CN109319820A - A method of chloride ion in removal nano-oxide is washed using plate compression - Google Patents
A method of chloride ion in removal nano-oxide is washed using plate compression Download PDFInfo
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- CN109319820A CN109319820A CN201811207610.3A CN201811207610A CN109319820A CN 109319820 A CN109319820 A CN 109319820A CN 201811207610 A CN201811207610 A CN 201811207610A CN 109319820 A CN109319820 A CN 109319820A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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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
- C01P2006/80—Compositional purity
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Abstract
The invention belongs to the preparation technical fields of rare earth compound, more particularly to a kind of method for washing chloride ion in removal nano-oxide using plate compression, the rare earth oxide prepared through the precipitation method is separated by solid-liquid separation using plate compression, the sheet frame for being used to wash is subjected to segmentation washing from front to back, then removing chloride is removed in washing simultaneously again, the method of the present invention has process conditions fairly simple, lower production costs, the advantages of industrialized production easy to accomplish, and whole preparation process meets environmental requirement.The chloride ion content of the oxide obtained through the method for the present invention is less than 20ppm, and primary particle size is 30-70nm, even particle distribution.
Description
Technical field
It is the invention belongs to the preparation technical field of rare earth compound, in particular to a kind of to be received using plate compression washing removal
The method of chloride ion in rice oxide.
Background technique
Oxide nano rare earth has good light, electricity, magnetic, mechanics and chemical characteristic, is widely used in function ceramics
The fields such as material, luminescent material, laser material.Not only to of nano RE oxide powder when being applied to above-mentioned field
Grain size has strict requirements, and also has higher requirement to non-rare earth impurity, when oxide nano rare earth is applied to chip
When in multilayer ceramic capacitor (MLCC), for the brightness for improving product, dispersion is reduced, extends its service life, generally requires nanometer
The lower the chloride ion content of oxide the better, because chloride ion content is higher, acid mist is corresponding also higher, leads to nano-oxide
Corrosion strength it is strong, will affect its performance when being used in MLCC, such as: the brightness of product, service life, or can cause
Short circuit etc..
The prior art prepares nano rareearth oxidate powder body using chemical precipitation method, by the way that precipitating reagent is added to rare-earth salts
So that anion in rare-earth salt solution is formed sediment in solution, is then filtered, washed, dries, thermally decomposing etc. and be prepared into
To nano rareearth oxidate powder body.Rare-earth salts usually selects rare earth-iron-boron, makees raw material instead of rare earth chlorine using rare earth nitrades
Compound, product chloride ion obtained is fewer, but cost will increase very much.Therefore, in view of to cost of material the considerations of, to being used for
It is required that the lower nano rareearth oxidate powder body of chloride ion content, removing chloride is needed in preparation process.
It prepares oxide nano rare earth and generallys use suction filtration bucket using vacuum pump suction filtration washing, but the suction filtration time is longer, use
Water is more, directly results in cost raising.Plate and frame filter press is the equipment for separating liquid and solid, but usually to separating
Solid there is no the requirement of impurity.
Summary of the invention
In order to meet the application requirement of oxide nano rare earth, its chloride ion content is reduced, the present invention provides one kind to adopt
The method for washing chloride ion in removal nano-oxide with plate compression, the specific method is as follows:
(1) it selects rare earth-iron-boron as raw material, and anionic surfactant (PEG2000) is added in feed liquid, adopt
Rare earth carbonate is obtained with alkaline precipitating agent precipitating rare earth ion；
Wherein, rare earth-iron-boron feed acidity is less than 0.3mol/l, and rare earth-iron-boron feed concentration is 0.2-0.8mol/l；
The mass percent that anionic surfactant dose accounts for rare-earth chlorination material liquid is 2%-5%；Alkaline precipitating agent is bicarbonate
Sodium or sodium carbonate, alkaline precipitating agent solution concentration are 0.4-1.0mol/l；The molar ratio of rare earth-iron-boron and precipitating reagent is 1:
1.5-1:4；
(2) rare earth carbonate for obtaining step (1) precipitation reaction after being aged 2h, is washed using segmented plate compression
Method washs rare earth carbonate to remove removing chloride, and chloride ion content control is made to be less than 20ppm；
Wherein, the washing temperature when washing of control plate and frame filter press are as follows: 50-60 DEG C, pressure when plate and frame filter press is washed
For 2Kg or so.
(3) by the rare earth carbonate calcination after step (2) washing, sieving prepares oxide nano rare earth, wherein calcination temperature
Degree is 750-900 DEG C, and calcination soaking time is 1-3 hours.
Segmented plate compression WATER-WASHING METHOD washs rare earth carbonate to remove the specific water-washing process of removing chloride are as follows:
(1), by the precipitation reaction of reaction kettle back warp and obtained rare earth carbonate feeding sheet frame is aged using pneumatic diaphragm pump
Filter press fills 40 blocks of plates, acts on using the centrifugation of filter cloth, then by the pressure of plate compression, filters moisture, keep slurry here
Material.
(2), first the inlet valve of the 1-10 sheet of plate and frame filter press to be closed, outlet valve is opened, the water inlet of 11-40 sheet,
Outlet valve is all closed, and 1-10 sheet is only washed, until being washed till water outlet silver nitrate titration without precipitating.Then by plate and frame filter press
The inlet valve of 11-20 sheet is closed, and outlet valve is opened, 1-10, the water inlet of 21-40 sheet, and outlet valve is all closed, and only washes 11-
20 sheets, until being washed till water outlet silver nitrate titration without precipitating, in this way and so on, 40 are successively washed from front to back
Plate；Finally the inlet valve of the 1-40 sheet of plate and frame filter press is closed again, outlet valve is opened, and 40 blocks of plates are washed 10min together, complete
At water-washing process.
First using the pressure that the purpose of segmentation washing is to increase water, enhance penetration when washing, due to diaphragm pump
Water supply hourly be it is certain, the piece number of washing is few, and pressure is big, and for impact force with regard to big, washing effect is all right, can be the inside
Chloride ion is all taken away.
(3), container bag is placed on cart when discharging, is pushed into below sheet frame, then the shovel in every sheet is entered container bag,
It is filled to container bag, tightens sack, weighed, stacked with driving neat.
In order to keep the particle of product uniform, the digestion time for the rare earth carbonate that precipitation reaction obtains must be consistent, so
One batch of material needs are disposably put down when blowing, and a batch of material can probably pile 40 blocks of plates, if disposable complete washing, chloride ion
Content is very high, generally 500-600ppm, sometimes even up to 1000ppm or more.
The method of the present invention washes 40 blocks of plates points 4 times, washes 10 blocks of plates every time, successively washes from front to back, all washes for 4 times
After good, then 40 blocks of plates are washed into 10min together, goes removing chloride effect clearly.
The utility model has the advantages that
The method of the present invention finds that the plate number washed is more, and pressure is smaller, and penetration power is weaker, water in water-washing process
The surface that every block of plate can only be washed during washing, cannot be penetrated into intralamellar part, be present in intralamellar part material washing less than, even if
The time for increasing washing, also it is unable to reach preferable effect.Therefore, the present invention is using segmentation washing, the sheet frame that will be used to wash
Segmentation washing is carried out from front to back, and under conditions of pressure is certain, in the case where plate number is less, penetration power is stronger, then again
Removing chloride is removed in washing simultaneously, so that the effect of washing is more preferable.
The advantages of the method for the present invention has process conditions fairly simple, lower production costs, industrialized production easy to accomplish,
And whole preparation process meets environmental requirement.The chloride ion of the oxide obtained through the method for the present invention, which contains, is less than 20ppm, and primary
Partial size is 30-70nm, even particle distribution.
Specific embodiment
The present invention will now be described in detail with reference to examples.
Embodiment 1
(1) carry out precipitation reaction: compound concentration is the yttrium chloride feed liquid of 0.4mol/l, and control yttrium chloride feed acidity is less than
0.3mol/l, according to the molar ratio of yttrium oxide and precipitating reagent are as follows: sodium carbonate is added in 1:1.6, and sodium carbonate liquor concentration is 0.5mol/
L adds 2% dispersing agent PEG2000, and just heavy shallow lake is added dropwise, and 1h is stirred after completion of dropwise addition, closes stirring ageing 2h.
(2) it washes:
The sediment in reaction kettle is sent into plate and frame filter press using pneumatic diaphragm pump, 40 blocks of plates is filled altogether, utilizes filter
The centrifugation of cloth, then acted on by the pressure of plate compression, moisture is filtered, keeps slurry here.When controlling plate and frame filter press washing
Washing temperature are as follows: 50 DEG C, plate and frame filter press wash when pressure be 2Kg, first by the inlet valve of plate and frame filter press 1-10 sheet
It closes, outlet valve is opened, the water inlet of 11-40, and outlet valve is all closed, and is only washed 1-10 sheet, is washed till water outlet silver nitrate titration
Until precipitating.It washes 11-20 sheet again after the same method, successively washes 40 sheets from front to back；Finally again by sheet frame pressure
The inlet valve of the 1-40 sheet of filter is closed, and outlet valve is opened, and 40 blocks of plates are washed 10min together, complete water-washing process.
The water-washing process used time is about 3.5h, electricity consumption: 30kw, with water: 12T.
(3) calcination: the carbonate washed above is placed on 850 DEG C of calcinations, 2h is kept the temperature, is finally sieved, obtains Nano Rare
Native yttrium oxide.
Through detecting: with Cl in spectrophotometer detection nano rare earth yttrium oxide-: its content are as follows: 20ppm；Nano rare earth oxygen
Change yttrium primary particle size is 30-70nm, even particle distribution.
Embodiment 2
(1) carry out precipitation reaction: compound concentration is the cerium chloride feed liquid of 0.3mol/l, and control cerium chloride feed acidity is less than
0.3mol/l, according to the molar ratio of cerium oxide and precipitating reagent are as follows: sodium bicarbonate is added in 1:3, and sodium bicarbonate solution concentration is
0.5mol/l adds 2.5% dispersing agent PEG2000, and just heavy shallow lake is added dropwise, and 1h is stirred after completion of dropwise addition, closes stirring ageing
2h。
(2) it washes:
The sediment in reaction kettle is sent into plate and frame filter press using pneumatic diaphragm pump, 40 blocks of plates is filled altogether, utilizes filter
The centrifugation of cloth, then acted on by the pressure of plate compression, moisture is filtered, keeps slurry here.
Control washing temperature when plate and frame filter press washing are as follows: 55 DEG C, pressure when plate and frame filter press is washed is 2Kg, first
The inlet valve of plate and frame filter press 1-10 sheet is closed, outlet valve is opened, the water inlet of 11-40, and outlet valve is all closed, and only washes 1-
10 sheets, until being washed till water outlet silver nitrate titration without precipitating.Wash 11-20 sheet again after the same method, from front to back according to
It is secondary to wash 40 sheets；Finally the inlet valve of the 1-40 sheet of plate and frame filter press is closed again, outlet valve is opened, together by 40 blocks of plates
10min is washed, water-washing process is completed.
Used time is about 3.8h, electricity consumption: 32kw, with water: 13.5T.
(3) calcination: the carbonate washed above is placed on 750 DEG C of calcinations, 3h is kept the temperature, is finally sieved, obtains Nano Rare
Native cerium oxide.
Through detecting: with Cl in spectrophotometer detection nano rare earth cerium oxide-: 18ppm, the primary grain of nano rare earth cerium oxide
Diameter is 30-70nm, even particle distribution.
Embodiment 3
(1) carry out precipitation reaction: compound concentration is the yttrium chloride feed liquid of 0.5mol/l, and control yttrium chloride feed acidity is less than
0.3mol/l, according to the molar ratio of yttrium oxide and precipitating reagent are as follows: sodium carbonate is added in 1:1.6, and sodium carbonate liquor concentration is 0.4mol/
L adds 2% dispersing agent PEG2000, and just heavy shallow lake is added dropwise, and 1h is stirred after completion of dropwise addition, closes stirring ageing 2h.
(2) it washes:
The sediment in reaction kettle is sent into plate and frame filter press using pneumatic diaphragm pump, 40 blocks of plates is filled altogether, utilizes filter
The centrifugation of cloth, then acted on by the pressure of plate compression, moisture is filtered, keeps slurry here.When controlling plate and frame filter press washing
Washing temperature are as follows: 60 DEG C, plate and frame filter press wash when pressure be 2Kg, first by the inlet valve of plate and frame filter press 1-10 sheet
It closes, outlet valve is opened, the water inlet of 11-40, and outlet valve is all closed, and is only washed 1-10 sheet, is washed till water outlet silver nitrate titration
Until precipitating.It washes 11-20 sheet again after the same method, successively washes 40 sheets from front to back；Finally again by sheet frame pressure
The inlet valve of the 1-40 sheet of filter is closed, and outlet valve is opened, and 40 blocks of plates are washed 10min together, complete water-washing process.
Used time is about 3.6h, electricity consumption: 32kw, with water: 12.5T.
(3) calcination: the carbonate washed above is placed on 900 DEG C of calcinations, 1.5h is kept the temperature, is finally sieved, obtains nanometer
Rare-earth oxidation yttrium.
Through detecting: with Cl in spectrophotometer detection nano rare earth yttrium oxide-: 20ppm, the primary grain of nano rare earth yttrium oxide
Diameter is 30-70nm, even particle distribution.
Comparative example 1
The precipitating of nano yttrium oxide, calcination mode is the same as embodiment 1.
Nano rare earth yttrium oxide primary particle size is 30-70nm, even particle distribution.
Water-washing method: the sediment in reaction kettle is sent into plate and frame filter press using pneumatic diaphragm pump, fills 40 pieces altogether
Plate is acted on using the centrifugation of filter cloth, then by the pressure of plate compression, filters moisture, keep slurry here.
Control washing temperature when plate and frame filter press washing are as follows: 50 DEG C, pressure when plate and frame filter press is washed is 2Kg, will
The inlet valve of the 1-40 sheet of plate and frame filter press is closed, and outlet valve is opened, and 40 blocks of plates are washed 10min together, complete water-washing process.
40 blocks of plates are washed together, while the material washed is too many, and washing is not thorough, lead to a height of 1000ppm of chloride ion or so.
Used time is about 5.5h, electricity consumption: 60kw, with water: 20T.
Comparative example 2
The precipitating of nano-cerium oxide, calcination mode is the same as embodiment 2.
Water-washing method: the sediment in reaction kettle is sent into plate and frame filter press using pneumatic diaphragm pump, fills 40 pieces altogether
Plate is acted on using the centrifugation of filter cloth, then by the pressure of plate compression, filters moisture, keep slurry here.
Control washing temperature when plate and frame filter press washing are as follows: 55 DEG C, pressure when plate and frame filter press is washed is 2Kg, first
The inlet valve of plate and frame filter press 1-20 sheet to be closed, outlet valve is opened, the water inlet of 21-40, and outlet valve is all closed, and first 20 pieces
Plate is first washed, until being washed till water outlet silver nitrate titration without precipitating.Wash 31-40 sheet again after the same method；Finally again by plate
The inlet valve of the 1-40 sheet of frame filter press is closed, and outlet valve is opened, and 40 blocks of plates are washed 10min together, complete water-washing process.
Used time is about 5h, electricity consumption: 50kw, with water: 18T.
Measuring chloride ion with spectrophotometer is 500-600ppm, is slightly improved or undesirable.
Comparative example 3
The precipitating of nano yttrium oxide, calcination mode is the same as embodiment 3.
Water-washing method: the valve of settling box is opened.Yttrium carbonate is put into and is filtered in bucket, using the centrifugation of filter cloth, is led to
Vacuum pump suction filtration is crossed, moisture is filtered, keeps slurry here.Then the pure water for being put into 60 DEG C in logical is being filtered again, is stirring, filters.It drains
Afterwards, discharge water washing for the second time.Silver nitrate titration is washed till without precipitating.
The whole process used time: 10h, electricity consumption 150kw, with water: 20T.
It is detected after calcination with spectrophotometer, Cl-: 200ppm.
Claims (6)
1. a kind of method for washing chloride ion in removal nano-oxide using plate compression, it is characterised in that: specific method step
It is rapid as follows:
(1) it selects rare earth-iron-boron as raw material, and anionic surfactant PEG2000 is added in feed liquid, using alkalinity
Precipitating reagent precipitating rare earth ion obtains rare earth carbonate；
(2) rare earth carbonate for obtaining step (1) precipitation reaction is washed after being aged 2h using segmented plate compression WATER-WASHING METHOD
Rare earth carbonate is washed to remove removing chloride, chloride ion content is made to be less than 20ppm；
(3) by the rare earth carbonate calcination after step (2) washing, sieving prepares oxide nano rare earth.
2. as described in claim 1 using the method for chloride ion in plate compression washing removal nano-oxide, feature exists
In: step (1) the rare earth-iron-boron feed acidity is less than 0.3mol/l, and rare earth-iron-boron feed concentration is 0.2-0.8mol/
l；The mass percent that anionic surfactant dose accounts for rare-earth chlorination material liquid is 2%-5%；Alkaline precipitating agent includes carbon
Sour hydrogen sodium or sodium carbonate, solution concentration 0.4-1.0mol/l；The molar ratio of rare earth-iron-boron and precipitating reagent is 1:1.5-1:4.
3. as described in claim 1 using the method for chloride ion in plate compression washing removal nano-oxide, feature exists
In: washing temperature when controlling plate and frame filter press washing in step (2) described water-washing process are as follows: 50-60 DEG C, plate and frame filter press water
Pressure when washing is 2Kg.
4. as described in claim 1 using the method for chloride ion in plate compression washing removal nano-oxide, feature exists
In: detailed process is as follows to remove removing chloride for step (2) the segmented plate compression WATER-WASHING METHOD washing rare earth carbonate:
(1), by the precipitation reaction of reaction kettle back warp and obtained rare earth carbonate feeding plate compression is aged using pneumatic diaphragm pump
Machine fills 40 blocks of plates, acts on using the centrifugation of filter cloth, then by the pressure of plate compression, filters moisture, keep slurry here；
(2), first the inlet valve of the 1-10 sheet of plate and frame filter press is closed, outlet valve is opened, the water inlet of 11-40 sheet, water outlet
Valve is all closed, and 1-10 sheet is only washed, until being washed till water outlet silver nitrate titration without precipitating；Then by the 11- of plate and frame filter press
The inlet valve of 20 sheets is closed, and outlet valve is opened, 1-10, the water inlet of 21-40 sheet, and outlet valve is all closed, and only washes 11-20 piece
Plate successively washes 40 sheets from front to back；Finally the inlet valve of the 1-40 sheet of plate and frame filter press is closed again, outlet valve is beaten
It opens, 40 blocks of plates is washed into 10min together, complete water-washing process；
(3), container bag is placed on cart, is pushed into below sheet frame, then the shovel in every sheet is entered container bag, it is packed to packaging
It is full, sack is tightened, is weighed, is stacked with driving neat.
5. as described in claim 1 using the method for chloride ion in plate compression washing removal nano-oxide, feature exists
In: step (3) calcination temperature is 750-900 DEG C, and calcination soaking time is 1-3 hours.
6. the application that a kind of method as described in claim 1 removes the nano-oxide of removing chloride, it is characterised in that: the removal
The nano-oxide of chloride ion is used for chip multilayer ceramic capacitor field.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811207610.3A CN109319820B (en) | 2018-10-17 | 2018-10-17 | Method for removing chloride ions in nano oxides by plate-and-frame filter pressing and washing |
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| CN201811207610.3A CN109319820B (en) | 2018-10-17 | 2018-10-17 | Method for removing chloride ions in nano oxides by plate-and-frame filter pressing and washing |
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Cited By (2)
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| CN112047371A (en) * | 2020-07-27 | 2020-12-08 | 常州市卓群纳米新材料有限公司 | Preparation method of low-Fe ion and low-Ca ion nano oxide serving as raw material for MLCC (MLCC) |
| CN112266243A (en) * | 2020-12-15 | 2021-01-26 | 安徽中创电子信息材料有限公司 | Method and device for washing superfine powder material for ceramic capacitor |
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| CN112266243A (en) * | 2020-12-15 | 2021-01-26 | 安徽中创电子信息材料有限公司 | Method and device for washing superfine powder material for ceramic capacitor |
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| CN109319820B (en) | 2019-12-17 |
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