CN103360232A - Method for converting yttrium oxide into yttrium acetate crystal - Google Patents
Method for converting yttrium oxide into yttrium acetate crystal Download PDFInfo
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- CN103360232A CN103360232A CN2012100856253A CN201210085625A CN103360232A CN 103360232 A CN103360232 A CN 103360232A CN 2012100856253 A CN2012100856253 A CN 2012100856253A CN 201210085625 A CN201210085625 A CN 201210085625A CN 103360232 A CN103360232 A CN 103360232A
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- China
- Prior art keywords
- acetic acid
- yttrium
- yttrium oxide
- liquid material
- crystal
- 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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- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000013078 crystal Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 26
- NFSAPTWLWWYADB-UHFFFAOYSA-N n,n-dimethyl-1-phenylethane-1,2-diamine Chemical compound CN(C)C(CN)C1=CC=CC=C1 NFSAPTWLWWYADB-UHFFFAOYSA-N 0.000 title abstract 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 57
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 229960000583 acetic acid Drugs 0.000 claims abstract description 22
- 239000011344 liquid material Substances 0.000 claims abstract description 19
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 238000001704 evaporation Methods 0.000 claims abstract description 9
- 230000008020 evaporation Effects 0.000 claims abstract description 9
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 9
- 239000000376 reactant Substances 0.000 claims abstract description 9
- DUSUCKWNBGMKRV-UHFFFAOYSA-N acetic acid;yttrium Chemical compound [Y].CC(O)=O DUSUCKWNBGMKRV-UHFFFAOYSA-N 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 11
- 238000002425 crystallisation Methods 0.000 claims description 9
- 230000008030 elimination Effects 0.000 claims description 8
- 238000003379 elimination reaction Methods 0.000 claims description 8
- 230000008025 crystallization Effects 0.000 claims description 7
- 230000008859 change Effects 0.000 claims description 6
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 230000002269 spontaneous effect Effects 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 15
- 230000008569 process Effects 0.000 abstract description 6
- -1 rare earth yttrium oxide Chemical class 0.000 abstract description 4
- 239000002932 luster Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 239000006260 foam Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for converting yttrium oxide into an yttrium acetate crystal. The method is characterized by comprising the following steps of: pumping analytically-pure glacial acetic acid and deionized water into a reaction kettle according to the volume ratio of 1:1, uniformly stirring and heating until the mixture is boiled; rotating a stirring paddle, and slowly adding the weighted yttrium oxide into the reaction kettle, wherein the mole rate of the addition of the yttrium oxide to the addition of acetic acid is 1:3.9; after the reaction is ended completely, heating a liquid material to 110-125 DEG C, and then, stopping heating to enable the liquid material in the reaction kettle to naturally cool and crystallize; when the liquid material is cooled to the temperature below 50 DEG C, enabling the stirring paddle to stop stirring, filtering a liquid through a filter tank, and centrifugally dewatering; and airing the dewatered reactant in a dust-free room to realize natural evaporation. The rare earth yttrium oxide is used for manufacturing the yttrium acetate crystal, so that the method is simple in process flow, high in production efficiency, low in energy consumption and capable of reducing the production cost and environment pollution; and the yttrium acetate crystal product is high in purity and total rare earth quantity, large in crystal particle and pure in color and luster, and the added value of a product can be increased.
Description
Technical field
The present invention relates to a kind of preparation method of rare earth acetate, especially relate to the method that a kind of yttrium oxide changes into acetic acid yttrium crystal.
Background technology
In recent years, development along with rare earth new material utilisation technology in the association areas such as electronics, chemical industry, environmental protection, rare earth material is being brought into play indispensable keying action in emerging green energy resource technology of modern times, high-new green technology and defence and military system, World Developed Countries is all classified rare earth as strategic resource, with Rare Earth Functional Materials research and related application industry as giving priority to the field, therefore, in order to improve the rare earth resources utilising efficiency, realize rare earth resources sustainable use and development, exploitation high added value, deep processing rare-earth products become an emphasis direction of scientific rersearch.At present, rare earth acetate product to high purity, highly water-soluble on the market presents very large demand, and the production technique of existing rare earth acetate product (as: acetic acid yttrium), exist complex manufacturing, production efficiency is low, consumes energy high, and production cost is high, to the problem such as seriously polluted of environment, the research and development of new production technique becomes a urgent task.
Summary of the invention
The applicant is studied improvement for above-mentioned problem, provides a kind of yttrium oxide to change into the method for acetic acid yttrium crystal, and technical process is simple, and production efficiency is high, consumes energy low, reduces production costs, and reduces the pollution to environment.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of yttrium oxide changes into the method for acetic acid yttrium crystal, comprises the steps:
A, with analytical pure Glacial acetic acid and deionized water by volume 1:1 pump in the reactor, stir and be heated to boiling;
B, rotate stirring rake and load weighted yttrium oxide is slowly added reactor, the mol ratio of yttrium oxide add-on and acetic acid is 1:3.9;
After C, the complete reaction, stopped heating during heating liquid material to 110 ℃-125 ℃ makes liquid material natural cooling crystallization in the reactor;
D, be cooled to below 50 ℃ when the liquid material temperature, stirring rake stops to stir, and is discharged in the strumbox liquid material and elimination liquid;
E, the reactant of elimination liquid was put into centrifuge dehydration 25 to 30 minutes;
F, the reactant after will dewatering dry in the air dustless spontaneous evaporation until the total amount of rare earth (REO) 〉=33% of acetic acid yttrium crystal.
Further:
Rotating speed of agitator is 60-80 rev/min among the described step B.
Adopt artificial fast crystallisation by cooling to substitute natural cooling crystallization among the described step C.
Dehydrating speed in the described step e is 900-1100 rev/min.
Adopt microwave evaporation or converter drying to substitute spontaneous evaporation in the described step F.
The purity of described yttrium oxide is 99.999%.
In technical scheme of the present invention, analytical pure Glacial acetic acid and deionized water are controlled at 1:1 by volume, it is 50% that Glacial acetic acid is diluted to total amount, this ratio be because the total amount of analytical pure Glacial acetic acid greater than 99%, if the acetic acid total amount is 50% then does not need thin up, consider the saving transportation cost, analytical pure Glacial acetic acid total amount is usually greater than 99%, and the ratio of acetic acid and deionized water preferably is controlled on the 1:1; If deionized water has been added, the acetic acid total amount is less than 50%, and will prolong heat-up time, and acidity is inadequate, and the reaction times also will prolong, and wastes energy; If deionized water adds few, the acetic acid total amount does not wait reaction to finish greater than 50%, and the material in the reactor has become mashed prod, dries easy caking after the dehydration, and the product product do not reach effect mutually.In the actual production, 1 mole of yttrium oxide needs 3 molar acetates, because continuous heating in the production process, the acetic acid highly volatile according to the data that experiment obtains, is made in the acetic acid yttrium process, acetic acid is wanted loss about 30%, therefore during actual production, acetic acid need to add 30%, and namely the mol ratio of yttrium oxide and acetic acid is 1:3.9.In addition, because this reaction belongs to thermopositive reaction, produce a large amount of foams in the reaction process, feed rate is too fast easily to cause " emitting groove ", therefore, reinforced in the reaction process, find foam get up will be slower reinforced, stop in case of necessity feeding in raw material, wait foam to reduce or do not had again slowly reinforced.
Technique effect of the present invention is:
A kind of yttrium oxide disclosed by the invention changes into the method for acetic acid yttrium crystal, utilizes the rare-earth oxidation yttrium to make acetic acid yttrium crystal, and technical process is simple, and production efficiency is high, consumes energy low, reduces production costs, and reduces the pollution to environment; Simultaneously, acetic acid yttrium crystal product purity is high, and total amount of rare earth is high, and crystal grain is thick, and color and luster is pure, has improved added value of product.
Embodiment
Be described in further detail below in conjunction with the specific embodiment of the present invention.
Embodiment 1,
The method that yttrium oxide changes into acetic acid yttrium crystal comprises the steps:
A, with analytical pure Glacial acetic acid and deionized water by volume 1:1 pump in the reactor, stir and be heated to boiling;
B, rotate stirring rake and be that 99.999% yttrium oxide slowly adds reactor with load weighted purity, the mol ratio of yttrium oxide add-on and acetic acid is 1:3.9, and rotating speed of agitator is 70 rev/mins; Rotating speed of agitator can not be too fast, and too fast consumed energy can not be too slow, affects too slowly the material speed of response, and according to experimental data, rotating speed of agitator is preferably 60 to 80 rev/mins of per minutes usually;
After C, the complete reaction, stopped heating during heating liquid material to 120 ℃ makes liquid material natural cooling crystallization in the reactor, and in the process of cooling, stirring rake continues to stir; So-called complete reaction is mainly according to visual inspection, and normal reaction is, after yttrium oxide adds and reacts for some time, do not had foam in the reactor, and it is limpid that feed liquid becomes, without outstanding absurd creature; According to experimental data, not only evaporate unnecessary moisture content but also be unlikely to moisture content is all evaporated when being heated to 120 ℃, can reach best crystallization effect; All evaporate such as moisture content, crystal grain is too thin, easily lumps after the cooling, and blowing is also pretty troublesome, has influence on follow-up work;
D, be cooled to below 50 ℃ when the liquid material temperature, stirring rake stops to stir, and is discharged in the strumbox liquid material and elimination liquid;
E, the reactant of elimination liquid was put into centrifuge dehydration 25 to 30 minutes, dehydrating speed is 1000 rev/mins, dewaters to water outlet to get final product without appreciable current;
F, the reactant after will dewatering dry in the air dustless spontaneous evaporation until the total amount of rare earth (REO) 〉=33% of acetic acid yttrium crystal.
Embodiment 2,
The method that yttrium oxide changes into acetic acid yttrium crystal comprises the steps:
A, with analytical pure Glacial acetic acid and deionized water by volume 1:1 pump in the reactor, stir and be heated to boiling;
B, rotate stirring rake and be that 99.999% yttrium oxide slowly adds reactor with load weighted purity, the mol ratio of yttrium oxide add-on and acetic acid is 1:3.9, and rotating speed of agitator is 60 rev/mins;
After C, the complete reaction, stopped heating during heating liquid material to 110 ℃,, adopt artificial fast cooling to make liquid material rapid crystallization in the reactor, in the process of cooling, stirring rake continues to stir;
D, be cooled to below 50 ℃ when the liquid material temperature, stirring rake stops to stir, and is discharged in the strumbox liquid material and elimination liquid;
E, the reactant of elimination liquid was put into centrifuge dehydration 25 to 30 minutes, dehydrating speed is 1100 rev/mins, dewaters to water outlet to get final product without appreciable current;
F, the reactant after will dewatering dry in the air at dustless with microwave evaporation or converter drying, until the total amount of rare earth (REO) 〉=33% of acetic acid yttrium crystal.
In above-described embodiment, the total amount of rare earth of acetic acid yttrium specifically refers to: a acetic acid yttrium is amounted to into the amount of yttrium oxide, and namely to amount to into yttrium oxide be 0.33 kilogram to one kilogram of acetic acid yttrium.
Claims (6)
1. a yttrium oxide changes into the method for acetic acid yttrium crystal, it is characterized in that comprising the steps:
A, with analytical pure Glacial acetic acid and deionized water by volume 1:1 pump in the reactor, stir and be heated to boiling;
B, rotate stirring rake and load weighted yttrium oxide is slowly added reactor, the mol ratio of yttrium oxide add-on and acetic acid is 1:3.9;
After C, the complete reaction, stopped heating during heating liquid material to 110 ℃-125 ℃ makes liquid material natural cooling crystallization in the reactor;
D, be cooled to below 50 ℃ when the liquid material temperature, stirring rake stops to stir, and is discharged in the strumbox liquid material and elimination liquid;
E, the reactant of elimination liquid was put into centrifuge dehydration 25 to 30 minutes;
F, the reactant after will dewatering dry in the air dustless spontaneous evaporation until the total amount of rare earth (REO) 〉=33% of acetic acid yttrium crystal.
2. change into the method for acetic acid yttrium crystal according to yttrium oxide claimed in claim 1, it is characterized in that: rotating speed of agitator is 60-80 rev/min among the described step B.
3. change into the method for acetic acid yttrium crystal according to yttrium oxide claimed in claim 1, it is characterized in that: adopt artificial fast crystallisation by cooling to substitute natural cooling crystallization among the described step C.
4. change into the method for acetic acid yttrium crystal according to yttrium oxide claimed in claim 1, it is characterized in that: the dehydrating speed in the described step e is 900-1100 rev/min.
5. change into the method for acetic acid yttrium crystal according to yttrium oxide claimed in claim 1, it is characterized in that: adopt microwave evaporation or converter drying to substitute spontaneous evaporation in the described step F.
6. change into the method for acetic acid yttrium crystal according to yttrium oxide claimed in claim 1, it is characterized in that: the purity of described yttrium oxide is 99.999%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100856253A CN103360232A (en) | 2012-03-28 | 2012-03-28 | Method for converting yttrium oxide into yttrium acetate crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100856253A CN103360232A (en) | 2012-03-28 | 2012-03-28 | Method for converting yttrium oxide into yttrium acetate crystal |
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| Publication Number | Publication Date |
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| CN103360232A true CN103360232A (en) | 2013-10-23 |
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| CN2012100856253A Pending CN103360232A (en) | 2012-03-28 | 2012-03-28 | Method for converting yttrium oxide into yttrium acetate crystal |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115838185A (en) * | 2022-12-09 | 2023-03-24 | 宣城晶瑞新材料有限公司 | Preparation method of nano yttrium oxide material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62209039A (en) * | 1986-03-08 | 1987-09-14 | Taki Chem Co Ltd | Aqueous solution of basic yttrium acetate and production thereof |
| CN101774641A (en) * | 2010-01-06 | 2010-07-14 | 哈尔滨工程大学 | Method for preparing yttrium vanadate crystals |
-
2012
- 2012-03-28 CN CN2012100856253A patent/CN103360232A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62209039A (en) * | 1986-03-08 | 1987-09-14 | Taki Chem Co Ltd | Aqueous solution of basic yttrium acetate and production thereof |
| CN101774641A (en) * | 2010-01-06 | 2010-07-14 | 哈尔滨工程大学 | Method for preparing yttrium vanadate crystals |
Non-Patent Citations (2)
| Title |
|---|
| R SKAUDZIUS ET AL.: "Synthesis and evolution of crystalline garnet phases in Y3Al5xInxO12", 《JOURNAL OF PHYSICS：CONFERENCE SERIES》, vol. 93, 31 December 2007 (2007-12-31), pages 1 - 8 * |
| 乔军等: "醋酸铈及醋酸稀土的研制工艺", 《中国稀土学报》, vol. 20, 31 October 2002 (2002-10-31), pages 143 - 148 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115838185A (en) * | 2022-12-09 | 2023-03-24 | 宣城晶瑞新材料有限公司 | Preparation method of nano yttrium oxide material |
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Application publication date: 20131023 |