CN1456510A - Process for preparing lanthanum hydroxide - Google Patents
Process for preparing lanthanum hydroxide Download PDFInfo
- Publication number
- CN1456510A CN1456510A CN 02110388 CN02110388A CN1456510A CN 1456510 A CN1456510 A CN 1456510A CN 02110388 CN02110388 CN 02110388 CN 02110388 A CN02110388 A CN 02110388A CN 1456510 A CN1456510 A CN 1456510A
- Authority
- CN
- China
- Prior art keywords
- lanthanum
- oven dry
- lanthanum hydroxide
- product
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- YXEUGTSPQFTXTR-UHFFFAOYSA-K lanthanum(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[La+3] YXEUGTSPQFTXTR-UHFFFAOYSA-K 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000005516 engineering process Methods 0.000 claims description 9
- 230000003068 static effect Effects 0.000 claims description 4
- 239000000047 product Substances 0.000 description 16
- 239000002245 particle Substances 0.000 description 6
- 238000004891 communication Methods 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 239000003985 ceramic capacitor Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- YPJKMVATUPSWOH-UHFFFAOYSA-N nitrooxidanyl Chemical compound [O][N+]([O-])=O YPJKMVATUPSWOH-UHFFFAOYSA-N 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
A process for preparing lanthanum hydroxide includes such steps as reacting of lanthanum oxide on water in Wt ratio of 1:(1-10) and baking. Its advantages are simple process, low cost, uniform granularity and high RE content up to 85.5%.
Description
Technical field
The present invention relates to the production technique of lanthanum hydroxide.
Background technology
End products such as computer, mobile phone, digital camera, opticfiber communication, micro-wave communication and automobile all be unable to do without the function ceramics element.Microwave ferrite that light efficiency amplifier, optoisolator, the micro-wave communication that the function ceramics element has laminated ceramic capacitor, opticfiber communication to use used and connection optical fiber ferrule etc.The ultra micro lanthanum hydroxide is mainly used in laminated ceramic capacitor, advantage such as purity height, granularity are little, narrow particle size distribution that it has, they mix the performance that can improve the function ceramics element greatly.
The method of traditional mode of production lanthanum hydroxide is that lanthanum trioxide changes into lanthanum nitrate with nitric acid dissolve, and lanthanum nitrate joins in the ammoniacal liquor and precipitates, and throw out washes with water removes nitrate radical, filters then, dries, pulverizes and obtain the lanthanum hydroxide product.The main drawback of this method is: 1, lanthanum hydroxide washing difficulty; 2, product contains nitrate ion, in the difficult index that reaches 84.0%-86.0% of amount of oxide compound total rare earth (TRE); 3, lanthanum hydroxide filtration difficulty is worn filter easily; 4, oven dry material caking needs to pulverize; 5, the Granularity Distribution of Fen Suiing is bad.Below be the product leading indicator of produced in conventional processes:
| Leading indicator | Index |
| TREO (in the amount of oxide compound total rare earth (TRE)) | 81.0％-83.5％ |
| NO3 | 2.5％-5.0％ |
| D50 (size of the product of 50% weight or meausurement) | 1.0～5.0μm |
Summary of the invention
Technical problem to be solved by this invention provides a kind of anionic impurity of not introducing, work simplification, and product granularity is little, the production technique of the lanthanum hydroxide of narrow particle size distribution.
The production technique of lanthanum hydroxide of the present invention is characterized in that being generated by lanthanum trioxide and water reaction, and resultant is through oven dry.
Lanthanum trioxide and water reaction, the theoretical consumption between them is La
2O
3: H
2O=1: 0.166 (weight ratio), can get final product more than or equal to this numerical value as the consumption of water, but consider the fairness that reliability, economy and the reaction of technology are carried out, the consumption of water is preferably 1～10 times of lanthanum trioxide weight, and preferred 3-6 is doubly.
The reaction of lanthanum trioxide and water belongs to thermopositive reaction, and reaction at room temperature can be carried out, and the starting temperature that the invention provides reaction is preferably 40～90 ℃.
The mode that the resultant of reaction is dried can be static (oven for drying), also can be dynamic (spraying oven dry).Bake out temperature is 100～300 ℃.
After reaction was finished, resultant just can reach requirement of the present invention through dynamically drying, and just can reach requirement of the present invention if resultant through static oven dry, grinds after the oven dry.
In order to guarantee quality product, the specification of lanthanum trioxide can be selected high-load, and 99.5～99.99%.
In order to guarantee quality product, the high purity water of wet concentration after with purifying treatment, its specific conductivity is less than 5.0us/cm
The outward appearance of the lanthanum hydroxide that obtains is: white powder.
Advantage of the present invention:
1, do not contain anionic impurity in the product, the total amount of rare earth of product (in oxide compound) reaches 85.5%, near theoretical amount.
2, save filtration, pulverizing process, simplified technology, reduced production cost.
3, product does not need to pulverize, and Granularity Distribution is narrow, and D50 is less than 3.0 μ m.
As Fig. 1, SEM photo (scanning electron microscope) can prove that the size ratio of product is less.
As Fig. 2, the XRD of product (spectrogram), with the standard spectrogram of pure lanthanum hydroxide relatively, relatively more consistent, illustrate that product is purified lanthanum hydroxide.
As Fig. 3, be the particle size distribution figure of lanthanum hydroxide, illustrate that the size-grade distribution of product is narrow, Fig. 4 forms contrast for particle size distribution figure and Fig. 3 of the lanthanum hydroxide that traditional processing technology obtains.
Description of drawings
Fig. 1 is the SEM photo of lanthanum hydroxide.
Fig. 2 is the XRD spectral line of lanthanum hydroxide.
Fig. 3 is the lanthanum hydroxide particle size distribution figure.
Fig. 4 is the particle size distribution figure of the lanthanum hydroxide that adopts traditional technology and obtain.
Embodiment
Embodiment one:
The water that adds 5 times of lanthanum trioxide weight in reactor slowly adds lanthanum trioxide under whipped state, starting temperature is 50 ℃, and along with a large amount of heat of adding reaction generation of lanthanum trioxide, temperature is elevated to more than 100 degree.After the lanthanum trioxide adding finishes, stir reaction down 2 hours, cool off blowing then.The oven dry of spraying under 200 ℃ obtains meeting the lanthanum hydroxide product shown in Fig. 1～3.
Embodiment two:
With embodiment one, different is that reaction finishes, and cooled material 105 ℃ of down static oven dry, grinds after the oven dry earlier, and the product effect that obtains is with embodiment one.
Claims (5)
1, the production technique of lanthanum hydroxide is characterized in that being generated by lanthanum trioxide and water reaction, and resultant is through oven dry.
2, technology according to claim 1, the consumption that it is characterized in that water are 1～10 times of lanthanum trioxide weight.
3, technology according to claim 1 is characterized in that the starting temperature of reacting is 40～90 ℃.
4, technology according to claim 1 is characterized in that the dynamically mode of oven dry of resultant oven dry employing.
5, technology according to claim 1 is characterized in that the static oven dry of resultant oven dry employing, grinds after the oven dry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02110388 CN1456510A (en) | 2002-05-10 | 2002-05-10 | Process for preparing lanthanum hydroxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02110388 CN1456510A (en) | 2002-05-10 | 2002-05-10 | Process for preparing lanthanum hydroxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1456510A true CN1456510A (en) | 2003-11-19 |
Family
ID=29410223
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02110388 Pending CN1456510A (en) | 2002-05-10 | 2002-05-10 | Process for preparing lanthanum hydroxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1456510A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1308242C (en) * | 2004-10-26 | 2007-04-04 | 有研稀土新材料股份有限公司 | Method for preparing great specific surface area rare-earth hydroxide |
| CN100391847C (en) * | 2005-04-05 | 2008-06-04 | 内蒙古包钢稀土高科技股份有限公司 | Preparation method and device of rare earth salt |
| CN100558639C (en) * | 2008-05-22 | 2009-11-11 | 同济大学 | A kind of double hydrolysis regulation prepares the method for basic lanthanum carbonate nano/micro crystal |
| CN101948128A (en) * | 2010-09-29 | 2011-01-19 | 东北师范大学 | Novel method for preparing lanthanum hydroxide crystals by fluxing agent method |
-
2002
- 2002-05-10 CN CN 02110388 patent/CN1456510A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1308242C (en) * | 2004-10-26 | 2007-04-04 | 有研稀土新材料股份有限公司 | Method for preparing great specific surface area rare-earth hydroxide |
| CN100391847C (en) * | 2005-04-05 | 2008-06-04 | 内蒙古包钢稀土高科技股份有限公司 | Preparation method and device of rare earth salt |
| CN100558639C (en) * | 2008-05-22 | 2009-11-11 | 同济大学 | A kind of double hydrolysis regulation prepares the method for basic lanthanum carbonate nano/micro crystal |
| CN101948128A (en) * | 2010-09-29 | 2011-01-19 | 东北师范大学 | Novel method for preparing lanthanum hydroxide crystals by fluxing agent method |
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