CN111302364A - Refining method and application of sodium carbonate - Google Patents

Refining method and application of sodium carbonate Download PDF

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Publication number
CN111302364A
CN111302364A CN202010122363.8A CN202010122363A CN111302364A CN 111302364 A CN111302364 A CN 111302364A CN 202010122363 A CN202010122363 A CN 202010122363A CN 111302364 A CN111302364 A CN 111302364A
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CN
China
Prior art keywords
sodium carbonate
carbonate
refining
concentration
ceramic membrane
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010122363.8A
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Chinese (zh)
Inventor
樊发英
唐志雷
邓小川
朱朝梁
卿彬菊
樊洁
史一飞
张毅
张文丁
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Qinghai Institute of Salt Lakes Research of CAS
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Qinghai Institute of Salt Lakes Research of CAS
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Priority to CN202010122363.8A priority Critical patent/CN111302364A/en
Publication of CN111302364A publication Critical patent/CN111302364A/en
Pending legal-status Critical Current

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Classifications

    • 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
    • C01D7/22—Purification
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/26—Carbonates or bicarbonates of ammonium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/08—Carbonates; Bicarbonates
    • 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
    • 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
    • C01F5/00—Compounds of magnesium
    • C01F5/24—Magnesium carbonates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G29/00—Compounds of bismuth

Abstract

The invention discloses a refining method of sodium carbonate and application thereof. The refining method comprises the following steps: mixing sodium carbonate to be refined with water to obtain a sodium carbonate solution; conveying the sodium carbonate solution to a separation assembly, and performing solid-liquid separation to obtain a liquid phase and a solid slurry, wherein the separation assembly comprises a ceramic membrane separation assembly; and concentrating and crystallizing the liquid phase to obtain the refined sodium carbonate. The method for continuously refining and removing the magnesium and the calcium from the sodium carbonate provided by the invention not only can realize deep removal of calcium and magnesium and obtain high-purity refined sodium carbonate, but also can realize continuous supply of a high-purity sodium carbonate solution.

Description

Refining method and application of sodium carbonate
Technical Field
The invention relates to a method for refining sodium carbonate, in particular to a method for pretreating refined sodium carbonate in the process of preparing carbonate and application thereof.
Background
Sodium carbonate is an important chemical raw material, and is often used for preparing carbonates such as lithium carbonate, calcium carbonate, magnesium carbonate and the like. However, industrial sodium carbonate usually contains certain impurities such as calcium ions and magnesium ions, which easily affect the quality of subsequent products. Especially, in the process of preparing high-purity lithium carbonate, the quality of lithium carbonate products is affected finally because the content of impurities such as magnesium, calcium and the like contained in sodium carbonate exceeds the standard. Therefore, the sodium carbonate solution needs to be refined to remove calcium and magnesium during the carbonate preparation process.
At present, the method for refining sodium carbonate mainly comprises a precipitation method, for example, sodium hydroxide is usually added in the refining of sodium carbonate solution, and then calcium and magnesium are removed by centrifugal separation, and patent CN109110786A discloses a method for removing trace calcium in the refining of sodium carbonate, and an ultrafiltration membrane is adopted. Furthermore, there are some conventional methods for removing calcium by centrifugation or pressure filtration, for example, CN103508469A discloses a method for purifying sodium carbonate solution in lithium carbonate production, but these methods are not easy to remove clean calcium or magnesium, and the operation is complicated, and the continuity and automation of production are not easy to achieve.
Disclosure of Invention
The invention aims to provide a refining method of sodium carbonate and application thereof, thereby overcoming the defects of the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a method for refining sodium carbonate, which comprises the following steps:
mixing sodium carbonate to be refined with water to obtain a sodium carbonate solution; or directly adopting a sodium carbonate solution (a solution without crystallization to remove sodium carbonate is also possible);
conveying the sodium carbonate solution to a separation assembly, and performing solid-liquid separation to obtain a liquid phase and a solid slurry, wherein the separation assembly comprises a ceramic membrane separation assembly;
and concentrating and crystallizing the liquid phase to obtain the refined sodium carbonate.
In some preferred embodiments, the sodium carbonate to be refined comprises Ca2+、Mg2+、Ba2+And the like, but is not limited thereto.
In some preferred embodiments, the concentration of the sodium carbonate solution is 0.01 to 10mol/L (or 1g/L to 500 g/L).
In some preferred embodiments, the method for refining sodium carbonate comprises: heating the sodium carbonate solution to 10-95 ℃, and conveying the sodium carbonate solution to a ceramic membrane separation assembly with the temperature of 10-95 ℃.
Furthermore, the aperture of the separation membrane in the ceramic membrane separation component is 2-200 nm.
In some preferred embodiments, the number of the ceramic membrane separation modules is more than one.
Furthermore, the number of the ceramic membrane separation modules is more than two, and two adjacent ceramic membrane separation modules are connected in series for use, so that the separation precision is improved.
In some preferred embodiments, the method for refining sodium carbonate comprises: and (4) conveying the liquid phase obtained after solid-liquid separation to a continuous crystallization device for evaporation and concentration.
Furthermore, the concentration of magnesium ions in the refined sodium carbonate obtained by the invention is lower than 50ppm, the concentration of calcium ions is lower than 50ppm, and the concentration of barium ions is lower than 50 ppm.
Further, the refined sodium carbonate solution obtained in the invention can be directly used for preparing carbonate after concentration adjustment, such as lithium carbonate, magnesium carbonate, calcium carbonate, strontium carbonate, zinc carbonate, barium carbonate, manganese carbonate, bismuth carbonate, basic magnesium carbonate, basic zinc carbonate, basic copper carbonate, and the like.
Further, the method for refining sodium carbonate further comprises the following steps: and (4) concentrating, drying and recovering the solid slurry obtained after solid-liquid separation.
In some more preferred embodiments, the method for refining sodium carbonate mainly comprises the following specific steps:
dissolving sodium carbonate to be refined in water to obtain an alkaline solution, feeding the solution into a ceramic membrane component, carrying out solid-liquid separation, and then carrying out liquid or concentration and crystallization to obtain the high-purity sodium carbonate. And (4) recovering the solid or after concentrating and drying.
The embodiment of the invention also provides application of the refined sodium carbonate prepared by the method in the fields of preparation of other carbonates, such as lithium carbonate, calcium carbonate, magnesium carbonate, potassium carbonate, barium carbonate, bismuth carbonate, ammonium bicarbonate, strontium carbonate or ammonium carbonate.
Compared with the prior art, the invention has the beneficial effects that:
the method for continuously refining and removing the magnesium and the calcium from the sodium carbonate provided by the invention not only can realize deep removal of calcium and magnesium and obtain high-purity refined sodium carbonate, but also can realize continuous supply of a high-purity sodium carbonate solution.
Detailed Description
In view of the shortcomings of the prior art, the present inventors have long studied and practiced a lot to provide the technical solution of the present invention, and further explain the technical solution, the implementation process and the principle thereof as follows.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention are described in detail below with reference to several preferred embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. The test methods in the following examples are carried out under conventional conditions without specifying the specific conditions. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
1. Dissolving 1kg of sodium carbonate in 3L of water, wherein the concentration of calcium ions is 100ppm, and the concentration of magnesium ions is 50ppm to obtain a solution A;
2. the solution A was transferred to a ceramic membrane module having a pore size of 10nm and filtered at room temperature.
3. And (3) evaporating and concentrating the liquid filtered and separated by the ceramic membrane component, and crystallizing to obtain sodium carbonate crystals, wherein the concentration of calcium ions in the obtained sodium carbonate crystals is 2ppm, and the concentration of magnesium ions in the obtained sodium carbonate crystals is 5 ppm.
Example 2
1. Dissolving 5kg of sodium carbonate in 10L of water, wherein the concentration of calcium ions is 500ppm, and the concentration of magnesium ions is 200ppm to obtain a solution A;
2. conveying the solution A to a first ceramic membrane module with the aperture of 200nm, and filtering at room temperature;
3. the liquid filtered and separated by the first ceramic membrane component is further conveyed to a second ceramic membrane component, wherein the pore diameter of the second ceramic membrane component is 20 nm;
4. and evaporating and concentrating the liquid separated by the second ceramic membrane component, and crystallizing to obtain sodium carbonate crystals, wherein the concentration of calcium ions in the obtained sodium carbonate crystals is 20ppm, and the concentration of magnesium ions in the obtained sodium carbonate crystals is 10 ppm.
Example 3
1. Dissolving 500g of crude sodium carbonate in 5L of water, wherein the concentration of calcium ions is 100ppm, the concentration of magnesium ions is 80ppm, and the concentration of barium ions is 50ppm to obtain a solution A;
2. conveying the solution A to a ceramic membrane component with 2nm pores, and filtering at room temperature;
3. storing the liquid filtered and separated by the ceramic membrane component in an alkali liquor tank to obtain sodium carbonate feed liquid with impurities removed;
4. and (3) adjusting the pH value of the feed liquid to 10 by using deionized water, conveying the feed liquid to the feed liquid containing lithium ions, reacting to obtain a lithium carbonate feed liquid, and separating and drying to obtain a lithium carbonate product.
Example 4
1. Dissolving 1.06g of sodium carbonate in 1L of water, wherein the concentration of calcium ions is 120ppm, and the concentration of magnesium ions is 50ppm to obtain a solution A;
2. and (3) heating the solution A to 90 ℃, conveying the solution A to a ceramic membrane module with the aperture of 10nm, and filtering at 90 ℃.
3. And (3) evaporating and concentrating the liquid filtered and separated by the ceramic membrane component, and crystallizing to obtain sodium carbonate crystals, wherein the concentration of calcium ions in the obtained sodium carbonate crystals is 2ppm, and the concentration of magnesium ions in the obtained sodium carbonate crystals is 4 ppm.
Example 5
1. Dissolving 10.6kg of sodium carbonate in 10L of water, wherein the concentration of calcium ions is 600ppm, and the concentration of magnesium ions is 200ppm to obtain a solution A;
2. conveying the solution A to a first ceramic membrane module with the aperture of 100nm, and filtering at 10 ℃;
3. the liquid filtered and separated by the first ceramic membrane component is further conveyed to a second ceramic membrane component, wherein the pore diameter of the second ceramic membrane component is 50 nm;
4. and evaporating and concentrating the liquid separated by the second ceramic membrane component, and crystallizing to obtain sodium carbonate crystals, wherein the concentration of calcium ions in the obtained sodium carbonate crystals is 25ppm, and the concentration of magnesium ions in the obtained sodium carbonate crystals is 8 ppm.
Comparative example 1
The comparative example differs from example 1 in that: and removing calcium ions and magnesium ions in the solution A by adopting a precipitation method, wherein the calcium ion concentration in the finally obtained sodium carbonate crystal is 100ppm, and the magnesium ion concentration is 150 ppm.
The aspects, embodiments, features and examples of the present invention should be considered as illustrative in all respects and not intended to be limiting of the invention, the scope of which is defined only by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed invention.
The use of headings and chapters in this disclosure is not meant to limit the disclosure; each section may apply to any aspect, embodiment, or feature of the disclosure.
Throughout this specification, where a composition is described as having, containing, or comprising specific components or where a process is described as having, containing, or comprising specific process steps, it is contemplated that the composition of the present teachings also consist essentially of, or consist of, the recited components, and the process of the present teachings also consist essentially of, or consist of, the recited process steps.
It should be understood that the order of steps or the order in which particular actions are performed is not critical, so long as the teachings of the invention remain operable. Further, two or more steps or actions may be performed simultaneously.
In addition, the inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
While the invention has been described with reference to illustrative embodiments, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims.

Claims (10)

1. A method for refining sodium carbonate, which is characterized by comprising:
mixing sodium carbonate to be refined with water to obtain a sodium carbonate solution;
conveying the sodium carbonate solution to a separation assembly, and performing solid-liquid separation to obtain a liquid phase and a solid slurry, wherein the separation assembly comprises a ceramic membrane separation assembly;
and concentrating and crystallizing the liquid phase to obtain the refined sodium carbonate.
2. The method for refining sodium carbonate according to claim 1, characterized in that: the sodium carbonate to be refined contains Ca2+、Mg2+、Ba2+Any one or a combination of two or more of them.
3. The method for refining sodium carbonate according to claim 1, characterized in that: the concentration of the sodium carbonate solution is 0.01-10 mol/L.
4. A refining process of sodium carbonate according to claim 1, characterized by comprising: heating the sodium carbonate solution to 10-95 ℃, and conveying the sodium carbonate solution to a ceramic membrane separation assembly with the temperature of 10-95 ℃.
5. The method for refining sodium carbonate according to claim 1, characterized in that: the aperture of a separation membrane in the ceramic membrane separation component is 2-200 nm.
6. The method for refining sodium carbonate according to claim 1, characterized in that: the number of the ceramic membrane separation assemblies is more than one; preferably, the number of the ceramic membrane separation modules is more than two, and two adjacent ceramic membrane separation modules are arranged in series.
7. A refining process of sodium carbonate according to claim 1, characterized by comprising: and (4) conveying the liquid phase obtained after solid-liquid separation to a continuous crystallization device for evaporation and concentration.
8. The method for refining sodium carbonate according to claim 1, characterized in that: the concentration of magnesium ions in the refined sodium carbonate is lower than 50ppm, the concentration of calcium ions is lower than 50ppm, and the concentration of barium ions is lower than 50 ppm.
9. The method for refining sodium carbonate according to claim 1, characterized by further comprising: and (4) concentrating, drying and recovering the solid slurry obtained after solid-liquid separation.
10. Use of the refined sodium carbonate obtained by the process according to any one of claims 1 to 9 in the field of the preparation of lithium carbonate, calcium carbonate, magnesium carbonate, potassium carbonate, barium carbonate, bismuth carbonate, ammonium bicarbonate, strontium carbonate or ammonium carbonate.
CN202010122363.8A 2020-02-27 2020-02-27 Refining method and application of sodium carbonate Pending CN111302364A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102432037A (en) * 2011-12-05 2012-05-02 中盐金坛盐化有限责任公司 Original halogen denitration production process and production equipment
CN106186002A (en) * 2016-07-22 2016-12-07 中国科学院青海盐湖研究所 A kind of preparation method of battery-level lithium carbonate
WO2018063797A1 (en) * 2016-09-30 2018-04-05 Veolia Water Solutions & Technologies Support Process for silica removal from sodium bicarbonate production wastewater

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102432037A (en) * 2011-12-05 2012-05-02 中盐金坛盐化有限责任公司 Original halogen denitration production process and production equipment
CN106186002A (en) * 2016-07-22 2016-12-07 中国科学院青海盐湖研究所 A kind of preparation method of battery-level lithium carbonate
WO2018063797A1 (en) * 2016-09-30 2018-04-05 Veolia Water Solutions & Technologies Support Process for silica removal from sodium bicarbonate production wastewater

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SERVAES, K ET AL.: "Purification and concentration of lignin from the spent liquor of the alkaline oxidation of woody biomass through membrane separation technology", 《INDUSTRIAL CROPS AND PRODUCTS》 *
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Application publication date: 20200619