CN109019655A - A kind of preparation method of large-specific surface area nano luteium oxide - Google Patents
A kind of preparation method of large-specific surface area nano luteium oxide Download PDFInfo
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- CN109019655A CN109019655A CN201710430812.3A CN201710430812A CN109019655A CN 109019655 A CN109019655 A CN 109019655A CN 201710430812 A CN201710430812 A CN 201710430812A CN 109019655 A CN109019655 A CN 109019655A
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- preparation
- nano oxidized
- specific surface
- surface area
- oxidized lutetium
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2006/12—Surface area
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- Inorganic Chemistry (AREA)
- Luminescent Compositions (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of preparation methods of large-specific surface area nano luteium oxide, it is characterised in that: the luteium oxide partial size of this method preparation is greater than 30m in 30-50nm, specific surface area2/ g, gained luteium oxide impurity is less, and even particle size, specific surface is larger, and dispersibility is relatively good.
Description
The invention belongs to field of material preparation more particularly to a kind of preparation methods of large-specific surface area nano luteium oxide.
Background technique
Scintillation material is the material that can be absorbed high energy particle or ray and issue optical photon, high-energy physics, nuclear medicine,
The fields such as space physics, geological prospecting extensive application, it is desirable that its to ionising radiation have high blocking ability (have high density and
Thick atom ordinal number).Luteium oxide has high density and thick atom ordinal number, good to the prevention effect of all kinds of rays；It its valence band and leads
Interband band gap is wide (6.5eV), can accommodate many activator ions as luminescent material matrix, therefore as scintillator matrix
Material is favored by people.Therefore, luteium oxide is a kind of luminescent ceramic matrix of great application prospect, and whether luteium oxide base is saturating
The preparation of bright ceramic material or luteium oxide base fluorescent powder, high quality luteium oxide powder is all key link.Different powder synthesis
The product of method has different granule-morphology and specific surface area, determines the property of final material.
Current combustion method is difficult to control to be unfavorable for producing, and hydro-thermal method is because equipment requirement is higher and the fertile amount of institute is limited
System, and the reaction time is longer, is unfavorable for producing in enormous quantities.In addition workshop section needed for sol-gal process is also more, and the production time is longer,
And the impurity introduced is difficult to remove.And traditional precipitation method are most useful for mass production and a kind of lower-cost method.Before
The precipitation method of all luteium oxides all use ammonium hydrogen carbonate or ammonium hydroxide and urea etc. to precipitate, and at present because of environmental grounds, own
The precipitating reagent for being related to ammonium ion and Nitrogen ion must all be abandoned.In addition luteium oxide is provided needed for present market require specific surface
Product is higher, and required luteium oxide shows better performance.The nano oxidized lutetium specific surface area that ordinary precipitation process prepares all only has
5,6 or so, not only epigranular is in 30-50nm or so for the luteium oxide that is precipitated out of the present invention, and dispersibility is preferably, in addition compares
Surface area is greater than 30m2/g。
Summary of the invention
The present invention provide it is a kind of precipitated with sodium carbonate or sodium bicarbonate, and specific surface area is greater than 30 or more nano oxidized lutetium
Preparation method.
The technical solution for realizing the object of the invention is a kind of preparation method of large-specific surface area nano luteium oxide；Including following
Step: the lutecium nitrate that first addition is 0.3mol/L-0.5mol/L with the concentration that pure water is prepared in a kettle, then weigh and use pure water
The concentration of preparation is the analysis pure sodium bicarbonate or sodium carbonate of 0.3mol/L-0.6mol/L；It weighs and is computed precipitated luteium oxide
The PEG 20000 surfactant of mass ratio 5%-15% be added in lutecium nitrate and stir 15-30min, then drop evenly
Precipitating reagent, after dissolved lauryl sodium sulfate or neopelex 2%-5% are added dropwise again, quickly stir
After 30min keeps its surfactant and sediment uniform, it is aged 2h, filters washing, gained filter cake is dried through 135 degree after being filtered dry,
Then it is greater than 30m after calcination 3-5h heat preservation 1h under 800 degree up to partial size 30-50nm, specific surface area2The nano oxidized lutetium of/g.
The present invention has the effect of positive: (1) luteium oxide is a kind of luminescent ceramic matrix of great application prospect, this side
The product of method synthesis has preferable granule-morphology, even particle size, and dispersibility preferably, and specific surface area is larger, and gained
The impurity that the luteium oxide arrived introduces is less, and quality is high, and the purity of the luteium oxide material excited and brightness are higher.This method
Luteium oxide obtained, even particle size, specific surface is larger, and dispersibility is relatively good.
(2) addition PEG 20000 is growth and reunion in order to effectively inhibit crystal grain, to its uniformity have can not or
Scarce effect is the crux for determining granular size.Temperature mistake in addition, temperature and time when calcination is also critically important, when calcination
Height, calcination time and the too long size that can all influence specific surface area of soaking time.
(3) after the lauryl sodium sulfate of its addition and neopelex coat sediment, played the role of
It is to make sediment reunite to reduce, sediment volume increases, and the oxide of same volume is gently more many than the meeting not added after calcination.Through examining
The specific surface area for measuring the oxide come is larger.
(4) Detailed description of the invention
In order that the present invention can be more clearly and readily understood, below according to specific embodiment and in conjunction with attached drawing, to this hair
Bright to be described in further detail, Fig. 1 and Fig. 2 are that transmission electron microscope TEM detects grain-size graph.
Specific embodiment:
Embodiment 1: precipitating the luteium oxide of 5KG, and being computed addition in a kettle and being configured to concentration with pure water is 0.4mol/L, body
Product is the lutecium nitrate of 62.85L, is 17 degree through measurement temperature, then weighs the pure sodium carbonate 4.26KG of analysis, is configured to concentration with pure water
For 0.4mol/L, volume 100.56L, temperature is 15 degree, weighs the PEG-20000 surface-active of the mass ratio 5% of oxide
250 grams of agent, 2.5L pure water is added, heating is allowed to be dissolved into liquid, PEG-20000 is put into lutecium nitrate, 15min is mixed,
Sodium carbonate is then dropped evenly, time for adding 45min, thus can calculate rate of addition is 2.23L/min, passes through governor
Flow and rate of addition are controlled, after dripping, 100 grams of lauryl sodium sulfate of 2% are added, is put into 1L pure water heating for dissolving,
It is added into the above slurry, quickly stirring 0.5 hour, is aged 2 hours, with 95 degree or more of hot pure water soaking water in filtering bucket
It washes, washes about 2500L, finally filter to doing, contained with earthen bowl, keep the temperature totally 4 hours in 850 degree of calcinations.Through detection gained oxygen
The specific surface area for changing lutetium is 32.
Embodiment 2: precipitating the luteium oxide of 10KG, is computed addition in a kettle and is configured to concentration with pure water and is
0.5mol/L, volume are the lutecium nitrate of 100.55L, are 25 degree through measurement temperature, then weigh analysis pure sodium bicarbonate 13.51KG,
Being configured to concentration with pure water is 0.6mol/L, and volume 268.14L, temperature is 22 degree, weighs the mass ratio 15% of oxide
1500 grams of PEG-20000 surfactant, 15L pure water is added, heating is allowed to be dissolved into liquid, and PEG-20000 is put into nitric acid
30min is mixed in lutetium, then drops evenly sodium bicarbonate, time for adding 65min, thus can calculate rate of addition is
4.13L/min controls flow and rate of addition by governor, and after dripping, 5% neopelex 500 is added
Gram, it is put into 5L pure water heating for dissolving, is added into the above slurry, quickly stirring 0.5 hour, is aged 2 hours, is used in filtering bucket
95 degree or more of hot pure water soaking and water washing washes about 5000L, finally filters to doing, is contained with earthen bowl, is protected in 800 degree of calcinations
Temperature totally 4 hours.Specific surface area through detection gained luteium oxide is 41.
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects
It describes in detail bright, it should be understood that the above is only a specific embodiment of the present invention, is not intended to restrict the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in guarantor of the invention
Within the scope of shield.
Claims (10)
1. a kind of preparation method of large-specific surface area nano luteium oxide, it is characterised in that include the following steps:
(A) lutecium nitrate solution is configured with pure water at 15-25 DEG C；
(B) surfactant is added in lutecium nitrate solution, stirs evenly；
(C) precipitating reagent is dropped evenly in above-mentioned lutecium nitrate solution, is continued that anionic additive is added dropwise after completion of dropwise addition, is uniformly stirred
It mixes, is aged after obtaining sediment；
(D) sediment obtains filter cake through suction filtration, washing, drying；
(E) to calcination is carried out after the drying of above-mentioned filter cake, product is nano oxidized lutetium.
2. the preparation method of nano oxidized lutetium according to claim 1, it is characterised in that: lutecium nitrate solution concentration is
0.3mol/L-0.5mol/L。
3. the preparation method of nano oxidized lutetium according to claim 1, it is characterised in that: the surface being added in step (B)
Activating agent is PEG 20000.
4. the preparation method of nano oxidized lutetium according to claim 1, it is characterised in that: the yin being added in step (C) from
Sub- additive is neopelex or lauryl sodium sulfate.
5. the preparation method of nano oxidized lutetium according to claim 1, it is characterised in that: precipitating reagent described in step (C)
It is sodium carbonate or sodium bicarbonate.
6. the preparation method of nano oxidized lutetium according to claim 4, it is characterised in that: in step (C) lutecium nitrate with point
The molar ratio for analysing pure sodium bicarbonate is 1:3-1:3.5；Lutecium nitrate and the molar ratio for analyzing pure sodium carbonate are 1:1.5-1:1.6.
7. the preparation method of nano oxidized lutetium according to claim 1, it is characterised in that: surfactant polyethylene
20000 by precipitating luteium oxide quality 5%-15%, dissolve by heating in pure water, mass concentration 10%.
8. the preparation method of nano oxidized lutetium according to claim 1, it is characterised in that: uniformly dripped described in step (C)
Adding precipitating reagent is controlled by governor, and duration 0.5h is stirred, and is aged duration 2h.
9. the preparation method of nano oxidized lutetium according to claim 1, it is characterised in that: filter water described in step (D)
Washing is in filtering bucket with 95 degree or more of hot pure water soaking and water washing, and the washing pure water amount and the mass ratio of obtained object when washing are
500:1;Filter cake is dried through 135 degree.
10. the preparation method of nano oxidized lutetium according to claim 1, it is characterised in that: filter cake is in 800- in step (E)
850 degree of lower calcination 3-5h keep the temperature 1h to get partial size 30-50nm, specific surface area and are greater than 30m2The nano oxidized lutetium of/g.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110104682A (en) * | 2019-05-29 | 2019-08-09 | 常州市卓群纳米新材料有限公司 | A kind of nano zirconium dioxide of high-specific surface area and preparation method thereof |
| CN110615461A (en) * | 2019-10-29 | 2019-12-27 | 常州市卓群纳米新材料有限公司 | A BET: ammonia-free environment-friendly preparation method of 20-30 uniformly dispersed nano samarium oxide |
| 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 |
| CN112479243A (en) * | 2020-12-17 | 2021-03-12 | 常州市卓群纳米新材料有限公司 | Method for preparing lutetium oxide with large specific surface area by secondary dispersion of nano lutetium oxide |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130059153A1 (en) * | 2011-09-02 | 2013-03-07 | The Government Of The United States Of America, As Represented By The Secretary Of The Navy | FLAME SPRAY SYNTHESIS OF Lu2O3 NANOPARTICLES |
| CN105084407A (en) * | 2014-05-22 | 2015-11-25 | 常州市卓群纳米新材料有限公司 | Ultrafine lanthanum oxide and preparation method thereof |
| CN105502467A (en) * | 2014-09-22 | 2016-04-20 | 常州市卓群纳米新材料有限公司 | Nanometer dysprosium oxide preparation method |
| CN106277021A (en) * | 2015-06-12 | 2017-01-04 | 常州卓煜新材料科技有限公司 | A kind of large-specific surface area nano Dineodymium trioxide preparation method |
| CN106830047A (en) * | 2015-12-04 | 2017-06-13 | 常州市卓群纳米新材料有限公司 | A kind of nano oxidized holmium preparation method |
-
2017
- 2017-06-09 CN CN201710430812.3A patent/CN109019655A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130059153A1 (en) * | 2011-09-02 | 2013-03-07 | The Government Of The United States Of America, As Represented By The Secretary Of The Navy | FLAME SPRAY SYNTHESIS OF Lu2O3 NANOPARTICLES |
| CN105084407A (en) * | 2014-05-22 | 2015-11-25 | 常州市卓群纳米新材料有限公司 | Ultrafine lanthanum oxide and preparation method thereof |
| CN105502467A (en) * | 2014-09-22 | 2016-04-20 | 常州市卓群纳米新材料有限公司 | Nanometer dysprosium oxide preparation method |
| CN106277021A (en) * | 2015-06-12 | 2017-01-04 | 常州卓煜新材料科技有限公司 | A kind of large-specific surface area nano Dineodymium trioxide preparation method |
| CN106830047A (en) * | 2015-12-04 | 2017-06-13 | 常州市卓群纳米新材料有限公司 | A kind of nano oxidized holmium preparation method |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110104682A (en) * | 2019-05-29 | 2019-08-09 | 常州市卓群纳米新材料有限公司 | A kind of nano zirconium dioxide of high-specific surface area and preparation method thereof |
| CN110615461A (en) * | 2019-10-29 | 2019-12-27 | 常州市卓群纳米新材料有限公司 | A BET: ammonia-free environment-friendly preparation method of 20-30 uniformly dispersed nano samarium oxide |
| CN110615461B (en) * | 2019-10-29 | 2022-05-03 | 常州市卓群纳米新材料有限公司 | A BET: ammonia-free environment-friendly preparation method of 20-30 uniformly dispersed nano samarium oxide |
| 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 |
| CN112010338B (en) * | 2020-07-27 | 2023-10-31 | 常州市卓群纳米新材料有限公司 | Method for preparing monodisperse low-sodium nanometer ytterbium oxide by sodium salt precipitation |
| CN112479243A (en) * | 2020-12-17 | 2021-03-12 | 常州市卓群纳米新材料有限公司 | Method for preparing lutetium oxide with large specific surface area by secondary dispersion of nano lutetium oxide |
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Application publication date: 20181218 |