CN117466251A - Method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide - Google Patents
Method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide Download PDFInfo
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- CN117466251A CN117466251A CN202311562447.3A CN202311562447A CN117466251A CN 117466251 A CN117466251 A CN 117466251A CN 202311562447 A CN202311562447 A CN 202311562447A CN 117466251 A CN117466251 A CN 117466251A
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- yttrium
- perchlorate
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- rare earth
- yttrium perchlorate
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- IYECSZYJKQPOOA-UHFFFAOYSA-K yttrium(3+);triperchlorate;hexahydrate Chemical compound O.O.O.O.O.O.[Y+3].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O IYECSZYJKQPOOA-UHFFFAOYSA-K 0.000 title claims abstract description 121
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 47
- -1 rare earth yttrium oxide Chemical class 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 28
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000013078 crystal Substances 0.000 claims abstract description 37
- 238000005406 washing Methods 0.000 claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 18
- 239000004094 surface-active agent Substances 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 230000010355 oscillation Effects 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- NASANMXFTVINAA-UHFFFAOYSA-N perchloric acid yttrium Chemical compound [Y].Cl(=O)(=O)(=O)O NASANMXFTVINAA-UHFFFAOYSA-N 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 22
- 239000000047 product Substances 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims description 12
- 239000000460 chlorine Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 7
- 229910052801 chlorine Inorganic materials 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 229910001923 silver oxide Inorganic materials 0.000 claims description 6
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 3
- 239000003945 anionic surfactant Substances 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 52
- 239000000523 sample Substances 0.000 description 6
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 4
- 238000011978 dissolution method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000005571 anion exchange chromatography Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- OSWPMRLSEDHDFF-UHFFFAOYSA-N methyl salicylate Chemical compound COC(=O)C1=CC=CC=C1O OSWPMRLSEDHDFF-UHFFFAOYSA-N 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 229910020366 ClO 4 Inorganic materials 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 150000003983 crown ethers Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229960001047 methyl salicylate Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B11/00—Oxides or oxyacids of halogens; Salts thereof
- C01B11/16—Perchloric acid
- C01B11/18—Perchlorates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide, which comprises the following steps: obtaining nano rare earth yttrium oxide powder and a strong acid solution dilute perchloric acid solution; adding rare earth yttrium oxide powder into a dilute perchloric acid solution in an excessive amount, and dissolving the rare earth yttrium oxide powder under the condition of low-speed stirring to generate a crude perchloric acid yttrium solution; enriching primary yttrium perchlorate crystals and washing for the first time; adjusting the yttrium perchlorate solution after primary washing to a semi-crystalline semi-solution state, adding a surfactant, performing ultrasonic oscillation, and calcining to obtain nano yttrium perchlorate crystals; and (5) performing secondary washing, and repeatedly performing dissolving and drying treatment until high-purity yttrium perchlorate crystals are obtained. After the primary product of yttrium perchlorate is produced, the microscopic morphology of the yttrium perchlorate is limited by utilizing an ultrasonic oscillation mode, so that the yttrium perchlorate product with high product controllability can be produced, and the method has the advantages of stable product quality and good repeatability.
Description
Technical Field
The invention relates to a preparation method of yttrium perchlorate, in particular to a method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide.
Background
Yttrium perchlorate is a perchlorate of yttrium and has the formula Y (ClO 4 ) 3 The mixture of yttrium perchlorate and methyl salicylate can be used for capturing, stably storing and measuring nitric oxide, and can also be used for protecting organic macromolecules such as proteins in organisms from being damaged by excessive nitric oxide, and meanwhile, the research of yttrium perchlorate in the direction of crown ether complexes is increasing. At present, yttrium perchlorate is generally synthesized by yttrium oxide and an acidic solution, and a synthesized product is directly evaporated into a crystalline state. However, the traditional yttrium perchlorate preparation method has simple synthesis mode, but the product particles are coarse, and the stability and repeatability of the product quality are poor, so that the performance of the yttrium perchlorate in application is unstable.
Disclosure of Invention
In order to solve the defects of the technology, the invention provides a method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide, which comprises the following steps:
s1, obtaining nano rare earth yttrium oxide powder;
s2, preparing a strong acid solution, wherein the strong acid solution is a dilute perchloric acid solution;
s3, adding the rare earth yttrium oxide powder into the dilute perchloric acid solution in an excessive manner, and dissolving the rare earth yttrium oxide powder under the condition of low-speed stirring to generate a crude perchloric acid yttrium solution;
s4, filtering out excessive rare earth yttrium oxide powder, and drying the obtained crude yttrium perchlorate solution to obtain enriched primary yttrium perchlorate crystals;
s5, dissolving primary yttrium perchlorate crystals into a concentrated solution and washing for the first time;
s6, adjusting the yttrium perchlorate solution after primary washing to a semi-crystalline semi-solution state, adding a surfactant, and carrying out ultrasonic oscillation at the temperature of 50-80 ℃ and under the neutral PH condition to obtain yttrium perchlorate suspension, wherein the suspension contains white precursor sediment;
s7, calcining to obtain nano yttrium perchlorate crystals;
s8, redissolving nano yttrium perchlorate crystals and performing secondary washing;
and S9, repeatedly dissolving and drying the yttrium perchlorate after the secondary washing until the high-purity yttrium perchlorate crystal is obtained.
Preferably, the preparation method of the strong acid diluted perchloric acid solution comprises the following steps: introducing chlorine into concentrated sulfuric acid solution, and reacting to produce perchloric acid, wherein the reaction equation is as follows:
Cl 2 +H 2 SO 4 →HClO 4 +HCl
adding silver oxide into the reaction product, precipitating silver chloride produced by the silver oxide and hydrochloric acid, removing HCl, filtering the precipitate to obtain a perchloric acid product, and dissolving the perchloric acid product to the concentration of 2-5mol/L.
Preferably, the drying treatment of the crude yttrium perchlorate solution in S4 and the drying method of the yttrium perchlorate after the secondary washing in S9 are as follows: the solution was transferred to a vacuum dryer containing phosphorus pentoxide, and the adsorbed water was dried using phosphorus pentoxide.
Preferably, the phosphorus pentoxide drying treatment temperature is 70 ℃.
Preferably, the dissolution method of the primary yttrium perchlorate crystal in S5, the dissolution method of the nano yttrium perchlorate crystal in S8 and the dissolution method of the yttrium perchlorate after the secondary washing in S9 are as follows: and (3) taking deionized water as a solvent, and completing dissolution treatment of yttrium perchlorate crystals at room temperature.
Preferably, the surfactant is an anionic surfactant including, but not limited to, sodium oleate.
Preferably, the calcination temperature of the nano yttrium perchlorate crystals is 200 to 240 ℃.
Preferably, in S5, the process of one washing is:
slowly adding diluted sodium hydroxide solution into the primary yttrium perchlorate solution, stirring and mixing at a low speed until the solution is neutral, and reacting sodium hydroxide with residual perchloric acid, wherein the reaction equation is as follows:
HClO 4 +NaOH→NaClO 4 +H 2 O
generated NaClO 4 The salt was removed by filtration and the filtered solution was collected.
Preferably, in S8, the secondary washing is performed by:
adding ethanol solution into the nano yttrium perchlorate solution, washing off surfactant impurities, enabling ethanol and yttrium perchlorate to exist in a complex form, and removing ethanol in a distillation mode to finish secondary washing.
Preferably, the yttrium perchlorate after the secondary washing is repeatedly dissolved and dried three times.
The invention discloses a method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide, which is characterized in that after an yttrium perchlorate primary product is produced, the microscopic morphology of the yttrium perchlorate is limited by utilizing an ultrasonic oscillation mode, and the yttrium perchlorate product with high product controllability can be produced.
Drawings
Fig. 1 is a schematic flow structure of the present invention.
FIG. 2 is a chromatogram of yttrium perchlorate in accordance with the present invention.
Detailed Description
The invention will be described in further detail with reference to the drawings and the detailed description.
The invention discloses a method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide, which is characterized in that the design idea of the method is as follows as can be seen from a flow chart shown in figure 1:
s1, acquiring a rare earth yttrium oxide raw material;
the nano-scale rare earth yttrium oxide is adopted as one of raw materials for synthesizing yttrium perchlorate, and the powder state of the rare earth yttrium oxide is checked, so that the rare earth yttrium oxide has no obvious moisture and no caking; if the rare earth yttrium oxide powder has the problems of dampness and caking, the moisture is removed by adopting a drying mode, and ball milling treatment is carried out under the condition of an argon protective atmosphere, so that the nano rare earth yttrium oxide powder with fine and uniform powder quality is obtained, and the subsequent full dissolution of the rare earth yttrium oxide raw material in an acid solution is facilitated.
S2, preparing a strong acid solution;
the specific preparation method of the strong acid solution is that the strong acid solution is a dilute perchloric acid solution, and the specific preparation method of the strong acid solution is that the chlorine method is adopted to prepare the strong acid dilute perchloric acid solution: under the safe condition, chlorine is introduced into a reaction kettle containing concentrated sulfuric acid solution, the chlorine is introduced in an aeration mode, the concentrated sulfuric acid and the chlorine meet to react to produce perchloric acid, and the reaction equation is as follows:
Cl 2 +H 2 SO 4 →HClO 4 +HCl
the concentrated sulfuric acid reacts with chlorine to generate perchloric acid product and hydrochloric acid impurity, silver oxide is added into the reaction product to remove hydrochloric acid, silver chloride precipitate can be produced by the reaction of silver oxide and hydrochloric acid, the impurity HCl is removed, the perchloric acid product is obtained after the precipitate is filtered, and the perchloric acid product is prepared into 2-5mol/L solution for reacting with rare earth yttrium oxide to generate yttrium perchlorate.
S3, synthesizing rare earth yttrium oxide and perchloric acid solution;
in order to ensure the sufficient production of yttrium perchlorate, excessive rare earth yttrium oxide powder is selected to be added, excessive rare earth yttrium oxide and perchloric acid also can fully react, so that perchloric acid solution is remained as little as possible to a certain extent, and the rare earth yttrium oxide is remained, so that the removal of precipitated impurities can be realized by a filtering mode, and the impurity removal treatment is greatly optimized.
The specific synthesis method comprises the following steps: and (3) adding the excessive rare earth yttrium oxide powder into a dilute perchloric acid solution, fully dissolving the rare earth yttrium oxide powder under the condition of low-speed stirring, and generating a crude perchloric acid yttrium solution through the synthesis reaction of the rare earth yttrium oxide and the perchloric acid solution.
S4, enriching yttrium perchlorate;
as described above, the crude yttrium perchlorate solution contains an excessive amount of rare earth yttrium oxide powder, and thus, the excessive amount of rare earth yttrium oxide powder is filtered off, and the crude yttrium perchlorate solution is obtained. And drying the obtained crude yttrium perchlorate solution to obtain enriched primary yttrium perchlorate crystals.
The drying treatment is carried out by introducing the crude yttrium perchlorate solution into a vacuum drier containing phosphorus pentoxide, drying and adsorbing hydrated moisture by phosphorus pentoxide, drying at 70deg.C to obtain primary yttrium perchlorate crystal.
S5, primary yttrium perchlorate crystals are washed once;
although the primary yttrium perchlorate crystals obtained hardly contain perchloric acid residues, in order to improve the product quality of the final yttrium perchlorate product, the treatment operation of perchloric acid residues is still carried out, deionized water is used as a solvent to dissolve the primary yttrium perchlorate crystals into a solution state, and then washing is carried out again.
The specific process of one-time washing is as follows:
slowly adding diluted sodium hydroxide solution into the primary yttrium perchlorate solution, stirring and mixing at a low speed until the solution is neutral, and reacting sodium hydroxide with residual perchloric acid, wherein the reaction equation is as follows:
HClO 4 +NaOH→NaClO 4 +H 2 O
generated NaClO 4 The salt can be removed by filtration, and the yttrium perchlorate solution is collected after the salt precipitate is removed by filtration.
S6, ultrasonically oscillating the yttrium perchlorate solution after primary washing;
and (3) carrying out moisture removal treatment on the yttrium perchlorate solution after primary washing collected in the step (S5) to enable the yttrium perchlorate solution to be in a semi-crystalline semi-solution state, and adding a surfactant, wherein the surfactant is an anionic surfactant including but not limited to sodium oleate. At this time, ultrasonic oscillation is carried out at a temperature of 50-80 ℃ and under a neutral pH condition, yttrium perchlorate is crushed into a specific structure by high-frequency mechanical waves of ultrasonic waves, and after ultrasonic treatment, an emulsified yttrium perchlorate suspension is obtained, wherein the suspension contains white precursor precipitate.
S7, calcining to obtain nano yttrium perchlorate crystals;
the semi-crystalline semi-solution is dispersed by resonance bubbles in an ultrasonic mode, precursor precipitates are adsorbed by a surfactant, so that the precursor precipitates grow on the surfactant, and nanoscale yttrium perchlorate crystals are separated out by controlling the calcination temperature. Through the combined action of the ultrasonic waves and the surfactant, the change of the shape of the yttrium perchlorate can be realized, and the nano yttrium perchlorate product with high product controllability is generated, and has the advantages of stable product quality and good repeatability. In addition, yttrium perchlorate is dehydrated at a temperature above 100 ℃ and starts to decompose at a temperature of 250-300 ℃, so that the calcination temperature is controlled between 200-240 ℃, and the rapid calcination crystallization is realized, so that the yttrium perchlorate is not decomposed.
S8, secondary washing of the nano yttrium perchlorate;
surfactant residues may be left in the nano yttrium perchlorate crystals obtained by calcination, so that the nano yttrium perchlorate crystals are dissolved again and subjected to secondary washing, wherein the secondary washing process comprises the following steps:
adding an ethanol solution into the nano yttrium perchlorate solution, and washing away surfactant impurities; the ethanol and the yttrium perchlorate exist in the form of a complex, and then the ethanol is removed by distillation, the distillation temperature is 80 ℃, and the secondary washing is completed.
S9, obtaining high-purity yttrium perchlorate crystals;
the step is a water washing process, and the yttrium perchlorate after the secondary washing is repeatedly dissolved and dried for three times until the high-purity yttrium perchlorate crystal is obtained. The dissolution method is that deionized water is used as a solvent, and the dissolution treatment of yttrium perchlorate crystals is completed under the condition of room temperature. The solution was transferred to a vacuum dryer containing phosphorus pentoxide, and the adsorbed water was dried using phosphorus pentoxide. The drying treatment temperature of phosphorus pentoxide is 70 ℃.
In summary, according to the method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide disclosed by the invention, the optimized post-treatment is carried out on the yttrium perchlorate, the ultrasonic treatment is adopted to carry out the dispersion treatment on the yttrium perchlorate, the nanoscale structure is formed, the ultrasonic oscillation mode only needs to control the temperature and PH, the controllability is strong, the product quality stability is high, and the advantages of good repeatability are achieved.
Further, the physical form of the high-purity yttrium perchlorate crystal is observed, the color form is uniform, and the crystal form is observed under a high-power mirror. The purity of the product is measured by adopting an anion chromatography method, a solution sample prepared by high-purity yttrium perchlorate crystals is injected into a chromatograph for measurement according to the same chromatographic conditions and steps as a standard curve, the solution sample is subjected to anion chromatography column exchange separation, a conductivity detector is used for detection, the product is qualitatively according to the retention time, the external standard method is used for quantification, and the mass concentration is calculated according to the following formula:
wherein ρ represents the mass concentration of yttrium perchlorate in a sample, mg/L;
h represents the peak area of yttrium perchlorate in the sample;
h0 represents the peak area of yttrium perchlorate in a blank sample;
a represents the intercept of the regression equation;
b represents the slope of the regression equation;
f represents the dilution factor of the sample.
As shown in figure 2, the chromatogram has single peak, reliable result, and the correlation coefficient r of the prepared sample concentration and the detection result is larger than 0.99, which indicates that the obtained yttrium perchlorate crystal has high reliability.
The above embodiments are not intended to limit the present invention, and the present invention is not limited to the above examples, but is also intended to be limited to the following claims.
Claims (10)
1. A method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide is characterized in that: the method comprises the following steps:
s1, obtaining nano rare earth yttrium oxide powder;
s2, preparing a strong acid solution, wherein the strong acid solution is a dilute perchloric acid solution;
s3, adding the rare earth yttrium oxide powder into the dilute perchloric acid solution in an excessive manner, and dissolving the rare earth yttrium oxide powder under the condition of low-speed stirring to generate a crude perchloric acid yttrium solution;
s4, filtering out excessive rare earth yttrium oxide powder, and drying the obtained crude yttrium perchlorate solution to obtain enriched primary yttrium perchlorate crystals;
s5, dissolving primary yttrium perchlorate crystals into a concentrated solution and washing for the first time;
s6, adjusting the yttrium perchlorate solution after primary washing to a semi-crystalline semi-solution state, adding a surfactant, and carrying out ultrasonic oscillation at the temperature of 50-80 ℃ and under the neutral PH condition to obtain yttrium perchlorate suspension, wherein the suspension contains white precursor sediment;
s7, calcining to obtain nano yttrium perchlorate crystals;
s8, redissolving nano yttrium perchlorate crystals and performing secondary washing;
and S9, repeatedly dissolving and drying the yttrium perchlorate after the secondary washing until the high-purity yttrium perchlorate crystal is obtained.
2. The method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide according to claim 1, wherein: the preparation method of the strong acid diluted perchloric acid solution comprises the following steps: introducing chlorine into concentrated sulfuric acid solution, and reacting to produce perchloric acid, wherein the reaction equation is as follows:
Cl 2 +H 2 SO 4 →HClO 4 +HCl
adding silver oxide into the reaction product, precipitating silver chloride produced by the silver oxide and hydrochloric acid, removing HCl, filtering the precipitate to obtain a perchloric acid product, and dissolving the perchloric acid product to the concentration of 2-5mol/L.
3. The method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide according to claim 1, wherein: the drying treatment of the coarse yttrium perchlorate solution in S4 and the drying method of the yttrium perchlorate after the secondary washing in S9 are as follows: the solution was transferred to a vacuum dryer containing phosphorus pentoxide, and the adsorbed water was dried using phosphorus pentoxide.
4. A method for preparing yttrium perchlorate by using rare earth yttrium oxide according to claim 3, wherein: the drying treatment temperature of the phosphorus pentoxide is 70 ℃.
5. The method for preparing yttrium perchlorate by using rare earth yttrium oxide according to any one of claims 2 to 4, wherein: the method for dissolving the primary yttrium perchlorate crystal in S5 and the nano yttrium perchlorate crystal in S8 and the method for dissolving the yttrium perchlorate after the secondary washing in S9 comprises the following steps: and (3) taking deionized water as a solvent, and completing dissolution treatment of yttrium perchlorate crystals at room temperature.
6. The method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide according to claim 5, wherein: the surfactant is an anionic surfactant including, but not limited to, sodium oleate.
7. The method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide according to claim 6, wherein: the calcination temperature of the nano yttrium perchlorate crystals is 200-240 ℃.
8. The method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide according to claim 7, wherein: in S5, the primary washing process is as follows:
slowly adding diluted sodium hydroxide solution into the primary yttrium perchlorate solution, stirring and mixing at a low speed until the solution is neutral, and reacting sodium hydroxide with residual perchloric acid, wherein the reaction equation is as follows:
HClO 4 +NaOH→NaClO 4 +H 2 O
generated NaClO 4 The salt was removed by filtration and the filtered solution was collected.
9. The method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide according to claim 8, wherein: in S8, the secondary washing process is as follows:
adding ethanol solution into the nano yttrium perchlorate solution, washing off surfactant impurities, enabling ethanol and yttrium perchlorate to exist in a complex form, and removing ethanol in a distillation mode to finish secondary washing.
10. The method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide according to claim 8, wherein: the times of dissolution and drying treatment of the yttrium perchlorate after the secondary washing are three times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311562447.3A CN117466251B (en) | 2023-11-22 | 2023-11-22 | Method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide |
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