CN113003595A - Method for separating calcium salt by alkali residue pretreatment - Google Patents

Method for separating calcium salt by alkali residue pretreatment Download PDF

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Publication number
CN113003595A
CN113003595A CN202110198916.2A CN202110198916A CN113003595A CN 113003595 A CN113003595 A CN 113003595A CN 202110198916 A CN202110198916 A CN 202110198916A CN 113003595 A CN113003595 A CN 113003595A
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China
Prior art keywords
caustic sludge
water
dechlorinated
calcium salt
slurry
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CN202110198916.2A
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贾志军
郭强
刘国振
贺佩
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Hebei Zhongke Tongchuang Technology Development Co ltd
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Hebei Zhongke Tongchuang Technology Development Co ltd
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Publication of CN113003595A publication Critical patent/CN113003595A/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/18—Carbonates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/46—Sulfates

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention provides a method for separating calcium salt by alkali residue pretreatment, belonging to the technical field of solid waste treatment. According to the invention, the caustic sludge is subjected to water leaching, chlorine-containing salts such as sodium chloride and potassium chloride in the caustic sludge can be dissolved in water to form water-soluble salts, the filtered filtrate can be crystallized to obtain corresponding chlorine salts, and the dechlorinated caustic sludge is obtained after removal. The alkaline residue pretreatment separation method provided by the invention is simple in process, easy to operate and suitable for industrial production.

Description

Method for separating calcium salt by alkali residue pretreatment
Technical Field
The invention relates to the technical field of solid waste treatment, in particular to a method for separating calcium salt by alkali residue pretreatment.
Background
In the industrial process of producing soda by an ammonia-soda process, a large amount of caustic sludge can be generated, the main components of the caustic sludge comprise calcium salt waste residues such as calcium carbonate, calcium sulfate, calcium chloride and the like, and also comprise components such as magnesium hydroxide, chloride, a small amount of sulfur dioxide and the like. Therefore, how to effectively utilize the alkaline residue and apply the alkaline residue to industrial production becomes a problem which needs to be solved urgently at present.
At present, aiming at different effective components and different purposes of soda ash residue, the recovery mode of soda residue can be roughly divided into: reclamation of land from sea, preparation of mortar modifier from soda residue, marine product cultivation and water quality modifier, preparation of building material from soda residue, preparation of compound fertilizer from soda residue, preparation of flue gas desulfurizer from soda residue, etc. (Wangzui et al, progress in the development and utilization of waste residue from soda production by ammonia-soda process [ J ]. soda industry, 2005 (6)). Calcium carbonate and calcium sulfate are used as important industrial raw materials and have wide industrial application, calcium salt is one of the main raw materials for preparing calcium carbonate, and if the calcium salt in the alkaline residue can be effectively converted into the calcium carbonate and the calcium sulfate under the condition of avoiding the adverse effects of other substances (such as corrosion of chloride and mixing of magnesium salts), the method has good environmental benefit and can add great economic benefit.
At present, researches on the industrial application of the alkaline residue mainly stay in the removal of chloride ions and the reuse of a mixed alkaline residue composition after chlorine removal, and no relevant documents report how to further separate the alkaline residue to obtain calcium carbonate and calcium sulfate and improve the product yield.
Disclosure of Invention
The invention aims to provide a method for separating calcium salt by pretreating alkaline residue, which can effectively separate calcium carbonate and calcium sulfate from the alkaline residue.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for separating calcium salt by alkaline residue pretreatment, which comprises the following steps:
soaking the caustic sludge in water, and filtering to obtain dechlorinated caustic sludge;
mixing the dechlorinated alkali residues with water to prepare slurry, and sorting the slurry through a concentrating table to obtain a calcium salt concentrate at a concentrate end; the calcium salt concentrate includes calcium carbonate and calcium sulfate.
Preferably, the alkaline residue is waste residue generated in the production of soda ash by an ammonia-soda process, and the content of calcium salt in the alkaline residue is 65-75 wt%.
Preferably, before the water leaching, the method further comprises crushing the caustic sludge, wherein the crushed caustic sludge is powdery.
Preferably, the mass ratio of the particles with the fineness of less than 200 meshes in the crushed alkaline residue is 60-70%.
Preferably, the water immersion is carried out under the condition of stirring, and the stirring time is 10-20 min.
Preferably, the water immersion temperature is 20-40 ℃.
Preferably, the mass ratio of water to alkaline residue in the water leaching is (2-3): 1.
preferably, the mass concentration of the dechlorinated alkali residues in the slurry is 25-35%.
Preferably, the stroke of the concentrating table is 8-12 mm.
Preferably, the inclination of the concentrating table is 3-5 degrees.
The invention provides a method for separating calcium salt by alkaline residue pretreatment, which comprises the following steps: soaking the caustic sludge in water, and filtering to obtain dechlorinated caustic sludge; and mixing the dechlorinated alkali residues with water to prepare slurry, sorting the slurry through a concentrating table to obtain calcium salt concentrate at a concentrate end, wherein the calcium salt concentrate comprises calcium carbonate and calcium sulfate.
According to the invention, the caustic sludge is subjected to water leaching, chlorine-containing salts such as sodium chloride and potassium chloride in the caustic sludge can be dissolved in water to form water-soluble salts, the filtered filtrate can be crystallized to obtain corresponding chlorine salts, and the dechlorinated caustic sludge is obtained after removal.
The alkaline residue pretreatment separation method provided by the invention is simple in process, easy to operate and suitable for industrial production.
Drawings
FIG. 1 is a flow chart of the method for separating calcium salt by alkaline residue pretreatment.
Detailed Description
The invention provides a method for separating calcium salt by alkaline residue pretreatment, which comprises the following steps:
soaking the caustic sludge in water, and filtering to obtain dechlorinated caustic sludge;
and mixing the dechlorinated alkali residues with water to prepare slurry, sorting the slurry through a concentrating table to obtain calcium salt concentrate at a concentrate end, wherein the calcium salt concentrate comprises calcium carbonate and calcium sulfate.
The invention carries out water leaching on the caustic sludge and obtains dechlorinated caustic sludge by filtering.
In the invention, the alkaline residue is preferably waste residue generated in the production of soda ash by an ammonia-soda process. In the invention, the main components of the caustic sludge are calcium salts (mainly comprising calcium carbonate and calcium sulfate), and other components comprise substances such as magnesium hydroxide, sodium chloride, potassium chloride and the like. In the invention, the content of the calcium salt in the alkaline residue is preferably 65-75 wt%, and more preferably 68-72%.
Before the water leaching, the invention preferably also comprises the step of crushing the caustic sludge, wherein the crushed caustic sludge is powdery. In the present invention, the crushing apparatus is preferably a small crusher. In the invention, the mass ratio of the particles with the fineness of less than 200 meshes in the alkali residue after crushing is 60-70%, and the preferable mass ratio is 65.3%. The invention aims to reduce the granularity of the alkaline residue by crushing the alkaline residue before water leaching, so that the alkaline residue is suitable for sorting by a shaking table.
In the invention, the water immersion temperature is preferably 20-40 ℃, and more preferably 25-35 ℃; the mass ratio of water to alkaline residue during water leaching is preferably (2-3): 1, more preferably (2.2 to 2.8): 1. in the invention, the water immersion is preferably carried out under stirring, and the stirring time is preferably 10-20 min, and more preferably 15 min. The present invention preferably performs said water immersion in a flotation cell. In the invention, the water leaching is used for dissolving sodium chloride and potassium chloride in the caustic sludge to form water-soluble chloride salt, and the water-soluble chloride salt is further removed through a subsequent filtering step, so that the dechlorination effect is achieved.
The filtration mode is not particularly limited in the invention, and the filtration mode can be realized by adopting the conventional filtration mode in the field. According to the invention, the alkali residue after water leaching is filtered to obtain a soluble salt solution and dechlorinated alkali residue, wherein the soluble salt solution can be used for extracting useful inorganic salt by a crystallization method, and the dechlorinated alkali residue is subjected to the next step of shaking table sorting.
After the dechlorinated alkali residues are obtained, the dechlorinated alkali residues and water are mixed to prepare slurry, the slurry is sorted by a concentrating table, and calcium salt enrichment is obtained at a concentrate end.
The preparation method of the slurry is not particularly limited, and a conventional method for preparing flotation slurry in the field is adopted, and the dechlorinated alkali residues are preferably dispersed in water and stirred to prepare the slurry; in the invention, the mass concentration of the dechlorinated alkaline residues in the slurry is preferably 25-35%, and more preferably 28-32%.
In the invention, the stroke of the concentrating table is preferably 8-12 mm, and more preferably 10 mm;
in the present invention, the inclination angle of the concentrating table is preferably 3 ° to 5 °, more preferably 3 ° or 5 °.
According to the density difference among the substances, the substances with different densities are distributed to different areas on the table concentrator, so that the calcium carbonate and the calcium sulfate with relatively higher densities are enriched at the concentrate end.
FIG. 1 is a flow chart of the method for separating calcium carbonate by alkaline residue pretreatment. Crushing caustic sludge, then soaking the crushed powdery caustic sludge in water, and filtering to obtain a soluble salt solution and dechlorinated caustic sludge; and mixing the dechlorinated alkali residues with water to prepare slurry, and sorting the slurry through a concentrating table to obtain enriched substances of calcium carbonate and calcium sulfate at a concentrate end.
The method for separating calcium carbonate by alkaline residue pretreatment according to the present invention will be described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
In the embodiment of the invention, the average content of calcium ions in the used caustic sludge is 195.13 mg/g.
Example 1
S1: smashing the caustic sludge into powder by using a small crusher, wherein the mass of particles with the fineness of less than 200 meshes accounts for 65.3%;
s2: soaking powdery caustic sludge in a flotation tank in water (the mass ratio of water to caustic sludge is 2:1.), stirring for 15min, filtering to obtain a soluble salt solution and dechlorinated caustic sludge, wherein the soluble salt solution is separately treated, and the dechlorinated caustic sludge enters the next process;
s3: mixing 5kg of dechlorinated alkaline residues with water to prepare slurry (the mass concentration of the dechlorinated alkaline residues in the slurry is 25%), sorting by a concentrating table, wherein the stroke of the table is set to be 8mm, the inclination angle is set to be 3 degrees, 1.96kg of calcium carbonate and calcium sulfate concentrates are obtained at a concentrate end, and the Ca concentration is detected by ICP2+The content was 327 mg/g.
Example 2
S1: smashing the caustic sludge into powder by using a small crusher, wherein the mass of particles with the fineness of less than 200 meshes accounts for 65.3%;
s2: soaking powdery caustic sludge in a flotation tank in water (the mass ratio of water to caustic sludge is 2:1), stirring for 15min, filtering to obtain a soluble salt solution and dechlorinated caustic sludge, wherein the soluble salt solution is separately treated, and the dechlorinated caustic sludge enters the next process;
s3: mixing 5kg of dechlorinated alkaline residues with water to prepare slurry (the mass concentration of the dechlorinated alkaline residues in the slurry is 30%), sorting by a concentrating table, wherein the stroke of the table is set to be 10mm, the inclination angle is set to be 3 degrees, 2.17kg of enriched calcium carbonate and calcium sulfate are obtained at the concentrate end, and the Ca content is detected by ICP2+The content was 319 mg/g.
Example 3
S1: smashing the caustic sludge into powder by using a small crusher, wherein the mass of particles with the fineness of less than 200 meshes accounts for 65.3%;
s2: soaking powdery caustic sludge in a flotation tank in water (the mass ratio of water to caustic sludge is 2:1), stirring for 15min, filtering to obtain a soluble salt solution and dechlorinated caustic sludge, wherein the soluble salt solution is separately treated, and the dechlorinated caustic sludge enters the next process;
s3: 5kg of dechlorinated alkali residues are taken and mixed with water to prepare slurry (the mass concentration of the dechlorinated alkali residues in the slurry is 35 percent), and the slurry is sorted by a concentrating tableWherein the stroke of the shaking table is set to be 12mm, the inclination angle is set to be 3 degrees, 2.28kg of enriched calcium carbonate and calcium sulfate are obtained at the concentrate end, and the Ca content is detected by ICP2+The content was 295 mg/g.
Example 4
S1: smashing the caustic sludge into powder by using a small crusher, wherein the mass of particles with the fineness of less than 200 meshes accounts for 65.3%;
s2: soaking powdery caustic sludge in a flotation tank in water (the mass ratio of water to caustic sludge is 2:1), stirring for 15min, filtering to obtain a soluble salt solution and dechlorinated caustic sludge, wherein the soluble salt solution is separately treated, and the dechlorinated caustic sludge enters the next process;
s3: mixing 5kg of dechlorinated alkaline residues with water to prepare slurry (the mass concentration of the dechlorinated alkaline residues in the slurry is 30%), sorting by a concentrating table, wherein the stroke of the table is set to be 10mm, the inclination angle is set to be 5 degrees, 1.92kg of enriched calcium carbonate and calcium sulfate are obtained at a concentrate end, and the Ca content is detected by ICP2+The content was 313 mg/g.
Comparative example 1
The difference from example 1 is only that the inclined angle of the table is set to 1 deg., and the Ca in the enriched calcium carbonate and calcium sulfate is obtained at the concentrate end2+The content was 282 mg/g.
From the results of example 1 and comparative example 1, it can be seen that the effect of calcium salt enrichment is reduced when the tilt angle of the table is increased beyond 3 to 5.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. The method for separating calcium salt by alkaline residue pretreatment is characterized by comprising the following steps:
soaking the caustic sludge in water, and filtering to obtain dechlorinated caustic sludge;
mixing the dechlorinated alkali residues with water to prepare slurry, and sorting the slurry through a concentrating table to obtain a calcium salt concentrate at a concentrate end; the calcium salt concentrate includes calcium carbonate and calcium sulfate.
2. The method according to claim 1, wherein the caustic sludge is waste residue generated in the production of soda ash by an ammonia-soda process, and the content of calcium salt in the caustic sludge is 65-75 wt%.
3. The method as claimed in claim 1, wherein before the water leaching, the method further comprises crushing caustic sludge, and the crushed caustic sludge is in powder form.
4. The method as claimed in claim 3, wherein the mass ratio of the particles with fineness less than 200 meshes in the alkali residue after crushing is 60-70%.
5. The method according to claim 1, wherein the water immersion is performed under stirring for 10 to 20 min.
6. The method according to claim 1, wherein the water immersion temperature is 20 to 40 ℃.
7. The method according to claim 1, wherein the mass ratio of water to caustic sludge in the water leaching is (2-3): 1.
8. the method according to claim 1, wherein the mass concentration of the dechlorinated caustic sludge in the slurry is 25-35%.
9. The method according to claim 1, wherein the stroke of the concentrating table is 8-12 mm.
10. A process according to claim 1 or 9, characterized in that the inclination of the concentrating table is 3 ° to 5 °.
CN202110198916.2A 2021-02-22 2021-02-22 Method for separating calcium salt by alkali residue pretreatment Withdrawn CN113003595A (en)

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Application Number Priority Date Filing Date Title
CN202110198916.2A CN113003595A (en) 2021-02-22 2021-02-22 Method for separating calcium salt by alkali residue pretreatment

Publications (1)

Publication Number Publication Date
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Application publication date: 20210622