CN115367782A - Method for preparing low-chlorine rare earth carbonate - Google Patents
Method for preparing low-chlorine rare earth carbonate Download PDFInfo
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- CN115367782A CN115367782A CN202211004731.4A CN202211004731A CN115367782A CN 115367782 A CN115367782 A CN 115367782A CN 202211004731 A CN202211004731 A CN 202211004731A CN 115367782 A CN115367782 A CN 115367782A
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- rare earth
- lifting ring
- earth carbonate
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 45
- -1 rare earth carbonate Chemical class 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000000460 chlorine Substances 0.000 title claims abstract description 22
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 22
- 230000007246 mechanism Effects 0.000 claims abstract description 85
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 66
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 57
- 238000005406 washing Methods 0.000 claims abstract description 43
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 33
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 6
- 238000001514 detection method Methods 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims description 41
- 239000007787 solid Substances 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 26
- 239000000706 filtrate Substances 0.000 claims description 25
- 238000007790 scraping Methods 0.000 claims description 22
- 239000000725 suspension Substances 0.000 claims description 20
- 238000003860 storage Methods 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 10
- 229910017569 La2(CO3)3 Inorganic materials 0.000 claims description 10
- NZPIUJUFIFZSPW-UHFFFAOYSA-H lanthanum carbonate Chemical compound [La+3].[La+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NZPIUJUFIFZSPW-UHFFFAOYSA-H 0.000 claims description 10
- 229960001633 lanthanum carbonate Drugs 0.000 claims description 10
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 7
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 7
- 241001330002 Bambuseae Species 0.000 claims description 7
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 7
- 239000011425 bamboo Substances 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 230000005540 biological transmission Effects 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 230000000630 rising effect Effects 0.000 claims description 6
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 4
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 4
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 4
- 239000001099 ammonium carbonate Substances 0.000 claims description 4
- 230000001174 ascending effect Effects 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 150000002910 rare earth metals Chemical class 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000000149 penetrating effect Effects 0.000 description 4
- 238000010924 continuous production Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/247—Carbonates
-
- 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
Abstract
The invention discloses a method for preparing low-chlorine rare earth carbonate, which relates to the technical field of rare earth materials and is realized by using equipment for preparing the low-chlorine rare earth carbonate, wherein the equipment for preparing the low-chlorine rare earth carbonate comprises a filtering and washing mechanism, the top of the filtering and washing mechanism is provided with a top frame, the top of the top frame is fixedly provided with a driving motor, the inner side of the top frame is provided with a suction mechanism, the driving motor drives a rotating shaft in the suction mechanism to rotate, the outer side of the suction mechanism is sleeved with a transparent observation barrel, and an annular piston in the suction mechanism is lifted at the inner side of the transparent observation barrel. The invention can automatically and continuously finish the detection of the washed washing water for multiple times without manually collecting the washing water and adding the silver nitrate solution, thereby saving the labor, reducing the operation difficulty and effectively reducing the preparation cost of the low-chlorine rare earth carbonate.
Description
Technical Field
The invention relates to the technical field of rare earth materials, in particular to a method for preparing low-chloride rare earth carbonate.
Background
The rare earth carbonate is used as a precursor for preparing rare earth fluorescent powder, rare earth polishing powder, rare earth permanent magnetic materials, hydrogen storage materials, structural materials and the like, various quality indexes are main factors influencing the physical and chemical properties of the rare earth carbonate, and with the further development of the high and new rare earth technology, many rare earth application enterprises have basic requirements on the chemical composition of rare earth products and also put forward new and higher requirements.
The invention patent of patent application publication No. CN104310456B discloses a production method of fine-grained low-chloride rare earth carbonate, which is mainly characterized in that: on a designed special precipitation reaction device, rare earth chloride and carbonate solution are added in a parallel-flow feeding mode, and the aging time of the rare earth carbonate is controlled by controlling the feeding speed and the discharging speed, so that the spatial separation of a reaction zone and a crystallization zone is realized, and the dual purposes of directly obtaining a fine-grained low-chlorine rare earth carbonate product by precipitation from a hydrochloric acid medium and continuous production are further achieved. The invention can directly obtain the fine-grained rare earth carbonate product with the chloride content of less than 50ppm in the hydrochloric acid medium by using the cheap ammonium bicarbonate, and the precipitation reaction device has simple structure and can realize continuous production.
After the production method finishes filtering the turbid liquid, the filtered solids are washed by normal-temperature water until the washing filtrate does not generate turbidity when contacting with the silver nitrate solution, and the obtained solids are the lanthanum carbonate product with fine granularity and low chlorine radicals.
Therefore, it is necessary to develop a method for preparing rare earth carbonate with low chloride to solve the above problems.
Disclosure of Invention
The present invention is directed to a method for preparing rare earth carbonate with low chloride to solve the above problems of the background art.
In order to achieve the purpose, the invention provides the following technical scheme: the utility model provides a method for preparing low chlorine root rare earth carbonate, the method for preparing low chlorine root rare earth carbonate uses the equipment realization of preparing low chlorine root rare earth carbonate, the equipment of preparing low chlorine root rare earth carbonate is including filtering washing mechanism, it is provided with the roof-rack to filter washing mechanism top, the fixed driving motor that is provided with in roof-rack top, the roof-rack inboard is provided with suction mechanism, the rotatory axle is rotatory in the driving suction mechanism of driving motor drive, the suction mechanism outside cup joints and is provided with transparent observation tube, annular piston goes up and down in transparent observation tube inboard in the suction mechanism, transparent observation tube outside cup joints and is provided with silver nitrate solution feed mechanism, silver nitrate solution feed mechanism is located and filters washing mechanism top, silver nitrate solution feed mechanism well L shape feed pipe pours into transparent observation tube inboard with silver nitrate solution, silver nitrate solution feed mechanism both sides all are provided with spacing scraping mechanism, spacing lagging plate drives the rotation of screw rod in the spacing scraping mechanism in the suction mechanism, the inside closed machanism that is provided with of suction mechanism, the catch bar rises in the lifting ring drive closed machanism.
Preferably, the filtering and washing mechanism comprises a shell, a turbid liquid input pipe, a cleaning water input pipe, a solid output pipe, a filtrate output pipe and a filter plate;
the cleaning device comprises a casing, a suspension input pipe, a cleaning water input pipe, a solid output pipe and a filtrate output pipe, wherein the suspension input pipe and the cleaning water input pipe are fixedly arranged at the top of the left side of the casing in a penetrating mode, the cleaning water input pipe is arranged at the bottom of the suspension input pipe, the solid output pipe and the filtrate output pipe are fixedly arranged at the bottom of the right side of the casing in a penetrating mode, and the filtrate output pipe is arranged at the bottom of the solid output pipe.
Preferably, the suction mechanism comprises a rotating shaft, a lifting ring, a limiting sleeve plate, a rotating ring, a longitudinal rod, an annular piston and an I-shaped channel;
the utility model discloses a portable electronic device, including a transparent observation tube, rotation axis top and driving motor transmission, the rotation axis outside is provided with reciprocal screw thread, the lifting ring is connected with the rotation axis transmission through reciprocal screw thread, the fixed cover of spacing lagging plate connects to be set up in the lifting ring outside, the swivel becket passes through the bearing and rotates nested the setting in the lifting ring bottom, the longitudinal rod is provided with two, two the longitudinal rod is fixed respectively and sets up in swivel becket bottom both sides, the annular piston slides and sets up in transparent observation tube inboard, and with two longitudinal rod bottom end fixed connection, the I shape passageway is seted up inside the rotation axis, I shape passageway one end extends to transparent observation tube inboard and the other end extends to casing inner chamber bottom.
Preferably, the silver nitrate solution feeding mechanism comprises an annular storage container, an L-shaped feeding pipe and a valve;
annular storage container is fixed to be set up in the casing top, L shape feeder pipe all is provided with two, two with the valve L shape feeder pipe is fixed respectively to run through and sets up in the inboard both sides of annular storage container, L shape feeder pipe end portion is fixed to run through and sets up in transparent observation tube side, two the valve is fixed respectively to be set up in two L shape feeder intraducts, be provided with the check valve on the L shape feeder pipe.
Preferably, the limiting scraping mechanism comprises a screw and a scraping plate;
the screw rod runs through the limiting sleeve plate and is in threaded connection with the limiting sleeve plate, the screw rod is rotatably connected with the shell through a bearing, the scraping plate is fixedly arranged at the bottom end of the screw rod, and the scraping plate is laminated on the top of the filter plate.
Preferably, the closing mechanism comprises an inverted T-shaped rod, a first spring, a push rod, a second spring, an accommodating groove and a closing plate;
the T-shaped rod that falls slides along vertical direction and sets up inside the rotation axis, and inside its bottom extended to I shape passageway, first spring fixed connection is on the T-shaped rod top that falls, catch bar fixed connection is on first spring top, and slides along vertical direction nestedly and set up inside the rotation axis, second spring bottom and catch bar fixed connection and top and rotation axis inner wall fixed connection, holding tank and closing plate all are provided with two, two the holding tank is all seted up on I shape passageway inner wall, two the closing plate slides respectively and sets up in two holding tanks inboardly, two the closing plate all with T-shaped rod fixed connection that falls.
Preferably, the method for preparing the low-chloride rare earth carbonate specifically comprises the following steps:
s1, preparing a suspension by using a precipitation reaction device by using lanthanum carbonate feed liquid and an ammonium bicarbonate solution as raw materials and lanthanum carbonate as seed crystals;
s2, inputting the turbid liquid into the shell through a turbid liquid input pipe, filtering the turbid liquid by the filter plate, discharging filtrate through a filtrate output pipe, retaining solids at the top of the filter plate, injecting cleaning water into the shell through a cleaning water input pipe, washing the solids by the cleaning water, and discharging the washed cleaning water through the filter plate and the filtrate output pipe;
s3, in the cleaning process, the driving motor drives the rotating shaft to rotate, the rotating shaft drives the lifting ring to ascend when rotating, the lifting ring drives the annular piston to ascend at the inner side of the transparent observation cylinder through the rotating ring and the longitudinal rod when ascending, and the cleaning water after being washed is sucked into the inner side of the transparent observation cylinder through the I-shaped channel;
s4, when the lifting ring rises, the pushing rod is pushed upwards, so that the pushing rod drives the sealing plate to rise through the first spring and the inverted T-shaped rod, the opening at the top of the I-shaped channel is sealed by the sealing plate along with the continuous rising of the lifting ring, and the washed washing water cannot continuously enter the transparent observation cylinder;
s5, with the continuous rising of the lifting ring, as the closing plate cannot move upwards continuously, the first spring is stretched, and meanwhile, the annular piston moves to the position above the L-shaped feeding pipe on the inner side of the transparent observation cylinder, so that the silver nitrate solution in the annular storage container is sucked into the inner side of the transparent observation cylinder through the L-shaped feeding pipe and is rapidly mixed with the washed washing water;
s6, observing a mixture of cleaning water and a silver nitrate solution through a transparent observation cylinder, stopping the input of the cleaning water if turbid matters are not generated, and simultaneously inputting residual cleaning water and solid matters into solid-liquid separation equipment through a solid matter output pipe for solid-liquid separation so as to obtain a lanthanum carbonate finished product with fine granularity and low chloride radicals;
s7, if turbid materials are generated, continuously injecting cleaning water, driving the lifting ring to slide downwards under the driving of the reciprocating screw threads when the lifting ring moves to the topmost part of the reciprocating screw threads, further pushing the annular piston through the rotating ring and the longitudinal rod, pressurizing the inner cavity of the transparent observation cylinder by the annular piston, and enabling the mixed liquid on the inner side of the transparent observation cylinder to not enter the annular storage container through the L-shaped feeding pipe due to the limitation of the one-way valve;
s8, in the descending process of the lifting ring, the second spring pushes the push rod to descend synchronously, the push rod firstly drives the stretched first spring to reset, then the first spring and the inverted T-shaped rod drive the closing plate to descend, and further the closing of the top opening of the I-shaped channel is removed, at the moment, mixed liquid on the inner side of the transparent observation cylinder is input to the bottom of the inner cavity of the shell through the I-shaped channel, then the mixed liquid is discharged through the filtrate output pipe, then the lifting ring moves to the lowest end of the reciprocating thread, and then the reciprocating thread drives the lifting ring to ascend again, so that the detection is carried out again.
The invention has the technical effects and advantages that:
according to the invention, the suction mechanism, the transparent observation cylinder, the silver nitrate solution feeding mechanism, the limiting scraping mechanism and the sealing mechanism are arranged, so that the driving motor can conveniently suck the washed washing water to the inner side of the transparent observation cylinder through the suction mechanism and drive the sealing mechanism, further, the silver nitrate solution in the silver nitrate solution feeding mechanism is sucked to the inner side of the transparent observation cylinder and is rapidly mixed with the washing water, meanwhile, the limiting scraping mechanism can be driven, further, the limiting scraping mechanism drives the solid to rotate, the washing efficiency of the solid is improved, meanwhile, the subsequent solid output is convenient, compared with the same type preparation method in the prior art, the detection of the washed washing water can be automatically and continuously completed for many times, the manual collection of the washing water and the addition of the silver nitrate solution are not needed, the labor is saved, the operation difficulty is reduced, and meanwhile, the preparation cost of the low-chlorine rare earth carbonate is effectively reduced.
Drawings
Fig. 1 is an overall front sectional structural view of the present invention.
Fig. 2 is a front sectional structural schematic view of a pumping mechanism and a silver nitrate solution feeding mechanism of the present invention.
Fig. 3 is a front sectional structural schematic view of the closing mechanism of the present invention.
In the figure: 1. a filtering and washing mechanism; 11. a housing; 12. a suspension liquid input pipe; 13. a cleaning water input pipe; 14. a solid matter output pipe; 15. a filtrate output pipe; 16. filtering a plate; 2. a top frame; 3. a drive motor; 4. a suction mechanism; 41. a rotating shaft; 42. a lifting ring; 43. a limiting sleeve plate; 44. a rotating ring; 45. a longitudinal rod; 46. an annular piston; 47. an I-shaped channel; 5. a transparent observation tube; 6. a silver nitrate solution feeding mechanism; 61. an annular storage container; 62. an L-shaped feed pipe; 63. a valve; 7. a limiting scraping mechanism; 71. a screw; 72. a scraping plate; 8. a closure mechanism; 81. an inverted T-shaped bar; 82. a first spring; 83. a push rod; 84. a second spring; 85. accommodating grooves; 86. and (3) closing the plate.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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 invention.
Example 1
The invention provides a method for preparing low-chlorine rare earth carbonate, which is realized by using equipment for preparing low-chlorine rare earth carbonate, and is shown in fig. 1-3, the equipment for preparing low-chlorine rare earth carbonate comprises a filtering and washing mechanism 1, the top of the filtering and washing mechanism 1 is provided with a top frame 2, the top of the top frame 2 is fixedly provided with a driving motor 3, the inner side of the top frame 2 is provided with a suction mechanism 4, the driving motor 3 drives a rotating shaft 41 in the suction mechanism 4 to rotate, the outer side of the suction mechanism 4 is sleeved with a transparent observation cylinder 5, an annular piston 46 in the suction mechanism 4 is lifted on the inner side of the transparent observation cylinder 5, the outer side of the transparent observation cylinder 5 is sleeved with a silver nitrate solution feeding mechanism 6, the silver nitrate solution feeding mechanism 6 is positioned on the top of the filtering and washing mechanism 1, an L-shaped feeding pipe 62 in the silver nitrate solution feeding mechanism 6 injects silver nitrate solution into the inner side of the transparent observation cylinder 5, both sides of the silver nitrate solution feeding mechanism 6 are provided with limiting and scraping mechanisms 7, a limiting sleeve plate 43 in the suction mechanism 4 drives a limiting and a lifting and pushing mechanism 8 in the suction mechanism 8.
As shown in fig. 1, the filtering and washing mechanism 1 includes a housing 11, a suspension input pipe 12, a cleaning water input pipe 13, a solids output pipe 14, a filtrate output pipe 15, and a filter plate 16, wherein the suspension input pipe 12 and the cleaning water input pipe 13 are both fixedly disposed at the top of the left side of the housing 11, the cleaning water input pipe 13 is disposed at the bottom of the suspension input pipe 12, the solids output pipe 14 and the filtrate output pipe 15 are both fixedly disposed at the bottom of the right side of the housing 11, and the filtrate output pipe 15 is disposed at the bottom of the solids output pipe 14.
By the above structure, the suspension is input into the casing 11 through the suspension input pipe 12, the suspension is filtered by the filter plate 16, the filtrate is discharged through the filtrate output pipe 15, the solids are retained on the top of the filter plate 16, the washing water is injected into the casing 11 through the washing water input pipe 13, the solids are washed by the washing water, and the washing water after washing passes through the filter plate 16 and is then discharged through the filtrate output pipe 15.
As shown in fig. 2, the suction mechanism 4 includes a rotation shaft 41, a lifting ring 42, a limiting sleeve plate 43, a rotation ring 44, longitudinal rods 45, an annular piston 46 and an i-shaped channel 47, wherein the top end of the rotation shaft 41 is in transmission connection with the driving motor 3, the outer side of the rotation shaft 41 is provided with reciprocating threads, the lifting ring 42 is in transmission connection with the rotation shaft 41 through the reciprocating threads, the limiting sleeve plate 43 is fixedly sleeved on the outer side of the lifting ring 42, the rotation ring 44 is nested in the bottom of the lifting ring 42 through a bearing, the longitudinal rods 45 are provided with two longitudinal rods 45, the longitudinal rods 45 are respectively fixedly arranged on two sides of the bottom of the rotation ring 44, the annular piston 46 is slidably arranged on the inner side of the transparent observation cylinder 5 and is fixedly connected with the bottom ends of the two longitudinal rods 45, the i-shaped channel 47 is arranged inside the rotation shaft 41, one end of the i-shaped channel 47 extends to the inner side of the transparent observation cylinder 5, and the other end extends to the bottom of the inner cavity of the housing 11.
By adopting the structure, the rotating shaft 41 drives the lifting ring 42 to ascend or descend when rotating, and further drives the annular piston 46 to ascend and descend through the rotating ring 44 and the longitudinal rod 45.
As shown in fig. 2, the silver nitrate solution feeding mechanism 6 includes an annular storage container 61, two L-shaped feeding pipes 62 and valves 63, wherein the annular storage container 61 is fixedly disposed on the top of the housing 11, the two L-shaped feeding pipes 62 and the two valves 63 are disposed, the two L-shaped feeding pipes 62 are respectively fixedly disposed on two inner sides of the annular storage container 61 in a penetrating manner, ends of the L-shaped feeding pipes 62 are fixedly disposed on the side of the transparent observation cylinder 5 in a penetrating manner, the two valves 63 are respectively fixedly disposed inside the two L-shaped feeding pipes 62, and a check valve is disposed on the L-shaped feeding pipes 62.
Through setting up above-mentioned structure to when the inboard cavity of a transparent observation section of thick bamboo 5 is the negative pressure, the inside silver nitrate solution of annular storage container 61 enters into a transparent observation section of thick bamboo 5 inboardly through L shape feed pipe 62, when the inboard cavity of a transparent observation section of thick bamboo 5 is the positive pressure simultaneously, under the blockking of check valve, the inboard mixed liquid of a transparent observation section of thick bamboo 5 can't enter into annular storage container 61 inside through L shape feed pipe 62.
As shown in fig. 1 and 2, the limiting scraping mechanism 7 includes a screw 71 and a scraping plate 72, wherein the screw 71 penetrates through the limiting sleeve plate 43 and is in threaded connection with the limiting sleeve plate 43, the screw 71 is rotatably connected with the housing 11 through a bearing, and the scraping plate 72 is fixedly disposed at the bottom end of the screw 71 and is attached to the top of the filter plate 16.
Through setting up above-mentioned structure to drive screw rod 71 rotatory when spacing sleeve plate 43 descends, and then make screw rod 71 drive scraping plate 72 stir the solid at filter plate 16 top, and then promote the solid washing effect.
As shown in fig. 3, the closing mechanism 8 includes an inverted T-shaped rod 81, a first spring 82, a push rod 83, a second spring 84, an accommodating groove 85 and a closing plate 86, wherein the inverted T-shaped rod 81 is slidably disposed inside the rotating shaft 41 along the vertical direction, and the bottom end of the inverted T-shaped rod extends into the i-shaped channel 47, the first spring 82 is fixedly connected to the top end of the inverted T-shaped rod 81, the push rod 83 is fixedly connected to the top end of the first spring 82 and is slidably nested inside the rotating shaft 41 along the vertical direction, the bottom end of the second spring 84 is fixedly connected to the push rod 83 and the top end of the second spring is fixedly connected to the inner wall of the rotating shaft 41, two accommodating grooves 85 and two closing plates 86 are disposed on the inner wall of the i-shaped channel 47, two closing plates 86 are respectively slidably disposed inside the two 85, and the two closing plates 86 are fixedly connected to the inverted T-shaped rod 81.
Through the arrangement of the structure, when the push rod 83 ascends, the two closing plates 86 are lifted through the first spring 82 and the inverted T-shaped rod 81, so that the closing plates 86 close the top opening of the I-shaped channel 47, and meanwhile, when the closing plates 86 cannot ascend continuously, the push rod 83 stretches the first spring 82 in the subsequent ascending process.
Example 2
The method for preparing the low-chloride rare earth carbonate specifically comprises the following steps:
s1, preparing a suspension by using a precipitation reaction device by using lanthanum carbonate feed liquid and an ammonium bicarbonate solution as raw materials and lanthanum carbonate as seed crystals;
s2, inputting the suspension into the shell 11 through the suspension input pipe 12, filtering the suspension by the filter plate 16, discharging the filtrate through the filtrate output pipe 15, retaining the solid on the top of the filter plate 16, injecting cleaning water into the shell 11 through the cleaning water input pipe 13, washing the solid by the cleaning water, enabling the washed cleaning water to pass through the filter plate 16, and then discharging the washing water through the filtrate output pipe 15;
s3, in the cleaning process, the driving motor 3 drives the rotating shaft 41 to rotate, the rotating shaft 41 drives the lifting ring 42 to ascend when rotating, the lifting ring 42 drives the annular piston 46 to ascend at the inner side of the transparent observation cylinder 5 through the rotating ring 44 and the longitudinal rod 45 when ascending, and the cleaned cleaning water is sucked into the inner side of the transparent observation cylinder 5 through the I-shaped channel 47;
s4, the push rod 83 is pushed upwards when the lifting ring 42 rises, the push rod 83 drives the sealing plate 86 to rise through the first spring 82 and the inverted T-shaped rod 81, the sealing plate 86 seals the top opening of the I-shaped channel 47 along with the continuous rising of the lifting ring 42, and the washed washing water cannot continuously enter the transparent observation cylinder 5;
s5, with the continuous rising of the lifting ring 42, as the closing plate 86 cannot move upwards continuously, the first spring 82 is stretched, and meanwhile, the annular piston 46 moves to the upper part of the L-shaped feeding pipe 62 on the inner side of the transparent observation cylinder 5, so that the silver nitrate solution in the annular storage container 61 is sucked into the inner side of the transparent observation cylinder 5 through the L-shaped feeding pipe 62 and is further quickly mixed with the washed washing water;
s6, observing a mixture of cleaning water and a silver nitrate solution through a transparent observation cylinder 5, stopping inputting the cleaning water if turbid matters are not generated, and simultaneously inputting residual cleaning water and solids into solid-liquid separation equipment through a solids output pipe 14 for solid-liquid separation to obtain a lanthanum carbonate finished product with fine particle size and low chlorine radicals;
s7, if turbid materials are generated, continuously injecting cleaning water, driving the lifting ring 42 to slide downwards under the driving of the reciprocating screw threads when the lifting ring moves to the topmost part of the reciprocating screw threads, further pushing the annular piston 46 through the rotating ring 44 and the longitudinal rod 45, pressurizing the inner cavity of the transparent observation cylinder 5 by the annular piston 46 at the moment, and preventing the mixed liquid inside the transparent observation cylinder 5 from entering the annular storage container 61 through the L-shaped feeding pipe 62 due to the limitation of the one-way valve;
s8, in the descending process of the lifting ring 42, the second spring 84 pushes the push rod 83 to descend synchronously, the push rod 83 firstly drives the stretched first spring 82 to reset, then the first spring 82 and the inverted T-shaped rod 81 drive the closing plate 86 to descend, and further the closing of the top opening of the I-shaped channel 47 is released, at the moment, the mixed liquid inside the transparent observation tube 5 is input to the bottom of the inner cavity of the shell 11 through the I-shaped channel 47 and is then discharged through the filtrate output tube 15, then the lifting ring 42 moves to the lowest end of the reciprocating thread, and then the reciprocating thread drives the lifting ring 42 to ascend again, so that the detection is carried out again.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (7)
1. A method for preparing low-chlorine rare earth carbonate is characterized by comprising the following steps: the method for preparing the low-chlorine rare earth carbonate is realized by using equipment for preparing the low-chlorine rare earth carbonate, the equipment for preparing the low-chlorine rare earth carbonate comprises a filtering and washing mechanism (1), an upper frame (2) is arranged at the top of the filtering and washing mechanism (1), a driving motor (3) is fixedly arranged at the top of the upper frame (2), a suction mechanism (4) is arranged on the inner side of the upper frame (2), a rotating shaft (41) in the driving suction mechanism (4) is rotated by the driving motor (3), a transparent observation barrel (5) is sleeved and arranged on the outer side of the suction mechanism (4), an annular piston (46) in the suction mechanism (4) is lifted on the inner side of the transparent observation barrel (5), a silver nitrate solution feeding mechanism (6) is sleeved and arranged on the outer side of the transparent observation barrel (5), the silver nitrate solution feeding mechanism (6) is arranged on the top of the filtering and washing mechanism (1), an L-shaped feeding pipe (62) in the silver nitrate solution feeding mechanism (6) injects a silver nitrate solution into the inner side of the transparent observation barrel (5), both sides of the silver nitrate solution feeding mechanism (6) are provided with a scraping and a limiting mechanism (7), a scraping mechanism (43) is arranged in the suction mechanism (4), and a closed screw rod (71) is arranged in the suction mechanism, the lifting ring (42) in the suction mechanism (4) drives the push rod (83) in the sealing mechanism (8) to ascend.
2. The method for preparing rare earth carbonate with low chloride content according to claim 1, wherein: the filtering and washing mechanism (1) comprises a shell (11), a suspension input pipe (12), a cleaning water input pipe (13), a solid output pipe (14), a filtrate output pipe (15) and a filter plate (16);
turbid liquid input tube (12) and washing water input tube (13) are all fixed to run through and set up in casing (11) left side top, washing water input tube (13) are located turbid liquid input tube (12) bottom, solid output tube (14) and filtrating output tube (15) are all fixed to run through and set up in casing (11) right side bottom, filtrating output tube (15) are located solid output tube (14) bottom.
3. The method for preparing rare earth carbonate with low chloride content according to claim 2, wherein: the suction mechanism (4) comprises a rotating shaft (41), a lifting ring (42), a limiting sleeve plate (43), a rotating ring (44), a longitudinal rod (45), an annular piston (46) and an I-shaped channel (47);
rotation axis (41) top is connected with driving motor (3) transmission, rotation axis (41) outside is provided with reciprocal screw thread, lifting ring (42) are connected through reciprocal screw thread and rotation axis (41) transmission, spacing lagging panel (43) are fixed to be cup jointed and are set up in lifting ring (42) outside, swivel becket (44) rotate the nestification through the bearing and set up in lifting ring (42) bottom, longitudinal rod (45) are provided with two, two longitudinal rod (45) are fixed respectively and set up in swivel becket (44) bottom both sides, annular piston (46) slide set up in transparent observation section of thick bamboo (5) inboard, and with two longitudinal rod (45) bottom fixed connection, rotation axis (41) are seted up inside I shape passageway (47), I shape passageway (47) one end extends to transparent observation section of thick bamboo (5) inboard and the other end extends to casing (11) inner chamber bottom.
4. The method for preparing rare earth carbonate with low chloride content according to claim 3, wherein: the silver nitrate solution feeding mechanism (6) comprises an annular storage container (61), an L-shaped feeding pipe (62) and a valve (63);
annular storage container (61) is fixed to be set up in casing (11) top, L shape feeder tube (62) all are provided with two, two with valve (63) L shape feeder tube (62) are fixed respectively to run through and set up in annular storage container (61) inboard both sides, L shape feeder tube (62) end fixing runs through and sets up in transparent observation section of thick bamboo (5) side, two valve (63) are fixed respectively to be set up inside two L shape feeder tubes (62), be provided with the check valve on L shape feeder tube (62).
5. The method for preparing rare earth carbonate with low chloride content according to claim 4, wherein: the limiting scraping mechanism (7) comprises a screw rod (71) and a scraping plate (72);
the screw rod (71) runs through the limiting sleeve plate (43) and is in threaded connection with the limiting sleeve plate (43), the screw rod (71) is rotatably connected with the shell (11) through a bearing, the scraping plate (72) is fixedly arranged at the bottom end of the screw rod (71), and the scraping plate is attached to the top of the filter plate (16).
6. The method for preparing rare earth carbonate with low chloride content according to claim 5, wherein: the closing mechanism (8) comprises an inverted T-shaped rod (81), a first spring (82), a push rod (83), a second spring (84), an accommodating groove (85) and a closing plate (86);
fall T shape pole (81) and slide along vertical direction and set up in rotation axis (41) inside, and its bottom extends to inside I shape passageway (47), first spring (82) fixed connection is in falling T shape pole (81) top, catch bar (83) fixed connection is on first spring (82) top, and slides along vertical direction nestedly and set up inside rotation axis (41), second spring (84) bottom and catch bar (83) fixed connection and top and rotation axis (41) inner wall fixed connection, holding tank (85) all are provided with two with closing plate (86), two on holding tank (85) all seted up on I shape passageway (47) inner wall, two closing plate (86) slide respectively and set up in two holding tank (85) inboards, two closing plate (86) all with fall T shape pole (81) fixed connection.
7. The method for preparing rare earth carbonate with low chloride content according to claim 6, wherein the method for preparing rare earth carbonate with low chloride content specifically comprises the following steps:
s1, preparing a suspension by using a precipitation reaction device by using lanthanum carbonate feed liquid and an ammonium bicarbonate solution as raw materials and lanthanum carbonate as a seed crystal;
s2, inputting the suspension into the shell (11) through a suspension input pipe (12), filtering the suspension by a filter plate (16), discharging the filtrate through a filtrate output pipe (15), retaining the solid on the top of the filter plate (16), injecting cleaning water into the shell (11) through a cleaning water input pipe (13), washing the solid by the cleaning water, enabling the washed cleaning water to pass through the filter plate (16), and then discharging the washing water through the filtrate output pipe (15);
s3, in the cleaning process, the driving motor (3) drives the rotating shaft (41) to rotate, the rotating shaft (41) drives the lifting ring (42) to ascend when rotating, the lifting ring (42) drives the annular piston (46) to ascend on the inner side of the transparent observation cylinder (5) through the rotating ring (44) and the longitudinal rod (45) when ascending, and the cleaning water after cleaning is sucked into the inner side of the transparent observation cylinder (5) through the I-shaped channel (47);
s4, the push rod (83) is pushed upwards when the lifting ring (42) rises, so that the push rod (83) drives the closing plate (86) to rise through the first spring (82) and the inverted T-shaped rod (81), the closing plate (86) closes the top opening of the I-shaped channel (47) along with the continuous rising of the lifting ring (42), and washing water after washing cannot continuously enter the transparent observation cylinder (5);
s5, with the continuous rising of the lifting ring (42), as the closing plate (86) cannot move upwards continuously, the first spring (82) is stretched, and meanwhile, the annular piston (46) moves to the position above the L-shaped feeding pipe (62) on the inner side of the transparent observation cylinder (5), so that the silver nitrate solution in the annular storage container (61) is sucked into the inner side of the transparent observation cylinder (5) through the L-shaped feeding pipe (62) and is further rapidly mixed with the washed washing water;
s6, observing a mixture of cleaning water and a silver nitrate solution through a transparent observation cylinder (5), stopping inputting the cleaning water if turbid matters are not generated, and simultaneously inputting residual cleaning water and solids into solid-liquid separation equipment through a solids output pipe (14) for solid-liquid separation to obtain a lanthanum carbonate finished product with fine granularity and low chlorine radicals;
s7, if turbid materials are generated, continuously injecting cleaning water, driving the lifting ring (42) to slide downwards under the driving of reciprocating threads when the lifting ring moves to the topmost part of the reciprocating threads, further pushing the annular piston (46) through the rotating ring (44) and the longitudinal rod (45), pressurizing the inner cavity of the transparent observation cylinder (5) by the annular piston (46), and enabling the mixed liquid inside the transparent observation cylinder (5) not to enter the annular storage container (61) through the L-shaped feeding pipe (62) due to the limitation of the one-way valve;
s8, in the descending process of the lifting ring (42), the second spring (84) pushes the pushing rod (83) to synchronously descend, the pushing rod (83) firstly drives the stretched first spring (82) to reset, then the first spring (82) and the inverted T-shaped rod (81) drive the closing plate (86) to descend, further the closing of the top opening of the I-shaped channel (47) is relieved, at the moment, the mixed liquid on the inner side of the transparent observation tube (5) is input to the bottom of the inner cavity of the shell (11) through the I-shaped channel (47), then the mixed liquid is discharged through the filtrate output tube (15), then the lifting ring (42) moves to the lowest end of the reciprocating thread, and then the reciprocating thread drives the lifting ring (42) to ascend again, so that the detection is carried out again.
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Denomination of invention: A method for preparing low chloride carbonate rare earth Effective date of registration: 20231228 Granted publication date: 20230818 Pledgee: Ganzhou Bank Co.,Ltd. Jishui Branch Pledgor: JISHUI JINCHENG NEW MATERIAL PROCESSING Co.,Ltd. Registration number: Y2023980075458 |
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