CN108793224B - Method for preparing narrow-distribution crystal form yttrium carbonate by sodium carbonate precipitation - Google Patents
Method for preparing narrow-distribution crystal form yttrium carbonate by sodium carbonate precipitation Download PDFInfo
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Abstract
The invention discloses a method for preparing narrow-distribution crystal form yttrium carbonate by sodium carbonate precipitation, which adopts sodium carbonate as a precipitator and yttrium chloride as a feed liquid, and strictly controls the reactionObtaining yttrium carbonate seed crystal under the conditions of temperature, yttrium chloride feed liquid feeding speed, pH value in the reaction process, parallel flow feeding position and the like, then carrying out precipitation reaction by taking the yttrium carbonate seed crystal slurry as a base solution, and controlling the precipitation temperature to be 70-90 DEGoC and precipitation reaction pH5.5-6.5 to obtain (D)90‑D10)/(2D50) Y of narrow distribution crystal form less than 0.82(CO3)3•3H2And O. The method obtains the crystal form yttrium carbonate with narrow distribution by strict control of the crystal seed preparation process and the precipitation process, has low consumption of the sodium carbonate precipitator, and avoids ammonia nitrogen pollution.
Description
Technical Field
The invention relates to the field of rare earth hydrometallurgy, in particular to a method for preparing narrow-distribution crystal form yttrium carbonate by sodium carbonate precipitation.
Background
Due to the unique 4f sublayer electronic structure, large atomic magnetic moment, strong spin-orbit coupling and variable coordination number of the rare earth element, the formed compound has very rich magnetic, optical, electric, catalytic and other functional properties, and is known as 'vitamin of modern industry' and 'treasure house of new materials'. The yttrium oxide is an important rare earth compound and is a key basic raw material for preparing high-grade new materials such as rare earth luminescent materials, crystal materials, ceramic materials, catalytic materials and the like. Because the precipitation method has the advantages of very accurate control of the chemical composition of the materials, low raw material cost, low requirement on equipment, simple process, convenient operation and the like, the precipitation method is generally adopted in industry to prepare the yttrium oxide precursor, and then the yttrium oxide precursor is roasted to obtain the yttrium oxide. The roasting process has certain inheritance, and a good-performance yttrium oxide precursor needs to be obtained to obtain good-performance yttrium oxide. At present, precipitation methods for preparing yttria precursors include the following methods.
(1) Oxalic acid precipitation method: the yttrium oxalate solution is precipitated by oxalic acid, so that the yttrium oxalate with higher purity can be obtained, but the oxalic acid is expensive and high in cost, and the oxalic acid residue in the mother liquor has adverse effects on human bodies and the environment. (2) Hydroxide precipitation method: the common precipitant for the hydroxide precipitation method comprises ammonia water, sodium hydroxide and the like, but ammonia nitrogen pollution also exists in the ammonia water precipitation, and the precipitation cost is increased by the sodium hydroxide precipitation; more importantly, the yttrium hydroxide obtained by the hydroxide precipitation method is easy to be gelatinous and has poor filtering performance. (3) Carbonate precipitation method. Ammonium bicarbonate is mostly adopted as a precipitator in the traditional yttrium feed liquid precipitation, and a lot of researches are carried out from the crystallization process of the yttrium feed liquid precipitation to industrial application. But ammonium bicarbonate precipitation can produce a large amount of ammonia nitrogen wastewater. The ammonia nitrogen wastewater has serious influence on the environment, so that the ammonium bicarbonate precipitation process faces the problem of standard discharge after severe water treatment. In recent years, replacing ammonium bicarbonate with sodium carbonate (soda ash) or sodium bicarbonate as yttrium precipitant has been a common concern in the industry. The sodium bicarbonate can obtain the yttrium carbonate with good crystallization performance and high total rare earth content by controlling conditions, but the unit consumption of sodium bicarbonate precipitation is high (6 mol of sodium bicarbonate is needed for precipitating 2mol of yttrium), and the cost is greatly increased. The consumption of yttrium precipitated by sodium carbonate is low (only 3mol of sodium carbonate is needed for precipitating 2mol of yttrium), but yttrium carbonate generated by yttrium precipitated by sodium carbonate is easy to form amorphous flocculent precipitate, contains a large amount of water and impurities, is large in volume, difficult to filter and low in total amount, and limits the popularization and application of sodium carbonate. In addition, the direct precipitation methods have the common problem that the concentration of a local precipitator is easily overhigh due to the direct addition of the precipitator, so that the supersaturation degree is uneven, and the products with narrow distribution range are difficult to obtain.
In conclusion, how to prepare yttrium carbonate with good crystallization, good filtration performance and narrow particle size distribution by using sodium carbonate precipitation is a technical problem to be solved at present.
Disclosure of Invention
The invention mainly aims to provide a method for preparing narrow-distribution crystal form yttrium carbonate by sodium carbonate precipitation so as to obtain yttrium carbonate with good crystallization, good filtering performance and narrow particle size distribution.
In order to achieve the purpose, the method for preparing the narrow-distribution crystal form yttrium carbonate by sodium carbonate precipitation specifically comprises the following steps.
(1) Preparing seed crystals: and adding bottom water into the reaction kettle, and controlling the bottom water to submerge the paddle of the stirring paddle. And then adding yttrium chloride feed liquid and sodium carbonate solution in a parallel flow manner for reaction, and filtering and washing after the reaction to obtain yttrium carbonate seed crystals. The concentration of yttrium chloride feed liquid is 0.05-0.15mol/L, the concentration of sodium carbonate solution is 0.05-0.30mol/L, the feeding speed of yttrium chloride feed liquid is controlled to be 1.0-3.0mL/min, the reaction temperature is controlled to be 75-85oAnd C, controlling the pH value in the reaction process to be 5.8-6.2.
(2) And (3) precipitation process: and (4) mixing the yttrium carbonate crystal seeds with water, and controlling the slurry to submerge a stirring paddle blade. And then adding yttrium chloride feed liquid and sodium carbonate solution in a parallel flow manner to carry out precipitation reaction, and filtering and washing after the reaction is finished to obtain an yttrium carbonate filter cake. The concentration of yttrium chloride feed liquid is 0.2-1.5mol/L, the concentration of sodium carbonate solution is 0.3-1.5mol/L, the feeding speed of yttrium chloride feed liquid is controlled to be 3.0-10.0mL/min, the precipitation temperature is controlled to be 70-90oAnd C, controlling the pH value in the precipitation process to be 5.5-6.5.
(3) And (3) drying: placing the yttrium carbonate filter cake in a temperature range of 40-80 DEG CoCDrying to finally obtain (D)90-D10)/(2D50) Y of narrow distribution crystal form less than 0.82(CO3)3•3H2O。
Further, the feeding positions of the yttrium chloride feed liquid and the sodium carbonate solution in the step (1) and the step (2) are below the liquid level and are distributed on two opposite sides.
Further, the precipitation end point pH in the step (2) is controlled to be 7.0-7.5.
Further, the stirring speed in the step (1) and the step (2) is 400 r/min.
Further, preparing the yttrium carbonate seed crystal by adopting a circulation method, specifically, the seed crystal obtained in the step (1) is slurried and returned to be used as the base solution in the step (1), new yttrium carbonate seed crystal is prepared and obtained through the reaction conditions in the step (1), and the yttrium carbonate seed crystal finally obtained after 2-4 times of circulation is reused in the step (2).
The invention adopts sodium carbonate as a precipitator and yttrium chloride as a feed liquid, and strictly controls the reaction temperature to be 75-85 DEGoC. Yttrium chloride feed liquid feeding speed is 1.0-3.0mL/min, reaction process pH is 5.8-6.2, parallel flow feeding position and other conditions are adopted to obtain yttrium carbonate seed crystal, then yttrium carbonate seed crystal slurry is used as base liquid to carry out precipitation reaction, and precipitation temperature and precipitation reaction pH are controlled to obtain (D) through precipitation preparation90-D10)/(2D50) Y of narrow distribution crystal form less than 0.82(CO3)3•3H2And O. The method obtains the crystal form yttrium carbonate with narrow distribution by strict control of the crystal seed preparation process and the precipitation process, has low consumption of the sodium carbonate precipitator, and avoids ammonia nitrogen pollution.
Drawings
Fig. 1 is an XRD pattern of amorphous yttrium carbonate obtained in comparative example 1.
FIG. 2 is Y obtained in example 12(CO3)3•3H2Particle size distribution plot of O.
FIG. 3 is Y obtained in example 12(CO3)3•3H2XRD pattern of O.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail with reference to examples.
At present, yttrium carbonate generated by yttrium precipitation of sodium carbonate is easy to form amorphous flocculent precipitate, contains a large amount of water, has large volume, is difficult to filter and has low total amount, thereby limiting the popularization and application of sodium carbonate. The invention provides a method for preparing narrow-distribution crystal form yttrium carbonate by sodium carbonate precipitation, which comprises the following steps.
(1) Preparing seed crystals: and adding bottom water into the reaction kettle, and controlling the bottom water to submerge the paddle of the stirring paddle. Then adding yttrium chloride feed liquid and sodium carbonate solution in a parallel flow manner for reaction,filtering and washing after the reaction is finished to obtain yttrium carbonate seed crystals. The concentration of yttrium chloride feed liquid is 0.05-0.15mol/L, the concentration of sodium carbonate solution is 0.05-0.30mol/L, the feeding speed of yttrium chloride feed liquid is controlled to be 1.0-3.0mL/min, the reaction temperature is controlled to be 75-85oAnd C, controlling the pH value in the reaction process to be 5.8-6.2.
The reaction conditions in the seed crystal preparation process must be strictly controlled, the concentration of yttrium chloride feed liquid is 0.05-0.15mol/L, the concentration of sodium carbonate feed liquid is 0.05-0.30mol/L, the feeding speed of yttrium chloride feed liquid is controlled to be 1.0-3.0mL/min, and the feeding speed of sodium carbonate solution is adjusted according to the control of pH in the reaction process. This is to prevent the rare earth carbonate from being locally supersaturated, and to form amorphous rare earth carbonate by the formation of a large number of nuclei of the rare earth carbonate. Furthermore, it is preferred to control the point of co-current feeding strictly, i.e. below the liquid level, while distributing on opposite sides, so as to better achieve the dispersion of sodium carbonate and yttrium chloride. More important is the control of temperature and pH. The selection of temperature and pH is greatly related to the types of rare earth elements and the types of precipitating agents, and different rare earth elements and precipitating agents have characteristic temperature and pH which jointly determine whether precipitates can be crystallized or not. The temperature and the pH value corresponding to different rare earth elements are different, for example, when praseodymium chloride is precipitated by sodium carbonate, the temperature is controlled to be about 50 ℃, and when neodymium chloride feed liquid is precipitated, the temperature is generally controlled to be 65-70 ℃, so that crystal form rare earth carbonate can be precipitated; and precipitating lanthanum chloride and cerium chloride solution by using sodium carbonate, wherein the pH value is preferably controlled to be 5-5.4, and the temperature is about 60 ℃. And the temperature and pH of different precipitants are different, for example, when ammonium bicarbonate is used for precipitating crystal form yttrium chloride, the precipitation pH is about 6.4, and the temperature is preferably 60 ℃. Likewise, for systems that precipitate yttrium chloride, temperature has an effect on the pH of the system, as well as on the kinetics and thermodynamics of yttrium carbonate precipitation. The pH can control the concentration of free yttrium and carbonate in the system, the pH is low, the concentration of yttrium in the precipitation solution is high, and the content of carbonate is high when the pH is high, so that the precipitation of the crystal form of yttrium carbonate is not facilitated. The yttrium carbonate crystal seed is prepared by the combined action of pH and temperature, if the pH and temperature are not strictly controlled, amorphous precipitate is easily obtained, and meanwhile, basic rare earth carbonate and rare earth carbonate-sodium carbonate double salt precipitate can also be obtained. The stirring speed in the process is controlled to be 100-. More particularly, the yttrium carbonate seed crystal is prepared by adopting a circulation method, specifically, the seed crystal obtained in the step (1) is slurried and returned to be used as the base solution in the step (1), new yttrium carbonate seed crystal is prepared and obtained through the reaction conditions in the step (1), and the yttrium carbonate seed crystal finally obtained after the circulation is performed for 2-4 times is reused in the step (2). The crystal seed obtained in the way has better crystallization performance, and the finally obtained crystal form yttrium carbonate has more uniform particle size distribution.
(2) And (3) precipitation process: and (4) mixing the yttrium carbonate crystal seeds with water, and controlling the slurry to submerge a stirring paddle blade. And then adding yttrium chloride feed liquid and sodium carbonate solution in a parallel flow manner to carry out precipitation reaction, and filtering and washing after the reaction is finished to obtain an yttrium carbonate filter cake. The concentration of yttrium chloride feed liquid is 0.2-1.5mol/L, the concentration of sodium carbonate solution is 0.3-1.5mol/L, the feeding speed of yttrium chloride feed liquid is controlled to be 3.0-10.0mL/min, the precipitation temperature is controlled to be 70-90oAnd C, controlling the pH value in the precipitation process to be 5.5-6.5.
On the premise of obtaining the yttrium carbonate seed crystal, precipitating yttrium carbonate, and expanding the control range of yttrium chloride feed liquid concentration, sodium carbonate solution concentration and yttrium chloride feed liquid feeding speed, wherein the yttrium chloride feed liquid concentration is 0.2-1.5mol/L, the sodium carbonate solution concentration is 0.3-1.5mol/L, the yttrium chloride feed liquid feeding speed is controlled to be 3.0-10.0mL/min, and the sodium carbonate solution feeding speed is adjusted according to the control of pH in the precipitation process. This is because the yttrium carbonate seed crystal can induce the carbonate and yttrium ions to form crystal form of rare earth carbonate. It should be noted, however, that the temperature and pH control is still critical and must be within a small range, with the precipitation temperature being controlled to 70-90 deg.CoAnd C, controlling the pH value in the precipitation process to be 5.5-6.5. Preferably, the co-current feed should also be located below the liquid level and distributed on opposite sides. In addition, in order to complete the yttrium precipitation, the precipitation end point pH can be controlled at 7.0-7.5 by slowly adding sodium carbonate to precipitate free yttrium ions. The stirring speed in the process is controlled to be 100-.
(3) And (3) drying: placing the yttrium carbonate filter cake in a temperature range of 40-80 DEG CoCDrying to finally obtain (D)90-D10)/(2D50) SmallY in the narrow distribution form of 0.82(CO3)3•3H2O。
The method for preparing narrow distribution crystal form yttrium carbonate by sodium carbonate precipitation provided by the invention is further illustrated by the following examples.
Comparative example 1
Adding bottom water into a reaction kettle, controlling the bottom water to submerge blades of a stirring paddle, then adding 0.1mol/L yttrium chloride feed liquid and 0.15mol/L sodium carbonate solution in a parallel flow manner for reaction, controlling the feeding positions of the yttrium chloride feed liquid and the sodium carbonate solution to be below the liquid level, and simultaneously distributing the yttrium chloride feed liquid and the sodium carbonate solution on two opposite sides, controlling the feeding speed of the yttrium chloride feed liquid to be 1.5mL/min, and controlling the reaction temperature to be 80 DEG CoAnd C, the pH value is 5.3 in the reaction process, the stirring speed is 300r/min, the reaction is stopped when the addition of the yttrium chloride feed liquid is 300mL, and the crystallization performance of the obtained yttrium carbonate seed crystal is poor. Filtering and washing to obtain a filter cake, mixing the filter cake with water, controlling the slurry to submerge a stirring paddle blade, then adding 1.0mol/L yttrium chloride feed liquid and 1.0mol/L sodium carbonate solution in a parallel flow manner for precipitation reaction, controlling the feeding positions of the yttrium chloride feed liquid and the sodium carbonate solution to be below the liquid level and distributed on two opposite sides, controlling the feeding speed of the yttrium chloride feed liquid to be 5.0mL/min and the precipitation temperature to be 80 DEGoC, the pH value in the precipitation process is 6.0, the stirring speed is 300r/min, when the addition amount of yttrium chloride is 400mL, the parallel flow feeding is stopped, then the pH value of the precipitation end point is adjusted to be 7.3 by adopting a sodium carbonate solution, the yttrium carbonate filter cake is obtained by filtering and washing, and the yttrium carbonate filter cake is placed in a place of 70oCDrying to finally obtain (D)90-D10)/(2D50) The amorphous yttrium carbonate is 2.5, the filtering crystallization performance is poor, and XRD of the amorphous yttrium carbonate is shown in figure 1.
Comparative example 2
Adding bottom water into a reaction kettle, controlling the bottom water to submerge blades of a stirring paddle, then adding 0.1mol/L yttrium chloride feed liquid and 0.15mol/L sodium carbonate solution in a parallel flow manner for reaction, controlling the feeding positions of the yttrium chloride feed liquid and the sodium carbonate solution to be below the liquid level, and simultaneously distributing the yttrium chloride feed liquid and the sodium carbonate solution on two opposite sides, controlling the feeding speed of the yttrium chloride feed liquid to be 1.5mL/min, and controlling the reaction temperature to be 80 DEG CoC, the pH value in the reaction process is 6.0, and the stirring speed is300r/min, when the addition of the yttrium chloride feed liquid is 300mL, the reaction is stopped, and the crystallization performance of the obtained yttrium carbonate seed crystal is good. Filtering and washing to obtain a filter cake, mixing the filter cake with water, controlling the slurry to submerge a stirring paddle blade, then adding 1.0mol/L yttrium chloride feed liquid and 1.0mol/L sodium carbonate solution in a parallel flow manner for precipitation reaction, controlling the feeding positions of the yttrium chloride feed liquid and the sodium carbonate solution to be below the liquid level and distributed on two opposite sides, controlling the feeding speed of the yttrium chloride feed liquid to be 5.0mL/min and the precipitation temperature to be 80 DEGoC, the pH value in the precipitation process is 5.3, the stirring speed is 300r/min, when the addition amount of yttrium chloride is 400mL, the parallel flow feeding is stopped, then the pH value of the precipitation end point is adjusted to be 7.3 by adopting a sodium carbonate solution, the yttrium carbonate filter cake is obtained by filtering and washing, and the yttrium carbonate filter cake is placed in a place of 70oCDrying to finally obtain (D)90-D10)/(2D50) The amorphous yttrium carbonate content of 1.8 is poor in filtering crystallization property.
Comparative example 3
Adding bottom water into a reaction kettle, controlling the bottom water to submerge blades of a stirring paddle, then adding 0.1mol/L yttrium chloride feed liquid and 0.15mol/L sodium carbonate solution in a parallel flow manner for reaction, controlling the feeding positions of the yttrium chloride feed liquid and the sodium carbonate solution to be below the liquid level, and simultaneously distributing the yttrium chloride feed liquid and the sodium carbonate solution on two opposite sides, controlling the feeding speed of the yttrium chloride feed liquid to be 1.5mL/min, and controlling the reaction temperature to be 60 DEG CoAnd C, the pH value is 6.0 in the reaction process, the stirring speed is 300r/min, the reaction is stopped when the addition of the yttrium chloride feed liquid is 300mL, and the crystallization performance of the obtained yttrium carbonate seed crystal is poor. Filtering and washing to obtain a filter cake, mixing the filter cake with water, controlling the slurry to submerge a stirring paddle blade, then adding 1.0mol/L yttrium chloride feed liquid and 1.0mol/L sodium carbonate solution in a parallel flow manner for precipitation reaction, controlling the feeding positions of the yttrium chloride feed liquid and the sodium carbonate solution to be below the liquid level and distributed on two opposite sides, controlling the feeding speed of the yttrium chloride feed liquid to be 5.0mL/min and the precipitation temperature to be 80 DEGoC, the pH value in the precipitation process is 6.0, the stirring speed is 300r/min, when the addition amount of yttrium chloride is 400mL, the parallel flow feeding is stopped, then the pH value of the precipitation end point is adjusted to be 7.3 by adopting a sodium carbonate solution, the yttrium carbonate filter cake is obtained by filtering and washing, and the yttrium carbonate filter cake is placed in a place of 70oCDrying to finally obtain (D)90-D10)/(2D50) The amorphous yttrium carbonate content of 2.4 is poor in filtering crystallization property.
Comparative example 4
Adding bottom water into a reaction kettle, controlling the bottom water to submerge blades of a stirring paddle, then adding 0.1mol/L yttrium chloride feed liquid and 0.15mol/L sodium carbonate solution in a parallel flow manner for reaction, controlling the feeding positions of the yttrium chloride feed liquid and the sodium carbonate solution to be below the liquid level, and simultaneously distributing the yttrium chloride feed liquid and the sodium carbonate solution on two opposite sides, controlling the feeding speed of the yttrium chloride feed liquid to be 1.5mL/min, and controlling the reaction temperature to be 80 DEG CoAnd C, the pH value is 6.0 in the reaction process, the stirring speed is 300r/min, the reaction is stopped when the addition of the yttrium chloride feed liquid is 300mL, and the crystallization performance of the obtained yttrium carbonate seed crystal is good. Filtering and washing to obtain a filter cake, mixing the filter cake with water, controlling the slurry to submerge a stirring paddle blade, then adding 1.0mol/L yttrium chloride feed liquid and 1.0mol/L sodium carbonate solution in a parallel flow manner for precipitation reaction, controlling the feeding positions of the yttrium chloride feed liquid and the sodium carbonate solution to be below the liquid level and distributed on two opposite sides, controlling the feeding speed of the yttrium chloride feed liquid to be 5.0mL/min and the precipitation temperature to be 60 DEGoC, the pH value in the precipitation process is 6.0, the stirring speed is 300r/min, when the addition amount of yttrium chloride is 400mL, the parallel flow feeding is stopped, then the pH value of the precipitation end point is adjusted to be 7.3 by adopting a sodium carbonate solution, the yttrium carbonate filter cake is obtained by filtering and washing, and the yttrium carbonate filter cake is placed in a place of 70oCDrying to finally obtain (D)90-D10)/(2D50) The amorphous yttrium carbonate content of 1.5 is poor in filtering crystallization property.
Comparative example 5
Adding bottom water into a reaction kettle, controlling the bottom water to submerge blades of a stirring paddle, then adding 0.4mol/L yttrium chloride feed liquid and 0.6mol/L sodium carbonate solution in a parallel flow manner for reaction, controlling the feeding positions of the yttrium chloride feed liquid and the sodium carbonate solution to be below the liquid level, and simultaneously distributing the yttrium chloride feed liquid and the sodium carbonate solution on two opposite sides, controlling the feeding speed of the yttrium chloride feed liquid to be 1.5mL/min, and controlling the reaction temperature to be 80 DEG CoAnd C, the pH value is 6.0 in the reaction process, the stirring speed is 300r/min, the reaction is stopped when the addition of the yttrium chloride feed liquid is 300mL, and the crystallization performance of the obtained yttrium carbonate seed crystal is poor. Filtering and washing to obtain filter cake, mixing the filter cake with water, and controlling slurryImmersing a stirring paddle blade, then adding 1.0mol/L yttrium chloride feed liquid and 1.0mol/L sodium carbonate solution in a parallel flow manner to carry out precipitation reaction, controlling the feeding positions of the yttrium chloride feed liquid and the sodium carbonate solution below the liquid level, simultaneously distributing the yttrium chloride feed liquid and the sodium carbonate solution at two opposite sides, controlling the feeding speed of the yttrium chloride feed liquid to be 5.0mL/min, and controlling the precipitation temperature to be 80 DEG CoC, the pH value in the precipitation process is 6.0, the stirring speed is 300r/min, when the addition amount of yttrium chloride is 400mL, the parallel flow feeding is stopped, then the pH value of the precipitation end point is adjusted to be 7.3 by adopting a sodium carbonate solution, the yttrium carbonate filter cake is obtained by filtering and washing, and the yttrium carbonate filter cake is placed in a place of 70oCDrying to finally obtain (D)90-D10)/(2D50) The amorphous yttrium carbonate content of 3.1 is poor in filtering crystallization property.
Example 1
Adding bottom water into a reaction kettle, controlling the bottom water to submerge blades of a stirring paddle, then adding 0.1mol/L yttrium chloride feed liquid and 0.15mol/L sodium carbonate solution in a parallel flow manner for reaction, controlling the feeding positions of the yttrium chloride feed liquid and the sodium carbonate solution to be below the liquid level, and simultaneously distributing the yttrium chloride feed liquid and the sodium carbonate solution on two opposite sides, controlling the feeding speed of the yttrium chloride feed liquid to be 1.5mL/min, and controlling the reaction temperature to be 80 DEG CoAnd C, the pH value is 6.0 in the reaction process, the stirring speed is 300r/min, the reaction is stopped when the addition of the yttrium chloride feed liquid is 300mL, and the crystallization performance of the obtained yttrium carbonate seed crystal is good. Filtering and washing to obtain a filter cake, mixing the filter cake with water, controlling the slurry to submerge a stirring paddle blade, then adding 1.0mol/L yttrium chloride feed liquid and 1.0mol/L sodium carbonate solution in a parallel flow manner for precipitation reaction, controlling the feeding positions of the yttrium chloride feed liquid and the sodium carbonate solution to be below the liquid level and distributed on two opposite sides, controlling the feeding speed of the yttrium chloride feed liquid to be 5.0mL/min and the precipitation temperature to be 80 DEGoC, the pH value in the precipitation process is 6.0, the stirring speed is 300r/min, when the addition amount of yttrium chloride is 400mL, the parallel flow feeding is stopped, then the pH value of the precipitation end point is adjusted to be 7.3 by adopting a sodium carbonate solution, the yttrium carbonate filter cake is obtained by filtering and washing, and the yttrium carbonate filter cake is placed in a place of 70oCDrying to finally obtain (D)90-D10)/(2D50) Y in the form of a narrow distribution of 0.52(CO3)3•3H2The corresponding particle size distribution and XRD pattern are shown in FIGS. 2 and 3.
Example 2
Adding bottom water into a reaction kettle, controlling the bottom water to submerge blades of a stirring paddle, then adding 0.05mol/L yttrium chloride feed liquid and 0.05mol/L sodium carbonate solution in a concurrent flow manner for reaction, controlling the feeding speed of the yttrium chloride feed liquid to be 2.0mL/min, and controlling the reaction temperature to be 75oAnd C, the pH value in the reaction process is 5.8, the stirring speed is 100r/min, the reaction is stopped when the addition of the yttrium chloride feed liquid is 300mL, and the crystallization performance of the obtained yttrium carbonate seed crystal is good. Filtering and washing to obtain a filter cake, mixing the filter cake with water, controlling the slurry to submerge a stirring paddle blade, then adding 0.2mol/L yttrium chloride feed liquid and 0.3mol/L sodium carbonate solution in a concurrent flow manner for precipitation reaction, controlling the feeding speed of the yttrium chloride feed liquid to be 10.0mL/min, and the precipitation temperature to be 70oC, the pH value in the precipitation process is 5.5, the stirring speed is 200r/min, when the addition amount of yttrium chloride is 400mL, the parallel flow feeding is stopped, then the pH value of the precipitation end point is adjusted to be 7.3 by adopting a sodium carbonate solution, the yttrium carbonate filter cake is obtained by filtering and washing, and the yttrium carbonate filter cake is placed at 40oCDrying to finally obtain (D)90-D10)/(2D50) Y in the narrow distribution form of 0.42(CO3)3•3H2O。
Example 3
Adding bottom water into a reaction kettle, controlling the bottom water to submerge a stirring paddle blade, then adding 0.08mol/L yttrium chloride feed liquid and 0.1mol/L sodium carbonate solution in a concurrent flow manner for reaction, controlling the feeding speed of the yttrium chloride feed liquid to be 1.0mL/min, and controlling the reaction temperature to be 80 DEG CoAnd C, the pH value in the reaction process is 5.8, the stirring speed is 200r/min, the reaction is stopped when the addition of the yttrium chloride feed liquid is 300mL, and the crystallization performance of the obtained yttrium carbonate seed crystal is good. Filtering and washing to obtain a filter cake, mixing the filter cake with water, controlling the slurry to submerge a stirring paddle blade, then adding 0.5mol/L yttrium chloride feed liquid and 0.8mol/L sodium carbonate solution in a concurrent flow manner for precipitation reaction, controlling the feeding speed of the yttrium chloride feed liquid to be 8.0mL/min and the precipitation temperature to be 90 DEG CoC, the pH value in the precipitation process is 5.5, the stirring speed is 300r/min, when the addition amount of yttrium chloride is 400mL, the parallel flow feeding is stopped, then the pH value of the precipitation end point is adjusted to be 7.5 by adopting a sodium carbonate solution, yttrium carbonate filter cakes are obtained by filtering and washing, and carbonic acid is addedThe yttrium filter cake is placed in 50oCDrying to finally obtain (D)90-D10)/(2D50) Y in the narrow distribution form of 0.72(CO3)3•3H2O。
Example 4
Adding bottom water into a reaction kettle, controlling the bottom water to submerge a stirring paddle blade, then adding 0.15mol/L yttrium chloride feed liquid and 0.3mol/L sodium carbonate solution in a concurrent flow manner for reaction, controlling the feeding speed of the yttrium chloride feed liquid to be 1.0mL/min and the reaction temperature to be 85 DEGoAnd C, the pH value in the reaction process is 6.2, the stirring speed is 200r/min, the reaction is stopped when the addition of the yttrium chloride feed liquid is 300mL, and the crystallization performance of the obtained yttrium carbonate seed crystal is good. Filtering and washing to obtain a filter cake, mixing the filter cake with water, controlling the slurry to submerge a stirring paddle blade, then adding 1.5mol/L yttrium chloride feed liquid and 1.2mol/L sodium carbonate solution in a concurrent flow manner for precipitation reaction, controlling the feeding speed of the yttrium chloride feed liquid to be 3.0mL/min, and the precipitation temperature to be 85 mL/minoC, the pH value in the precipitation process is 6.2, the stirring speed is 100r/min, when the addition amount of yttrium chloride is 400mL, the parallel flow feeding is stopped, then the pH value of the precipitation end point is adjusted to be 7.0 by adopting a sodium carbonate solution, the yttrium carbonate filter cake is obtained by filtering and washing, and the yttrium carbonate filter cake is placed at 80 DEG CoCDrying to finally obtain (D)90-D10)/(2D50) Y in the narrow distribution form of 0.62(CO3)3•3H2O。
Example 5
Adding bottom water into a reaction kettle, controlling the bottom water to submerge a stirring paddle blade, then adding 0.15mol/L yttrium chloride feed liquid and 0.2mol/L sodium carbonate solution in a concurrent flow manner for reaction, controlling the feeding speed of the yttrium chloride feed liquid to be 3.0mL/min, and controlling the reaction temperature to be 80 DEG CoAnd C, the pH value in the reaction process is 6.2, the stirring speed is 400r/min, the reaction is stopped when the addition of the yttrium chloride feed liquid is 300mL, and the crystallization performance of the obtained yttrium carbonate seed crystal is good. Filtering and washing to obtain a filter cake, mixing the filter cake with water, controlling the slurry to submerge a stirring paddle blade, then adding 1.2mol/L yttrium chloride feed liquid and 1.5mol/L sodium carbonate solution in a concurrent flow manner for precipitation reaction, controlling the feeding speed of the yttrium chloride feed liquid to be 4.0mL/min and the precipitation temperature to be 85 mL/minoC, precipitatingThe process pH is 6.5, the stirring speed is 400r/min, when the adding amount of yttrium chloride is 400mL, the parallel flow feeding is stopped, then the precipitation end point pH is adjusted to 7.0 by adopting a sodium carbonate solution, the yttrium carbonate filter cake is obtained by filtering and washing, and the yttrium carbonate filter cake is placed at 70oCDrying to finally obtain (D)90-D10)/(2D50) Y in the form of a narrow distribution of 0.52(CO3)3•3H2O。
Example 6
Adding bottom water into a reaction kettle, controlling the bottom water to submerge blades of a stirring paddle, then adding 0.12mol/L yttrium chloride feed liquid and 0.24mol/L sodium carbonate solution in a concurrent flow manner for reaction, controlling the feeding speed of the yttrium chloride feed liquid to be 2.5mL/min, and controlling the reaction temperature to be 85 DEGoAnd C, the pH value in the reaction process is 6.1, the stirring speed is 250r/min, the reaction is stopped when the addition amount of the yttrium chloride feed liquid is 300mL, and the crystallization performance of the obtained yttrium carbonate seed crystal is good. Mixing the yttrium carbonate crystal seed, controlling the slurry to submerge a stirring paddle blade, then adding 0.12mol/L yttrium chloride feed liquid and 0.24mol/L sodium carbonate solution in a flowing manner for reaction, controlling the feeding speed of the yttrium chloride feed liquid to be 2.5mL/min, and controlling the reaction temperature to be 85 DEGoAnd C, the pH value in the reaction process is 6.1, the stirring speed is 250r/min, the reaction is stopped when the addition amount of the yttrium chloride feed liquid is 300mL, and the crystallization performance of the obtained yttrium carbonate seed crystal is good. Filtering and washing to obtain a filter cake, mixing the filter cake with water, controlling the slurry to submerge a stirring paddle blade, then adding 0.8mol/L yttrium chloride feed liquid and 1.2mol/L sodium carbonate solution in a concurrent flow manner for precipitation reaction, controlling the feeding speed of the yttrium chloride feed liquid to be 6.0mL/min, and the precipitation temperature to be 75oC, the pH value in the precipitation process is 6.4, the stirring speed is 100r/min, when the addition amount of yttrium chloride is 400mL, the parallel flow feeding is stopped, then the pH value of the precipitation end point is adjusted to be 7.2 by adopting a sodium carbonate solution, the yttrium carbonate filter cake is obtained by filtering and washing, and the yttrium carbonate filter cake is placed at 60 DEGoCDrying to finally obtain (D)90-D10)/(2D50) Y of narrow distribution crystal form of 0.352(CO3)3•3H2O。
Claims (5)
1. A method for preparing narrow-distribution crystal form yttrium carbonate by sodium carbonate precipitation is characterized by comprising the following steps:
(1) preparing seed crystals: adding bottom water into the reaction kettle, controlling the bottom water to submerge a stirring paddle blade, then adding yttrium chloride feed liquid and sodium carbonate solution in a parallel flow manner for reaction, and filtering and washing after the reaction is finished to obtain yttrium carbonate seed crystals; the concentration of yttrium chloride feed liquid is 0.05-0.15mol/L, the concentration of sodium carbonate solution is 0.05-0.30mol/L, the feeding speed of yttrium chloride feed liquid is controlled to be 1.0-3.0mL/min, the reaction temperature is controlled to be 75-85 ℃, and the pH value in the reaction process is controlled to be 5.8-6.2;
(2) and (3) precipitation process: mixing yttrium carbonate seed crystals with water, controlling the slurry to submerge a stirring paddle blade, then adding yttrium chloride feed liquid and sodium carbonate solution in a parallel flow manner for precipitation reaction, and filtering and washing after the reaction is finished to obtain yttrium carbonate filter cakes; the concentration of yttrium chloride feed liquid is 0.2-1.5mol/L, the concentration of sodium carbonate solution is 0.3-1.5mol/L, the feeding speed of yttrium chloride feed liquid is controlled to be 3.0-10.0mL/min, the precipitation temperature is controlled to be 70-90oC, controlling the pH value in the precipitation process to be 5.5-6.5;
(3) and (3) drying: drying the yttrium carbonate filter cake at 40-80 ℃ to finally obtain (D)90-D10)/(2D50) Y of narrow distribution crystal form less than 0.82(CO3)3•3H2O。
2. The method according to claim 1, wherein the feeding positions of the yttrium chloride feed liquid and the sodium carbonate solution in the step (1) and the step (2) are below the liquid level and are distributed on two opposite sides.
3. The method according to claim 1, wherein the precipitation end point pH in the step (2) is controlled to be 7.0 to 7.5.
4. The method as claimed in claim 1, wherein the stirring speed in step (1) and step (2) is 400 r/min.
5. The method according to claim 1, wherein the yttrium carbonate seed crystal is prepared by a circulation method, specifically, the seed crystal obtained in the step (1) is slurried and returned to be used as the base solution in the step (1), new yttrium carbonate seed crystal is prepared and obtained through the reaction conditions in the step (1), and the finally obtained yttrium carbonate seed crystal is reused in the step (2) after 2-4 times of circulation.
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