CN105038604A - Composition and preparation method of fluorine-containing rare-earth composite oxides - Google Patents
Composition and preparation method of fluorine-containing rare-earth composite oxides Download PDFInfo
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- CN105038604A CN105038604A CN201510287748.9A CN201510287748A CN105038604A CN 105038604 A CN105038604 A CN 105038604A CN 201510287748 A CN201510287748 A CN 201510287748A CN 105038604 A CN105038604 A CN 105038604A
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- 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
Abstract
The invention relates to a composition and preparation method of fluorine-containing rare-earth composite oxides. The preparation method comprises the following steps: by using a rare-earth salt mixture as a raw material, adding a precipitant to firstly prepare a rare-earth mixture precipitate, adding a fluorinating agent, carrying out constant-temperature fluoridation, filtering, drying and roasting to obtain the fluorine-containing rare-earth composite oxide powder. The prepared powder comprises 20-99.9% of CeO2 and the balance of fluorine-containing rare-earth composite oxides RE1O2.RE2OF.RE3F3 (RE1 is Ce, and RE2 and RE3 are respectively one or more of lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium and gadolinium). The structural form is shell-type nano particles, and the fluorine-containing rare-earth composite oxides are coated on the cerium oxide nano core. The fluorine-containing rare-earth composite oxide powder prepared by the method has the advantages of uniform particle size distribution and low aggregation. The preparation method and after-treatment are simple, and can easily implement industrialized production.
Description
Technical field
The present invention relates to a kind of composition and preparation method of fluorine-containing complex rare-earth oxidate containing valuable metal, belong to field of inorganic material preparing technology.
Background technology
Rare earth element has 4f track and the level structure of abundant underfilling electronics, thus gives the chemical property of rare earth element uniqueness, thus obtains purposes widely in making it in a lot of fields.In numerous earth oxide products, RE oxide powder is exactly a wherein very important class, and such as cerium oxide or CeO2-ZrO2 solid solution are hydrogen-storing materials important in motor vehicle tail-gas purifying three-way catalyst; Cerium base oxide powder or fluorine-containing cerium oxide composite oxide powder are important polishing materials; Nano rareearth oxidate powder body is important rubber filler; Also have in the preparation of various pottery, according to different purposes, also need nano rare earth powder miscellaneous as raw material, etc.But any one RE oxide powder is different due to the field used, and has different requirements to its composition and performance, therefore, in the preparation of RE oxide powder, one relates to its composition, and two relate to its technology of preparing.
Due to the importance of RE oxide powder technology of preparing, investigators carry out a large amount of research work for this reason, and comprise the impact of composition on performance, preparation method and parameter are on the impact of its performance.In these RE oxide powder, using the widest should be nano-cerium oxide or cerium oxide base composite oxides, therefore conducts a research to it also more extensive.The method prepared for rare earth oxide at present also has multiple, and conventional has the precipitator method, hydrothermal method, sol-gel method, microemulsion method, spray pyrolysis and mechanico-chemical reaction method etc.The rare earth oxide (as cerium oxide) that research finds different material, prepared by different preparation method has visibly different physico-chemical property.But; that commonly uses at these prepares in the method for rare earth oxide; also there is problem more or less; during as produced complex rare-earth oxidate containing valuable metal with coprecipitation method mass-producing; in order to obtain the composite oxides of high-ratio surface; precipitation agent used is essentially the bases such as ammoniacal liquor, bicarbonate of ammonia, therefore annual by producing a large amount of ammonia nitrogen waste waters, causes severe contamination to environment.Be process ammonia nitrogen waste water on the one hand in addition, need the environmental protection equipment investment and the wastewater treatment running cost that increase additional expensive.For this reason, technology of preparing of the present invention eliminates Ammonia Nitrogen Precipitation from Simulated system, adopts sodium carbonate or sodium hydroxide to replace ammoniacal liquor, bicarbonate of ammonia to produce rare earth carbonate.
For the preparation method of fluorine-containing complex rare-earth oxidate containing valuable metal, be all first prepare rare earth carbonate and rare earth fluorine usually, then mixed grinding, roasting forms.Patent (CN101155891A) discloses a kind of preparation method that can be used as the fluorine-containing complex rare-earth oxidate containing valuable metal that polishing powder uses, comprise the following steps: in the aqueous solution of the light rare earths salt containing cerium, add precipitation agent, light rare earths is salted out, obtains the slurries A containing light rare earths salt particle; In the slurries containing light rare earths salt particle, add fluorizating agent, light rare earths salt and fluorizating agent are reacted, obtain the slurries B containing light rare earth fluorides particle; Obtain mixed serum after being mixed by slurries A and slurries B, after drying and roasting, obtain fluorine-containing complex rare-earth oxidate containing valuable metal.
Patent (CN101010402A) discloses a kind of method preparing fluorine-containing complex rare-earth oxidate containing valuable metal, is mixed by rare earth oxide with rare earth fluoride, after grinding, drying, roasting, the standby process of grading system, just can prepare fluorine-containing complex rare-earth oxidate containing valuable metal.The method will use the compounding process of fluorochemical and oxide compound simultaneously, before mixture, preroasting process to be carried out to two kinds of particles, therefore there is the phenomenon of double sintering in the method, partial particulate can produce abnormal growth after re-baking, form the big particle of local, thus cause surface tear in its polishing use procedure.
In order to overcome or solve above-mentioned existing problem, the invention discloses a kind of method of direct employing rare earth fluoride mixed sediment, then the preparation method of obtained rare earth fluoride composite oxides after aging, dry and roasting, thus decrease the step prepared rare earth oxide and rare earth fluoride oxide compound respectively, then carry out mixed grinding, the nano-powder of fluorine-containing complex rare-earth oxidate containing valuable metal can be obtained by method of the present invention, and even particle size distribution, reunion are few, preparation method and aftertreatment simply, easily realize suitability for industrialized production.
Summary of the invention
The object of the present invention is to provide a kind of composition and preparation method of fluorine-containing complex rare-earth oxidate containing valuable metal.It is characterized in that add precipitation agent first obtained rare earth mixed precipitation, then fluoridize constant temperature is fluoridized, and filtration, drying and roasting obtain fluorine-containing complex rare-earth oxidate containing valuable metal nano-powder with rare earth mixing salt for raw material.
The composition of a kind of fluorine-containing complex rare-earth oxidate containing valuable metal of the present invention, is characterized in that CeO
2and RE
1o
2rE
2oFRE
3f
3the mixture of (RE is the code name of rare earth, RareEarth), wherein CeO
2weight be 20.0 ~ 99.9%, all the other are the complex rare-earth oxidate containing valuable metal RE containing F
1o
2rE
2oFRE
3f
3, wherein RE
1for Ce, RE
2and RE
3for one or more in lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium; Fluorine-containing composite oxides are shell type nano bead, and fluorine-containing composite oxides are wrapped on cerium oxide nano core;
The preparation method of fluorine-containing complex rare-earth oxidate containing valuable metal of the present invention comprises following process:
(1) the rare-earth salts mixture that will weigh, dissolving or in deionized water dispersed, concentration is 0.2 ~ 0.6mol/L; (2) in the aqueous solution or suspension of soluble rare-earth salt, add precipitation agent makes soluble ion produce precipitation; (3) above-mentioned solid-water compound is placed in the fluorizating agent constant temperature adding metering after oil bath rises to certain temperature to fluoridize; (4), after standing aging, drying, roasting obtain fluorine-containing complex rare-earth oxidate containing valuable metal.
In above-mentioned preparation method, it is characterized in that described rare-earth salts is muriate, nitrate or carbonate; Rare-earth salts mixture is the mixture of cerium salt and other rare-earth saltss; Other described rare earths are one or more in lanthanum, praseodymium, neodymium, promethium, samarium, europium, gadolinium; The mol ratio of cerium salt and other rare-earth saltss is 1/10 ~ 10/1.
Described precipitation agent is one or more in sodium bicarbonate, sodium carbonate, sodium hydroxide;
Described temperature of fluoridizing is 20 ~ 110 DEG C, fluoridizes 1 ~ 12 hour time; Fluorizating agent is Neutral ammonium fluoride or Sodium Fluoride or the mixture of the two; The molar weight adding fluorochemical is 1 ~ 7 times of rare earth (except cerium) molar weight;
Described standing digestion time is 1 ~ 48 hour; Maturing temperature is 450 ~ 1200 DEG C, and roasting time is 2 ~ 7 hours.
Adopt the D of the fluorine-containing complex rare-earth oxidate containing valuable metal prepared by preparation method disclosed by the invention
50be 0.3 ~ 5.0 μm, specific surface area is 2 ~ 10m
2/ g.The polishing material that can be used as glass material containing fluorine composite oxide prepared by present method, stock removal rate can reach 0.11mg/ (cm
2min), cut qualification rate is more than 95%; Add in rubber can greatly improve its wear resisting property as weighting agent.There is even particle size distribution, reunite less, production cost is low, the features such as technological process is simple.
Embodiment
The present invention will be further described below to use case study on implementation.Scope is not by the restriction of these case study on implementation.
embodiment 1:
Take 17.37g(0.04mol) cerous nitrate (Ce (NO
3)
36H
2o) and 3.25g(0.01mol) lanthanum nitrate (La (NO
3)
3nH
2o), be dissolved under stirring (strength of solution is 0.2mol/L) in the water of 250mL, adding 8.00g sodium carbonate makes it precipitate completely, oil bath is warming up to 90 DEG C, add 1.26g Sodium Fluoride constant temperature and fluoridize 2 hours, leave standstill through drying after aging 2 hours, 900 DEG C of roastings obtain the fluorine-containing complex rare-earth oxidate containing valuable metal powder that lanthanum/cerium mol ratio is 1:4, fluorine/lanthanum mol ratio is 3:1 after 2 hours.
embodiment 2:
Compared with embodiment 1, difference is with 16.68g(0.04mol) praseodymium nitrate (Pr (NO
3)
35H
2o) 4.34g(0.01mol used instead by alternative 3.25g lanthanum nitrate and cerous nitrate), Sodium Fluoride uses 5.04g instead, and other processes are identical with embodiment 1 with operational condition, and the praseodymium/cerium mol ratio of the fluorine-containing complex rare-earth oxidate containing valuable metal of gained is 4:1, and fluorine/praseodymium mol ratio is 3:1.
embodiment 3:
Compared with embodiment 1, difference is that the water yield reduces to 100mL from 250mL, and ie in solution concentration is increased to 0.5mol/L from 0.2mol/L, and other processes are identical with embodiment 1 with operational condition, the fluorine-containing complex rare-earth oxidate containing valuable metal lanthanum/cerium mol ratio of gained is 1:4, and fluorine/lanthanum mol ratio is 3:1.
embodiment 4:
Compared with embodiment 1, difference is that precipitation agent 12.60g sodium bicarbonate replaces 8.00g sodium carbonate, and other processes are identical with embodiment 1 with operational condition, and the lanthanum/cerium mol ratio of the fluorine-containing complex rare-earth oxidate containing valuable metal of gained is 1:4, and fluorine/lanthanum mol ratio is 3:1.
embodiment 5:
Compared with embodiment 1, difference is to replace 8.00g sodium carbonate with 6.30g sodium carbonate and 3.00g sodium hydroxide mixture, other processes are identical with embodiment 1 with operational condition, and the lanthanum/cerium mol ratio of the fluorine-containing complex rare-earth oxidate containing valuable metal of gained is 1:4, and fluorine/lanthanum mol ratio is 3:1.
embodiment 6:
Compared with embodiment 1, difference is that oil bath temperature reduces to 30 DEG C by 90 DEG C, and other processes are identical with embodiment 1 with operational condition, and the lanthanum/cerium mol ratio of the fluorine-containing complex rare-earth oxidate containing valuable metal of gained is 1:4, and fluorine/lanthanum mol ratio is 3:1.
embodiment 7:
Compared with embodiment 1, difference is to replace 1.26g Sodium Fluoride with 1.12g Neutral ammonium fluoride, and other processes are identical with embodiment 1 with operational condition, and the lanthanum/cerium mol ratio of the fluorine-containing complex rare-earth oxidate containing valuable metal of gained is 1:4, and fluorine/lanthanum mol ratio is 3:1.
embodiment 8:
Compared with embodiment 1, it is 10 hours that difference is that the time of fluoridizing increased by 2 hours, and other processes are identical with embodiment 1 with operational condition, and the lanthanum/cerium mol ratio of the fluorine-containing complex rare-earth oxidate containing valuable metal of gained is 1:4, and fluorine/lanthanum mol ratio is 3:1.
embodiment 9:
Compared with embodiment 1, difference is that the consumption of Sodium Fluoride is increased to 2.52g by 1.26g, and other processes are identical with embodiment 1 with operational condition, and the fluorine-containing complex rare-earth oxidate containing valuable metal lanthanum/cerium mol ratio of gained is 1:4, and fluorine/lanthanum mol ratio is 6:1.
embodiment 10:
Compared with embodiment 1, difference is that the digestion time after fluoridizing extended to 24 hours by 2 hours, and other processes are identical with embodiment 1 with operational condition, and the lanthanum/cerium mol ratio of the fluorine-containing complex rare-earth oxidate containing valuable metal of gained is 1:4, and fluorine/lanthanum mol ratio is 3:1.
embodiment 11:
Compared with embodiment 1, difference is that maturing temperature is reduced to 500 DEG C by 900 DEG C, and other processes are identical with embodiment 1 with operational condition, and the fluorine-containing complex rare-earth oxidate containing valuable metal lanthanum/cerium mol ratio of gained is 1:4, and fluorine/lanthanum mol ratio is 3:1.
embodiment 12:
Compared with embodiment 1, difference is that roasting time extended to 7 hours by 2 hours, and other processes are identical with embodiment 1 with operational condition, and the lanthanum/cerium mol ratio of the fluorine-containing complex rare-earth oxidate containing valuable metal of gained is 1:4, and fluorine/lanthanum mol ratio is 3:1.
embodiment 13:
Take 14.18g(0.04mol) Cerium II Chloride (CeCl
36H
2o) and 3.53g(0.01mol) Lanthanum trichloride (LaCl
36H
2o), be dissolved under stirring (strength of solution is 0.2mol/L) in the water of 250mL, adding 8.00g sodium carbonate makes it precipitate completely, oil bath is warming up to 90 DEG C, add 1.26g Sodium Fluoride constant temperature and fluoridize 2 hours, leave standstill through drying after aging 2 hours, 900 DEG C of roastings obtain the fluorine-containing complex rare-earth oxidate containing valuable metal powder that lanthanum/cerium mol ratio is 1:4, fluorine/lanthanum mol ratio is 3:1 after 2 hours.
embodiment 14:
Take 14.18g(0.04mol) Cerium II Chloride (CeCl
36H
2o) and 3.53g(0.01mol) Lanthanum trichloride (LaCl
36H
2o), be dissolved under stirring (strength of solution is 0.5mol/L) in the water of 100mL, adding 8.00g sodium carbonate makes it precipitate completely, oil bath is warming up to 30 DEG C, add 2.24g Neutral ammonium fluoride constant temperature and fluoridize 6 hours, leave standstill through drying after aging 10 hours, 600 DEG C of roastings obtain the fluorine-containing complex rare-earth oxidate containing valuable metal powder that lanthanum/cerium mol ratio is 1:4, fluorine/lanthanum mol ratio is 6:1 after 5 hours.
embodiment 15:
Take 14.18g(0.04mol) Cerium II Chloride (CeCl
36H
2o) and 3.53g(0.01mol) Lanthanum trichloride (LaCl
36H
2o), be dissolved under stirring (strength of solution is 0.25mol/L) in the water of 200mL, adding 8.00g sodium carbonate makes it precipitate completely, oil bath is warming up to 50 DEG C, add 2.99g Neutral ammonium fluoride constant temperature and fluoridize 4 hours, leave standstill through drying after aging 6 hours, 800 DEG C of roastings obtain the fluorine-containing complex rare-earth oxidate containing valuable metal powder that lanthanum/cerium mol ratio is 1:4, fluorine/lanthanum mol ratio is 4:1 after 3 hours.
embodiment 16:
Take 19.85g(0.04mol) cerous carbonate (Ce
2(CO
3)
32H
2o) and 4.94g(0.01mol) Phosbloc (La
2(CO
3)
32H
2o), be dissolved under stirring (strength of solution is 0.2mol/L) in the water of 500mL, oil bath is warming up to 90 DEG C, add 2.52g Sodium Fluoride constant temperature and fluoridize 2 hours, leave standstill through drying after aging 2 hours, 900 DEG C of roastings obtain the fluorine-containing complex rare-earth oxidate containing valuable metal powder that lanthanum/cerium mol ratio is 1:4, fluorine/lanthanum mol ratio is 3:1 after 2 hours.
embodiment 17:
Take 19.85g(0.04mol) cerous carbonate (Ce
2(CO
3)
32H
2o) and 4.94g(0.01mol) Phosbloc (La
2(CO
3)
32H
2o), be dissolved under stirring (strength of solution is 0.5mol/L) in the water of 200mL, oil bath is warming up to 70 DEG C, add 2.96g Neutral ammonium fluoride constant temperature and fluoridize 4 hours, leave standstill through drying after aging 24 hours, 1100 DEG C of roastings obtain the fluorine-containing complex rare-earth oxidate containing valuable metal powder that lanthanum/cerium mol ratio is 1:4, fluorine/lanthanum mol ratio is 4:1 after 4 hours.
embodiment 18:
Take 4.96g(0.01mol) cerous carbonate (Ce
2(CO
3)
32H
2o) and 4.94g(0.01mol) Phosbloc (La
2(CO
3)
32H
2o), be dissolved under stirring (strength of solution is 0.2mol/L) in the water of 500mL, oil bath is warming up to 30 DEG C, add 2.52g Sodium Fluoride constant temperature and fluoridize 3 hours, leave standstill through drying after aging 15 hours, 850 DEG C of roastings obtain the fluorine-containing complex rare-earth oxidate containing valuable metal powder that lanthanum/cerium mol ratio is 1:1, fluorine/lanthanum mol ratio is 3:1 after 2 hours.
Foregoing be only the present invention conceive under basic explanation, and according to any equivalent transformation that technical scheme of the present invention is done, all should protection scope of the present invention be belonged to.
Claims (5)
1. the composition of fluorine-containing complex rare-earth oxidate containing valuable metal and a preparation method, is characterized in that the main component of composite oxides is CeO
2and RE
1o
2rE
2oFRE
3f
3(RE is the code name of rare earth, RareEarth), wherein CeO
2weight be 20.0 ~ 99.9%, all the other are fluorine-containing composite oxides is RE
1o
2rE
2oFRE
3f
3, wherein RE
1for Ce, RE
2and RE
3for one or more in lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium; Fluorine-containing composite oxides are shell type nano bead, and fluorine-containing composite oxides are wrapped on cerium oxide nano core;
The preparation method of described fluorine-containing complex rare-earth oxidate containing valuable metal comprises following process:
(1) the rare-earth salts mixture that will weigh, dissolving or in deionized water dispersed, concentration is 0.2 ~ 0.6mol/L;
(2) in the aqueous solution or suspension of soluble rare-earth salt, add precipitation agent makes soluble ion produce precipitation;
(3) be placed in by above-mentioned solid-water compound after oil bath is heated to certain temperature, the fluorizating agent constant temperature adding metering is fluoridized;
(4), after standing aging, drying, roasting obtain fluorine-containing complex rare-earth oxidate containing valuable metal.
2. the preparation method of a kind of fluorine-containing complex rare-earth oxidate containing valuable metal according to claim 1, is characterized in that described rare-earth salts is muriate, nitrate or carbonate; Rare-earth salts mixture is the mixture of cerium salt and other rare-earth saltss; Other described rare earths are one or more in lanthanum, praseodymium, neodymium, promethium, samarium, europium, gadolinium; The molar ratio of cerium salt and other rare-earth saltss is 1/10 ~ 10/1.
3. the preparation method of a kind of fluorine-containing complex rare-earth oxidate containing valuable metal according to claim 1, is characterized in that described precipitation agent is one or more in sodium bicarbonate, sodium carbonate, sodium hydroxide.
4. the preparation method of a kind of fluorine-containing complex rare-earth oxidate containing valuable metal according to claim 1, is characterized in that: fluoridizing temperature is 20 ~ 110 DEG C, fluoridizes 1 ~ 12 hour time; Fluorizating agent is Neutral ammonium fluoride or Sodium Fluoride or the mixture of the two; The molar weight adding fluorochemical is 1 ~ 7 times of rare earth (except cerium) molar weight.
5. the preparation method of a kind of fluorine-containing complex rare-earth oxidate containing valuable metal according to claim 1, is characterized in that: standing digestion time is 1 ~ 48 hour; Maturing temperature is 450 ~ 1200 DEG C, and roasting time is 2 ~ 7 hours.
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| CN109104866B (en) * | 2016-04-20 | 2021-04-27 | 信越化学工业株式会社 | Polishing agent for synthetic quartz glass substrate and method for polishing synthetic quartz glass substrate |
| US11180677B2 (en) | 2016-04-20 | 2021-11-23 | Shin-Etsu Chemical Co., Ltd. | Polishing agent for synthetic quartz glass substrate and method for polishing synthetic quartz glass substrate |
| CN107502762A (en) * | 2017-08-29 | 2017-12-22 | 江西理工大学 | The method that ion type rareearth leaches mother liquor one-step method removing impurity by means of precipitation Extraction of rare earth |
| CN107502762B (en) * | 2017-08-29 | 2022-01-07 | 江西理工大学 | Method for extracting rare earth by one-step precipitation and impurity removal of ionic rare earth leaching mother liquor |
| CN111115677A (en) * | 2020-01-13 | 2020-05-08 | 赣州有色冶金研究所 | Preparation method of rare earth fluoride |
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