CN102092766B - Preparation method of ultrafine lanthanum oxide powder - Google Patents
Preparation method of ultrafine lanthanum oxide powder Download PDFInfo
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- CN102092766B CN102092766B CN 201110053742 CN201110053742A CN102092766B CN 102092766 B CN102092766 B CN 102092766B CN 201110053742 CN201110053742 CN 201110053742 CN 201110053742 A CN201110053742 A CN 201110053742A CN 102092766 B CN102092766 B CN 102092766B
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- lanthanum
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- oxalate
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- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000000843 powder Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 38
- 238000010791 quenching Methods 0.000 claims abstract description 29
- 230000000171 quenching effect Effects 0.000 claims abstract description 29
- 238000001556 precipitation Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 14
- OXHNIMPTBAKYRS-UHFFFAOYSA-H lanthanum(3+);oxalate Chemical compound [La+3].[La+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O OXHNIMPTBAKYRS-UHFFFAOYSA-H 0.000 claims abstract description 13
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- -1 rare earth lanthanum oxide Chemical class 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 16
- 239000012498 ultrapure water Substances 0.000 claims description 12
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 5
- YXEUGTSPQFTXTR-UHFFFAOYSA-K lanthanum(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[La+3] YXEUGTSPQFTXTR-UHFFFAOYSA-K 0.000 claims description 5
- NZPIUJUFIFZSPW-UHFFFAOYSA-H lanthanum carbonate Chemical compound [La+3].[La+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NZPIUJUFIFZSPW-UHFFFAOYSA-H 0.000 claims description 4
- 238000001354 calcination Methods 0.000 abstract description 26
- 229910001404 rare earth metal oxide Inorganic materials 0.000 abstract description 11
- 230000002776 aggregation Effects 0.000 abstract description 7
- 239000000047 product Substances 0.000 abstract description 6
- 238000005406 washing Methods 0.000 abstract description 6
- 238000005054 agglomeration Methods 0.000 abstract description 4
- 238000000227 grinding Methods 0.000 abstract description 4
- 239000002243 precursor Substances 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract 2
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000000967 suction filtration Methods 0.000 description 5
- 239000000460 chlorine Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 3
- 150000004703 alkoxides Chemical class 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 239000012716 precipitator Substances 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 2
- 239000001099 ammonium carbonate Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 208000031968 Cadaver Diseases 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 240000004859 Gamochaeta purpurea Species 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 230000004931 aggregating effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Abstract
The invention discloses a preparation method of ultrafine rare earth lanthanum oxide powder. The method comprises the following steps of: quickly calcining precipitates which are produced in a reaction by a direct precipitation method and serve as a precursor at a high temperature; and putting the calcined precipitates into water for quenching to obtain high-purity lanthanum oxide ultrafine powder. By the method, the problems of difficulty in washing and low product purity during precipitation, hard agglomeration of rare earth oxide particles during calcining, wide particle distribution and the like in the prior art are solved, and more importantly, the problem of synthesis of precursors such as ultrafine lanthanum oxalate and the like with very high costs can be solved. The method can be directly applied on the basis of the original precipitation and calcining, complex grinding or smashing operation is not required, and the environmental protection pressure cannot be too high under the condition that an appropriate precipitating agent is selected; moreover, the method is low in preparation cost, and is easy to operate and popularize.
Description
Technical field
The present invention relates to a kind of preparation method of ultrafine lanthanum oxide powder.
Technical background
The method for preparing the superfine rare-earth oxide compound has the precipitator method, sol-gel processing, hydrothermal method, microemulsion method, spray heating decomposition etc., and wherein the precipitator method are research and the production methods that the most generally adopt.The method has that raw materials cost is low, low for equipment requirements, technique is simple, easy and simple to handle, can accurately control chemical constitution, easily make the ultra-micro powder of Multiple components homogeneous, control the advantages such as the shape of particle and granularity easily.
The precipitator method commonly used prepare the superfine rare-earth oxide compound to be had:
(1) direct precipitation method: add the precipitation agents such as oxyhydroxide, oxalate or bicarbonate of ammonia in containing the solution of rare earth ion, directly reacting produces precipitation.But research finds, during precipitation of hydroxide, the rare earth hydrate of generation is that a kind of height is assembled, the throw out of unformed, viscose glue, be difficult to washing, the hard coacervate of the rear generation of dry, calcining need grind, and can't directly generate the superfine rare-earth oxide compound; During oxalate precipitation, because Cl
-More, very easily form crystal salt in the sintering process, form the solid phase bridge, make particle produce hard aggregation and big particle agglomerate, and under comparatively high temps, agglomeration is more serious, also can't directly generate the superfine rare-earth oxide powder; It is low that ammonium bicarbonate precipitation method has a raw materials cost, and the product yield advantages of higher can form the less rare earth oxide of particle diameter after calcining, but the high-concentration ammonia nitrogenous wastewater that ammonium bicarbonate method produces is difficult to process, and therefore limited its application.
(2) sluggish precipitation: utilize a certain chemical reaction make in the solution configurational ion by in the solution lentamente, discharge equably, after washing, oven dry, calcining, can form epigranular, densification, rare earth oxide that purity is high, normal precipitation agent is urea at present, but this production technique productive rate is lower, and environmental protection pressure is larger.
(3) alkoxide hydrolysis: utilize the rare earth metal organic alkoxide can be dissolved in organic solvent and hydrolysis occurs to generate oxyhydroxide preparation superfine rare-earth oxide powder.But this method expense of raw materials is very high, and the preparation alkoxide needs to react operational difficulty under anhydrous atmosphere.
(4) complex-precipitation method: the complexing agents such as rare earth ion and EDTA generate the complex compound of ambient stable, and complex compound is destroyed under proper temperature and pH value, and rare earth ion discharges again, with the OH in the solution
-And add precipitation agent effect generation throw out, further processing can prepare the superfine rare-earth oxide powder, but technique is loaded down with trivial details, is unsuitable for industrial production, and cost is high.
Summary of the invention
For above problem, the preparation method who the purpose of this invention is to provide a kind of ultrafine lanthanum oxide powder, can on the basis of original precipitation and calcining, directly use, need not loaded down with trivial details grinding or fragmentation procedure, under the condition of selecting suitable precipitation agent, not only do not have too large environmental protection pressure, and cost of manufacture is low, simple to operate, be easy to promote.
In order to reach above-mentioned purpose, solution of the present invention is:
A kind of preparation method of superfine rare-earth lanthanum oxide powder, the throw out that direct precipitation method reaction is produced is as presoma, and behind the high temperature quick burning, the entry quenching is prepared into the high purity lanthanum oxide superfine powder.
Described presoma is to add precipitation agent oxyhydroxide, oxalate or bicarbonate of ammonia, lanthanum oxalate, Phosbloc or lanthanum hydroxide that reaction produces in containing the solution of rare earth ion.
Described presoma lanthanum oxalate, Phosbloc or lanthanum hydroxide particle diameter are 5～6 μ m.
900～1000 ℃ of the temperature of described high temperature quick burning, time 1～3h.
The time 6h of described high temperature quick burning, the section that wherein heats up 3 h, holding-zone 3 h.
Described quenching water is the high purity water under room temperature or the low temperature.
The high purity water that described quenching water is 10～40 ℃ (under low temperature) (water that chemical purity is high, the content of impurity wherein is less than 0.1mg/L).
Described high purity lanthanum oxide superfine powder D
50=0.8～0.9 μ m.
Described quenching water is the recirculated water of recycling.
After adopting such scheme, do presoma as example take lanthanum oxalate, step of the present invention is:
(1) oxalate precipitation.Oxalate precipitation technique is simple, the cycle is short, productive rate is high, but because during oxalic acid precipitation, the crystal grain formation speed is very fast, usually obtain oarse-grained oxalate, generate in order to suppress crystal grain, improve aggregating state, add organic dispersing agent in the precipitation process of being everlasting, and in the oxalate as contain more Cl
-, produce easily hard aggregation during calcining, so cost is higher, and is difficult to prepare the superfine rare-earth oxide compound.Adopt technique of the present invention, not only the control of oxalate precipitation process conditional does not need very accurately, and need not add dispersion agent, makes things convenient for manual operation, and has reduced production cost.
(2) suction filtration and washing.The oxalate particle is larger, make things convenient for suction filtration, but contained chlorine root easily forms parcel, difficulty is washed, adopt technique of the present invention to prepare ultrafine lanthanum oxide, most of impurity can be discharged by the fracture of quenching, therefore can reduce the washing times of chlorine root and impurity, enhance productivity, reduce production costs.
(3) calcining and liquid cooling.In the industrial production, the temperature of calcining lanthanum oxalate is generally 1000 ℃, the lanthanum trioxide granularity that generates under this temperature is large (3-10 μ m), if lanthanum oxalate is oven dry not, easier generation agglomeration, it is larger that granularity becomes, and skewness, technique of the present invention can be under existing working condition, the lanthanum trioxide chamber of pouring into behind the high-temp combustion is overflow or low temperature under high purity water in, pass through quenching, make it to produce the fracture of quenching, but repeated hardening makes it to produce repeated stress failure in case of necessity, and it is minimum to get granularity, the lanthanum oxide powder that is evenly distributed.
(4) oven dry and batch mixing packing.According to the practical situation of producing, dry and batch mixing is packed and got final product by existing technique.
In a word, the present invention is compared with prior art: traditional technology calcining lanthanum oxalate etc. needs higher temperature, and be preferably under the atmosphere of oxygen abundance, calcination process is difficult to avoid the particle agglomeration phenomenon, therefore the preparation ultrafine lanthanum oxide powder all needs trickleer precursor particle at present, cause the production operation difficulty, facility investment and process costs are very high.Part company adopts the method that grinds after the calcining, and not only workman's complex operation, severe operational environment, energy consumption are high, and product particle distributes widely, often brings pollution substance when grinding simultaneously into.The present invention is by this technology, and when the temperature quenching, the lanthanum trioxide coacervate ruptures automatically, and drying can make ultra-fine lanthanum oxide powder.Industrial production is convenient in the present invention, grinding or fragmentation procedure that prepared lanthanum trioxide need not be loaded down with trivial details, and high purity water reusable edible, but decrease production cost.
Washing difficulty when the invention solves present precipitation, the problem such as product purity is not high, prepares the rare earth oxide particles hard aggregation during calcination, and size distribution is wide be the more important thing is the composition problem of the precursors such as ultra-fine lanthanum oxalate that avoidable cost is very high.
For the use-pattern of technique of the present invention is described, take following specific embodiment to be elaborated.
Embodiment
Embodiment 1
Get 2 Kg lanthanum oxalates (not oven dry), under the atmosphere of anoxic, put into 900 ℃ of calcinings of retort furnace, 6 h(intensification section, 3 h, holding-zone 3 h), without temperature descending section, directly the lanthanum trioxide that burns till is taken out, in 2/3 high purity water of pouring under 20 ℃ of 5 L, suction filtration, then 100 ℃ of lower oven dry 12 h, lanthanum trioxide with remaining 1/3 and the detection granularity of taking away through the lanthanum trioxide of the fracture post-drying of quenching, the result is: without the lanthanum trioxide D of the fracture of quenching
50=8.78, D
90=18.50, through the lanthanum trioxide D of the fracture of quenching
50=0.80, D
90=0.87, and experimental repeatability is good.
Embodiment 2
Get 2 Kg Phosblocs (not oven dry), under the atmosphere of anoxic, put into 1000 ℃ of calcinings of retort furnace, 6 h(intensification section, 3 h, holding-zone 3 h), without temperature descending section, directly the lanthanum trioxide that burns till is taken out, in 2/3 high purity water of pouring under 20 ℃ of 5 L, suction filtration, then 100 ℃ of lower oven dry 12 h, lanthanum trioxide with remaining 1/3 and the detection granularity of taking away through the lanthanum trioxide of the fracture post-drying of quenching, the result is: without the lanthanum trioxide D of the fracture of quenching
50=13.42, D
90=28.92, through the lanthanum trioxide D of the fracture of quenching
50=0.76, D
90=0.87, and experimental repeatability is good.
Embodiment 3
Get 2 Kg lanthanum hydroxides (not oven dry), under the atmosphere of anoxic, put into 900 ℃ of calcinings of retort furnace, 6 h(intensification section, 3 h, holding-zone 3 h), without temperature descending section, directly the lanthanum trioxide that burns till is taken out, in 2/3 high purity water of pouring under 20 ℃ of 5 L, suction filtration, then 100 ℃ of lower oven dry 12 h, lanthanum trioxide with remaining 1/3 and the detection granularity of taking away through the lanthanum trioxide of the fracture post-drying of quenching, the result is: without the lanthanum trioxide D of the fracture of quenching
50=1.21, D
90=1.64, through the lanthanum trioxide D of the fracture of quenching
50=0.79, D
90=0.91, and experimental repeatability is good.
Embodiment 4
Get 2 Kg lanthanum oxalates (not oven dry), under the atmosphere of anoxic, put into 1000 ℃ of calcinings of retort furnace, 6 h(intensification section, 3 h, holding-zone 3 h), without temperature descending section, directly the lanthanum trioxide that burns till is taken out, pour respectively water temperature into and be in 10 ℃, 20 ℃, 30 ℃ the high purity water, when experiment finds that water temperature is 10 ℃, by the lanthanum trioxide D of the fracture generation of quenching
50=0.95, D
90=1.12; When water temperature is 20 ℃, by the lanthanum trioxide D of the fracture generation of quenching
50=0.81, D
90=0.88; When water temperature is 30 ℃, by the lanthanum trioxide D of the fracture generation of quenching
50=0.91, D
90=1.07, illustrate that normal conditions at room temperature can use this technique.
Key of the present invention is the control of calcining temperature and the selection of calcining heating curve, also different through the granularity of the prepared lanthanum trioxide of repeated stress failure under the highest calcining temperature of difference, heat-up rate and whether be incubated the lanthanum trioxide particle size influences very large, satisfying on the basis that lanthanum oxalate fully decomposes, heat-up rate is faster, soaking time is shorter, and quenched products granularity and distribution are thinner.
Experiment by repeatedly finds that calcining temperature is 800 ℃, and during 20 ℃ of water temperatures, the lanthanum trioxide great majority that generate by the fracture of quenching concentrate on D
50=1.39, D
90=1.89; Calcining temperature is 900 ℃, during 20 ℃ of water temperatures, and the lanthanum trioxide D that generates by the fracture of quenching
50=0.80, D
90=0.87; Calcining temperature is 1000 ℃, during 20 ℃ of water temperatures, and the lanthanum trioxide D that generates by the fracture of quenching
50=0.81, D
90=0.88; Calcining temperature is 1100 ℃, during 20 ℃ of water temperatures, and the lanthanum trioxide D that generates by the fracture of quenching
50=0.83, D
90=0.87, this process repeatability is good,
But the present invention in case of necessity repeated hardening diplomatic corps aggressiveness produces the fracture of quenching further to reduce product cut size, and drying can make ultra-fine lanthanum oxide powder.
High purity water of the present invention can recycle.Because this process using oxalic acid precipitation, the lanthanum trioxide purity of calcining out is higher, it is less to produce the impurity that discharges when quenching fracture, but so high purity water recycled for multiple times, in addition, because lanthanum trioxide is slightly soluble in water, so when if high purity water Rare-Earth Content and foreign matter content are higher, can return sour molten workshop again and again dissolve.
It below only is preferred implementation of the present invention; it is not the restriction to protection scope of the present invention; all and of the present invention gordian techniquies do not have to produce difference in essence, to the deduction or replace of above-mentioned embodiment, all should be regarded as falling within the protection domain of this case.
Claims (1)
1. the preparation method of a superfine rare-earth lanthanum oxide powder, it is characterized in that: direct precipitation method is reacted the throw out of generation as presoma, presoma is to add precipitation agent oxyhydroxide, oxalate or bicarbonate of ammonia in containing the solution of rare earth ion, lanthanum oxalate, Phosbloc or lanthanum hydroxide that reaction produces, presoma lanthanum oxalate, Phosbloc or lanthanum hydroxide particle diameter are 5～6 μ m; Under the atmosphere of anoxic, 900～1000 ℃, high temperature quick burning, time 6h, the section that wherein heats up 3 h, holding-zone 3 h are behind the high temperature quick burning, without temperature descending section, directly the lanthanum trioxide that burns till is taken out, the entry quenching, the quenching water is 10～40 ℃ high purity water, is prepared into high purity lanthanum oxide superfine powder D
50=0.8～0.9 μ m.
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| CN105271353B (en) * | 2015-09-23 | 2017-01-18 | 北方稀土生一伦高科技有限公司 | Calcination method for raising daily output of rare earth carbonate |
| CN108585015A (en) * | 2018-06-19 | 2018-09-28 | 四川江铜稀土有限责任公司 | A kind of method that microwave calcination prepares lanthana |
| CN111115675B (en) * | 2018-10-11 | 2023-03-10 | 有研稀土新材料股份有限公司 | High-purity light lanthanum carbonate or lanthanum oxide and preparation method thereof |
| CN115010163B (en) * | 2022-05-20 | 2024-04-09 | 全南县新资源稀土有限责任公司 | Rare earth oxide with low apparent density and preparation method thereof |
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| CN101151214A (en) * | 2004-12-28 | 2008-03-26 | 纳米科技创造私人有限公司 | Nanostructured zinc oxide and a method of producing the same |
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| CN101151214A (en) * | 2004-12-28 | 2008-03-26 | 纳米科技创造私人有限公司 | Nanostructured zinc oxide and a method of producing the same |
Non-Patent Citations (1)
| Title |
|---|
| 韩江.碳酸氢铵沉淀生产碳酸镧氧化镧.《稀有金属快报》.2001,(第11期),17-19. * |
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Application publication date: 20110615 Assignee: GUANGZHOU ZHUJIANG PHOTOELECTRIC NEW MATERIALS Co.,Ltd. Assignor: FUJIAN CHANGTING GOLDEN DRAGON RARE-EARTH Co.,Ltd. Contract record no.: 2013990000326 Denomination of invention: Preparation method of ultrafine lanthanum oxide powder Granted publication date: 20130313 License type: Exclusive License Record date: 20130619 |
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Address after: 366300 new industrial zone, Changting Economic Development Zone, Longyan City, Fujian Province Patentee after: Fujian Jinlong Rare Earth Co.,Ltd. Country or region after: China Address before: 366300 Changting Jinlong Rare Earth Co., Ltd., Industrial New District, Changting Economic Development Zone, Longyan City, Fujian Province Patentee before: FUJIAN CHANGTING GOLDEN DRAGON RARE-EARTH Co.,Ltd. Country or region before: China |