CN115321577A - Preparation method of yttrium oxide - Google Patents
Preparation method of yttrium oxide Download PDFInfo
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- CN115321577A CN115321577A CN202211051777.1A CN202211051777A CN115321577A CN 115321577 A CN115321577 A CN 115321577A CN 202211051777 A CN202211051777 A CN 202211051777A CN 115321577 A CN115321577 A CN 115321577A
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- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/218—Yttrium oxides or hydroxides
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- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P2006/80—Compositional purity
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Abstract
The invention discloses a preparation method of yttrium oxide, which comprises the following steps: s1, adding hydrochloric acid into yttrium-containing raw materials, enabling the hydrochloric acid and the yttrium-containing raw materials to fully react, filtering, adding inorganic acid into filtrate, fully reacting, evaporating partial hydrochloric acid after the reaction is finished, adding distilled water, recovering the evaporated hydrochloric acid, centrifuging and washing after the solution is fully crystallized to obtain crude yttrium salt; the crude yttrium salt is treated by two methods: firstly, firing is carried out; secondly, purifying; the purification preparation steps are as follows: s2, adding distilled water and a small amount of hydrochloric acid into the crude yttrium to dissolve the crude yttrium, heating the crude yttrium to crystallize the solution, and centrifuging and washing the crude yttrium after the crystallization of the solution is finished to obtain fine yttrium salt; s3, firing the refined yttrium salt to obtain yttrium oxide; the invention adopts a closed cycle process, can effectively recycle and reutilize raw materials in the preparation process, and avoids environmental pollution; the preparation method is simple, the cost of raw materials is extremely low, and the production cost is greatly saved in industrial production.
Description
Technical Field
The invention relates to the technical field of chemical preparation, in particular to a preparation method of yttrium oxide.
Background
Chemical formula Y 2 O 3 White yellowish powder, insoluble in water and alkali, soluble in acid. It is mainly used for making magnetic material for microwave and important material for military industry (single crystal, yttrium iron garnet, yttrium aluminium garnet, etc. composite oxide), and also can be used as optical glass, ceramic material additive, high-brightness fluorescent powder for large-screen TV and other kinescope coating material. And also for the production of thin-film capacitors and special refractory materials, and also for the production of blister materials for high-pressure mercury lamps, lasers, storage elements, etc.The addition of yttrium oxide during sintering can effectively reduce the grain size of the tungsten alloy. The manufacture of light sources in infrared spectrometers, mantles for acetylene and gas lamps, phosphors for color television tubes, stabilizers for zirconia refractory materials, phosphors, synthetic gemstone laser crystals, superconductors and many advanced applications in the electronics industry.
Most of the yttrium oxide powder is prepared by an oxalic acid precipitation process or a multistage extraction process at present, oxalic acid is required to be added in the preparation process by adopting the oxalic acid precipitation process, the price of the oxalic acid is high, and the oxalic acid is difficult to treat after the preparation is finished, so that the environmental pollution is caused; in the multistage extraction process, organic reagents are usually adopted as the extracting agents, for example, a mode of performing three-stage extraction by adopting Cyanex272 is provided in the application number CN201610525689.9, the preparation steps are complex, the price of the extracting agents is high, the cost is high, the large-area application to industrial production is difficult, and most of the organic extracting agents are easy to diffuse into the air in the process of preparing yttrium oxide, so that the environmental pollution is caused.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the preparation method of the yttrium oxide, and the method adopts a closed cycle process, can effectively recycle and reutilize raw materials in the preparation process and avoids environmental pollution; the preparation method is simple, and greatly saves the production cost.
The purpose of the invention is realized by the following technical scheme:
a preparation method of yttrium oxide comprises the following steps:
s1, adding hydrochloric acid into yttrium-containing raw materials, enabling the hydrochloric acid and the yttrium-containing raw materials to fully react, filtering after the reaction is finished, adding inorganic acid into filtrate, fully reacting, evaporating partial hydrochloric acid after the reaction is finished, adding distilled water, recovering the evaporated hydrochloric acid, centrifuging and washing solids after the solution is fully crystallized, and obtaining crude yttrium salt;
the crude yttrium salt is treated by two methods: firstly, firing; secondly, purifying;
the purification preparation steps are as follows:
s2, adding distilled water and a small amount of hydrochloric acid into the crude yttrium to dissolve the crude yttrium, heating the crude yttrium to crystallize the solution, and centrifuging and washing the solid after the crystallization of the solution is finished to obtain refined yttrium salt;
s3, burning the refined yttrium salt to obtain the yttrium oxide.
As some possible embodiments of the present application, in S1, the reaction temperature of the yttrium ore and the hydrochloric acid is 80-95 ℃, and the reaction time is 1-1.5h.
As some possible embodiments of the present application, in the S1, the temperature at the time of filtration is 50 to 60 ℃.
As some possible embodiments of the present application, after the inorganic acid is added to S1, the reaction temperature is 60-80 ℃ and the reaction time is 5.5-6.5h.
As some possible embodiments of the present application, in S2, the temperature for increasing the temperature is 80 to 95 ℃.
As some possible embodiments of the present application, the temperature of the distilled water added in S2 is 7 to 20 ℃.
As some possible embodiments herein, the mineral acid is sulfuric acid.
As some possible embodiments of the present application, the yttrium-containing feedstock is an yttria-containing ore.
As some possible embodiments of the present application, the centrifugation speed in S1 and S2 is 800-1200r/min.
As some possible embodiments of the present application, the temperature of washing in S1 and S2 is 80-95 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. the cost of the invention is low, and at least comprises the following two reasons:
(1) the chemical raw materials in the invention are hydrochloric acid and sulfuric acid, which have low cost and convenient acquisition, and overcome the defect of high cost caused by adopting high-price oxalic acid or high-price organic extractant and other raw materials to prepare yttrium oxide in the prior art; (2) the preparation method has the advantages of few preparation steps, low preparation temperature and simple preparation method, can greatly save the production cost and energy consumption, and is suitable for industrial production. According to the calculation: the invention prepares one ton of yttrium oxide with purity more than 99.95%, and the cost is about 9900-11900 yuan, which is far lower than the prior art, such as oxalic acid precipitation method or multistage series extraction method.
2. The invention adopts a closed loop mode, the volatilized hydrochloric acid can be directly recycled in the closed loop, the waste of the hydrochloric acid or the environmental pollution caused by the emission of the hydrochloric acid to the atmosphere is avoided, meanwhile, compared with an organic extractant, the sulfuric acid in the invention can not volatilize, and the treatment is convenient after the preparation, and the environmental pollution can not be generated.
3. According to different industrial requirements on the purity of the yttrium oxide, the invention provides two preparation methods, wherein the purity of the yttrium oxide prepared by one preparation method is more than 99 percent; the purity of the yttrium oxide prepared by the second step is not less than 99.95 percent, the yield is not less than 97.35 percent, the particle size distribution is 2.5-3 mu m, the particle size distribution is uniform, and the density is high.
Description of the drawings:
FIG. 1: the preparation scheme in example 1;
FIG. 2: preparation schemes in examples 2-4.
Detailed Description
The technical solutions in the embodiments of the present application will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
In the prior art, most of yttrium oxide powder is prepared by an oxalic acid precipitation process or a multi-stage extraction process, oxalic acid is required to be added in the preparation process by adopting the oxalic acid precipitation process, the price of the oxalic acid is high, and the oxalic acid is difficult to treat after the preparation is finished, so that the environmental pollution is caused; in the multistage extraction process, an organic reagent is usually adopted as an extractant, the preparation steps are complex, the price of the extractant is high, the cost is high, the large-area application to industrial production is difficult, and most organic extractants are easy to diffuse into the air, so that the environment pollution is caused.
Based on the above, the invention provides a preparation method of yttrium oxide, which comprises the following steps:
s1, adding hydrochloric acid into yttrium-containing raw materials, enabling the hydrochloric acid and the yttrium-containing raw materials to fully react, filtering after the reaction is finished, adding inorganic acid into filtrate, fully reacting, evaporating partial hydrochloric acid after the reaction is finished, adding distilled water, recovering the evaporated hydrochloric acid, centrifuging and washing solids after the solution is fully crystallized, and obtaining crude yttrium salt;
the crude yttrium salt is treated by two methods: firstly, firing is carried out; secondly, purifying;
the purification preparation steps are as follows:
s2, adding distilled water and a small amount of hydrochloric acid into the crude yttrium to dissolve the crude yttrium, heating the crude yttrium to crystallize the solution, and centrifuging and washing the solid after the crystallization of the solution is finished to obtain fine yttrium salt;
s3, burning the refined yttrium salt to obtain the yttrium oxide.
Firstly, reacting yttrium-containing raw materials with hydrochloric acid to generate yttrium chloride solution, then adding inorganic acid into the yttrium chloride solution, fully reacting to generate yttrium salt precipitate, then evaporating partial hydrochloric acid, adding a small amount of water to increase acidity in turbid liquid, so as to reduce solubility of yttrium salt, so that yttrium salt precipitate is more fully separated out, and then centrifugally washing the precipitate to obtain crude yttrium salt, wherein the crude yttrium salt can be treated by two modes, one mode can be directly fired, and the content of yttrium oxide after firing is about 99%, so that the crude yttrium salt can be directly sold; secondly, the purification can be continued, and the purification process is as follows: adding hydrochloric acid and distilled water into the crude yttrium salt to increase the acidity of turbid liquid and improve the solubility of the crude yttrium salt, after the dissolution is finished, heating to reduce the solubility of the yttrium salt so as to recrystallize the yttrium salt, centrifuging and washing to obtain refined yttrium salt, and keeping other impurities in mother liquor; sintering the refined yttrium salt at high temperature to obtain yttrium oxide with the purity of more than or equal to 99.95. The yttrium oxide is prepared in a closed cycle mode, so that the environment pollution caused by the volatilization of hydrochloric acid can be avoided, and the environment pollution caused by improper treatment after the reaction is finished can be avoided by using inorganic acid as a raw material; the yttrium oxide prepared by the two methods provided by the invention has higher purity and the cost is far lower than that of the prior art.
In order to further improve the purity and yield of the yttrium oxide and reduce the particle size of the yttrium oxide, as some possible embodiments of the present application, the reaction temperature and reaction time of the yttrium-containing raw material and hydrochloric acid are further limited, that is, in S1, the reaction temperature of the yttrium-containing raw material and hydrochloric acid is 80-95 ℃ and the reaction time is 1-1.5h. At the temperature and the reaction time, the yttrium oxide can fully react with the hydrochloric acid, so that the reaction speed is improved; in addition, the solubility of the yttrium chloride can be improved by properly increasing the temperature, and the problem that the purity of the yttrium chloride is reduced due to crystallization of the yttrium chloride at low temperature is avoided; the problem that the reaction of yttrium oxide is insufficient due to too high temperature to volatilize hydrochloric acid too fast can be avoided, and the yield and the purity of yttrium oxide are reduced; if the reaction time is too long, more heat energy is consumed, resulting in cost waste.
In order to further improve the purity and yield of the yttrium oxide and reduce the particle size of the yttrium oxide, as some possible embodiments of the present application, the filtering temperature in step S1 is further defined, i.e. in S1, the filtering temperature is 50-60 ℃.
In order to further improve the purity and yield of the yttrium oxide and reduce the particle size of the yttrium oxide, as some possible embodiments of the present application, the reaction temperature and the reaction time after the addition of the inorganic acid in step S1 are further limited, i.e. in step S1, after the addition of the inorganic acid, the reaction temperature is 60 to 80 ℃ and the reaction time is 5.5 to 6.5 hours. The solubility of the yttrium salt is reduced along with the increase of the temperature, and the reaction can accelerate the reaction speed and reduce the solubility of the yttrium salt at the temperature, so that the reaction is promoted to be carried out towards the generation direction of the yttrium salt all the time, and the conversion rate of the yttrium salt is improved.
In order to further improve the purity and yield of the yttria and reduce the grain size of the yttria, as some possible embodiments of the present application, the temperature increase in step S2 is further defined, that is, in S2, the temperature increase is 80-95 ℃. As the solubility of the yttrium salt is reduced along with the increase of the temperature, the solubility of the yttrium salt can be greatly reduced by increasing the temperature to 80-95 ℃, and then the precipitation of the yttrium salt is promoted.
In order to further improve the purity and yield of the yttria and reduce the grain size of the yttria, as some possible embodiments of the present application, the temperature of the distilled water in the step S1 is further limited, that is, in the step S2, the temperature of the added distilled water is 7-20 ℃. At this temperature, the solubility of yttrium salt is about 7.4-8, and the solubility is greater, which promotes dissolution of yttrium salt.
In order to further improve the purity and yield of the yttria and reduce the particle size of the yttria, as some possible embodiments of the present application, the type of the inorganic acid is further defined, i.e., the inorganic acid is sulfuric acid. The properties of the sulfuric acid meet the requirements of the invention on the inorganic acid, and the purity and yield of the yttrium oxide can be greatly improved by using the sulfuric acid as the inorganic acid.
In order to further increase the purity and yield of the yttrium oxide, and to reduce the particle size of the yttrium oxide, as some possible embodiments of the present application, further limitations are made on the type of yttrium-containing raw material, i.e., various types of ores containing yttrium oxide.
In order to further improve the purity of the yttria and the grain size uniformity of the yttria, as some possible embodiments of the present application, the centrifugation speed in steps S1 and S2 is further limited, that is, the centrifugation speed in S1 and S2 is 800-1200r/min.
In order to further improve the purity of the yttria and the grain size uniformity of the yttria, as some possible embodiments of the present application, the washing speed in steps S1 and S2 is further limited, that is, the temperature in washing in S1 and S2 is 80-95 ℃. The solubility of the yttrium salt is reduced along with the rise of the temperature, and the dissolution of the yttrium salt can be reduced and the yield solubility of the yttrium salt is improved by controlling the washing temperature.
The preparation of the yttria described herein is described in further detail below with reference to specific embodiments; it is worth mentioning that: the various starting materials in the examples are commercially available products.
Example 1 (preparation scheme shown in FIG. 1)
S1, weighing 10kg of ore containing 20% of yttrium oxide and 8kg of 31% hydrochloric acid in a reaction kettle, heating the ore and the hydrochloric acid to enable the ore and the hydrochloric acid to react for 1.5h at 80 ℃, cooling the ore to 50 ℃, filtering the ore, adding 3.5kg of 98% concentrated sulfuric acid into filtrate, reacting for 6h at 65 ℃, evaporating partial hydrochloric acid after the reaction is finished, adding distilled water to enable yttrium sulfate to be fully crystallized, centrifuging the solution at the speed of 800r/min, and washing and precipitating the solution by using hot water at 80 ℃ to obtain crude yttrium sulfate; in the process, the evaporated hydrochloric acid needs to be recovered to realize closed circulation in the preparation process; and then burning the crude yttrium sulfate to obtain yttrium oxide.
The hydrochloric acid recovered as described above may be used for the reaction with the ore in step S1.
The purity of the obtained yttrium oxide is 99.03 percent and the particle size distribution is uniform by detecting according to the national standard.
The preparation schemes of the following examples 2-4 are shown in FIG. 2, and specifically as follows:
example 2
S1, weighing 10.5kg of ore containing 25% of yttrium oxide and 8.3kg of 31% hydrochloric acid into a reaction kettle, heating the ore and the hydrochloric acid to enable the ore and the hydrochloric acid to react for 1.2h at the temperature of 85 ℃, cooling the ore to 60 ℃, filtering the ore, adding 4.5kg of 98% concentrated sulfuric acid into the filtrate, reacting for 6.5h at the temperature of 60 ℃, evaporating partial hydrochloric acid after the reaction is finished, adding distilled water to fully crystallize yttrium sulfate, centrifuging the yttrium sulfate at the speed of 1000r/min, and washing and precipitating the yttrium sulfate by using hot water at the temperature of 90 ℃ to obtain crude yttrium sulfate; in the process, the evaporated hydrochloric acid needs to be recovered to realize closed circulation;
s2, adding distilled water at 10 ℃ and a small amount of hydrochloric acid into the crude yttrium sulfate, heating to 90 ℃ after the crude yttrium sulfate is completely dissolved, fully crystallizing, centrifuging at the speed of 1000r/min, and washing with hot water at 90 ℃ to obtain refined yttrium sulfate;
s3, burning the refined yttrium sulfate to obtain yttrium oxide.
The hydrochloric acid recovered as described above may be used for the reaction with the ore in step S1, and may also be used for dissolving the crude sulfuric acid ore in step S2.
Detecting the obtained yttrium oxide according to the national standard, wherein the purity of the yttrium oxide is 99.95 percent, and the yield of the yttrium oxide is 97.35 percent; the obtained yttrium oxide is tested by a laser particle size analyzer, the particle size distribution is 2.5-3 mu m, the particle size distribution is uniform, and the density is high; the cost for preparing 1 ton of yttrium oxide according to the method is 9900-10200 yuan.
Example 3
S1, weighing 9.7kg of ore containing 50.7% of yttrium oxide and 17.1kg of 35% hydrochloric acid in a reaction kettle, heating the ore and the hydrochloric acid to enable the ore and the hydrochloric acid to react at the temperature of 90 ℃ for 1 hour, cooling the ore and the hydrochloric acid to 50 ℃ and filtering the ore and the hydrochloric acid, adding 42.98kg of 94% concentrated sulfuric acid into the filtrate, reacting the filtrate at the temperature of 80 ℃ for 5.5 hours, evaporating partial hydrochloric acid after the reaction is finished, adding distilled water to fully crystallize yttrium sulfate, centrifuging the crystallized product at the speed of 1100r/min, and washing and precipitating the crystallized product with hot water at the temperature of 85 ℃ to obtain crude yttrium sulfate; in the process, the evaporated hydrochloric acid needs to be recovered to realize closed circulation;
s2, adding distilled water at 10 ℃ and a small amount of hydrochloric acid into the crude yttrium sulfate, heating to 90 ℃ after the crude yttrium sulfate is completely dissolved, fully crystallizing, centrifuging at the speed of 1100r/min, and washing with hot water at 85 ℃ to obtain refined yttrium sulfate;
s3, burning the refined yttrium sulfate to obtain yttrium oxide with the purity of 99.94.
Detecting the obtained yttrium oxide according to national standard, wherein the purity is 99.961 percent, and the yield is 97.57 percent; the obtained yttrium oxide is tested by a laser particle size analyzer, the particle size distribution is 2.6-3 mu m, the particle size distribution is uniform, and the density is high; the cost required for preparing 1 ton of yttrium oxide according to the method is 10000-11500 yuan.
Example 4
S1, weighing 10.7kg of ore containing 57% of yttrium oxide and 8.3kg of 35% hydrochloric acid in a reaction kettle, heating the ore and the hydrochloric acid to enable the ore and the hydrochloric acid to react for 1.2h at the temperature of 85 ℃, cooling the ore to 55 ℃, filtering the ore, adding 4.5kg of 98% concentrated sulfuric acid into filtrate, reacting for 5.8h at the temperature of 75 ℃, evaporating partial hydrochloric acid after the reaction is finished, adding distilled water to enable yttrium sulfate to be fully crystallized, centrifuging the solution at the speed of 1000r/min, and washing and precipitating the solution by using hot water at the temperature of 85 ℃ to obtain crude yttrium sulfate; in the process, the evaporated hydrochloric acid needs to be recovered to realize closed circulation;
s2, adding distilled water at 10 ℃ and a small amount of hydrochloric acid into the crude yttrium sulfate, heating to 85 ℃ after the crude yttrium sulfate is completely dissolved, fully crystallizing, centrifuging at the speed of 1000r/min, and washing with hot water at 85 ℃ to obtain refined yttrium sulfate;
s3, burning the refined yttrium sulfate to obtain yttrium oxide.
Detecting the obtained yttrium oxide according to the national standard, wherein the purity is 100.02 percent, and the yield is 97.73 percent; the obtained yttrium oxide is tested by a laser particle size analyzer, the particle size distribution is 2.5-2.85 μm, the particle size distribution is uniform, and the density is high; the cost for preparing 1 ton of yttrium oxide according to the method is 10700-11900 yuan.
It is worth mentioning that: the dosage in the embodiments 1 to 4 is experimental dosage, that is, experimental data of early-stage testing, the actual dosage can be adjusted according to actual requirements and proportion, and particularly in industrial plants, the addition proportion can be selected according to the scale of the plant; as can be seen from the cost in examples 2-4, a ton of yttria with a purity of > 99.95% was prepared according to any of the methods of examples 2-4 of the present invention, at a cost of about 9900-11900 RMB; the cost is lower because of the fewer steps in example 1.
Comparative example 1
Compared with the example 1, the reaction temperature of the ore and the hydrochloric acid is changed to normal temperature, and the rest steps and parameters are the same as the example 1.
The purity of the prepared yttrium oxide is 92.47 percent by national standard detection.
Comparative example 2
The temperature of the water washing in step S1 and step S2 was adjusted to room temperature as compared with example 4, and the rest of the steps and parameters were the same as those in example 4.
The purity of the prepared yttrium oxide is 94.31 percent by detection according to the national standard.
Comparative example 3
Compared with the example 4, the water washing temperature in the step S1 and the step S2 is adjusted to normal temperature, and the rest steps and parameters are the same as those in the example 4.
The purity of the prepared yttrium oxide is 95.19 percent by detection according to the national standard.
Comparative example 4
Taking 10.1kg of ore containing 57% of yttrium oxide, and preparing yttrium oxide according to an oxalic acid precipitation method; the purity of the yttrium oxide is 99.41 percent and the yield is 96.2 percent through the inspection of national standard; testing the obtained yttrium oxide by using a laser particle size analyzer, wherein the particle size distribution is 2.7-3.5 mu m, the particle size distribution is uniform, and the particle size is not much different from that of the yttrium oxide; the cost for preparing one ton of yttrium oxide by oxalic acid precipitation method is 58000-61000 yuan.
As can be seen from examples 1 to 4 and comparative examples 1 to 4: the purity of the yttrium oxide prepared by the method in the embodiment 1 is 99.03 percent, the purity of the yttrium oxide prepared by the method in the embodiments 2-4 is not lower than 99.95 percent, the yield is not lower than 97.35 percent, the particle size distribution is 2.5-3 mu m, and the density is high; while comparative examples 1-3 were not prepared exactly as in the present invention and were of lower purity, comparative example 4 was prepared according to the prior art process with yttrium oxide of higher purity than comparative examples 1-3; compared with the examples 2-4 in the invention, the grain size of the yttrium oxide in the comparative example 4 is not much different from that of the invention, and both the yttrium oxide and the yttrium oxide belong to micron-sized grain sizes, but both the yttrium oxide and the yttrium oxide have uniform grain size distribution, and are both suitable for preparing large-grain-size grains; however, the purity and yield of yttrium oxide in comparative example 4 are lower than those of the present invention, and most importantly, the cost in comparative example 4 is much higher than that of the present invention, and the residual oxalic acid in comparative example 4 causes environmental pollution and also causes investment cost in oxalic acid treatment.
As can be seen from comparative example 4 and inventive examples 2 to 4: the invention provides a preparation method of micron-level yttrium oxide with the grain diameter equivalent to that of the prior art (oxalic acid precipitation method), but the purity and the yield are higher than those of the prior art, the production cost is far lower than that of the prior art, the preparation method is extremely suitable for industrial plants, and the preparation method of the yttrium oxide has high efficiency and low cost; in addition, the method in the embodiment 1 is very effective, the purity is more than 99 percent, the cost is very low, the method in the embodiment 1 or the method in the embodiment 2 to 4 can be selected according to the requirement during the actual production, the purity and the price are different greatly, namely, the purity is higher, the selling price is higher, the difficulty in industrial production is higher, and the cost performance is very high by analyzing the cost, the preparation steps, the purity, the yield and the pollution degree of air.
The foregoing is merely a preferred embodiment of the invention, it is to be understood that the invention is not limited to the forms disclosed herein, but is not intended to be exhaustive or to limit the invention to other embodiments, and to various other combinations, modifications, and environments and may be modified within the scope of the inventive concept as expressed herein, by the teachings or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of yttrium oxide is characterized by comprising the following steps:
s1, adding hydrochloric acid into yttrium-containing raw materials, enabling the hydrochloric acid and the yttrium-containing raw materials to fully react, filtering after the reaction is finished, adding inorganic acid into filtrate, fully reacting, evaporating partial hydrochloric acid after the reaction is finished, adding distilled water, recycling the evaporated hydrochloric acid, and centrifuging and washing solids after the solution is fully crystallized to obtain crude yttrium salt;
the crude yttrium salt is treated by two methods: firstly, firing; secondly, purifying;
the purification preparation steps are as follows:
s2, adding distilled water and a small amount of hydrochloric acid into the crude yttrium to dissolve the crude yttrium, heating the crude yttrium to crystallize the solution, and centrifuging and washing the solid after the crystallization of the solution is finished to obtain fine yttrium salt;
s3, burning the refined yttrium salt to obtain the yttrium oxide.
2. A process according to claim 1, wherein the reaction temperature of the yttrium ore and hydrochloric acid in S1 is 80-95 ℃ and the reaction time is 1-1.5h.
3. The method according to claim 1, wherein the temperature during filtration in S1 is 50-60 ℃.
4. The method according to claim 1, wherein the reaction temperature of S1 is 60-80 ℃ and the reaction time is 5.5-6.5h after the addition of the inorganic acid.
5. The method according to claim 1, wherein the temperature of the step S2 is increased to 80 to 95 ℃.
6. The method according to claim 1, wherein the temperature of the distilled water added in S2 is 7 to 20 ℃.
7. A process according to claim 1, wherein the inorganic acid is sulfuric acid.
8. A process according to claim 1, wherein the yttrium-containing source material is an yttrium oxide-containing ore.
9. The method according to claim 1, wherein the centrifugation speed of each of S1 and S2 is 800-1200r/min.
10. The method according to claim 1, wherein the washing temperature of each of S1 and S2 is 80-95 ℃.
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| CN202211051777.1A CN115321577A (en) | 2022-08-29 | 2022-08-29 | Preparation method of yttrium oxide |
| CN202311090329.7A CN117208952A (en) | 2022-08-29 | 2023-08-28 | Preparation method of yttrium oxide |
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| CN202211051777.1A Withdrawn CN115321577A (en) | 2022-08-29 | 2022-08-29 | Preparation method of yttrium oxide |
| CN202311090329.7A Pending CN117208952A (en) | 2022-08-29 | 2023-08-28 | Preparation method of yttrium oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115838185A (en) * | 2022-12-09 | 2023-03-24 | 宣城晶瑞新材料有限公司 | Preparation method of nano yttrium oxide material |
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| US20170107597A1 (en) * | 2015-10-20 | 2017-04-20 | National Chung Shan Institute Of Science And Technology | Method of purifying yttrium |
| CN108910932A (en) * | 2018-09-02 | 2018-11-30 | 江西理工大学 | A kind of method that sodium carbonate precipitating prepares narrow ditribution ultrafine yttria |
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- 2022-08-29 CN CN202211051777.1A patent/CN115321577A/en not_active Withdrawn
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- 2023-08-28 CN CN202311090329.7A patent/CN117208952A/en active Pending
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| CN115838185A (en) * | 2022-12-09 | 2023-03-24 | 宣城晶瑞新材料有限公司 | Preparation method of nano yttrium oxide material |
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