CN106044832A - Preparation method of yttrium oxide with central grain size being 20-50 microns - Google Patents
Preparation method of yttrium oxide with central grain size being 20-50 microns Download PDFInfo
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- CN106044832A CN106044832A CN201610396407.XA CN201610396407A CN106044832A CN 106044832 A CN106044832 A CN 106044832A CN 201610396407 A CN201610396407 A CN 201610396407A CN 106044832 A CN106044832 A CN 106044832A
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- preparation
- oxalic acid
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- particle diameter
- yttrium
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Abstract
The invention discloses a preparation method of yttrium oxide with central grain size being 20-50 microns. The preparation method comprises steps as follows: 30-60 L of deionized water at a temperature of 35-45 DEG C is added to a precipitation pot; mixing is started, a yttrium chloride solution and an oxalic acid solution are added to the precipitation pot, wherein the rare earth concentration of the yttrium chloride solution is 30-70 g/L, the acidity is 3-5 mol/L and is adjusted with hydrochloric acid, the concentration of the oxalic acid solution is 100-120 g/L, the mass ratio of the added yttrium chloride solution to the oxalic acid solution is controlled to be 1:1.5-1:2, and the oxalic acid is replenished after the addition, the mass ratio of the yttrium chloride solution and the oxalic acid solution is controlled to be 1:2.5-1:3; after complete reaction, steam is opened, the mixture is heated to 95-100 DEG C for constant-temperature distillation, and heating is stopped after the endpoint acidity is 6-8 mol/L; discharging is performed, yttrium oxalate is washed and burnt, and large-granularity yttrium oxide with central grain size being 20-50 microns can be obtained.
Description
Technical field
The present invention relates to a kind of prepare the method that medium particle diameter is 20-50 micron yittrium oxide.
Background technology
Yittrium oxide is a kind of important rare earth compound, has the thermostability of uniqueness, corrosion resistance, high-temperature stability, height
Dielectric constant and a series of excellent optical property, be widely used in advanced ceramic, optoelectronics, catalyst and function and service
The fields such as material efficient additive.
The development of rare-earth trade in recent years, rare earth application deepens continuously, and new material technology is flourish, the dilutest
Soil oxide application in new material is further extensive, more and more higher to the physical property requirements of oxide powder therewith, example
As to specific surface area, granularity, the requirement of mobility, the difference of diameter of particle size, the demand in market is the most different, past little granule
Rare earth oxide has special application, and current large particle rare-earth oxide the most also has certain market, dives in market
Power is huge.
About the preparation of yttrium oxide powder, it is concentrated mainly on Nano grade, and to the medium particle diameter oxidation more than 20 microns
The preparation research of yttrium powder body is less.Patent CN200710121460.X describes the preparation method of a kind of big granularity yittrium oxide, with
Ammonium hydrogen carbonate is precipitant, though available big granularity yittrium oxide, but ammonia nitrogen in waste water will be caused to exceed standard, it is unsatisfactory for discharge of wastewater mark
Accurate.
Summary of the invention
It is an object of the invention to provide the preparation method that a kind of medium particle diameter is 20-50 micron yittrium oxide, production process
Simple to operate, and can reach the requirement of properties of product.
In order to reach above-mentioned purpose, the solution of the present invention is:
A kind of medium particle diameter is the preparation method of 20-50 micron yittrium oxide, adds deionized water, open stirring in clarifying kettle,
Yttrium chloride solution and oxalic acid solution are joined in clarifying kettle, after question response is complete, opens steam, be heated to 95-100 DEG C, enter
Row constant temperature distills, until after terminal acidity, carrying out blowing washing yttrium oxalate, calcination, i.e. can get big granularity yittrium oxide.
Described clarifying kettle is enamel pan, and adding deionized water volume is 30-60L, and temperature is 35-45 DEG C.
Described yttrium chloride solution rare earth concentration is 30-70 g/L, and acidity is 3-5mol/L, and acidity is regulated by hydrochloric acid.
The concentration of described oxalic acid solution is 100-120g/L.
Described it is precipitated as parallel-flow precipitation.
Described yttrium chloride solution and oxalic acid solution join the mass ratio in clarifying kettle and control at 1:1.5-1:2, wait to add
After, add oxalic acid, make the mass ratio of yttrium chloride solution and oxalic acid solution control at 1:2.5-1:3, to reach reaction completely.
After described precipitation is complete, stir 10 minutes, open steam heating, constant temperature distillation, treat that terminal acidity reaches 6-
8mol/L, stops heating.
The filtration washing of described yttrium oxalate, is to be washed with deionized 6-10 time, then drains.
Described calcination, is in atmosphere furnace, in 950-1050 DEG C, is incubated 3-5 hour.
After using such scheme, the present invention is molten by the volume and temperature, yttrium chloride solution and oxalic acid changing deionized water
The terminal acidity that the quality of the concentration of liquid and acidity, yttrium chloride solution and oxalic acid solution is when distilled, is steamed by high temperature highly acidity
Evaporating, little granule constantly dissolves, and bulky grain is constantly grown up, thus obtains large-particle yttrium oxide.
Invent simple to operate, and favorable reproducibility.Yttrium oxalate is sizing precipitation, and granule is thick, it is easy to filtration washing.Mother solution is
Hydrochloric acid, it is easy to process.The yittrium oxide granularity obtained is 20-50 micron, and apparent density is big, and properties of product meet customer requirement
。
Accompanying drawing explanation
Fig. 1 is the particle size distribution schematic diagram of embodiment 1；
Fig. 2 is the particle size distribution schematic diagram of embodiment 2.
Detailed description of the invention
Embodiment 1:
Adding 30L deionized water in enamel pan, temperature is 35 DEG C, opens stirring.Yttrium chloride solution concentration is 50g/L, acidity
For 3mol/L, oxalic acid solution concentration is 117g/L.Yttrium chloride solution and oxalic acid solution are joined clarifying kettle with 1:1.8 mass ratio
In, after adding, add oxalic acid, make mass ratio reach 1:2.5.After reaction completely, stir 10 minutes.Open steam to heat,
Temperature controls at 95-100 DEG C, when terminal acidity reaches 6.8mol/L, stops heating.Blowing.It is washed with deionized 6-10
Time, after draining.It is incubated 3 hours in 1000 DEG C.Obtain yittrium oxide.Medium particle diameter D50=27.31 microns, apparent density is 1.32g/
cm3, specific surface area is 26070 cm2/ g, total amount of rare earth is 99.02%, impurity content: Fe2O3For less than 2ppm, SiO2For being less than
10ppm, CaO are 8ppm.Particle size distribution such as Fig. 1.
Embodiment 2:
Adding 40L deionized water in enamel pan, temperature is 45 DEG C, opens stirring.Yttrium chloride solution concentration is 62g/L, acidity
For 3.5mol/L, oxalic acid solution concentration is 108g/L.Yttrium chloride solution and oxalic acid solution are joined clarifying kettle with 1:2 mass ratio
In, after adding, add oxalic acid, make mass ratio reach 1:2.5.After reaction completely, stir 10 minutes.Open steam to heat,
Temperature controls at 95-100 DEG C, when terminal acidity reaches 8mol/L, stops heating.Blowing.It is washed with deionized 6-10 time,
After draining.It is incubated 4 hours in 1000 DEG C.Obtain yittrium oxide.Medium particle diameter D50=45.21 microns, apparent density is 1.42g/cm3,
Specific surface area is 20000 cm2/ g, total amount of rare earth is 99.15%, impurity content: Fe2O3For less than 2ppm, SiO2For being less than
10ppm, CaO are 10ppm.Particle size distribution such as Fig. 2.
Claims (6)
1. a medium particle diameter is the preparation method of 20-50 micron yittrium oxide, it is characterised in that:
Adding deionized water in clarifying kettle, 30-60L, temperature is 35-45 DEG C；
Opening stirring, join in clarifying kettle by yttrium chloride solution and oxalic acid solution, yttrium chloride solution rare earth concentration is 30-70
G/L, acidity is 3-5mol/L, and acidity is regulated by hydrochloric acid, and the concentration of oxalic acid solution is 100-120g/L, yttrium chloride solution and oxalic acid
Solution joins the mass ratio in clarifying kettle and controls, at 1:1.5-1:2, after adding, to add oxalic acid, makes yttrium chloride solution and grass
The mass ratio of acid solution controls at 1:2.5-1:3；
After question response is complete, opens steam, be heated to 95-100 DEG C, carry out constant temperature distillation, until after terminal acidity 6-8mol/L,
Stop heating；
Carrying out blowing washing yttrium oxalate, calcination, i.e. can get medium particle diameter is 20-50 micron yittrium oxide.
A kind of medium particle diameter the most as claimed in claim 1 is the preparation method of 20-50 micron yittrium oxide, it is characterised in that: institute
Stating clarifying kettle is enamel pan.
A kind of medium particle diameter the most as claimed in claim 1 is the preparation method of 20-50 micron yittrium oxide, it is characterised in that: institute
State and be precipitated as parallel-flow precipitation.
A kind of medium particle diameter the most as claimed in claim 1 is the preparation method of 20-50 micron yittrium oxide, it is characterised in that: institute
State precipitation complete after, stir 10 minutes, be then turned on steam heating, constant temperature distillation.
A kind of medium particle diameter the most as claimed in claim 1 is the preparation method of 20-50 micron yittrium oxide, it is characterised in that: institute
State the filtration washing of yttrium oxalate, be to be washed with deionized 6-10 time, then drain.
A kind of medium particle diameter the most as claimed in claim 1 is the preparation method of 20-50 micron yittrium oxide, it is characterised in that: institute
State calcination, be in atmosphere furnace, in 950-1050 DEG C, be incubated 3-5 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610396407.XA CN106044832A (en) | 2016-06-07 | 2016-06-07 | Preparation method of yttrium oxide with central grain size being 20-50 microns |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115010163A (en) * | 2022-05-20 | 2022-09-06 | 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 |
| CN117401706A (en) * | 2023-12-11 | 2024-01-16 | 赣州晨光稀土新材料有限公司 | Preparation method and application of large-particle rare earth oxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037217A (en) * | 2007-03-22 | 2007-09-19 | 广东富远稀土新材料股份有限公司 | Production method of ultra granule yttria |
| CN102139908A (en) * | 2011-04-21 | 2011-08-03 | 赣州虔东稀土集团股份有限公司 | Submicron yttrium oxide and preparation method thereof |
| CN102205985A (en) * | 2011-04-02 | 2011-10-05 | 南昌大学 | Preparation method for yttrium oxide with different specific surface area |
| CN103803630A (en) * | 2014-01-27 | 2014-05-21 | 福建省长汀金龙稀土有限公司 | Method for preparing yttria of different sizes and different appearances |
-
2016
- 2016-06-07 CN CN201610396407.XA patent/CN106044832A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037217A (en) * | 2007-03-22 | 2007-09-19 | 广东富远稀土新材料股份有限公司 | Production method of ultra granule yttria |
| CN102205985A (en) * | 2011-04-02 | 2011-10-05 | 南昌大学 | Preparation method for yttrium oxide with different specific surface area |
| CN102139908A (en) * | 2011-04-21 | 2011-08-03 | 赣州虔东稀土集团股份有限公司 | Submicron yttrium oxide and preparation method thereof |
| CN103803630A (en) * | 2014-01-27 | 2014-05-21 | 福建省长汀金龙稀土有限公司 | Method for preparing yttria of different sizes and different appearances |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115010163A (en) * | 2022-05-20 | 2022-09-06 | 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 |
| 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 |
| CN117401706A (en) * | 2023-12-11 | 2024-01-16 | 赣州晨光稀土新材料有限公司 | Preparation method and application of large-particle rare earth oxide |
| CN117401706B (en) * | 2023-12-11 | 2024-03-26 | 赣州晨光稀土新材料有限公司 | Preparation method and application of large-particle rare earth oxide |
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Application publication date: 20161026 |