CN109205655A - A kind of preparation method for the nano oxidized gadolinium that partial size is 80-100nm - Google Patents
A kind of preparation method for the nano oxidized gadolinium that partial size is 80-100nm Download PDFInfo
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- CN109205655A CN109205655A CN201811404108.1A CN201811404108A CN109205655A CN 109205655 A CN109205655 A CN 109205655A CN 201811404108 A CN201811404108 A CN 201811404108A CN 109205655 A CN109205655 A CN 109205655A
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- C—CHEMISTRY; METALLURGY
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- 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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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention discloses a kind of preparation methods for the nano oxidized gadolinium that partial size is 80-100nm, include the following steps: first, the sodium bicarbonate solution that concentration is 0.1mol/L-0.6mol/L and temperature is 0-5 DEG C is dropped evenly with the speed of 3-6L/min into the gadolinium chloride solution containing polyethylene glycol 10000 and/or PEG 20000, continue to stir 0.5-1h after completion of dropwise addition, it is still aging under conditions of 0-5 DEG C again, the mother liquor containing sediment is made, temperature of reaction system is 0-5 DEG C during this, and the environment temperature of operation maintains 26-28 DEG C.Then washing is filtered, the suction filtration water-washing method is 95 DEG C or more of the multiple soaking and water washing of hot pure water, and the filter cake after filtering washing is placed at 0-5 DEG C more than for 24 hours, then the calcination 1-2h at 800-850 DEG C, obtains the nano oxidized gadolinium that partial size is 80-100nm.
Description
Technical field
The invention belongs to a kind of systems for the nano oxidized gadolinium that nano-powder technical field more particularly to partial size are 80-100nm
Preparation Method.
Background technique
Gadolinium oxide is widely used in catalysis, ceramics, glass industry, solid oxide fuel cell, luminescent material, polishing material
The fields such as material and nuclear material.Gadolinium oxide can also be used as the main component in solid fuel cell.For nano oxidized gadolinium powder
Synthesis, the use of commonplace method is at present sol-gal process, chemical precipitation method." the micro-nano gadolinium oxide of electrically conductive polyaniline
The synthesis and characterization of composite material " Lixia ZHANG etc., Guangxi Teachers College's journal (natural science edition), 2007,66-68, using change
The gadolinium oxide flaky powder that the precipitation method prepare micro/nano level is learned, but the powder prepared is easy to reunite, obtained gadolinium oxide size
It is larger, in 50~800nm or so；" preparation of nano oxidized gadolinium/NBR composite material and its shielding properties research " Zhao Yongfeng etc.,
Rubber industry, 2010,581-585, it is combined using coprecipitation and spray drying process and has prepared nanoscale through high-temperature calcination
Gadolinium oxide, but comparatively preparation process duration, technique are relatively cumbersome.
With the development of science and technology, also there is higher requirement in manufacturer to the physical property of gadolinium oxide.It is open at present
The technology of preparing of RE oxide powder largely use ammonium hydrogen carbonate, crystal seed will be also added as precipitating reagent in urea sometimes
Or the other materials such as ammonium salt.Ammonium hydrogen carbonate or ammonium salt can generate a large amount of ammonia nitrogen waste water, bring great difficulty to wastewater to reach standard；
The method that crystal seed is added simultaneously, first has to obtain preferable crystal seed, and the preparation difficulty of crystal seed is larger, and precipitation process is not easily-controllable
System.
Summary of the invention
The present invention is provided and a kind of more environmentally friendly, energy-efficient prepares partial size to overcome above-mentioned problems of the prior art
For the method for the nano oxidized gadolinium of 80-100nm.
The technical scheme adopted by the invention is as follows: a kind of partial size is described in the preparation method of the nano oxidized gadolinium of 80-100nm
Method includes the following steps:
(1) the gadolinium chloride solution that addition is 0.1mol/L-0.6mol/L with the concentration that pure water is prepared in a kettle, then
The polyethylene glycol 10000 and/or PEG 20000 surfactant of the 10%-15% of gadolinium chloride quality are added thereto, stirs
It mixes to evenly dispersed and sufficiently dissolve, adjustment system temperature is 0-5 DEG C.
Then, under conditions of maintenance system temperature is 0-5 DEG C, use is dropped evenly with the speed of 3-6L/min into system
The sodium bicarbonate precipitating reagent that the concentration that pure water is prepared is 0.1mol/L-0.6mol/L and temperature is 0-5 DEG C；Precipitating reagent waits that knot is added dropwise
Shu Hou continues to stir 0.5-1h, then still aging under conditions of 0-5 DEG C, and the mother liquor containing sediment is made.Speed is wherein added dropwise
Degree can also suitably increase according to production amplification factor, but should increase mixing speed simultaneously.The environment temperature operated above is tieed up
26-28 DEG C is held, particle can be made to become larger if being higher than this temperature, specific surface becomes smaller, this environment temperature is very crucial, is lower than this
Temperature particle can be small, and specific surface is bigger.
(2) mother liquor containing sediment made from step (1) is subjected to suction filtration washing, the suction filtration water-washing method is to take out
With 95 DEG C or more of the multiple soaking and water washing of hot pure water in lauter tub, the time impregnated every time washes after 15-20min, filters washing
Environment temperature be maintained at 26-28 DEG C；Then the filter cake filtered after washing is placed 24 hours or more under conditions of 0-5 DEG C,
Then again at 800-850 DEG C after calcination 1-2h, the nano oxidized gadolinium that partial size is 80-100nm is obtained.
For the ease of granularity control, advanced optimize, the molar ratio of gadolinium chloride described in step (1) and sodium bicarbonate is
1:3-1:3.2。
It for more preferable control system temperature, advanced optimizes, the system temperature in step (1) in reaction kettle is by circulation ice
Water management.
In order to the more uniform distribution of particle, it is preferred that in step (1) after precipitating reagent completion of dropwise addition, continue mixing time
For 0.5h, digestion time 2h.
In order to promote burning effect and guarantee distribution of particles, it is further preferred that calcination described in step (2) is in trolley
It is carried out in formula rare earth roaster.
Advantageous effects obtained by the present invention are as follows: 1) prepare the nano oxidized of the uniform 80-100nm of particle diameter distribution
Gadolinium；2) multiple using 95 DEG C or more of hot pure water soaking and water washing, under the premise of effectively removing impurity, effectively avoid water washed
The defect that particle agglomeration becomes larger in journey, and gadolinium oxide particle dispersion obtained is preferable；3)；The environment temperature for filtering washing is kept
At 26-28 DEG C, grain graininess is also effectively ensured.4) filter cake is first placed 24 hours or more under conditions of 0-5 DEG C and is burnt again after washing
It burns, further ensures the good dispersion of particle, guarantee that particle is not reunited and become larger.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of nano oxidized gadolinium particle made from embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of nano oxidized gadolinium particle made from embodiment 2；
Fig. 3 is the scanning electron microscope (SEM) photograph of nano oxidized gadolinium particle made from embodiment 3；
Fig. 4 is the scanning electron microscope (SEM) photograph of nano oxidized gadolinium particle made from embodiment 4；
Fig. 5 is the scanning electron microscope (SEM) photograph of nano oxidized gadolinium particle made from comparative example 1；
Fig. 6 is the scanning electron microscope (SEM) photograph of nano oxidized gadolinium particle made from comparative example 2；
Fig. 7 is the scanning electron microscope (SEM) photograph of nano oxidized gadolinium particle made from comparative example 3；
Fig. 8 is the scanning electron microscope (SEM) photograph of nano oxidized gadolinium particle made from comparative example 4；
Fig. 9 is the scanning electron microscope (SEM) photograph of nano oxidized gadolinium particle made from comparative example 5.
Specific embodiment
The present invention is described in further detail below with reference to embodiment:
Embodiment 1:
The nano oxidized gadolinium powder that present embodiment uses following technical scheme to prepare partial size as 80-100nm: pass through
External temperature controlling instruments (can be air-conditioning) control environment temperature is 26 DEG C.The gadolinium chloride solution of high concentration is taken, pure water dilution is added
Compound concentration is the gadolinium chloride solution of 0.3mol/L, and the gadolinium chloride solution 91.95L that concentration is 0.3mol/L is then put into spacer
It is 2 DEG C that solution system temperature in circulation ice water control spacer reaction kettle is passed through in reaction kettle, in spacer.Then 500 grams are weighed to gather
Ethylene glycol 20000 is added in above-mentioned spacer reaction kettle with the solution that pure water is dissolved into 2L, is by concentration after stirring 30min
0.3mol/L temperature is that 2 DEG C of sodium bicarbonate solution uniformly spray and is added dropwise in spacer reaction kettle, and rate of addition 4L/min drips
Continue to stir 30min after adding, then still aging 2 hours under conditions of 2 DEG C, the mother liquor containing sediment is made.More than
It is 2 DEG C that operation, which all keeps the temperature of reaction system in spacer reaction kettle,.
The preparation method of precipitating reagent are as follows: weigh sodium bicarbonate 6.95kg, addition pure water 275.85L stirring is configured to concentration and is
0.3mol/L sodium bicarbonate solution.
The mother liquor obtained above containing sediment is filtered after ageing, it is pure then to add 95 DEG C or more of heat
The soaked wash water of water logging is washed.With each 500L soaking and water washing, the time impregnated every time in 15min, is washed 5 times, total 2500L heat is pure
Water, the environment temperature for filtering washing are maintained at 26-28 DEG C.Filter cake is placed 24 under conditions of 0-5 DEG C after suction filtration excessive moisture
Hour, it is then placed in cart furnace calcination, calcination temperature is 800 DEG C, and soaking time is 1 hour.The nano oxidized gadolinium of gained is examined through SEM
Survey granularity is 80-100nm, specific surface area 8.81m2/g。
Embodiment 2
The nano oxidized gadolinium powder that present embodiment uses following technical scheme to prepare partial size as 80-100nm: pass through
External temperature controlling instruments (can be air-conditioning) control environment temperature is 28 DEG C.The gadolinium chloride solution of high concentration is taken, pure water dilution is added
Compound concentration be 0.2mol/L gadolinium chloride solution, then by concentration be 0.2mol/L gadolinium chloride solution 275.86L be put into every
It covers in reaction kettle, it is 0 DEG C that solution system temperature in circulation ice water control spacer reaction kettle is passed through in spacer.Then 1500 grams are weighed
Polyethylene glycol 10000 is added in above-mentioned spacer reaction kettle with the solution that pure water is dissolved into 6L, is by concentration after stirring 30min
0.2mol/L temperature is that 0 DEG C of sodium bicarbonate solution uniformly spray and is added dropwise in spacer reaction kettle, and rate of addition 6L/min drips
Continue to stir 30min after adding, the mother liquor containing sediment is made within still aging 2 hours.The above operation all keeps spacer reaction
Temperature of reaction system in kettle is 0 DEG C.
The preparation method of precipitating reagent are as follows: weigh sodium bicarbonate 14.83kg, pure water 441.38L stirring is added and is configured to concentration
For 0.4mol/L sodium bicarbonate solution.
The mother liquor obtained above containing sediment is filtered after ageing, it is pure then to add 95 DEG C or more of heat
Water washing.With each 500L washing, wash 10 times, total 5000L hot pure water, the environment temperature for filtering washing is maintained at 26-28 DEG C.
Filter cake is placed 24 hours under conditions of 0-5 DEG C after filtering excessive moisture, is then placed in cart furnace calcination, calcination temperature is
800 DEG C, soaking time is 1 hour.The nano oxidized gadolinium of gained is 80-100nm, specific surface area 7.46m through SEM detection granularity2/g。
Embodiment 3
The nano oxidized gadolinium powder that present embodiment uses following technical scheme to prepare partial size as 80-100nm: pass through
External temperature controlling instruments (can be air-conditioning) control environment temperature is 27 DEG C.The gadolinium chloride solution of high concentration is taken, pure water dilution is added
Compound concentration is the gadolinium chloride solution of 0.1mol/L solubility, then by the gadolinium chloride solution by concentration for 0.1mol/L
441.38L is put into spacer reaction kettle, and it is 3 DEG C that circulation ice water control solution system temperature is passed through in spacer.Then 960 grams are weighed
Polyethylene glycol 10000 is added in above-mentioned spacer reaction kettle with the solution that pure water is dissolved into 3.84L, is by concentration after stirring 30min
0.4mol/L temperature is that 3 DEG C of sodium bicarbonate solution uniformly spray and is added dropwise in spacer reaction kettle, and rate of addition 5L/min drips
Continue to stir 30min after adding, be then allowed to stand ageing 2 hours, the mother liquor containing sediment is made.The above operation all keeps spacer
Temperature of reaction system in reaction kettle is 3 DEG C.The preparation method of precipitating reagent are as follows: weigh sodium bicarbonate 14.83kg, pure water is added
It is 0.4mol/L sodium bicarbonate solution that 342.07L stirring, which is configured to concentration,.
The mother liquor obtained above containing sediment is filtered after ageing, it is pure then to add 95 DEG C or more of heat
Water washing.With each 500L washing, wash 8 times, total 4000L hot pure water, the environment temperature for filtering washing is maintained at 26-28 DEG C.
Filter cake is placed 24 hours under conditions of 0-5 DEG C after filtering excessive moisture, is then placed in cart furnace calcination, calcination temperature is
800 DEG C, soaking time is 1 hour.The nano oxidized gadolinium of gained is 80-100nm, specific surface area 9.86m through SEM detection granularity2/g。
Embodiment 4
The nano oxidized gadolinium powder that present embodiment uses following technical scheme to prepare partial size as 80-100nm: pass through
External temperature controlling instruments (can be air-conditioning) control environment temperature is 28 DEG C.The gadolinium chloride solution of high concentration is taken, pure water dilution is added
Compound concentration is the gadolinium chloride solution of 0.6mol/L, and the gadolinium chloride solution 55.17L that concentration is 0.6mol/L is then put into spacer
It is 5 degree that solution system temperature in circulation ice water control spacer reaction kettle is passed through in reaction kettle, in spacer, then weighs 780 grams and gathers
Ethylene glycol 20000 is added in above-mentioned spacer reaction kettle with the solution that pure water is dissolved into 3.12L, is by concentration after stirring 30min
0.1mol/L, temperature are that 5 degree of sodium bicarbonate solution is uniformly sprayed and is added dropwise in spacer reaction kettle, rate of addition 6L/min,
Continue after completion of dropwise addition stir 30min, still aging 2 hours.All keeping system temperature above is 5 DEG C.
Sodium bicarbonate 8.62KG is weighed, it is 0.1mol/L sodium bicarbonate solution that pure water 1026.16L, which is added, and stirs into concentration.
The mother liquor obtained above containing sediment is filtered after ageing, then adds 95 DEG C or more of hot pure water washing.
With each 500L washing, wash 6 times, total 3000L hot pure water, the environment temperature for filtering washing is maintained at 26-28 DEG C.It is extra to filter
Filter cake is placed 24 hours under conditions of 0-5 DEG C after moisture content, is then placed in cart furnace calcination, calcination temperature is 800 DEG C, heat preservation
Time is 1 hour.The nano oxidized gadolinium of gained is 80-100nm, specific surface area 7.86m through SEM detection granularity2/g。
Comparative example 1
The nano oxidized gadolinium powder that present embodiment uses following technical scheme to prepare partial size as 80-100nm: pass through
External temperature controlling instruments (can be air-conditioning) control environment temperature is 35 DEG C.The gadolinium chloride solution of high concentration is taken, pure water dilution is added
Compound concentration is the gadolinium chloride solution of 0.3mol/L, and the gadolinium chloride solution 91.95L that concentration is 0.3mol/L is then put into spacer
It is 2 DEG C that solution system temperature in circulation ice water control spacer reaction kettle is passed through in reaction kettle, in spacer, weighs 500 grams of poly- second two
Alcohol 20000 is added in above-mentioned spacer reaction kettle with the solution that pure water is dissolved into 2L, and stirring concentration after 30min is 0.3mol/L temperature
Degree is uniformly sprayed for 2 DEG C of sodium bicarbonate solution and is added dropwise in spacer reaction kettle, rate of addition 4L/min, and completion of dropwise addition is subsequent
Continuous stirring 30min, is then allowed to stand ageing 2 hours, the mother liquor containing sediment is made.The above operation is all kept in spacer reaction kettle
Temperature of reaction system is 2 DEG C.The preparation method of precipitating reagent are as follows: weigh sodium bicarbonate 6.6.95kg, pure water 275.85L stirring is added
Being configured to concentration is 0.3mol/L sodium bicarbonate solution.The mother liquor obtained above containing sediment is taken out after ageing
Then filter adds 95 DEG C or more of hot pure water washing.It with each 500L washing, washes 5 times, total 2500L hot pure water, filters water
The environment temperature washed is maintained at 26-28 DEG C.It filters and filter cake is placed 24 hours under conditions of 0-5 DEG C after excessive moisture, then
It is put into cart furnace calcination, calcination temperature is 800 DEG C, and soaking time is 1 hour.The nano oxidized gadolinium of gained detects granularity through SEM
100nm or more, specific surface area 5.43m2/g。
Comparative example 2
The nano oxidized gadolinium powder that present embodiment uses following technical scheme to prepare partial size as 80-100nm: pass through
External temperature controlling instruments (can be air-conditioning) control environment temperature is 32 degree.The gadolinium chloride solution of high concentration is taken, pure water dilution is added
Compound concentration is the gadolinium chloride solution of 0.3mol/L, and the gadolinium chloride solution 91.95L that concentration is 0.3mol/L is then put into spacer
In reaction kettle, solution system temperature is room temperature in spacer, then weighs 500 grams of PEG 20000s with pure water and is dissolved into 2L's
Solution is added in above-mentioned spacer reaction kettle, and the sodium bicarbonate solution that concentration is 0.3mol/L is uniformly sprayed drop after stirring 30min
It adds in spacer reaction kettle, rate of addition 4L/min, continues to stir 30min after completion of dropwise addition, be then allowed to stand ageing 2 hours,
The mother liquor containing sediment is made.Temperature of reaction system in the above operation spacer reaction kettle is room temperature.
The preparation method of precipitating reagent are as follows: at room temperature, weigh sodium bicarbonate 6.95kg, pure water 275.85L stirring is added and prepares
It is 0.3mol/L sodium bicarbonate solution at concentration.The mother liquor obtained above containing sediment is filtered after ageing, so
95 DEG C or more of hot pure water washing is added afterwards.With each 500L washing, wash 5 times, total 2500L hot pure water filters washing
Environment temperature is maintained at 26-28 DEG C.Filter cake is placed 24 hours under conditions of 0-5 DEG C after filtering excessive moisture, is then placed in
Cart furnace calcination, calcination temperature are 800 DEG C, and soaking time is 1 hour.The nano oxidized gadolinium of gained is 200nm through SEM detection granularity
The above irregular particle, specific surface area 2.94m2/g。
Comparative example 3
The nano oxidized gadolinium powder that present embodiment uses following technical scheme to prepare partial size as 80-100nm: pass through
External temperature controlling instruments (can be air-conditioning) control environment temperature is 26 DEG C.The gadolinium chloride solution of high concentration is taken, pure water dilution is added
Be configured to concentration be 0.6mol/L gadolinium chloride solution, then by concentration be 0.6mol/L gadolinium chloride solution 45.98L be put into every
It covers in reaction kettle, it is 2 DEG C that solution system temperature in circulation ice water control spacer reaction kettle is passed through in spacer.Then 500 grams are weighed
PEG 20000 is added in above-mentioned spacer reaction kettle with the solution that pure water is dissolved into 2L, is by concentration after stirring 30min
0.8mol/L temperature is that 2 DEG C of sodium bicarbonate solution uniformly spray and is added dropwise in spacer reaction kettle, and rate of addition 4L/min drips
Continue to stir 30min after adding, be then allowed to stand ageing 2 hours, the mother liquor containing sediment is made.The above operation all keeps spacer
Temperature of reaction system in reaction kettle is 2 DEG C.
The preparation method of precipitating reagent are as follows: weigh sodium bicarbonate 6.95kg, addition pure water 103.42L is configured to concentration and is
0.8mol/L sodium bicarbonate solution.The mother liquor obtained above containing sediment is filtered after ageing, is then added
95 DEG C or more of hot pure water washing.With each 500L washing, wash 5 times, total 2500L hot pure water filters the environment temperature of washing
It is maintained at 26-28 DEG C.Filter cake is placed 24 hours under conditions of 0-5 DEG C after filtering excessive moisture, cart furnace is then placed in and burns
It burns, calcination temperature is 800 degree, and soaking time is 1 hour.The nano oxidized gadolinium of gained is 80-100nm through SEM detection granularity, compares table
Area 6.58m2/g。
Comparative example 4
The nano oxidized gadolinium powder that present embodiment uses following technical scheme to prepare partial size as 80-100nm: pass through
External temperature controlling instruments (can be air-conditioning) control environment temperature is 20 DEG C.The gadolinium chloride solution of high concentration is taken, pure water dilution is added
Compound concentration is the gadolinium chloride solution of 0.3mol/L, and the gadolinium chloride solution 91.95L that concentration is 0.3mol/L is then put into spacer
It is 0 DEG C that solution system temperature in circulation ice water control spacer reaction kettle is passed through in reaction kettle, in spacer.Then 500 grams are weighed to gather
The solution that ethylene glycol 20000 is dissolved into 2L is added in above-mentioned spacer reaction kettle, and stirring concentration after 30min is 0.3mol/L temperature
It uniformly sprays and is added dropwise in spacer reaction kettle for 2 DEG C of sodium bicarbonate solutions, rate of addition 4L/min continues after completion of dropwise addition
30min is stirred, ageing 2 hours is then allowed to stand, the mother liquor containing sediment is made.The above operation all keeps anti-in spacer reaction kettle
Answering system temperature is 0 DEG C.
The preparation method of precipitating reagent are as follows: weigh sodium bicarbonate 6.95kg, addition pure water 275.85L stirring is configured to concentration and is
0.3mol/L sodium bicarbonate solution.
The mother liquor obtained above containing sediment is filtered after ageing, it is pure then to add 95 DEG C or more of heat
Water washing.With each 500L washing, wash 5 times, total 2500L hot pure water, the environment temperature for filtering washing is maintained at 26-28 DEG C.
Filter cake is placed 24 hours under conditions of 0-5 DEG C after filtering excessive moisture, is then placed in cart furnace calcination, calcination temperature is
800 DEG C, soaking time is 1 hour.The nano oxidized gadolinium of gained is 60-80nm, specific surface area 11.53m through SEM detection granularity2/g.
Comparative example 5
The nano oxidized gadolinium powder that present embodiment uses following technical scheme to prepare partial size as 80-100nm: pass through
External temperature controlling instruments (can be air-conditioning) control environment temperature is 26 DEG C.The gadolinium chloride solution of high concentration is taken, pure water dilution is added
Compound concentration is the gadolinium chloride solution of 0.3mol/L, and the gadolinium chloride solution 91.95L that concentration is 0.3mol/L is then put into spacer
It is 2 DEG C that solution system temperature in circulation ice water control spacer reaction kettle is passed through in reaction kettle, in spacer.Then 500 grams are weighed to gather
Ethylene glycol 20000 is added in above-mentioned spacer reaction kettle with the solution that pure water is dissolved into 2L, is by concentration after stirring 30min
0.3mol/L temperature is that 2 DEG C of sodium bicarbonate solution uniformly spray and is added dropwise in spacer reaction kettle, and rate of addition 4L/min drips
Continue to stir 30min after adding, be then allowed to stand ageing 2 hours, the mother liquor containing sediment is made.The above operation all keeps spacer
Temperature of reaction system in reaction kettle is 2 DEG C.
The preparation method of precipitating reagent are as follows: weigh sodium bicarbonate 6.6.95kg, pure water 275.85L stirring is added and is configured to concentration
For 0.3mol/L sodium bicarbonate solution.
The mother liquor obtained above containing sediment is filtered after ageing, then adds the washing of room temperature pure water.
With each 500L washing, wash 5 times, total 2500L hot pure water, the environment temperature for filtering washing is maintained at 26-28 DEG C.It is extra to filter
Filter cake is placed 24 hours under conditions of 0-5 DEG C after moisture content, is then placed in cart furnace calcination, calcination temperature is 800 DEG C, heat preservation
Time is 1 hour.The nano oxidized gadolinium of gained is 100nm or more, specific surface area 4.08m through SEM detection granularity2/g。
Claims (5)
1. the preparation method that a kind of partial size is the nano oxidized gadolinium of 80-100nm；It is characterized by: the method includes following steps
It is rapid:
(1) the gadolinium chloride solution that addition is 0.1mol/L-0.6mol/L with the concentration that pure water is prepared in a kettle, then to it
The polyethylene glycol 10000 and/or PEG 20000 surfactant of the middle 10%-15% that gadolinium chloride quality is added, stirring is extremely
Evenly dispersed and sufficiently dissolve, adjustment system temperature is 0-5 DEG C；
Then, under conditions of maintenance system temperature is 0-5 DEG C, the speed into system with 3-6L/min, which drops evenly, uses pure water
The sodium bicarbonate precipitating reagent that the concentration of preparation is 0.1mol/L-0.6mol/L and temperature is 0-5 DEG C after completion of dropwise addition, continues to stir
0.5-1h is mixed, it is then still aging under conditions of 0-5 DEG C, the mother liquor containing sediment is made；
The environment temperature operated above maintains 26-28 DEG C；
(2) mother liquor containing sediment made from step (1) is subjected to suction filtration washing, the suction filtration water-washing method is to filter bucket
The multiple soaking and water washing of the middle hot pure water with 95 DEG C or more, the time impregnated every time wash after 15-20min, filter the ring of washing
Border temperature is maintained at 26-28 DEG C；Then the filter cake after washing will be filtered places 24 hours or more under conditions of 0-5 DEG C, then
Again at 800-850 DEG C after calcination 1-2h, the nano oxidized gadolinium that partial size is 80-100nm is obtained.
2. the preparation method that partial size according to claim 1 is the nano oxidized gadolinium of 80-100nm, it is characterised in that: step
(1) molar ratio of gadolinium chloride described in and sodium bicarbonate is 1:3-1:3.2.
3. the preparation method that partial size according to claim 2 is the nano oxidized gadolinium of 80-100nm, it is characterised in that: step
(1) system temperature in reaction kettle is controlled by circulation ice water.
4. the preparation method that partial size according to claim 1 is the nano oxidized gadolinium of 80-100nm, it is characterised in that: step
(1) in after precipitating reagent completion of dropwise addition, continuation mixing time is 0.5h, digestion time 2h.
5. the preparation method that grain according to claim 1 passes through the nano oxidized gadolinium for 80-100nm, it is characterised in that: step
(2) calcination described in is carried out in car-type rare earth roaster.
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| CN201811404108.1A CN109205655B (en) | 2018-11-23 | 2018-11-23 | Preparation method of nano gadolinium oxide with particle size of 80-100nm |
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| CN112010338A (en) * | 2020-07-27 | 2020-12-01 | 常州市卓群纳米新材料有限公司 | Method for preparing low-sodium nanometer ytterbium oxide with good monodispersity by sodium salt precipitation |
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