CN115784291A - Device for removing europium oxide from high-purity gadolinium oxide - Google Patents
Device for removing europium oxide from high-purity gadolinium oxide Download PDFInfo
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- CN115784291A CN115784291A CN202211443553.5A CN202211443553A CN115784291A CN 115784291 A CN115784291 A CN 115784291A CN 202211443553 A CN202211443553 A CN 202211443553A CN 115784291 A CN115784291 A CN 115784291A
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- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910001938 gadolinium oxide Inorganic materials 0.000 title claims abstract description 19
- 229940075613 gadolinium oxide Drugs 0.000 title claims abstract description 19
- 229910001940 europium oxide Inorganic materials 0.000 title claims abstract description 18
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 66
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000000746 purification Methods 0.000 claims abstract description 22
- 230000009194 climbing Effects 0.000 claims abstract description 16
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 13
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims abstract description 13
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 239000002274 desiccant Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 65
- 239000007788 liquid Substances 0.000 claims description 43
- 238000001035 drying Methods 0.000 claims description 31
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 239000003638 chemical reducing agent Substances 0.000 claims description 14
- 239000011347 resin Substances 0.000 claims description 13
- 229920005989 resin Polymers 0.000 claims description 13
- 239000000872 buffer Substances 0.000 claims description 12
- 230000000903 blocking effect Effects 0.000 claims description 11
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 5
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 abstract description 78
- 235000005074 zinc chloride Nutrition 0.000 abstract description 39
- 239000011592 zinc chloride Substances 0.000 abstract description 39
- 239000000843 powder Substances 0.000 abstract description 22
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 12
- MEANOSLIBWSCIT-UHFFFAOYSA-K gadolinium trichloride Chemical compound Cl[Gd](Cl)Cl MEANOSLIBWSCIT-UHFFFAOYSA-K 0.000 abstract description 12
- 239000002245 particle Substances 0.000 abstract description 12
- 239000011701 zinc Substances 0.000 abstract description 12
- 229910052725 zinc Inorganic materials 0.000 abstract description 12
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 abstract description 12
- 229940007718 zinc hydroxide Drugs 0.000 abstract description 12
- 229910021511 zinc hydroxide Inorganic materials 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 9
- 239000007787 solid Substances 0.000 abstract description 7
- 230000007935 neutral effect Effects 0.000 abstract description 6
- 238000005406 washing Methods 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 description 15
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 7
- 229910003317 GdCl3 Inorganic materials 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- 229910052688 Gadolinium Inorganic materials 0.000 description 4
- 230000003472 neutralizing effect Effects 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 3
- 229910052771 Terbium Inorganic materials 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- -1 gadolinium ions Chemical class 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- 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
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to the technical field of separation and purification of substances, in particular to a device for removing europium oxide from high-purity gadolinium oxide, which comprises a purification device and a climbing frame, wherein the purification device is positioned in the middle of the climbing frame and is connected with the climbing frame, and the purification device comprises an europium removing component: further comprising: according to the calcining component connected with the europium-removing component, zinc particles react with a dilute hydrochloric acid solution to prepare a zinc chloride solution, zinc hydroxide powder is utilized to neutralize the zinc chloride solution to enable the zinc chloride solution to be neutral, a weakly alkaline solid drying agent is utilized to absorb redundant dilute hydrochloric acid, and an NH4OH solution is vaporized by using a vortex effect, so that the purpose of adjusting the pH value in the heating crucible 115 is achieved, and the problems that the existing water washing method cannot completely wash off acidity in the solution, the concentration of the zinc chloride solution is reduced, and the existing alkaline environment adjusting method cannot react with gadolinium chloride to generate gadolinium oxide are solved.
Description
Technical Field
The invention relates to the technical field of separation and purification of substances, in particular to a device for removing europium oxide from high-purity gadolinium oxide.
Background
In the arrangement sequence of rare earth elements, europium, gadolinium and terbium are adjacent elements, and on a leaching curve for separating the three elements, curve crossing of europium and gadolinium can be obviously seen, and the crossing does not exist between terbium and gadolinium, so that europium is difficult to be completely removed when high-purity gadolinium oxide is prepared, and further spectral research and application of gadolinium oxide are influenced;
the existing method for removing europium oxide from high-purity gadolinium oxide has the following defects;
1. when europium oxide in high-purity gadolinium oxide is removed, a reducing agent is usually adopted to reduce Eu < 3+ > in the europium oxide into Eu < 2+ >, and a high-reducing agent is also adopted to reduce gadolinium ions, so that a neutral zinc chloride solution is adopted to reduce the high-purity gadolinium oxide, and a zinc chloride solution is prepared at proper time, the traditional preparation method is to adopt zinc particles to react with an HCL solution, the zinc chloride solution prepared by the method has certain acidity, and the traditional method is to adopt water washing to adjust the pH value, so that the acidity in the solution cannot be completely washed away, and part of the zinc chloride solution can be washed away in the water washing process, so that the concentration of the zinc chloride solution is reduced, the europium oxide cannot be reduced easily, and the Eu < 3+ > cannot be completely removed;
2. when gadolinium chloride is converted into gadolinium oxide, oxalate needs to be added into gadolinium chloride for precipitation, meanwhile, the pH value of gadolinium chloride is adjusted to achieve the pH =1-2, the traditional adjustment method is to add a certain amount of alkaline solution, and the excessive alkaline solution is added to rapidly react with oxalate, so that oxygen atoms in oxalate are replaced, and the gadolinium chloride is difficult to react with the oxalate;
therefore, it is necessary to develop a device for removing europium oxide from high-purity gadolinium oxide.
Disclosure of Invention
Therefore, the invention provides a device for removing europium oxide from high-purity gadolinium oxide, zinc particles are used for reacting with a dilute hydrochloric acid solution to prepare a zinc chloride solution, zinc hydroxide powder is used for neutralizing the zinc chloride solution to be neutral, a weakly alkaline solid drying agent is used for absorbing redundant dilute hydrochloric acid, and an NH4OH solution is vaporized by using a vortex effect to achieve the purpose of adjusting the pH value in a heating crucible 115, so that the problems that the acidity in the solution cannot be completely washed away by the existing water washing method, the concentration of the zinc chloride solution is reduced, and the existing alkaline environment adjusting method is difficult to react with gadolinium chloride to generate gadolinium oxide are solved.
In order to achieve the above purpose, the invention provides the following technical scheme: the device for removing europium oxide from high-purity gadolinium oxide comprises a purification device and a climbing frame, wherein the purification device is positioned in the middle of the climbing frame and is connected with the climbing frame, and the purification device comprises a europium removal component: further comprising: the calcining component is connected with the europium removing component;
the calcining assembly comprises an annular loading seat, a heated tank is fixedly mounted in the middle of the annular loading seat, an air inlet is formed in the top of the heated tank, the inner walls of two sides of the annular loading seat are fixedly provided with the same eddy current heating coil, the eddy current heating coil is wound on the outer wall of the heated tank and is not in contact with the heated tank, the inner side wall of the heated tank is fixedly provided with a heating crucible, the outer wall of the heating crucible is hermetically connected with the inner wall of the heated tank, a heat transfer area is formed between the outer wall of the heating crucible and the inner wall of the heated tank, and high-concentration hydrogen is filled in the heat transfer area;
an outer tank body is fixedly installed in the middle of the climbing frame, the calcining assembly is located in the outer tank body, the outer wall of the bottom of the annular loaded seat is fixedly connected with the inner wall of the outer tank body, a PH adjusting area is formed between the outer wall of the heated tank and the inner wall of the outer tank body located at the upper portion of the annular loaded seat, and high-concentration volatile NH4OH solution is filled in the PH adjusting area;
the liquid outlet channel is formed in the bottom of the outer tank body, the blocking block is clamped in the liquid outlet channel, a hydrochloric acid buffer area is formed between the bottom of the annular loaded seat and the inner wall of the outer tank body located at the bottom of the annular loaded seat, and HCl solution is filled in the hydrochloric acid buffer area.
Preferably, there is the cover at the outer jar of body top through bolt fixed mounting, cover top fixed mounting has servo motor, be equipped with the threaded rod on the inside the central axis of cover, servo motor output shaft and threaded rod top fixed connection, threaded rod lateral wall thread meshing has the internal thread sleeve, internal thread sleeve bottom fixed mounting has the jam ball, it is located the jar inside being heated to block up the ball, it is greater than the inlet port aperture to block up the biggest internal diameter of ball, cover top inner wall fixed mounting has spacing traveller, internal thread sleeve one side fixed mounting has the stopper, spacing traveller slides and runs through the stopper.
Preferably, the purification device still includes except that the europium subassembly, it is equipped with two sets ofly to remove the europium subassembly, it includes the outer sleeve, and is two sets of to remove the europium subassembly the outer sleeve is all fixed to run through the cover and the tank deck portion of being heated, and is two sets of the outer sleeve is the symmetry setting, and all has the inclination to set up, outer sleeve inner wall fixed mounting receives to water the resin post, it is equipped with same group of helical coiled passage with the outer sleeve inner wall to receive to water resin post outer wall, outer sleeve outer wall fixed mounting has multiunit heating plate, multiunit the heating plate is circumference array and arranges.
Preferably, the purification device further comprises a reducing agent allocation assembly, the reducing agent allocation assembly is provided with two sets, the reducing agent allocation assembly comprises a solid-liquid circulation pipe, the solid-liquid circulation pipe penetrates through the bottom of the outer tank body, the solid-liquid circulation pipe is symmetrically arranged and has inclination arrangement, the reducing agent allocation assembly is located inside the hydrochloric acid buffer area, a allocation barrel is fixedly arranged on one side of the solid-liquid circulation pipe, multiple sets of liquid inlet holes are formed in the outer wall of the barrel on the upper half portion of the allocation barrel and are arranged in a circumferential array mode, flow control valves are fixedly arranged at the bottom of the solid-liquid circulation pipe, drying pipelines are fixedly arranged on the other sides of the flow control valves, multiple sets of capillary holes are formed in the outer side wall of each drying pipeline, multiple sets of capillary holes are arranged in a circumferential array mode, drying sleeves are sleeved on the outer side wall of each drying pipeline, alkaline solid drying agents are filled in the drying sleeves, reaction collection tanks are connected to the bottom of each drying pipeline through threads, and are connected to the top of the outer sleeves through threads.
The invention has the beneficial effects that:
1. injecting HCl solution into a hydrochloric acid buffer zone by opening a plugging block, opening a cylinder cover of a blending cylinder body, and adding high-purity zinc particles and a small amount of zinc hydroxide powder into the blending cylinder body, wherein the high-purity zinc particles in the blending cylinder body react with the small amount of zinc hydroxide powder and the HCl solution to generate high-purity zinc chloride solution, meanwhile, the small amount of zinc hydroxide powder can adjust the pH value in the blending cylinder body, so that the zinc chloride solution in a solid-liquid circulating pipe is kept neutral, after the high-purity zinc particles in the blending cylinder body react, opening a flow control valve, slowly allowing the zinc chloride solution and part of the zinc chloride powder in the solid-liquid circulating pipe to enter a reaction collecting tank through a drying pipeline, and drying the zinc chloride solution and part of the zinc chloride powder which pass through the drying pipeline by using an alkaline solid drying agent in a drying sleeve to absorb dilute hydrochloric acid and aqueous solution in the zinc chloride solution, so as to achieve the effect of neutralizing the zinc chloride solution;
2. let in the alternating current for eddy current heating coil, based on the vortex effect, the bottom of the heating tank is heated, the heating tank heats for the NH4OH solution that is located the PH regulatory region, thereby make NHOH solution vaporization, NHOH solution after the vaporization enters into in the heating crucible through the inlet port, thereby reach the effect that changes the interior PH value of heating crucible, when pH =1-2 in the heating crucible, through starting servo motor, servo motor output shaft drives the threaded rod and rotates, under the effect of stopper and spacing traveller, the internal thread sleeve drives and blocks up the ball and move, make and block up the inlet port, make the inside confined space that forms of heating crucible, add certain dose of oxalate simultaneously and precipitate, after the completion of precipitation, increase the voltage that lets in eddy current heating coil, make the heat that receives of heating tank grow, the heating tank passes through the hydrogen transmission in the heat transfer district for the heating crucible, thereby can obtain the Gd2O3 powder of utmost point high purity, reached the mesh of getting rid of europium oxide.
Drawings
FIG. 1 is a schematic structural diagram of the apparatus provided by the present invention;
FIG. 2 is a schematic illustration of the outer can body and can lid of the present invention in assembled form;
FIG. 3 is a partial cross-sectional view of the apparatus provided by the present invention;
FIG. 4 is a schematic structural diagram of a purification apparatus provided in the present invention;
FIG. 5 is a schematic structural diagram of a reductant dispensing assembly according to the present invention;
fig. 6 is an enlarged view of a portion a of fig. 3 according to the present invention.
In the figure: the device comprises a purification device 100, a calcination component 110, an annular loaded seat 111, a heated tank 112, an air inlet 113, a vortex heating coil 114, a heating crucible 115, a heat transfer zone 116, a pH adjusting zone 117, an europium-removing component 120, an outer sleeve 121, a poured resin column 122, a heating plate 123, a spiral channel 124, a reducing agent preparing component 130, a solid-liquid flow pipe 131, a preparing cylinder 132, a liquid inlet hole 133, a flow control valve 134, a drying pipeline 135, a capillary hole 136, a drying sleeve 137, a reaction collecting tank 138, a climbing frame 200, an outer tank body 210, a liquid outlet channel 211, a blocking block 212, a hydrochloric acid buffer zone 213, a tank cover 220, a servo motor 221, a threaded rod 222, an internal threaded sleeve 223, a blocking ball 224, a limiting block 225 and a limiting sliding column 226.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Referring to fig. 1-6, the present invention provides an apparatus for removing europium oxide from high-purity gadolinium oxide, including a purification apparatus 100 and a climbing frame 200, wherein the purification apparatus 100 is located in the middle of the climbing frame 200 and is connected to the climbing frame 200, the purification apparatus 100 includes a europium removal assembly 120: further comprising: a calcining component 110 connected with the europium-removing component 120;
the calcining component 110 comprises an annular receiving seat 111, a heated tank 112 is fixedly installed in the middle of the annular receiving seat 111, an air inlet 113 is formed in the top of the heated tank 112, the same eddy current heating coil 114 is fixedly installed on the inner walls of two sides of the annular receiving seat 111, the eddy current heating coil 114 is wound on the outer wall of the heated tank 112 and is not in contact with the heated tank 112, a heating crucible 115 is fixedly installed on the inner side wall of the heated tank 112, the outer wall of the heating crucible 115 is hermetically connected with the inner wall of the heated tank 112, a heat transfer area 116 is formed between the heating crucible and the inner wall of the heated tank 112, high-concentration hydrogen is filled in the heat transfer area 116, an outer tank body 210 is fixedly installed in the middle of the climbing frame 200, the calcining component 110 is located in the outer tank body 210, the outer wall of the bottom of the annular receiving seat 111 is fixedly connected with the inner wall of the outer tank body 210, a PH adjusting area 117 is formed between the outer wall of the heated tank 112 and the inner wall of the outer tank body 210 located at the upper portion of the annular receiving seat 111, high-concentration volatile NH4OH solution is filled in the PH adjusting area 117, specifically, alternating current is introduced into the eddy current heating coil 114, based on an eddy current effect, the bottom of the heating tank 112 is heated, the heating tank 112 heats the NH4OH solution in the PH adjusting region 117, so that the NH4OH solution is vaporized, the vaporized NH4OH solution enters the heating crucible 115 through the air inlet 113, so that an effect of changing the PH value in the heating crucible 115 is achieved, the PH =1-2 in the heating crucible 115 is achieved, meanwhile, a certain amount of oxalate is added for precipitation, after the precipitation is completed, the voltage introduced into the eddy current heating coil 114 is increased, so that the heat received by the heating tank 112 is increased, the heat is transferred to the heating crucible 115 through hydrogen in the heat transfer region 116 by the heating tank 112, and therefore, extremely high-purity Gd2O3 powder can be obtained, and the purpose of removing europium oxide is achieved;
Further, a tank cover 220 is fixedly installed at the top of the outer tank body 210 through a bolt, a servo motor 221 is fixedly installed at the top of the tank cover 220, a threaded rod 222 is arranged on the central axis inside the tank cover 220, an output shaft of the servo motor 221 is fixedly connected with the top of the threaded rod 222, an inner threaded sleeve 223 is meshed with the outer side wall of the threaded rod 222 in a threaded manner, a blocking ball 224 is fixedly installed at the bottom of the inner threaded sleeve 223, the blocking ball 224 is located inside the heated tank 112, the maximum inner diameter of the blocking ball 224 is larger than the aperture of the air inlet 113, a limiting sliding column 226 is fixedly installed on the inner wall of the top of the tank cover 220, a limiting block 225 is fixedly installed on one side of the inner threaded sleeve 223, the limiting sliding column 226 penetrates through the limiting block 225 in a sliding manner, specifically, the servo motor 221 is started, the output shaft of the servo motor 221 drives the threaded rod 222 to rotate, under the action of the limiting block 225 and the limiting sliding column 226, the inner threaded sleeve 223 drives the blocking ball 224 to move, so that the air inlet 113 can be blocked by the blocking ball 224, and a closed space can be formed inside the heated crucible 115.
Further, the purification apparatus 100 further includes an europium-removing component 120, two sets of the europium-removing component 120 are provided, the europium-removing component 120 includes outer sleeves 121, the two sets of the outer sleeves 121 are both fixedly penetrated through the top of the tank cover 220 and the heated tank 112, the two sets of the outer sleeves 121 are symmetrically arranged and are both arranged at an inclination, a poured resin column 122 is fixedly installed on the inner wall of the outer sleeve 121, the same set of spiral passages 124 are provided on the outer wall of the poured resin column 122 and the inner wall of the outer sleeve 121, a plurality of sets of heating fins 123 are fixedly installed on the outer wall of the outer sleeve 121, the plurality of sets of heating fins 123 are arranged in a circumferential array, specifically, the reaction collection tank 138 is meshed with the outer sleeves 121, at this time, the material liquid in the reaction collection tank 138 can enter the heating crucible 115 in the heated tank 112 along with the spiral passages 124 on the poured resin column 122 (the heating fins 123 are started to keep the poured resin column 122 at a constant temperature of 50 ℃), at this time, eu2+ in Gd2O3 with a purity greater than 99.9% can be adsorbed by the poured resin column 122, and therefore, the GdCl3 solution flowing into the heating crucible 115 does not contain Eu ions.
Further, the purification apparatus 100 further comprises a reducing agent preparing assembly 130, two groups of reducing agent preparing assemblies 130 are provided, each reducing agent preparing assembly 130 comprises a solid-liquid flow pipe 131, the two groups of solid-liquid flow pipes 131 are fixedly penetrated through the bottom of the outer tank 210, the two groups of solid-liquid flow pipes 131 are symmetrically arranged and are arranged with slopes, the solid-liquid flow pipes 131 are arranged with slopes, so that zinc chloride solution and zinc hydroxide powder in the solid-liquid flow pipes 131 can enter the reaction collection tank 138 under the action of gravity, a preparing cylinder 132 is fixedly installed on one side of the solid-liquid flow pipes 131 in the hydrochloric acid buffer area 213, a plurality of groups of liquid inlet holes 133 are formed in the outer wall of the upper half part of the preparing cylinder 132, the liquid inlet holes 133 are formed in the upper half part of the preparing cylinder 132, so that raw material powder in the preparing cylinder 132 can be prevented from spilling, the plurality of groups of liquid inlet holes 133 are arranged in a circumferential array, flow control valves 134 are fixedly installed at the bottoms of the solid-liquid flow pipes 131, a drying pipe 135 is fixedly installed on the other side of the flow control valve 134, a plurality of groups of capillary holes 136 are formed in the outer side wall of the drying pipe 135, the plurality of groups of capillary holes 136 are arranged in a circumferential array, a drying sleeve 137 is sleeved on the outer side wall of the drying pipe 135, an alkaline solid drying agent is filled in the drying sleeve 137, a reaction collecting tank 138 is connected to the bottom of the drying pipe 135 in a threaded manner, the reaction collecting tank 138 is connected to the top of the outer sleeve 121 in a threaded manner, specifically, a high-purity zinc particle and a small amount of zinc hydroxide powder are added into the mixing cylinder 132 by opening a cylinder cover of the mixing cylinder 132, at the moment, the high-purity zinc particle and the small amount of zinc hydroxide powder in the mixing cylinder 132 react with an HCl solution, so that a high-purity zinc chloride solution is generated, meanwhile, the PH value in the mixing cylinder 132 can be adjusted by the small amount of zinc hydroxide powder, so that the zinc chloride solution in the solid-liquid circulation pipe 131 is kept neutral, after the high-purity zinc particles in the blending cylinder 132 react, the flow control valve 134 is opened, the zinc chloride solution and part of the zinc chloride powder in the solid-liquid flow pipe 131 slowly enter the reaction collecting tank 138 through the drying pipeline 135, at this time, the zinc chloride solution and part of the zinc chloride powder passing through the drying pipeline 135 are dried by the alkaline solid desiccant in the drying sleeve 137, so that the dilute hydrochloric acid and the aqueous solution in the zinc chloride solution are sucked, the effect of neutralizing the zinc chloride solution is achieved, meanwhile, a 20 mg/ml-concentration GdCl3 solution prepared from Gd2O3 with the purity of more than 99.9% is added into the reaction collecting tank 138, and the acidic solution with a certain dosage is added, so that the pH inside of the reaction collecting tank 138 is less than or equal to 1.5, and meanwhile, the zinc chloride solution in the drying pipeline 135 can react with the GdCl3 solution, so that Eu3+ in the feed liquid can be reduced to be Eu2+.
The using process of the invention is as follows: a person skilled in the art injects an HCl solution into the hydrochloric acid buffer zone 213 by opening the plugging block 212, and opens the cover of the blending cylinder 132 to add high-purity zinc particles and a small amount of zinc hydroxide powder into the blending cylinder 132, at this time, the high-purity zinc particles and the small amount of zinc hydroxide powder in the blending cylinder 132 react with the HCl solution, so as to generate a high-purity zinc chloride solution, meanwhile, the small amount of zinc hydroxide powder can adjust the PH value in the blending cylinder 132, so that the zinc chloride solution in the solid-liquid flow pipe 131 is kept neutral, after the high-purity zinc particles in the blending cylinder 132 react, the flow control valve 134 is opened, the zinc chloride solution and part of the zinc chloride powder in the solid-liquid flow pipe 131 slowly enter the reaction collection tank 138 through the drying pipe 135, at this time, the zinc chloride solution and part of the zinc chloride powder passing through the drying pipe 135 are dried by the alkaline solid desiccant in the drying sleeve 137, so as to absorb hydrochloric acid and the aqueous solution in the zinc chloride solution, thereby achieving the effect of neutralizing the zinc chloride solution;
meanwhile, 20mg/ml GdCl3 solution prepared from Gd2O3 with purity of more than 99.9 percent is added into the reaction and collection tank 138, and the reaction and collection tank 138 is added with a certain amount of acid solution, so that the pH value in the reaction and collection tank is less than or equal to 1.5, and the zinc chloride solution in the drying pipeline 135 can react with the GdCl3 solution, so that Eu & lt 3+ & gt in the feed liquid can be reduced to Eu & lt 2+ & gt, after the reaction is completed, the reaction and collection tank 138 is meshed with the outer sleeve 121, at the moment, the feed liquid in the reaction and collection tank 138 can enter the heating crucible 115 in the heating tank 112 along with the spiral channel 124 on the poured resin column 122 (the heating sheet 123 is started to keep the temperature of the poured resin column 122 constant by 50 ℃), at the moment, eu & lt 2+ & gt in the Gd2O3 with purity of more than 99.9 percent can be adsorbed by the poured resin column 122, so that the GdCl3 solution flowing into the heating crucible 115 does not contain Eu ions;
meanwhile, alternating current is introduced into the eddy current heating coil 114, the bottom of the heating tank 112 is heated based on the eddy current effect, the NH4OH solution in the pH adjusting region 117 is heated by the heating tank 112, so that the NH4OH solution is vaporized, the vaporized NH4OH solution enters the heating crucible 115 through the air inlet hole 113, so that the effect of changing the pH value in the heating crucible 115 is achieved, when the pH =1-2 in the heating crucible 115, the servo motor 221 is started, the output shaft of the servo motor 221 drives the threaded rod 222 to rotate, under the action of the limiting block 225 and the limiting sliding column 226, the internal threaded sleeve 223 drives the blocking ball 224 to move, so that the blocking ball 224 can block the air inlet hole 113, a closed space is formed inside the heating crucible 115, meanwhile, a certain amount of oxalate is added for precipitation, after the precipitation is completed, the voltage introduced into the eddy current heating coil 114 is increased, so that the heat received by the heating tank 112 is increased, and the heat is transferred to the heating crucible 115 through hydrogen in the heat transfer region 116 by the heating tank 112, so that extremely high-purity 2O3 powder can be obtained, and the purpose of removing europium oxide is achieved.
The above description is only a preferred embodiment of the present invention, and any person skilled in the art may modify the present invention or modify it into an equivalent technical solution by using the technical solution described above. Therefore, any simple modifications or equivalent substitutions made in accordance with the technical solution of the present invention are within the scope of the claims of the present invention.
Claims (4)
1. A device for removing europium oxide from high-purity gadolinium oxide, which comprises a purification device (100) and a climbing frame (200), wherein the purification device (100) is positioned in the middle of the climbing frame (200) and is connected with the climbing frame (200), and is characterized in that: the purification device (100) comprises a europium-removing component (120): further comprising: a calcination component (110) connected with the europium-removing component (120);
the calcining assembly (110) comprises an annular loaded seat (111), a heated tank (112) is fixedly installed in the middle of the annular loaded seat (111), an air inlet hole (113) is formed in the top of the heated tank (112), the inner walls of two sides of the annular loaded seat (111) are fixedly provided with the same vortex heating coil (114), the vortex heating coil (114) is wound on the outer wall of the heated tank (112) and is not in contact with the heated tank (112), a heating crucible (115) is fixedly installed on the inner side wall of the heated tank (112), the outer wall of the heating crucible (115) is hermetically connected with the inner wall of the heated tank (112), a heat transfer area (116) is formed between the outer wall and the inner wall of the heated tank (112), and high-concentration hydrogen is filled in the heat transfer area (116);
an outer tank body (210) is fixedly installed in the middle of the climbing frame (200), the calcining assembly (110) is located inside the outer tank body (210), the outer wall of the bottom of the annular loading seat (111) is fixedly connected with the inner wall of the outer tank body (210), a PH adjusting area (117) is formed between the outer wall of the heating tank (112) and the inner wall of the outer tank body (210) located at the upper part of the annular loading seat (111), and high-concentration volatile NH4OH solution is filled in the PH adjusting area (117);
a liquid outlet channel (211) is formed in the bottom of the outer tank body (210), a blocking block (212) is clamped in the liquid outlet channel (211), a hydrochloric acid buffer area (213) is formed between the bottom of the annular receiving seat (111) and the inner wall of the outer tank body (210) located at the bottom of the annular receiving seat (111), and HCl solution is filled in the hydrochloric acid buffer area (213).
2. The apparatus of claim 1, wherein the apparatus comprises: the utility model discloses a heating tank, including outer jar body (210), threaded rod (223), servo motor (222), stopper ball (224) is located heated tank (112), stopper ball (224) maximum internal diameter is greater than inlet port (113) aperture, jar cover (220) top fixed mounting has servo motor (221), be equipped with threaded rod (222) on jar cover (220) the inside central axis, servo motor (221) output shaft and threaded rod (222) top fixed connection, threaded rod (222) lateral wall threaded engagement has internal thread sleeve (223), internal thread sleeve (223) bottom fixed mounting has stopper ball (224), stopper ball (224) is located heated tank (112) inside, stopper ball (224) maximum internal diameter is greater than inlet port (113) aperture, jar cover (220) top inner wall fixed mounting has spacing traveller (226), internal thread sleeve (223) one side fixed mounting has stopper (225), stopper traveller (226) slide and run through stopper (225).
3. The apparatus of claim 2, wherein the europium oxide is removed from high-purity gadolinium oxide by: purification device (100) still includes except europium subassembly (120), it is equipped with two sets ofly to remove europium subassembly (120), it includes outer sleeve (121) to remove europium subassembly (120), and is two sets of outer sleeve (121) is all fixed to run through cover (220) and be heated jar (112) top, and is two sets of outer sleeve (121) are the symmetry and set up, and all have the slope setting, outer sleeve (121) inner wall fixed mounting has and receives to water resin column (122), it is equipped with same a set of screw channel (124) with outer sleeve (121) inner wall to receive to water resin column (122) outer wall, outer sleeve (121) outer wall fixed mounting has multiunit heating plate (123), multiunit heating plate (123) are the circumference array and arrange.
4. The apparatus of claim 3, wherein the europium oxide is removed from high-purity gadolinium oxide by: the purification device (100) further comprises a reducing agent allocation assembly (130), the reducing agent allocation assembly (130) is provided with two groups, the reducing agent allocation assembly (130) comprises solid-liquid flow pipes (131), the two groups of solid-liquid flow pipes (131) fixedly penetrate through the bottom of the outer tank body (210), the two groups of solid-liquid flow pipes (131) are symmetrically arranged and are arranged with slopes, an allocation barrel (132) is fixedly installed on one side of each solid-liquid flow pipe (131) inside the hydrochloric acid cache region (213), multiple groups of liquid inlet holes (133) are formed in the outer wall of the upper half barrel of the allocation barrel (132), the multiple groups of liquid inlet holes (133) are arranged in a circumferential array mode, flow control valves (134) are fixedly installed at the bottoms of the solid-liquid flow pipes (131), drying pipelines (135) are fixedly installed on the other sides of the flow control valves (134), multiple groups of capillary holes (136) are formed in the outer side wall of the drying pipelines (135), the multiple groups of the capillary holes (136) are arranged in a circumferential array mode, drying sleeves (137) are sleeved on the outer side wall of the drying pipelines (135), alkaline solid-liquid flow pipes (137) are filled with alkaline drying agents, the bottoms of the drying pipelines (135) are connected with a screw thread connection reaction tank (138), and the top of a reaction tank (121) and connected with a reaction tank.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211443553.5A CN115784291B (en) | 2022-11-18 | 2022-11-18 | Device for removing europium oxide from high-purity gadolinium oxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211443553.5A CN115784291B (en) | 2022-11-18 | 2022-11-18 | Device for removing europium oxide from high-purity gadolinium oxide |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1125260A (en) * | 1995-07-12 | 1996-06-26 | 中国科学院长春应用化学研究所 | Method for removing europium oxide from high pure gadolinium oxide |
| CN1931724A (en) * | 2006-10-09 | 2007-03-21 | 江阴加华新材料资源有限公司 | Prepn process of high purity yttrium europium oxide |
| WO2014167534A1 (en) * | 2013-04-12 | 2014-10-16 | University Of Kwazulu-Natal | Recovery of yttrium and europium compounds |
| CN107326200A (en) * | 2017-05-25 | 2017-11-07 | 广东省稀有金属研究所 | The method of europium is enriched with a kind of chloride solution from sm-eu-gd |
-
2022
- 2022-11-18 CN CN202211443553.5A patent/CN115784291B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1125260A (en) * | 1995-07-12 | 1996-06-26 | 中国科学院长春应用化学研究所 | Method for removing europium oxide from high pure gadolinium oxide |
| CN1931724A (en) * | 2006-10-09 | 2007-03-21 | 江阴加华新材料资源有限公司 | Prepn process of high purity yttrium europium oxide |
| WO2014167534A1 (en) * | 2013-04-12 | 2014-10-16 | University Of Kwazulu-Natal | Recovery of yttrium and europium compounds |
| CN107326200A (en) * | 2017-05-25 | 2017-11-07 | 广东省稀有金属研究所 | The method of europium is enriched with a kind of chloride solution from sm-eu-gd |
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| CN115784291B (en) | 2024-01-30 |
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