CN115159558B - Precipitation method of rare earth carbonate - Google Patents
Precipitation method of rare earth carbonate Download PDFInfo
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- CN115159558B CN115159558B CN202210794478.0A CN202210794478A CN115159558B CN 115159558 B CN115159558 B CN 115159558B CN 202210794478 A CN202210794478 A CN 202210794478A CN 115159558 B CN115159558 B CN 115159558B
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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
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/247—Carbonates
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- C—CHEMISTRY; METALLURGY
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract
The invention discloses a precipitation method of rare earth carbonate, which comprises the following steps of carrying out precipitation reaction on soluble rare earth salt and a precipitant in the presence of seed crystals in a positive sequence feeding mode; wherein, the diammonium tartrate with the yield of 0.2 to 0.5 weight percent of theoretical rare earth carbonate is further added. According to the method, polyethyleneimine PEI is added in the seed crystal preparation, after surface adsorption, the polyethyleneimine PEI and diammonium tartrate further form a bridging effect, so that aggregation and growth of a precipitant and rare earth carbonate on the seed crystal are promoted, and the obtained rare earth carbonate is favorable for obtaining rare earth oxide with larger bulk density and fluidity.
Description
Technical Field
The invention belongs to the technical field of rare earth materials, and relates to a precipitation method of rare earth carbonate.
Background
Rare earth is called as a 'treasury' of new materials, is a group of elements which are most concerned by material scientists at home and abroad, and is listed as a key element for developing high-technology industry in the United states, japan and other countries. The rare earth compound has unique 4f electron energy level, and thus, exhibits unique optical, electrical, magnetic, etc. properties. The rare earth element emits light from the 4f electron transition of the inner layer, and the inner layer electron is less influenced by chemical environment, and meanwhile, the 4f layer transition is forbidden transition, so that the rare earth element emission spectrum is linear, and the fluorescence lifetime is longer.
Rare earth products are various and widely used, and rare earth carbonates are generally not separated when the rare earth products are prepared. Rare earth carbonate is widely used for the industrial production of rare earth, can be used as intermediate raw materials for preparing rare earth oxides, other rare earth salts, rare earth complexes and rare earth enrichment, and plays an extremely important role in industry. Through a great deal of research and production practice, an effective method capable of promoting the crystallization of rare earth carbonate has been found, and rare earth carbonates with different crystal forms can be prepared. Some high purity rare earth products may require oxalic acid for precipitation during preparation, most of the rest are precipitated by carbonate, and the existing carbonate precipitation process basically replaces the oxalic acid precipitation process.
The preparation method of rare earth carbonate mainly comprises a homogeneous precipitation method, a hydrothermal growth method, a high-pressure carbon dioxide method, a hydroxide-carbon dioxide method, a carbonate precipitation method, a bicarbonate precipitation method and the like. However, the former methods have long precipitation reaction period, complicated operation and partial requirement of high pressure and high temperature, and are not suitable for large-scale production. Therefore, carbonate and bicarbonate precipitation methods and the like are mainly adopted at home and abroad.
Chinese patent application CN86100671a discloses a method for precipitating and separating rare earth compounds from rare earth feed liquid by using ammonium bicarbonate as precipitant, which is suitable for rare earth precipitation and separation of rare earth feed liquid obtained by different approaches. The precipitation treatment process mainly comprises two stages of pretreatment and precipitation. The invention can greatly reduce the production cost of rare earth, and has no toxicity to human body, no environmental pollution, the precipitation rate is more than 95 percent, and the purity of rare earth products is more than 92 percent.
Chinese patent CN101798627B discloses a new method for precipitating rare earth, which uses pure magnesium bicarbonate and/or calcium bicarbonate aqueous solution prepared by calcining, digesting and carbonizing calcium or/and magnesium minerals as raw materials as precipitant to precipitate rare earth, to obtain rare earth carbonate, hydroxide, basic carbonate or their mixture, and then preparing rare earth oxide by roasting. The invention uses cheap calcium or/and magnesium minerals to replace ammonium bicarbonate to precipitate rare earth, which can eliminate the pollution of ammonia nitrogen wastewater to the environment and greatly reduce the production cost of rare earth carbonate or rare earth oxide.
Chinese patent application CN103436697a discloses a method for precipitating rare earth carbonate crystals for treating aluminum-containing rare earth feed liquid, which reduces the influence of impurities on the crystallization of rare earth carbonate by controlling the reaction and aging temperatures and the proportion of raw materials, and obtains rare earth carbonate with high total rare earth content, fast crystallization speed and convenient filtration and washing. With the increase of the ratio of the carbonate to the rare earth, the crystallization speed is slowed down, the required aging time is prolonged, and the chloride content is reduced. The feeding mode can be any one of positive sequence, reverse sequence and synchronous feeding. The method has the advantages of high crystallization speed, high total rare earth content in the product, high bulk density and low consumption of precipitant.
However, when rare earth carbonate is used as an intermediate for preparing rare earth oxide, if rare earth carbonate particles are fine, the prepared rare earth oxide is usually fine in particles, small in bulk density, poor in sedimentation, and not easy to mix with other raw materials. Another performance indicator of interest is the flowability of the rare earth oxide produced. Poor fluidity and is not easy to be mixed with other raw materials uniformly.
Accordingly, in view of the drawbacks of the prior art, there is an urgent need to provide a precipitation method of rare earth carbonate that can provide higher bulk density and fluidity.
Disclosure of Invention
The invention aims to provide a precipitation method of rare earth carbonate.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the precipitation method of rare earth carbonate is characterized by that in the presence of seed crystal a precipitation reaction is implemented between soluble rare earth salt and precipitant; wherein, the diammonium tartrate with the yield of 0.2 to 0.5 weight percent of theoretical rare earth carbonate is further added.
The precipitation method according to the present invention, wherein the seed crystal is added together with the precipitant.
The precipitation method according to the invention, wherein the seed is added in an amount of 2-8wt% of the theoretical rare earth carbonate yield.
The precipitation method according to the present invention, wherein the rare earth carbonate is selected from cerium carbonate or a hydrate thereof.
The precipitation method according to the invention, wherein the precipitation method is specifically as follows: taking cerium nitrate aqueous solution with the concentration of 0.5-5mol/L, and adjusting the pH value to be 3.0-5.0; adding diammonium tartrate, and stirring to uniformly mix the materials; firstly uniformly mixing seed crystals and 0.5-5mol/L magnesium bicarbonate aqueous solution, then adding the seed crystals and the magnesium bicarbonate aqueous solution into cerium nitrate aqueous solution at the speed of 1-10mL/min, adjusting the pH value to be 7.0-8.0 after the addition, and continuously stirring for 5-60min; after stopping stirring, aging for 10-50h at room temperature; filtering the solid precipitate, washing with distilled water, and vacuum drying to obtain rare earth carbonate crystal.
The precipitation method according to the present invention, wherein the seed crystal is selected from cerium carbonate octahydrate seed crystals adsorbed on the surface of polyethylenimine PEI.
The precipitation method according to the present invention, wherein the seed crystal is selected from lanthanite type cerium carbonate pdf#38-0377.
The precipitation method according to the present invention, wherein the seed crystal has an average particle diameter of not less than 4. Mu.m.
The precipitation method according to the present invention, wherein the weight average molecular weight mw=70000 of the polyethylenimine PEI; the molar ratio of primary amine and tertiary amine was 25% each and the molar ratio of secondary amine was 50%.
The precipitation method according to the invention, wherein the seed crystal is prepared as follows: taking cerium nitrate aqueous solution with the concentration of 0.5-5mol/L, and adjusting the pH value to be 3.0-5.0; adding polyethylenimine PEI, stirring to mix uniformly; adding 0.5-5mol/L magnesium bicarbonate aqueous solution at a speed of 1-10mL/min until the ratio of cerium ions to bicarbonate ions reaches the theoretical molar ratio, adjusting pH=7.0-8.0 after the addition, and continuously stirring for 5-60min; after stopping stirring, aging for 4-12h at room temperature; filtering the solid precipitate, washing with distilled water, and vacuum drying to obtain cerium carbonate octahydrate seed crystal.
Compared with the prior art, the rare earth carbonate obtained by the precipitation method is more beneficial to obtaining rare earth oxide with larger bulk density and fluidity.
Without wishing to be bound by any theory, polyethyleneimine PEI is added in the preparation of the seed crystal, and after surface adsorption, the polyethyleneimine PEI further forms a bridging effect with diammonium tartrate, so that aggregation and growth of the precipitant and rare earth carbonate on the seed crystal are promoted, and the obtained rare earth carbonate is beneficial to obtaining the rare earth oxide with larger bulk density and fluidity.
Detailed Description
It must be noted that, as used in this specification and the appended claims, the singular forms "a," "an," and "the" include both a reference and a plurality of references (i.e., more than two, including two) unless the context clearly dictates otherwise.
Unless otherwise indicated, the numerical ranges in the present invention are approximate, and thus values outside the ranges may be included. The numerical ranges may be expressed herein as from "about" one particular value, and/or to "about" another particular value. When such a range is expressed, another aspect includes from the one particular value and/or to the other particular value. Similarly, when values are expressed as approximations, by use of the antecedent "about," it will be understood that the particular value forms another aspect. It will also be understood that the endpoints of each of the numerical ranges are significant both in relation to the other endpoint, and independently of the other endpoint.
References in the specification and the claims to parts by weight of a particular element or component in a composition or article refer to the relationship by weight between that element or component and any other element or component in the composition or article.
In the present invention, unless specifically indicated to the contrary, or implied by the context of the context or conventional means in the art, the solutions referred to in the present invention are aqueous solutions; when the solute of the aqueous solution is a liquid, all fractions and percentages are by volume, and the volume percent of the component is based on the total volume of the composition or product comprising the component; when the solute of the aqueous solution is a solid, all fractions and percentages are by weight, and the weight percentages of the components are based on the total weight of the composition or product comprising the components.
References to "comprising," "including," "having," and similar terms in this invention are not intended to exclude the presence of any optional components, steps or procedures, whether or not any optional components, steps or procedures are specifically disclosed. For the avoidance of any doubt, unless stated to the contrary, all methods claimed through use of the term "comprising" may include one or more additional steps, apparatus parts or components and/or materials. In contrast, the term "consisting of … …" excludes any component, step or procedure not specifically recited or enumerated. The term "or" refers to members recited individually as well as in any combination unless otherwise specified.
Furthermore, the contents of any of the referenced patent documents or non-patent documents in the present invention are incorporated by reference in their entirety, especially with respect to the definitions and general knowledge disclosed in the art (in case of not inconsistent with any definitions specifically provided by the present invention).
In the present invention, parts are parts by weight unless otherwise indicated, temperatures are expressed in degrees celsius or at ambient temperature, and pressures are at or near atmospheric. Room temperature represents 20-30 ℃. There are numerous variations and combinations of reaction conditions (e.g., component concentrations, solvents needed, solvent mixtures, temperatures, pressures, and other reaction ranges) and conditions that can be used to optimize the purity and yield of the product obtained by the process. Only reasonable routine experimentation will be required to optimize such process conditions.
Example 1
Taking 1L of cerium nitrate aqueous solution with the concentration of 2mol/L, and adjusting the pH value to be 4.0; 10g of polyethylenimine PEI (weight average molecular weight Mw=70000; the molar ratio of primary amine to tertiary amine is 25% respectively, the molar ratio of secondary amine is 50%) was added and stirred to mix them well; adding 2mol/L magnesium bicarbonate aqueous solution at a speed of 5mL/min until the molar ratio of cerium ions to bicarbonate ions is 1:1.5, adjusting pH to 7.0-8.0 after the addition,stirring was continued for 30min. After stopping stirring, the mixture was aged at room temperature for 8 hours. Filtering the solid precipitate, washing with distilled water, and vacuum drying at 90 ℃ to obtain the cerium carbonate octahydrate seed crystal. The powder XRD characterization proves that the cerium carbonate octahydrate seed crystal is consistent with the characteristic peaks of the standard (pdf#38-0377) lanthanite type cerium carbonate. The IR spectrum shows that a small amount of polyethyleneimine PEI molecules are adsorbed on the surface of the cerium carbonate octahydrate seed crystal, and 3200cm of polyethyleneimine PEI molecules are adsorbed on the surface of the cerium carbonate octahydrate seed crystal -1 Near 2934cm -1 、2830cm -1 、1650cm -1 、1470cm -1 、1120cm -1 、858cm -1 、726cm -1 An absorption peak appears. The particle size analyzer determined that the particle size of the cerium carbonate octahydrate seed crystal was (mean) 6.4.+ -. (SD) 1.3. Mu.m.
Example 2
Taking 1L of cerium nitrate aqueous solution with the concentration of 2mol/L, and adjusting the pH value to be 4.0; adding 4g of diammonium tartrate, and stirring to uniformly mix the materials; 60.5g of the cerium carbonate octahydrate seed crystal of the embodiment 1 and 3L of 2mol/L magnesium bicarbonate aqueous solution are uniformly mixed, then added into cerium nitrate aqueous solution at a speed of 5mL/min, pH=7.0-8.0 is adjusted after the addition, and stirring is continued for 30min. After stopping stirring, aging was carried out at room temperature for 30 hours. Filtering the solid precipitate, washing with distilled water, and vacuum drying at 90 ℃ to obtain cerium carbonate octahydrate crystal. The powder XRD characterization proves that the cerium carbonate octahydrate crystals are consistent with the characteristic peaks of the standard (PDF # 38-0377) lanthanite type cerium carbonate. The IR spectrum shows that a small amount of diammonium tartrate molecules are further adsorbed on the surface of the crystal of cerium carbonate octahydrate. The particle size analyzer determined that the particle size of the cerium carbonate octahydrate crystals was (mean) 29.6.+ -. (SD) 8.7. Mu.m.
Comparative example 1
Taking 1L of cerium nitrate aqueous solution with the concentration of 2mol/L, and adjusting the pH value to be 4.0; adding 2mol/L magnesium bicarbonate aqueous solution at a speed of 5mL/min until the molar ratio of cerium ions to bicarbonate ions is 1:1.5, adjusting pH to 7.0-8.0 after the addition, and continuously stirring for 30min. After stopping stirring, the mixture was aged at room temperature for 8 hours. Filtering the solid precipitate, washing with distilled water, and vacuum drying at 90 ℃ to obtain the cerium carbonate octahydrate seed crystal. The powder XRD characterization proves that the cerium carbonate octahydrate seed crystal is consistent with the characteristic peaks of the standard (pdf#38-0377) lanthanite type cerium carbonate. The particle size analyzer determined that the particle size of the cerium carbonate octahydrate seed crystal was (mean) 1.4.+ -. (SD) 0.35. Mu.m.
Comparative example 2
The cerium carbonate octahydrate seed crystal of example 1 was replaced with that of comparative example 1, and the rest was the same as example 2. The powder XRD characterization proves that the cerium carbonate octahydrate crystals are consistent with the characteristic peaks of the standard (PDF # 38-0377) lanthanite type cerium carbonate. The particle size analyzer determined that the particle size of the cerium carbonate octahydrate crystals was (mean) 10.2.+ -. (SD) 2.9. Mu.m.
Comparative example 3
The procedure of example 2 is followed except that no diammonium tartrate is added. The powder XRD characterization proves that the cerium carbonate octahydrate crystals are consistent with the characteristic peaks of the standard (PDF # 38-0377) lanthanite type cerium carbonate. The particle size of the cerium carbonate octahydrate crystals was (mean) 21.3.+ -. (SD) 6.5. Mu.m.
Performance testing
The cerium carbonate octahydrate crystals obtained in example 2 and comparative examples 2 to 3 were placed in a muffle furnace, and the temperature was raised to 1000 ℃ and kept for 4 hours to obtain cerium oxide powder.
The apparent density of the different cerium oxide powders was measured according to the national standard GB/T16913.3-2008.
And (3) measuring powder parameters such as the repose angle, the compression degree, the spatula angle, the uniformity, the condensation degree and the like of different cerium oxide powders by using a powder comprehensive property tester, and calculating the flowability parameters of different cerium oxide powders according to a Carr calculation method.
The results are shown in Table 1.
TABLE 1
| Bulk density (g/cm) 3 ) | Fluidity parameters (100 minutes system) | |
| Example 2 | 2.29 | 82 |
| Comparative example 2 | 1.15 | 67 |
| Comparative example 3 | 1.76 | 74 |
As can be seen from table 1, the rare earth carbonate obtained using the precipitation method of the present invention is more advantageous in obtaining larger bulk density and flowability parameters than the comparative example.
Further, it should be understood that various changes, substitutions, omissions, modifications, or adaptations to the present invention may be made by those skilled in the art after having read the present disclosure, and such equivalent embodiments are within the scope of the present invention as defined in the appended claims.
Claims (5)
1. The precipitation method of rare earth carbonate is characterized by that in the presence of seed crystal a precipitation reaction is implemented between soluble rare earth salt and precipitant; it is characterized in that the diammonium tartrate with the yield of 0.2 to 0.5 weight percent of theoretical rare earth carbonate is further added; the addition amount of the seed crystal is 2-8wt% of the theoretical rare earth carbonate yield;
the precipitation method comprises the following steps: taking cerium nitrate aqueous solution with the concentration of 0.5-5mol/L, and adjusting the pH value to be 3.0-5.0; adding diammonium tartrate, and stirring to uniformly mix the materials; firstly uniformly mixing seed crystals and 0.5-5mol/L magnesium bicarbonate aqueous solution, then adding the seed crystals and the magnesium bicarbonate aqueous solution into cerium nitrate aqueous solution at the speed of 1-10mL/min, adjusting the pH value to be 7.0-8.0 after the addition, and continuously stirring for 5-60min; after stopping stirring, aging for 10-50h at room temperature; filtering the solid precipitate, washing with distilled water, and vacuum drying to obtain rare earth carbonate crystal;
the seed crystal is selected from cerium carbonate octahydrate seed crystal adsorbed on the surface of polyethyleneimine PEI.
2. The precipitation method according to claim 1, wherein the seed crystal is selected from the group consisting of lanthanite type cerium carbonate pdf#38-0377.
3. The precipitation method according to claim 1, wherein the seed crystal has an average particle diameter of not less than 4 μm.
4. Precipitation process according to claim 1, characterized in that the weight average molecular weight mw=70000 of polyethylenimine PEI; the molar ratio of primary amine and tertiary amine was 25% each and the molar ratio of secondary amine was 50%.
5. The precipitation method according to claim 1, wherein the seed crystal is prepared by the following method: taking cerium nitrate aqueous solution with the concentration of 0.5-5mol/L, and adjusting the pH value to be 3.0-5.0; adding polyethylenimine PEI, stirring to mix uniformly; adding 0.5-5mol/L magnesium bicarbonate aqueous solution at a speed of 1-10mL/min until the ratio of cerium ions to bicarbonate ions reaches the theoretical molar ratio, adjusting pH=7.0-8.0 after the addition, and continuously stirring for 5-60min; after stopping stirring, aging for 4-12h at room temperature; filtering the solid precipitate, washing with distilled water, and vacuum drying to obtain cerium carbonate octahydrate seed crystal.
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