CN116553597A - Optical coating ytterbium fluoride processing technology - Google Patents
Optical coating ytterbium fluoride processing technology Download PDFInfo
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- CN116553597A CN116553597A CN202310271734.2A CN202310271734A CN116553597A CN 116553597 A CN116553597 A CN 116553597A CN 202310271734 A CN202310271734 A CN 202310271734A CN 116553597 A CN116553597 A CN 116553597A
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- Prior art keywords
- nitric acid
- ytterbium
- fixedly connected
- mixing barrel
- optical coating
- Prior art date
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- XASAPYQVQBKMIN-UHFFFAOYSA-K ytterbium(iii) fluoride Chemical compound F[Yb](F)F XASAPYQVQBKMIN-UHFFFAOYSA-K 0.000 title claims abstract description 28
- 230000003287 optical effect Effects 0.000 title claims abstract description 22
- 239000011248 coating agent Substances 0.000 title claims abstract description 20
- 238000000576 coating method Methods 0.000 title claims abstract description 20
- 238000005516 engineering process Methods 0.000 title claims abstract description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 101
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 101
- 238000002156 mixing Methods 0.000 claims abstract description 71
- 238000003756 stirring Methods 0.000 claims abstract description 43
- 230000007246 mechanism Effects 0.000 claims abstract description 27
- 238000001125 extrusion Methods 0.000 claims abstract description 19
- KUBYTSCYMRPPAG-UHFFFAOYSA-N ytterbium(3+);trinitrate Chemical compound [Yb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O KUBYTSCYMRPPAG-UHFFFAOYSA-N 0.000 claims description 21
- 238000007789 sealing Methods 0.000 claims description 20
- JCDQGOSXWGXOQQ-UHFFFAOYSA-H ytterbium(3+);tricarbonate Chemical compound [Yb+3].[Yb+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O JCDQGOSXWGXOQQ-UHFFFAOYSA-H 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000000376 reactant Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 8
- -1 rare earth ytterbium oxide Chemical class 0.000 claims description 8
- 229940075624 ytterbium oxide Drugs 0.000 claims description 7
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- 239000012065 filter cake Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000009616 inductively coupled plasma Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000012488 sample solution Substances 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 3
- AUYOHNUMSAGWQZ-UHFFFAOYSA-L dihydroxy(oxo)tin Chemical compound O[Sn](O)=O AUYOHNUMSAGWQZ-UHFFFAOYSA-L 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 230000005484 gravity Effects 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 239000000523 sample Substances 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- SJHMKWQYVBZNLZ-UHFFFAOYSA-K ytterbium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Yb+3] SJHMKWQYVBZNLZ-UHFFFAOYSA-K 0.000 claims description 3
- 239000000243 solution Substances 0.000 description 34
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 4
- 235000017491 Bambusa tulda Nutrition 0.000 description 4
- 241001330002 Bambuseae Species 0.000 description 4
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 4
- 239000011425 bamboo Substances 0.000 description 4
- 238000005304 joining Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000005383 fluoride glass Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000005304 optical glass Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 230000007306 turnover Effects 0.000 description 2
- 206010034972 Photosensitivity reaction Diseases 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 229910001618 alkaline earth metal fluoride Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 230000036211 photosensitivity Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
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
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/253—Halides
- C01F17/265—Fluorides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/05—Stirrers
- B01F27/11—Stirrers characterised by the configuration of the stirrers
- B01F27/19—Stirrers with two or more mixing elements mounted in sequence on the same axis
- B01F27/191—Stirrers with two or more mixing elements mounted in sequence on the same axis with similar elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/71—Feed mechanisms
- B01F35/712—Feed mechanisms for feeding fluids
-
- 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
- C01F17/276—Nitrates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Accessories For Mixers (AREA)
Abstract
The invention discloses an optical coating ytterbium fluoride processing technology, and relates to the technical field of optical coating; the invention solves the problems that repeated adding operation and repeated observation by staff are needed, and comprises a mixing barrel, wherein a nitric acid tank is fixedly connected to the inner surface of the mixing barrel, an extrusion plate is connected to the inner surface of the nitric acid tank in a sliding manner, a threaded cylinder is fixedly connected to the top of the extrusion plate, one end of the threaded cylinder penetrates through the mixing barrel and extends to the outside of the mixing barrel, and a threaded rod is connected to the inner surface of the threaded cylinder in a threaded manner; according to the invention, through the arrangement of the extrusion plate, the extrusion plate moves downwards to extrude the nitric acid in the extrusion plate, so that the nitric acid solution is added into the mixing barrel, and through the arrangement of the cam, the extrusion plate can reciprocate, so that the nitric acid is added in batches, repeated addition is not needed, a certain amount of labor force is saved, and through the arrangement of the stirring mechanism, the solution in the mixing barrel is stirred, so that the solution is uniformly mixed.
Description
Technical Field
The invention relates to the technical field of optical coating, in particular to an optical coating ytterbium fluoride processing technology.
Background
At present, fluoride optical glass material needs are growing year by year, and are mainly applied to the fields of optical fiber communication, medicine and the like. The fluoride optical glass mainly comprises alkaline earth metal fluoride and rare earth fluoride. Ytterbium fluoride is added to fluoride glasses to give the fluoride glasses excellent near infrared and special optical properties.
The existing optical coating ytterbium fluoride processing technology needs to add nitric acid into rare earth ytterbium oxide and deionized water in batches, repeatedly adds a certain amount of labor force, influences processing efficiency, and in the processing process, the reactant needs to be clear and transparent, namely certain acidity is kept in the reaction process, if the reactant is not clear and transparent, nitric acid is added, so that the reactant is clear and transparent, the operation needs to be repeatedly observed by staff, and then nitric acid is added, so that the operation is more troublesome.
In order to solve the above problems, the inventors propose an optical coating ytterbium fluoride processing technology for solving the above problems.
Disclosure of Invention
In order to solve the problem that the repeated adding operation is needed and the repeated observation is needed by the staff; the invention aims to provide an optical coating ytterbium fluoride processing technology.
In order to solve the technical problems, the invention adopts the following technical scheme: the method comprises the following steps:
uniformly mixing rare earth ytterbium oxide and deionized water according to a weight ratio of 3:10;
step two, adding nitric acid in batches, keeping the whole reaction temperature at 70 ℃ and the PH value at the reaction end point at 2.5 to obtain ytterbium nitrate solution;
step three, in the whole reaction process, the reactant is kept clear and transparent, namely certain acidity is kept in the reaction process, and if the reactant is not clear and transparent, nitric acid is added to make the reactant clear and transparent;
fourthly, adding the ytterbium nitrate solution into deionized water, flushing the specific gravity of the diluted ytterbium nitrate solution to 1.15, heating to 105 ℃, preserving heat for 3 hours, removing the head, and filtering into another container;
adding ytterbium hydroxide into the ytterbium nitrate filtrate obtained in the step four, adjusting the pH value of the solution to 3.5, adding a metastannic acid solution with the concentration of 6%, uniformly stirring, heating to 105 ℃, preserving heat for 30 minutes, removing the head, and filtering into another container to obtain ytterbium nitrate filtrate;
step six, sampling from ytterbium nitrate filtrate, detecting the content of metal element Fe, cu, ni, cr, co, mn, ti, V, pb in the sample solution by ICP (inductively coupled plasma mass spectrometer), and checking whether the sample solution is qualified or not;
step seven, concentrating to prepare ytterbium nitrate crystals;
step eight, preparing ytterbium carbonate filter cakes;
step nine, adding water into a ytterbium carbonate filter cake, stirring the mixture into paste with the solid content of 35%, heating the mixture to 45 ℃, adding a small amount of ytterbium carbonate paste into high-purity hydrofluoric acid, stopping adding the ytterbium carbonate paste, slowly adding the ytterbium carbonate paste after large-particle ytterbium fluoride refined seeds are formed, and obtaining ytterbium fluoride precipitate, wherein the pH value of the synthesis reaction end point is 1-2;
and step ten, roasting ytterbium fluoride.
Preferably, the device comprises a mixing barrel, wherein a nitric acid tank is fixedly connected to the inner surface of the mixing barrel, an extruding plate is slidably connected to the inner surface of the nitric acid tank, a threaded barrel is fixedly connected to the top of the extruding plate, one end of the threaded barrel penetrates through the mixing barrel and extends to the outside of the mixing barrel, a threaded rod is connected to the inner surface of the threaded barrel in a threaded manner, a retaining plate is rotated to enable the threaded rod to be retracted into the threaded barrel, the threaded rod drives the retaining plate to descend, the descending distance of the retaining plate is adjusted, the descending distance of the extruding plate is adjusted, the amount of nitric acid extruded for a single time can be adjusted, the applicability of the device is improved, the retaining plate is fixedly connected to one end of the threaded rod, a first reset spring is sleeved on the outer surface of the threaded rod, a rotating shaft is connected to the top of the mixing barrel, a cam is sleeved and fixedly connected to the outer surface of the rotating shaft, and a motor is fixedly connected to the top of the mixing barrel, one end of the output shaft of the motor is fixedly connected with one end of the rotating shaft, the stirring mechanism is arranged in the mixing barrel, the closing mechanism is arranged at the bottom of the nitric acid tank, the photosensitive mechanism is arranged at the bottom of the mixing barrel, the extruding plate moves downwards to extrude nitric acid in the extruding plate through the arrangement of the extruding plate, so that nitric acid solution is added into the mixing barrel, the extruding plate can reciprocate through the arrangement of the cam, nitric acid is added in batches, repeated addition is not needed, a certain amount of labor force is saved, the solution in the mixing barrel is stirred through the arrangement of the stirring mechanism, the solution is uniformly mixed, the outer surface of the mixing barrel is communicated with a first adding pipe, the outer surface of the nitric acid tank is communicated with a second adding pipe, one end of the second adding pipe penetrates through the mixing barrel and extends to the outer part of the mixing barrel, the bottom of the mixing barrel is communicated with a liquid outlet pipe, the first adding pipe is used for adding mixed solution into the mixing barrel, and the second adding pipe is used for adding nitric acid solution into the nitric acid tank.
Preferably, the stirring mechanism comprises a stirring rod, the top of the mixing bucket is rotationally connected with the outer surface of the stirring rod through a bearing, the stirring rack is fixedly connected with the outer surface of the stirring rod, the top end of the stirring rod is fixedly connected with a first bevel gear, the outer surface of the rotating shaft is sleeved with a second bevel gear which is fixedly connected with the stirring rod, the stirring rod is used for installing the stirring rack, and the first bevel gear and the second bevel gear are arranged, so that the rotating shaft can drive the stirring rod to rotate, the use of a motor is reduced, and the manufacturing cost of the device is further reduced.
Preferably, the closing mechanism comprises a sealing plate, the nitric acid through-hole has been seted up to the bottom of nitric acid case, the bottom fixedly connected with bracket of closing plate is used for shutoff nitric acid through-hole, prevents that the solution in the nitric acid case from flowing out, and the bracket is used for installing the closing plate, the bottom of nitric acid case and the both sides that are located the nitric acid through-hole are all fixedly connected with spring barrel, the internal surface fixedly connected with second reset spring of spring barrel, the one end fixedly connected with spring bar of second reset spring, the elasticity messenger closing plate and nitric acid through-hole in close contact with prevent that the solution in the nitric acid case from flowing out, the one end of spring bar and the top fixed connection of bracket, the top of closing plate and the bottom in close contact with of nitric acid case, the bottom intercommunication of nitric acid case has the intake pipe, the surface of intake pipe is provided with the check valve, and the intake pipe is used for installing the check valve, and the setting of check valve makes the outside air of nitric acid case can get into the nitric acid case through the intake pipe, and solution and the air in the nitric acid case can not flow through the intake pipe, and the model of check valve is SS-4C2-1/3.
Preferably, the photosensitive mechanism comprises a searchlight, the surface of searchlight and the bottom fixed connection of nitric acid case, the searchlight has been seted up to the bottom of hybrid bucket, and the searchlight is used for sending the optical signal, cooperates photosensitive switch to use, the bottom of hybrid bucket and the below fixedly connected with sealed transparent glass that is located the searchlight hole, sealed transparent glass's bottom fixedly connected with black box, the internal surface of black box is provided with photosensitive switch, and photosensitive switch's model is KG-F, and photosensitive switch is photosensitive switch that sensitization can be adjusted, and sealed transparent glass is used for sealed searchlight hole, the balancing hole has been seted up at the top of stripper plate, the top intercommunication of hybrid bucket has the balance pipe, the surface of balance pipe is provided with electromagnetic control valve, and when solution in the hybrid bucket was transparent, reciprocating motion of stripper plate made the atmospheric pressure in the nitric acid case pass through the balance pipe business turn over to do not influence the use of stirring mechanism, electromagnetic control valve and external power source electric connection, control through photosensitive switch.
Compared with the prior art, the invention has the beneficial effects that:
1. through the arrangement of the extrusion plate, the extrusion plate moves downwards to extrude nitric acid in the extrusion plate, so that nitric acid solution is added into the mixing barrel, and through the arrangement of the cam, the extrusion plate can reciprocate, so that nitric acid is added in batches, repeated addition is not needed, a certain amount of labor force is saved, and through the arrangement of the stirring mechanism, the solution in the mixing barrel is stirred, so that the solution is uniformly mixed;
2. through searchlight and photosensitive switch's setting, detect the solution in the mixing drum and whether turbid, if turbid, realize automatic add nitric acid, do not need the staff to observe repeatedly and add nitric acid, easy operation is convenient, saves a certain amount of labour.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic diagram of the overall structure of the present invention.
Fig. 2 is a schematic view of the internal structure of the mixing tub according to the present invention.
Fig. 3 is a schematic structural view of the extrusion plate of the present invention.
Fig. 4 is a schematic structural view of the threaded rod of the present invention.
Fig. 5 is a schematic view of the structure of the nitric acid tank of the present invention.
Fig. 6 is a schematic structural view of the sealing plate of the present invention.
Fig. 7 is a schematic structural view of the spring barrel of the present invention.
Fig. 8 is a schematic structural view of the black box of the present invention.
In the figure: 1. a mixing drum; 2. a nitric acid tank; 3. an extrusion plate; 4. a thread cylinder; 5. a threaded rod; 6. a retaining plate; 7. a first return spring; 8. a rotating shaft; 9. a cam; 10. a motor; 11. a stirring mechanism; 12. a closing mechanism; 13. a photosensitive mechanism; 14. a first addition pipe; 15. a second addition pipe; 16. a liquid outlet pipe; 111. a stirring rod; 112. a stirring rack; 113. a first bevel gear; 114. a second bevel gear; 121. nitric acid through holes; 122. a sealing plate; 123. a bracket; 124. a spring barrel; 125. a second return spring; 126. a spring rod; 127. an air inlet pipe; 128. a one-way valve; 131. a searchlight; 132. a probe hole; 133. sealing transparent glass; 134. a black box; 135. a photosensitive switch; 136. a balance hole; 137. a balance tube; 138. an electromagnetic control valve.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
As shown in fig. 1-8, the invention provides an optical coating ytterbium fluoride processing technology, which comprises the following steps:
uniformly mixing rare earth ytterbium oxide and deionized water according to a weight ratio of 3:10;
step two, adding nitric acid in batches, keeping the whole reaction temperature at 70 ℃ and the PH value at the reaction end point at 2.5 to obtain ytterbium nitrate solution;
step three, in the whole reaction process, the reactant is kept clear and transparent, namely certain acidity is kept in the reaction process, and if the reactant is not clear and transparent, nitric acid is added to make the reactant clear and transparent;
fourthly, adding the ytterbium nitrate solution into deionized water, flushing the specific gravity of the diluted ytterbium nitrate solution to 1.15, heating to 105 ℃, preserving heat for 3 hours, removing the head, and filtering into another container;
adding ytterbium hydroxide into the ytterbium nitrate filtrate obtained in the step four, adjusting the pH value of the solution to 3.5, adding a metastannic acid solution with the concentration of 6%, uniformly stirring, heating to 105 ℃, preserving heat for 30 minutes, removing the head, and filtering into another container to obtain ytterbium nitrate filtrate;
step six, sampling from ytterbium nitrate filtrate, detecting the content of metal element Fe, cu, ni, cr, co, mn, ti, V, pb in the sample solution by an ICP inductively coupled plasma mass spectrometer, and checking whether the sample solution is qualified or not;
step seven, concentrating to prepare ytterbium nitrate crystals;
step eight, preparing ytterbium carbonate filter cakes;
step nine, adding water into a ytterbium carbonate filter cake, stirring the mixture into paste with the solid content of 35%, heating the mixture to 45 ℃, adding a small amount of ytterbium carbonate paste into high-purity hydrofluoric acid, stopping adding the ytterbium carbonate paste, slowly adding the ytterbium carbonate paste after large-particle ytterbium fluoride refined seeds are formed, and obtaining ytterbium fluoride precipitate, wherein the pH value of the synthesis reaction end point is 1-2;
and step ten, roasting ytterbium fluoride.
Including mixing barrel 1, the internal surface fixedly connected with nitric acid case 2 of mixing barrel 1, the internal surface sliding connection of nitric acid case 2 has stripper plate 3, the top fixedly connected with screw thread section of thick bamboo 4 of stripper plate 3, the one end of screw thread section of thick bamboo 4 runs through mixing barrel 1 and extends to the outside of mixing barrel 1, the internal surface threaded connection of screw thread section of thick bamboo 4 has threaded rod 5, rotate the butt plate 6, make threaded rod 5 take in screw thread section of thick bamboo 4, threaded rod 5 drive butt plate 6 descend, thereby adjust the decline distance of butt plate 6, thereby adjust the decline distance of stripper plate 3, and then can adjust the quantity of single extrusion nitric acid, the suitability of device increases, the one end fixedly connected with butt plate 6 of threaded rod 5, the surface cover of threaded rod 5 is equipped with first reset spring 7, the top rotation of mixing barrel 1 is connected with axis of rotation 8, the surface cover of axis of rotation 8 is established and fixedly connected with cam 9, the top fixedly connected with motor 10 of mixing barrel 1, the one end of motor 10 output shaft and the one end fixedly connected with of axis of rotation 8, the inside of mixing barrel 1 is provided with rabbling mechanism 11, the bottom of nitric acid case 2 is provided with closing mechanism 12, the bottom of mixing barrel 1 is provided with photosensitive mechanism 13.
Through adopting above-mentioned technical scheme, through the setting of stripper plate 3, the stripper plate 3 downwardly moving extrudes the nitric acid in the stripper plate 3 to add the nitric acid solution in to mixing drum 1, through the setting of cam 9, make stripper plate 3 can carry out reciprocating motion, thereby add the nitric acid in batches, do not need the manual work to add repeatedly, save a certain amount of labour, through the setting of rabbling mechanism 11, stir the solution in the mixing drum 1, make solution misce bene.
The surface intercommunication of mixing drum 1 has first joining pipe 14, and the surface intercommunication of nitric acid case 2 has second joining pipe 15, and the one end of second joining pipe 15 runs through mixing drum 1 and extends to the outside of mixing drum 1, and the bottom intercommunication of mixing drum 1 has drain pipe 16.
By adopting the above technical scheme, the first adding pipe 14 is used for adding the mixed solution into the mixing tank 1, and the second adding pipe 15 is used for adding the nitric acid solution into the nitric acid tank 2.
The stirring mechanism 11 comprises a stirring rod 111, the top of the mixing drum 1 is rotatably connected with the outer surface of the stirring rod 111 through a bearing, a stirring frame 112 is fixedly connected with the outer surface of the stirring rod 111, a first bevel gear 113 is fixedly connected with the top end of the stirring rod 111, and a second bevel gear 114 is sleeved on the outer surface of the rotating shaft 8 and fixedly connected with the outer surface of the stirring rod.
Through adopting above-mentioned technical scheme, puddler 111 is used for installing stirring frame 112, and first bevel gear 113 and the setting of second bevel gear 114 make axis of rotation 8 can drive puddler 111 rotation to reduce the use of motor, and then reduce the manufacturing cost of device.
The closing mechanism 12 comprises a sealing plate 122, a nitric acid through hole 121 is formed in the bottom of the nitric acid tank 2, and a bracket 123 is fixedly connected to the bottom of the sealing plate 122.
By adopting the above technical scheme, the sealing plate 122 is used for plugging the nitric acid through hole 121, preventing the solution in the nitric acid tank 2 from flowing out, and the bracket 123 is used for installing the sealing plate 122.
The bottom of the nitric acid tank 2 and two sides of the nitric acid through hole 121 are fixedly connected with a spring barrel 124, the inner surface of the spring barrel 124 is fixedly connected with a second return spring 125, and one end of the second return spring 125 is fixedly connected with a spring rod 126.
By adopting the above technical scheme, the elastic force of the second return spring 125 makes the sealing plate 122 closely contact with the nitric acid through hole 121, preventing the solution in the nitric acid tank 2 from flowing out.
One end of the spring rod 126 is fixedly connected with the top of the bracket 123, the top of the sealing plate 122 is tightly contacted with the bottom of the nitric acid tank 2, the bottom of the nitric acid tank 2 is communicated with an air inlet pipe 127, and the outer surface of the air inlet pipe 127 is provided with a one-way valve 128.
Through adopting above-mentioned technical scheme, intake pipe 127 is used for installing check valve 128, and the setting of check valve 128 makes the outside air of nitric acid case 2 can get into nitric acid case 2 through intake pipe 127, and solution and the air in the nitric acid case 2 can not flow out through intake pipe 127, and the model of check valve 128 is SS-4C2-1/3.
The photosensitive mechanism 13 comprises a searchlight 131, the outer surface of the searchlight 131 is fixedly connected with the bottom of the nitric acid tank 2, and a searchlight hole 132 is formed in the bottom of the mixing drum 1.
By adopting the above technical scheme, the searchlight 131 is used for emitting light signals and is matched with the photosensitive switch 135 for use.
The bottom of mixing bucket 1 and be located the below fixedly connected with sealed transparent glass 133 of searchlight hole 132, the bottom fixedly connected with black box 134 of sealed transparent glass 133, the internal surface of black box 134 is provided with photosensitive switch 135.
By adopting the above technical scheme, the model of the photosensitive switch 135 is KG-F, and the photosensitive switch 135 is a photosensitive switch with adjustable photosensitivity, and the sealing transparent glass 133 is used for sealing the probe hole 132.
The balance hole 136 has been seted up at the top of stripper plate 3, and the top intercommunication of mixing drum 1 has balance pipe 137, and the surface of balance pipe 137 is provided with electromagnetic control valve 138.
Through adopting above-mentioned technical scheme, when the solution in the mixing drum 1 is transparent, the reciprocating motion of stripper plate 3 makes the atmospheric pressure in the nitric acid case 2 pass through balance pipe 137 business turn over to do not influence the use of rabbling mechanism 11, electromagnetic control valve 138 and external power supply electric connection, control through photosensitive switch 135.
Working principle: adding nitric acid solution into the nitric acid tank 2 through a second adding pipe 15, adding rare earth ytterbium oxide and deionized water into the mixing drum 1 through a first adding pipe 14, adding the rare earth ytterbium oxide and the deionized water according to the weight ratio of 3:10, starting a motor 10 to drive a rotating shaft 8 to rotate a second bevel gear 114, the second bevel gear 114 drives a first bevel gear 113 to rotate a stirring rod 111, the stirring rod 111 drives a stirring rack 112 to rotate, thereby mixing the rare earth ytterbium oxide and the deionized water, simultaneously, the rotating shaft 8 drives a cam 9 to rotate, the cam 9 presses a resisting plate 6 to shrink a first reset spring 7, the resisting plate 6 drives a threaded rod 5 to descend, the threaded drum 4 drives a pressing plate 3 to descend, the pressing plate 3 descends to extrude nitric acid in the nitric acid tank 2 through a nitric acid through hole 121, and when the nitric acid is extruded through the nitric acid through hole 121, a sealing plate 122 drives a bracket 123 to descend a spring rod 126, when the spring rod 126 drives the second reset spring 125 to extend and the extrusion plate 3 rises, the second reset spring 125 contracts to drive the spring rod 126 to enable the bracket 123 to rise, the bracket 123 drives the sealing plate 122 to enable the nitric acid through hole 121 to be plugged, meanwhile, the extrusion plate 3 rises to enable air outside the nitric acid tank 2 to enter the nitric acid tank 2 through the air inlet pipe 127, so that pressure balance in the nitric acid tank 2 is ensured, solution in the mixing tank 1 is gradually transparent through continuously adding nitric acid in batches, when the solution is transparent, light emitted by the searchlight 131 sequentially enters the black tank 134 through the searchlight hole 132 and the sealing transparent glass 133, due to the arrangement of the photosensitive switch 135, the photosensitive switch 135 receives a light signal to open the electromagnetic control valve 138, after the electromagnetic control valve 138 is opened, the extrusion plate 3 descends to enable the air in the nitric acid tank 2 to sequentially pass through the balance hole 136 and the balance pipe 137, when the extrusion plate 3 ascends, air outside the mixing barrel 1 enters the nitric acid tank 2 through the balance pipe 137, so that the pressure balance in the nitric acid tank 2 is ensured, and meanwhile, nitric acid in the nitric acid tank 2 is not extruded by the reciprocating motion of the extrusion plate 3, so that the addition of nitric acid is stopped.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (10)
1. The optical coating ytterbium fluoride processing technology is characterized by comprising the following steps of:
uniformly mixing rare earth ytterbium oxide and deionized water according to a weight ratio of 3:10;
step two, adding nitric acid in batches, keeping the whole reaction temperature at 70 ℃ and the PH value at the reaction end point at 2.5 to obtain ytterbium nitrate solution;
step three, in the whole reaction process, the reactant is kept clear and transparent, namely certain acidity is kept in the reaction process, and if the reactant is not clear and transparent, nitric acid is added to make the reactant clear and transparent;
fourthly, adding the ytterbium nitrate solution into deionized water, flushing the specific gravity of the diluted ytterbium nitrate solution to 1.15, heating to 105 ℃, preserving heat for 3 hours, removing the head, and filtering into another container;
adding ytterbium hydroxide into the ytterbium nitrate filtrate obtained in the step four, adjusting the pH value of the solution to 3.5, adding a metastannic acid solution with the concentration of 6%, uniformly stirring, heating to 105 ℃, preserving heat for 30 minutes, removing the head, and filtering into another container to obtain ytterbium nitrate filtrate;
step six, sampling from ytterbium nitrate filtrate, detecting the content of metal element Fe, cu, ni, cr, co, mn, ti, V, pb in the sample solution by ICP (inductively coupled plasma mass spectrometer), and checking whether the sample solution is qualified or not;
step seven, concentrating to prepare ytterbium nitrate crystals;
step eight, preparing ytterbium carbonate filter cakes;
step nine, adding water into a ytterbium carbonate filter cake, stirring the mixture into paste with the solid content of 35%, heating the mixture to 45 ℃, adding a small amount of ytterbium carbonate paste into high-purity hydrofluoric acid, stopping adding the ytterbium carbonate paste, slowly adding the ytterbium carbonate paste after large-particle ytterbium fluoride refined seeds are formed, and obtaining ytterbium fluoride precipitate, wherein the pH value of the synthesis reaction end point is 1-2;
and step ten, roasting ytterbium fluoride.
2. The optical coating ytterbium fluoride processing device of claim 1, comprising a mixing barrel (1), wherein the inner surface of the mixing barrel (1) is fixedly connected with a nitric acid box (2), the inner surface of the nitric acid box (2) is slidingly connected with a squeeze plate (3), the top of the squeeze plate (3) is fixedly connected with a threaded barrel (4), one end of the threaded barrel (4) penetrates through the mixing barrel (1) and extends to the outside of the mixing barrel (1), the inner surface of the threaded barrel (4) is in threaded connection with a threaded rod (5), one end of the threaded rod (5) is fixedly connected with a retaining plate (6), the utility model discloses a mixing barrel, including threaded rod (5), rotary shaft (8), rotary shaft (1), cam (9) are established and fixedly connected with to the top rotation of mixing barrel (1), top fixedly connected with motor (10) of mixing barrel (1), the one end of motor (10) output shaft and the one end fixed connection of rotary shaft (8), the inside of mixing barrel (1) is provided with rabbling mechanism (11), the bottom of nitric acid case (2) is provided with closing mechanism (12), the bottom of mixing barrel (1) is provided with photosensitive mechanism (13).
3. The optical coating ytterbium fluoride processing device according to claim 1, wherein the outer surface of the mixing barrel (1) is communicated with a first adding pipe (14), the outer surface of the nitric acid tank (2) is communicated with a second adding pipe (15), one end of the second adding pipe (15) penetrates through the mixing barrel (1) and extends to the outside of the mixing barrel (1), and the bottom of the mixing barrel (1) is communicated with a liquid outlet pipe (16).
4. The optical coating ytterbium fluoride processing device according to claim 1, wherein the stirring mechanism (11) comprises a stirring rod (111), the top of the mixing drum (1) is rotatably connected with the outer surface of the stirring rod (111) through a bearing, a stirring frame (112) is fixedly connected with the outer surface of the stirring rod (111), a first bevel gear (113) is fixedly connected with the top end of the stirring rod (111), and a second bevel gear (114) is sleeved on the outer surface of the rotating shaft (8) and fixedly connected with the outer surface of the stirring rod.
5. The optical coating ytterbium fluoride processing device according to claim 1, wherein the closing mechanism (12) comprises a sealing plate (122), a nitric acid through hole (121) is formed in the bottom of the nitric acid tank (2), and a bracket (123) is fixedly connected to the bottom of the sealing plate (122).
6. The optical coating ytterbium fluoride processing device according to claim 5, wherein spring barrels (124) are fixedly connected to the bottom of the nitric acid tank (2) and located on two sides of the nitric acid through hole (121), a second return spring (125) is fixedly connected to the inner surface of each spring barrel (124), and a spring rod (126) is fixedly connected to one end of each second return spring (125).
7. The optical coating ytterbium fluoride processing device according to claim 6, wherein one end of the spring rod (126) is fixedly connected with the top of the bracket (123), the top of the sealing plate (122) is in close contact with the bottom of the nitric acid tank (2), the bottom of the nitric acid tank (2) is communicated with an air inlet pipe (127), and a one-way valve (128) is arranged on the outer surface of the air inlet pipe (127).
8. The optical coating ytterbium fluoride processing device according to claim 1, wherein the photosensitive mechanism (13) comprises a searchlight (131), the outer surface of the searchlight (131) is fixedly connected with the bottom of the nitric acid tank (2), and a searchlight hole (132) is formed in the bottom of the mixing drum (1).
9. The optical coating ytterbium fluoride processing device of claim 8, wherein a sealing transparent glass (133) is fixedly connected to the bottom of the mixing barrel (1) and below the probe hole (132), a black box (134) is fixedly connected to the bottom of the sealing transparent glass (133), and a photosensitive switch (135) is arranged on the inner surface of the black box (134).
10. The optical coating ytterbium fluoride processing device according to claim 9, wherein a balance hole (136) is formed in the top of the extrusion plate (3), a balance pipe (137) is communicated with the top of the mixing barrel (1), and an electromagnetic control valve (138) is arranged on the outer surface of the balance pipe (137).
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| CN202310271734.2A CN116553597A (en) | 2023-03-20 | 2023-03-20 | Optical coating ytterbium fluoride processing technology |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117584310A (en) * | 2024-01-19 | 2024-02-23 | 纳琳威纳米科技（上海）有限公司 | Raw material mixing device for optical film production |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117584310A (en) * | 2024-01-19 | 2024-02-23 | 纳琳威纳米科技（上海）有限公司 | Raw material mixing device for optical film production |
| CN117584310B (en) * | 2024-01-19 | 2024-05-10 | 纳琳威纳米科技（上海）有限公司 | Raw material mixing device for optical film production |
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