CN117945450A - Production process of nano rare earth polishing solution - Google Patents
Production process of nano rare earth polishing solution Download PDFInfo
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- CN117945450A CN117945450A CN202410116854.XA CN202410116854A CN117945450A CN 117945450 A CN117945450 A CN 117945450A CN 202410116854 A CN202410116854 A CN 202410116854A CN 117945450 A CN117945450 A CN 117945450A
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- 238000005498 polishing Methods 0.000 title claims abstract description 38
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 20
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 68
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000001238 wet grinding Methods 0.000 claims abstract description 18
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 17
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 230000001590 oxidative effect Effects 0.000 claims abstract description 10
- 238000003825 pressing Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 238000001704 evaporation Methods 0.000 claims abstract description 5
- 230000008020 evaporation Effects 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 36
- 239000000463 material Substances 0.000 claims description 34
- 239000002351 wastewater Substances 0.000 claims description 31
- 238000005086 pumping Methods 0.000 claims description 22
- 239000002002 slurry Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 19
- 238000007254 oxidation reaction Methods 0.000 claims description 15
- 238000003860 storage Methods 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 13
- 239000012065 filter cake Substances 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 10
- 238000011049 filling Methods 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 8
- 239000002912 waste gas Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 6
- 229920002313 fluoropolymer Polymers 0.000 claims description 5
- 238000003786 synthesis reaction Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 8
- 238000001035 drying Methods 0.000 abstract description 2
- 239000007800 oxidant agent Substances 0.000 abstract description 2
- 239000012716 precipitator Substances 0.000 abstract description 2
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 45
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 13
- 239000000843 powder Substances 0.000 description 10
- 239000002245 particle Substances 0.000 description 7
- 229910021529 ammonia Inorganic materials 0.000 description 6
- 238000009837 dry grinding Methods 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 238000004880 explosion Methods 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 239000011858 nanopowder Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000007517 polishing process Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 208000004998 Abdominal Pain Diseases 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 201000004569 Blindness Diseases 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 206010008479 Chest Pain Diseases 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 208000000059 Dyspnea Diseases 0.000 description 1
- 206010013975 Dyspnoeas Diseases 0.000 description 1
- 208000007101 Muscle Cramp Diseases 0.000 description 1
- 208000007542 Paresis Diseases 0.000 description 1
- 206010040026 Sensory disturbance Diseases 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000036760 body temperature Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- DPUCLPLBKVSJIB-UHFFFAOYSA-N cerium;tetrahydrate Chemical compound O.O.O.O.[Ce] DPUCLPLBKVSJIB-UHFFFAOYSA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000006735 deficit Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 230000001787 epileptiform Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000010129 solution processing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 230000008673 vomiting Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 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
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/235—Cerium oxides or hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a production process of nano rare earth polishing solution, which comprises the specific steps of taking ultra-high purity cerium nitrate crystal as a raw material, dissolving and preparing by pure water to obtain high purity cerium nitrate feed liquid, taking hydrogen peroxide as an oxidant, taking ammonia water as a precipitator, reversely precipitating, heating at high temperature, washing, plate-frame filter pressing, flash evaporation and drying, oxidizing roasting and wet grinding to obtain the high purity nano polishing solution.
Description
Technical Field
The invention relates to the technical field of polishing solution processing technology, in particular to a production technology of nano rare earth polishing solution.
Background
The rare earth element is applied to polishing solution or polishing powder, the rare earth polishing solution has the characteristics of low hardness, less scratch, high polishing speed, high precision and the like, in the polishing process, the rare earth polishing solution mainly plays a role in forming a layer of film on the surface of a workpiece through chemical action, then the abrasive in the polishing solution removes the film through mechanical action, and finally the chemical mechanical polishing process is finished, and the existing rare earth polishing solution has complex preparation process and high cost.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a production process of nano rare earth polishing solution, which solves the problems that the purity of the existing rare earth polishing solution preparation process is relatively low and damage is brought to electronic products such as grinding.
A production process of nano rare earth polishing solution comprises the following steps:
Step one, preparing cerium nitrate solution
Pumping quantitative pure water into a solution tank from a pure water storage tank through a pump, adding cerium nitrate crystals into the solution tank through a vacuum suction machine, stirring in the solution tank until the cerium nitrate crystals are completely dissolved to obtain high-purity cerium nitrate feed liquid, and pumping the high-purity cerium nitrate feed liquid into a storage tank through a centrifugal pump;
step two, oxidation reaction
Pumping the cerium nitrate solution prepared in the first step into a high-level metering tank through a centrifugal pump from a storage tank, quantitatively adding the cerium nitrate solution into the solution tank through the high-level metering tank, quantitatively adding hydrogen peroxide into the solution tank, mixing the hydrogen peroxide and the cerium nitrate solution in the storage tank to perform oxidation reaction, and pumping the cerium nitrate solution into the high-level metering tank through the centrifugal pump after the oxidation reaction is completed;
Step three, synthesis reaction
Pumping quantitative ammonia water into a reaction kettle from an ammonia water storage tank through a centrifugal pump, adding the reaction materials in the second step into the reaction kettle quantitatively, mixing the reaction materials in the reaction kettle to react, heating the materials in the reaction kettle by steam after the reaction of the materials is finished, and standing and cooling the materials after the heating is finished;
Step four, washing and filter pressing
Discharging the supernatant fluid of the materials in the reaction kettle in the third step to a wastewater receiving tank, adding pure water into the slurry for washing for 1-3 times, placing the slurry into the slurry receiving tank, pumping the slurry from the slurry receiving tank into a filter press for press filtration by a feed pump, enabling the wastewater pressed by the filter press to enter the wastewater receiving tank, and pumping the wastewater to a wastewater tank by a centrifugal pump;
step five, roasting and oxidizing
Conveying the filter cake generated in the step four to an electric kiln workshop through a forklift, roasting at a high temperature through an electric kiln, treating waste gas generated by roasting through a spraying system, discharging the waste gas through an exhaust pipe, roasting the filter cake at the high temperature to enable the filter cake to undergo an oxidation reaction, and oxidizing to obtain high-purity cerium oxide;
Step six, grinding
Then, carrying out wet grinding on the high-purity cerium oxide generated in the step five;
Seventh, filling
And (5) after wet grinding, filling the finished product into a high-purity nano polishing solution product.
In one embodiment of the invention, the materials in the reaction kettle are heated by steam in the third step to 95-120 ℃.
In one embodiment of the invention, in the fourth step, the filter cake is baked at a high temperature by an electric kiln, wherein the baking temperature is 600-800 ℃.
In one embodiment of the invention, the centrifugal pump is a fluoroplastic centrifugal pump.
In one embodiment of the invention, the waste gas generated in the third step and the fifth step is input into a spraying system for treatment and then is discharged.
In one embodiment of the invention, the wastewater generated in the fourth step and the spraying system is discharged into a four-effect evaporation processor for treatment, and the treated water is recycled.
In one embodiment of the invention, the materials in the reaction kettle are stirred while the reaction kettle is heated in the third step.
The invention provides a production process of a nano rare earth polishing solution, which has the following beneficial effects:
The preparation of the polishing solution comprises the steps of firstly preparing cerium nitrate solution, then carrying out oxidation reaction on the cerium nitrate solution, then carrying out synthesis reaction on materials obtained by oxidation, then washing and filter pressing the synthesized materials, roasting and oxidizing a filter cake, then carrying out wet grinding on the roasted materials, and finally filling a finished polishing solution product.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a flow chart of the production process of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
In the description of the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "coupled," and the like are to be construed broadly and may be, for example, fixedly attached, detachably attached, or integrally attached; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention.
Examples
The high-purity nano polishing liquid product takes ultra-high-purity cerium nitrate crystals as raw materials, pure water is used for dissolution and blending to obtain high-purity cerium nitrate feed liquid, hydrogen peroxide is used as an oxidant, ammonia water is used as a precipitator, reverse precipitation is carried out, and the high-purity nano polishing liquid is obtained through high-temperature heating, washing, plate and frame filter pressing, flash evaporation drying, oxidizing roasting and wet grinding. The chemical reaction equation involved is as follows:
2Ce(NO3)3+3H2O2+6NH3·H2O→2Ce(OH)3OOH+6NH4NO3+2H2O
Ce(OH)3OOH→Ce(OH)4+1/2O2↑
Quality standard: polishing the SiO2 insulating layer on the integrated circuit chip by using CeO 2-based polishing solution, wherein the polishing speed is more than or equal to 100nm/min and the surface roughness Ra is less than or equal to 1nm under proper process conditions;
product parameters: the total concentration of harmful impurity ions in the CeO2 polishing solution reaches the sub-ppm level; ceO2 has narrow size distribution, the central value of the primary particle size is 100+/-30 nm, and the maximum particle size in the polishing solution is less than 300nm.
A production process of nano rare earth polishing solution comprises the following steps:
Step one, preparing cerium nitrate solution
Pumping quantitative pure water into a solution tank from a pure water storage tank through a pump, adding raw material cerium nitrate into the solution tank through a vacuum suction machine, utilizing the air pressure difference between vacuum and an environment space by the vacuum suction machine to form air flow in a pipeline to drive the raw material cerium nitrate to move, thereby completing the transportation of the raw material, wherein the annual usage amount of the raw material cerium nitrate is 108t, the pure water amount required for preparing a cerium nitrate solution is 612t/a, stirring in the solution tank until the raw material cerium nitrate is completely dissolved to obtain high-purity cerium nitrate feed liquid, pumping the high-purity cerium nitrate feed liquid into the solution tank through a fluoroplastic centrifugal pump, and waiting for entering the next oxidation synthesis reaction process;
step two, oxidation reaction
Pumping the high-purity cerium nitrate solution prepared in the first step into a high-level metering tank through a fluoroplastic centrifugal pump from a storage tank, quantitatively adding the high-level metering tank into a solution tank, quantitatively adding hydrogen peroxide into the solution tank (pumping the hydrogen peroxide into the high-level metering tank through the fluoroplastic centrifugal pump from a hydrogen peroxide storage tank), mixing the hydrogen peroxide and the cerium nitrate solution in the storage tank to perform oxidation reaction, and pumping the mixture into the high-level metering tank through the centrifugal pump after the oxidation reaction is finished; hydrogen peroxide: colorless transparent liquid with weak special smell, and is soluble in water, alcohol and ether, insoluble in benzene and petroleum ether. Melting point: -2 ℃ (anhydrous), boiling point: 158 ℃ (anhydrous), saturated vapor pressure 0.13
(15.3 ℃), Relative density (water=1): 1.46 (anhydrous) relative density (air=1): 3.5. hydrogen peroxide is not combustible, but can react with combustible materials to release a large amount of heat and oxygen to cause ignition explosion. The PH value of hydrogen peroxide is most stable at 3.5-4.5, is easy to decompose in alkaline solution, and can decompose when encountering strong light, especially when irradiated by wave rays. When heated above 100 ℃, rapid decomposition begins. It forms an explosive mixture with many organic substances, such as sugar, starch, alcohols, petroleum products, etc., and can explode under the action of impact, heat or electric spark. Hydrogen peroxide can be rapidly decomposed to cause explosion after contacting with a plurality of inorganic compounds or impurities, and a large amount of heat, oxygen and water vapor are emitted. Most heavy metals (such as iron, copper, silver, lead, mercury, zinc, cobalt, nickel, chromium, manganese, etc.) and their oxides and salts are active catalysts, and dust, soot, carbon powder, rust, etc. can also accelerate decomposition. Hydrogen peroxide at a concentration exceeding 74% can cause gas phase explosions in closed containers with appropriate ignition sources or temperatures. Inhalation of the product vapor or mist is strongly irritating to the respiratory tract. Direct eye contact with liquids can lead to irreversible loss and even blindness. Oral poisoning may occur as abdominal pain, chest pain, dyspnea, vomiting, chronokinesia and sensory disturbance, elevated body temperature, etc. Individual cases present with vision impairment, epileptiform cramps, paresis, etc.
The chemical reaction equation involved in this process is as follows:
2Ce(NO3)3+3H2O2+4H2O→2Ce(OH)3OOH+6HNO3
Step three, synthesis reaction
The ammonia water contains NH 3·H2 O as main component, is aqueous ammonia solution, has molecular weight of 35, is colorless and transparent, and has pungent smell. Ammonia has a melting point of-77.773 ℃, a boiling point of-33.34 ℃ and a density of 0.91g/cm 3. Ammonia is easily dissolved in water and ethanol. Is volatile, has partial alkali permeability, and is prepared by introducing ammonia into water. Ammonia is toxic, has irritation and corrosiveness to eyes, nose and skin, can suffocate people, and has the maximum allowable concentration of 30mg/m 3 in air. Industrial ammonia water is an aqueous solution containing 25% -28% ammonia, and only a small part of ammonia molecules in the ammonia water react with water to form ammonia monohydrate, which is a weak base only existing in the ammonia water. The freezing point of ammonia water is related to the concentration of ammonia water, and the common (wt) concentration freezing point is about-35 ℃, and the ammonia water reacts with acid to generate heat, so that the risk of combustion explosion exists. Pumping quantitative ammonia water into a reaction kettle from an ammonia water storage tank through a centrifugal pump, adding the reaction materials in the second step into the reaction kettle quantitatively, mixing the reaction materials in the reaction kettle to react, heating the reaction kettle, stirring the materials in the reaction kettle, heating the materials in the reaction kettle by steam after the reaction of the materials in the reaction kettle is finished, heating the materials to a temperature of more than 95 ℃ for 120 ℃, and standing and cooling the materials after the heating is finished;
Step four, washing and filter pressing
Discharging the supernatant fluid obtained after the materials in the reaction kettle in the third step are kept still to a wastewater receiving tank, adding pure water into the slurry of the precipitation reactant to wash for 1-3 times, wherein the pure water is 4950t/a, placing the slurry into the slurry receiving tank, pumping the slurry from the slurry receiving tank into a filter press for filter pressing by a feed pump, allowing the wastewater subjected to filter pressing by a plate-and-frame filter press to enter the wastewater receiving tank, and pumping the wastewater into a wastewater tank by a centrifugal pump;
step five, roasting and oxidizing
Conveying the filter cake produced in the fourth step to an electric kiln workshop through a forklift, roasting at a high temperature of 600-800 ℃ through an electric kiln, treating waste gas produced by roasting through a spraying system, discharging the waste gas through an exhaust pipe, and roasting the filter cake at a high temperature to enable the filter cake to undergo an oxidation reaction to obtain high-purity cerium oxide;
Step six, grinding
Then, carrying out wet grinding on the high-purity cerium oxide generated in the step five, wherein the pure water amount used in the process is 252t/a;
The physical mechanical grinding method can lead the powder material to reach the nanometer, namely dry grinding and wet grinding, and for the manufacture of nanometer powder, it is of course desirable to obtain the final nanometer powder by a dry grinding method. However, when the powder is mechanically ground, the temperature of the powder is rapidly increased by the introduction of a large amount of energy during the grinding process, and it is difficult to control the grinding machine as to how to avoid the explosion-proof problem after the particles are refined. Therefore, in general, the particle size of dry milling can only be milled to 8. Mu.m. If a particle size of 8 μm or less is to be obtained, wet milling must be used. Grinding the resulting powder with a wet grinder is the most efficient and economical method. The method avoids the high cost of chemical nano powder manufacture and the defect that the mechanical dry grinding fineness is difficult to reach nano powder.
Wet grinding is to mix the nano powder with a proper solvent to prepare a proper material. In order to avoid the phenomenon of powder agglomeration in the grinding process, proper dispersing agents or auxiliary agents are needed to be added as grinding aids.
If the final nanoscale product is desired to be a powder rather than a slurry, consideration must be given to how to filter the large particles in the slurry first and how to dry the filtered slurry to obtain the nanoscale powder. The bead mill for wet grinding is to determine how large zirconia beads are selected according to the initial particle size and the final fineness of the materials.
The dry grinding particle size can only be ground to about 8um, if the grinding operation is to be performed in a finer or nanoscale manner, the wet grinding is performed by using wet grinding, wherein the water content of the material is not more than 4%, and the wet grinding is performed by suspending the raw material in carrier liquid flow for grinding, and adding additives such as dispersing agents and the like to assist the grinding. When the water content of the material in the wet grinding machine exceeds 50%, the problem of dust flying can be overcome. In food processing, the ground material is often used as a preliminary operation for leaching, making the components easy to dissolve out, and is therefore well suited for wet grinding processes. Wet operations generally consume more energy than dry operations and the wear of equipment is also more severe.
Seventh, filling
And after wet grinding, filling the slurry into a high-purity nano polishing solution finished product, wherein the filling of the polishing solution is common knowledge of a person skilled in the art and is not described in detail again.
Step four, wastewater generated by the spraying system is discharged into a four-effect evaporation processor for treatment, the treated water is recycled, specifically, after slurry generated by precipitation reaction is kept stand, generated waste supernatant is discharged into a wastewater receiving tank and finally enters a wastewater land tank, the wastewater is discharged into the wastewater receiving tank after the wastewater is treated by a four-effect evaporator, the non-discharged precipitation reactant slurry is washed by pure water, and finally enters the wastewater land tank, and the wastewater is treated by the four-effect evaporator and is not discharged; the washed slurry is subjected to plate and frame filter pressing to generate filter pressing wastewater which is discharged to a wastewater receiving tank and finally enters a wastewater land tank, and the wastewater is not discharged when being treated by a four-effect evaporator; the wastewater of the water spray tower is recycled after being subjected to sedimentation treatment in a sedimentation tank, and is not discharged; the waste water of the alkali spray tower is recycled after being treated by a plate-and-frame filter press, and is not discharged.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, and various modifications and variations may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A production process of nano rare earth polishing solution is characterized in that: the method comprises the following steps:
Step one, preparing cerium nitrate solution
Pumping quantitative pure water into a solution tank from a pure water storage tank through a pump, adding cerium nitrate crystals into the solution tank through a vacuum suction machine, stirring in the solution tank until the cerium nitrate crystals are completely dissolved to obtain high-purity cerium nitrate feed liquid, and pumping the high-purity cerium nitrate feed liquid into a storage tank through a centrifugal pump;
step two, oxidation reaction
Pumping the cerium nitrate solution prepared in the first step into a high-level metering tank through a centrifugal pump from a storage tank, quantitatively adding the cerium nitrate solution into the solution tank through the high-level metering tank, quantitatively adding hydrogen peroxide into the solution tank, mixing the hydrogen peroxide and the cerium nitrate solution in the storage tank to perform oxidation reaction, and pumping the cerium nitrate solution into the high-level metering tank through the centrifugal pump after the oxidation reaction is completed;
Step three, synthesis reaction
Pumping quantitative ammonia water into a reaction kettle from an ammonia water storage tank through a centrifugal pump, adding the reaction materials in the second step into the reaction kettle quantitatively, mixing the reaction materials in the reaction kettle to react, heating the materials in the reaction kettle by steam after the reaction of the materials is finished, and standing and cooling the materials after the heating is finished;
Step four, washing and filter pressing
Discharging the supernatant fluid of the materials in the reaction kettle in the third step to a wastewater receiving tank, adding pure water into the slurry for washing for 1-3 times, placing the slurry into the slurry receiving tank, pumping the slurry from the slurry receiving tank into a filter press for press filtration by a feed pump, enabling the wastewater pressed by the filter press to enter the wastewater receiving tank, and pumping the wastewater to a wastewater tank by a centrifugal pump;
step five, roasting and oxidizing
Conveying the filter cake generated in the step four to an electric kiln workshop through a forklift, roasting at a high temperature through an electric kiln, treating waste gas generated by roasting through a spraying system, discharging the waste gas through an exhaust pipe, roasting the filter cake at the high temperature to enable the filter cake to undergo an oxidation reaction, and oxidizing to obtain high-purity cerium oxide;
Step six, grinding
Then, carrying out wet grinding on the high-purity cerium oxide generated in the step five;
Seventh, filling
And (5) after wet grinding, filling the finished product into a high-purity nano polishing solution product.
2. The process for producing the nano rare earth polishing solution according to claim 1, which is characterized in that: and in the third step, the materials in the reaction kettle are heated by steam to 95-120 ℃.
3. The process for producing the nano rare earth polishing solution according to claim 1, which is characterized in that: and in the fourth step, the filter cake is roasted at a high temperature by an electric kiln, wherein the roasting temperature is 600-800 ℃.
4. The process for producing the nano rare earth polishing solution according to claim 1, which is characterized in that: the centrifugal pump is a fluoroplastic centrifugal pump.
5. The process for producing the nano rare earth polishing solution according to claim 1, which is characterized in that: and the waste gas generated in the third step and the fifth step is input into a spraying system for treatment and then is discharged.
6. The process for producing the nano rare earth polishing solution according to claim 5, wherein the process comprises the following steps: and step four, the wastewater generated by the spraying system is discharged into a four-effect evaporation processor for treatment, and the treated water is recycled.
7. The process for producing the nano rare earth polishing solution according to claim 1, which is characterized in that: and in the third step, the materials in the reaction kettle are stirred while the reaction kettle is heated.
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