material of the sodium bicarbonate is below 5 percent, the energy consumption of the subsequent working section is reduced, the salt content in the soda ash is also reduced, and the salt content in the product is less than 0.1 percent.
Drawings
FIG. 1 is a flow chart of the process for jointly producing soda ash by using mirabilite and ammonium bicarbonate as raw materials.
Detailed Description
In order to make the disclosure of the present invention more comprehensible, the self-sintered carbon graphite sealing material and the preparation method thereof are further described in the following with reference to specific embodiments. It should not be understood that the scope of the above-described subject matter of the present invention is limited to the following examples.
Unless otherwise specified,% "in the present invention means the mass percentage, i.e., wt%.
Example 1:
the present embodiment provides a method for producing soda ash by using mirabilite and ammonium bicarbonate as raw materials, wherein the flow chart is shown in fig. 1, and the specific steps are as follows:
(1) simultaneously adding ammonium bicarbonate, sodium sulfate and water into a premixing tank with a stirrer, and carrying out primary reaction on the materials in the premixing tank to generate sodium bicarbonate crystals, wherein the mass ratio of the water to the ammonium bicarbonate to the sodium sulfate is 1:1.1:0.9, the retention time of the materials in the premixing tank is 1h, and the temperature of the premixing tank is 25 ℃;
(2) feeding the mixed material (including sodium bicarbonate crystals) in the step (1) into a reaction crystallizer, and further reacting the material to grow the sodium bicarbonate crystals, wherein the temperature of the reaction crystallizer is 45 ℃, the pressure is 0.3MPa, and the reaction time is 1 h;
(3) and (4) conveying the material discharged from the reaction crystallizer to a vacuum belt filter for vacuum dehydration, washing for multiple times in a subarea manner, and washing to remove salt on the surface of the sodium bicarbonate. Wherein, the washing water in the fifth area is desalted water, the washing water in the fourth area is the filtrate of a centrifuge in the rear working section, the washing water in the third area is the filtrate in the fifth area, and the filtrate in the third area and the filtrate in the fourth area are mixed and then the materials in the second area are washed;
(4) sending the sodium bicarbonate slurry obtained in the step (3) to a centrifuge for centrifugal dehydration to obtain a sodium bicarbonate wet material with the water content of 3.5 percent, wherein the average particle size of the wet material is 187 mu m, and returning the filtered mother liquor to a vacuum belt filter to be used as washing water for washing the sodium bicarbonate wet material;
(5) the wet sodium bicarbonate material is sent to a calcination working section, and calcined to obtain soda ash, wherein the purity of the soda ash is 99.6 percent, and the salt content is 0.08 percent;
(6) the vacuum filter filters the mother liquor and sends the mother liquor to the subsequent working section for processing, and the conversion rate of the sodium sulfate can be calculated to be 74.5 percent according to the components of the mother liquor.
Example 2
The embodiment provides a method for producing soda ash by using mirabilite and ammonium bicarbonate as raw materials, as shown in fig. 1, the specific steps are as follows:
(1) simultaneously adding ammonium bicarbonate, sodium sulfate and water into a premixing tank with a stirrer, and carrying out primary reaction on the materials in the premixing tank to generate sodium bicarbonate crystals, wherein the mass ratio of the water to the ammonium bicarbonate to the sodium sulfate is 1:1:1, the retention time of the materials in the premixing tank is 0.5h, and the temperature of the premixing tank is 30 ℃;
(2) feeding the mixed material into a reaction crystallizer, further reacting the material to grow sodium bicarbonate crystals, wherein the temperature of the reaction crystallizer is 50 ℃, the pressure is 0.3MPa, and the reaction time is 0.5 h;
(3) discharging the reaction crystallizer, conveying the discharged material to a vacuum belt filter for vacuum dehydration, washing the discharged material for multiple times in a subarea manner, and washing off salt on the surface of the sodium bicarbonate; wherein, the washing water in the fifth area is desalted water, the washing water in the fourth area is the filtrate of a centrifuge in the rear working section, the washing water in the third area is the filtrate in the fifth area, and the filtrate in the third area and the filtrate in the fourth area are mixed and then the materials in the second area are washed;
(4) conveying the sodium bicarbonate slurry to a centrifuge for centrifugal dehydration to obtain a sodium bicarbonate wet material with the water content of 3.8 percent, wherein the average particle size of the wet material is 211 mu m, and returning filtered mother liquor to a vacuum belt filter to be used as washing water for washing the sodium bicarbonate wet material;
(5) the wet sodium bicarbonate material is sent to a calcination working section, and calcined to obtain soda ash, wherein the purity of the soda ash is 99.7 percent, and the salt content is 0.08 percent;
(6) the vacuum filter filters the mother liquor and sends the mother liquor to the subsequent working section for processing, and the conversion rate of the sodium sulfate can be calculated to be 75.3 percent according to the components of the mother liquor.
Example 3:
the embodiment provides a method for producing soda ash by using mirabilite and ammonium bicarbonate as raw materials, as shown in fig. 1, the specific steps are as follows:
(1) simultaneously adding ammonium bicarbonate, sodium sulfate and water into a premixing tank with a stirrer, and carrying out primary reaction on the materials in the premixing tank to generate sodium bicarbonate crystals; wherein the mass ratio of the water to the ammonium bicarbonate to the sodium sulfate is 1:1.2:1, the retention time of the materials in the premixing tank is 1.5h, and the temperature of the premixing tank is 30 ℃;
(2) feeding the mixed material into a reaction crystallizer, further reacting the material to grow sodium bicarbonate crystals, wherein the temperature of the reaction crystallizer is 60 ℃, the pressure is 0.5MPa, and the reaction time is 1 h;
(3) discharging the reaction crystallizer, conveying the discharged material to a vacuum belt filter for vacuum dehydration, washing the discharged material for multiple times in a subarea manner, and washing off salt on the surface of the sodium bicarbonate; wherein, the washing water in the fifth area is desalted water, the washing water in the fourth area is the filtrate of a centrifuge in the rear working section, the washing water in the third area is the filtrate in the fifth area, and the filtrate in the third area and the filtrate in the fourth area are mixed and then the materials in the second area are washed;
(4) sending the sodium bicarbonate slurry to a centrifuge for centrifugal dehydration to obtain a sodium bicarbonate wet material with the water content of 4.0 percent, wherein the average particle size of the wet material is 226 mu m; returning the filtered mother liquor to a vacuum belt filter to be used as washing water for washing a sodium bicarbonate wet material;
(5) the wet sodium bicarbonate material is sent to a baking soda drying section and dried to obtain baking soda, wherein the purity of the baking soda is 99.3 percent, and the salt content is 0.09 percent;
(6) the vacuum filter filters the mother liquor and sends the mother liquor to the subsequent working section for processing, and the conversion rate of the sodium sulfate can be calculated to be 74.8 percent according to the components of the mother liquor.
Example 4:
the embodiment provides a method for producing soda ash by using mirabilite and ammonium bicarbonate as raw materials, as shown in fig. 1, the specific steps are as follows:
(1) simultaneously adding ammonium bicarbonate, sodium sulfate and water into a premixing tank with a stirrer, and carrying out primary reaction on the materials in the premixing tank to generate sodium bicarbonate crystals, wherein the mass ratio of the water to the ammonium bicarbonate to the sodium sulfate is 1:1.2:0.5, the retention time of the materials in the premixing tank is 1h, and the temperature of the premixing tank is 28 ℃;
(2) feeding the mixed material into a reaction crystallizer, further reacting the material to grow sodium bicarbonate crystals, wherein the temperature of the reaction crystallizer is 55 ℃, the pressure is 0.5MPa, and the reaction time is 1 h;
(3) discharging the reaction crystallizer, conveying the discharged material to a vacuum belt filter for vacuum dehydration, washing the discharged material for multiple times in a subarea manner, and washing off salt on the surface of the sodium bicarbonate; wherein, the washing water in the fifth area is desalted water, the washing water in the fourth area is the filtrate of a centrifuge in the rear working section, the washing water in the third area is the filtrate in the fifth area, and the filtrate in the third area and the filtrate in the fourth area are mixed and then the materials in the second area are washed;
(4) sending the sodium bicarbonate slurry to a centrifuge for centrifugal dehydration to obtain a sodium bicarbonate wet material with the moisture content of 3.8 percent, wherein the average particle size of the wet material is 203 mu m; returning the filtered mother liquor to a vacuum belt filter to be used as washing water for washing a sodium bicarbonate wet material;
(5) the wet sodium bicarbonate material is sent to a baking soda drying section and dried to obtain baking soda, wherein the purity of the baking soda is 99.3 percent, and the salt content is 0.09 percent;
(6) the vacuum filter filters the mother liquor and sends the mother liquor to the subsequent working section for treatment, and the conversion rate of the sodium sulfate is only 64.1 percent due to the overhigh proportion of water and the sodium sulfate in the reaction.
Example 5:
the embodiment provides a method for producing soda ash by using mirabilite and ammonium bicarbonate as raw materials, as shown in fig. 1, the specific steps are as follows:
(1) simultaneously adding ammonium bicarbonate, sodium sulfate and water into a premixing tank with a stirrer, and carrying out primary reaction on the materials in the premixing tank to generate sodium bicarbonate crystals, wherein the mass ratio of the water to the ammonium bicarbonate to the sodium sulfate is 1:1.2:1, the retention time of the materials in the premixing tank is 10min, and the temperature of the premixing tank is 28 ℃;
(2) feeding the mixed material into a reaction crystallizer, further reacting the material to grow sodium bicarbonate crystals, wherein the temperature of the reaction crystallizer is 60 ℃, the pressure is 0.5MPa, and the reaction time is 20 min;
(3) discharging the reaction crystallizer, conveying the discharged material to a vacuum belt filter for vacuum dehydration, washing the discharged material for multiple times in a subarea manner, and washing off salt on the surface of the sodium bicarbonate; wherein, the washing water in the fifth area is desalted water, the washing water in the fourth area is the filtrate of a centrifuge in the rear working section, the washing water in the third area is the filtrate in the fifth area, and the filtrate in the third area and the filtrate in the fourth area are mixed and then the materials in the second area are washed;
(4) sending the sodium bicarbonate slurry to a centrifuge for centrifugal dehydration to obtain a sodium bicarbonate wet material with the water content of 12.4 percent, wherein the average particle size of the wet material is 83 mu m; returning the filtered mother liquor to a vacuum belt filter to be used as washing water for washing a sodium bicarbonate wet material;
(5) the wet sodium bicarbonate material is sent to a calcination working section, and calcined to obtain sodium carbonate, wherein the purity of the sodium carbonate is 99.4 percent, and the salt content is 0.28 percent;
(6) the vacuum filter filters the mother liquor and sends the mother liquor to the subsequent working section for treatment, and the conversion rate of the sodium sulfate is only 73.3 percent calculated by the components of the mother liquor.
The above examples are merely illustrative for clarity and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (1)
1. A method for producing soda ash and ammonium sulfate by using mirabilite and ammonium bicarbonate as raw materials is characterized by comprising the following steps:
(1) simultaneously adding ammonium bicarbonate, sodium sulfate and water into a premixing tank with a stirrer, and carrying out primary reaction on the materials in the premixing tank to generate sodium bicarbonate crystals; the mass ratio of water, ammonium bicarbonate and sodium sulfate is 1: 0.6-1.2: 0.9-1.5; the retention time of the mixed materials in the premixing tank is 0.5h, and the temperature of the premixing tank is 30 ℃;
(2) feeding the mixed material containing sodium bicarbonate crystals obtained in the step (1) into a reaction crystallizer for further reaction to grow sodium bicarbonate crystals; the temperature of the reaction crystallizer is 50 ℃, the pressure is 0.3MPa, and the reaction time is 0.5 h;
(3) conveying the mixed material in the step (2) to a vacuum belt filter for vacuum dehydration, washing for multiple times in a subarea manner, and washing off salt on the surface of sodium bicarbonate, wherein the washing water is desalted water;
(4) conveying the sodium bicarbonate slurry obtained in the step (3) to a centrifugal machine for centrifugal dehydration, wherein a filter cake is a wet sodium bicarbonate material, and filtering mother liquor to return to a vacuum belt filter to be used as washing water for washing the wet sodium bicarbonate material;
(5) sending the wet sodium bicarbonate material in the step (4) to a drying section, and drying to obtain baking soda; or the calcined soda is sent to a calcination working section and calcined to obtain soda;
(6) the vacuum filtration mother liquor in the step (4) is sent to a subsequent working section for treatment;
washing the solid materials in the vacuum belt filter in the step (3) in a subarea mode when filtering the sodium bicarbonate slurry, wherein five-area washing water is desalted water, four-area washing water is filtrate of a centrifuge in a rear working section, three-area washing water is filtrate of the five areas, and the second-area materials are washed after the three-area filtrate and the four-area filtrate are mixed; the sodium bicarbonate filtered by the vacuum belt filter in the step (4) is sent to a centrifuge for centrifugal dehydration, a filter cake is a sodium bicarbonate wet material, and a filtrate is used as washing water to wash materials in four areas of the vacuum filter; the conversion rate of the sodium sulfate reaches over 75 percent.
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| CN1091395A (en) * | 1994-01-19 | 1994-08-31 | 李兴德 | The method of soda production from sodium sulfate |
| US5830422A (en) * | 1995-06-23 | 1998-11-03 | Ormiston Mining And Smelting Co. Ltd. | Method for production of sodium bicarbonate, sodium carbonate and ammonium sulfate from sodium sulfate |
| US7393378B2 (en) * | 2003-02-11 | 2008-07-01 | Airborne Industrial Minerals Inc. | Method for recovering purified sodium bicarbonate and ammonium sulfate |
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