CN106882813A - A kind of utilization inorganic raw material synthesizes the method for nano hydrated silicon metal sodium titanate - Google Patents
A kind of utilization inorganic raw material synthesizes the method for nano hydrated silicon metal sodium titanate Download PDFInfo
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- CN106882813A CN106882813A CN201710086483.5A CN201710086483A CN106882813A CN 106882813 A CN106882813 A CN 106882813A CN 201710086483 A CN201710086483 A CN 201710086483A CN 106882813 A CN106882813 A CN 106882813A
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- 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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/38—Particle morphology extending in three dimensions cube-like
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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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
Abstract
The invention discloses a kind of method that utilization inorganic raw material synthesizes nano hydrated silicon metal sodium titanate.It is with Na2Si2O3·9H2O and NaOH is silicon source, with TiCl4Ethanol solution be titanium source, the nanometer CST crystal without dephasign is successfully prepared using collosol and gel hydrothermal synthesis method, solve CST and prepare the problem containing dephasign, and operating cost is low, preparation process is simple.
Description
Technical field
Radioactive waste recycling treatment the present invention relates to be subordinated to field of environment protection, is related to one kind effectively to locate
Manage the synthetic method of the functional material of the radioactive wastewater of strontium containing caesium, and in particular to a kind of nano hydrated silicon metal sodium titanate(CST)
Synthetic method.
Background technology
With the fast development of nuclear power, people are increasingly paid close attention to nuclear waste safe handling disposal.In high activity liquid waste90Sr
(T1/2=28.79 years, 100% β decays, Eβ=546 keV)With137Cs(T1/2=30.02 years, 100% β decays, association gamma-rays
ENERGY Eγ=661 keV)It is the heat release fission product high of long half-lift, removal contains137Cs+/90Sr2+It is high level liquid waste processing disposal
One of key of technical research.At present, contain137Cs+/90Sr2+The method of radioactive liquid waste safe disposal mainly has precipitation, film point
From, extraction, ion exchange, evaporation etc..Ion-exchange is to realize that radioactive nucleus waste liquid pre-processes the best way.With it is organic from
Sub- exchanger is compared, the good anti-radiation performance of inorganic ion exchanger, chemical stability, heat endurance and mechanical stability,
With exchanging with irreversibility for radionuclide ion, to Na+There is high selectivity Deng competing ions, can industrialization and cost
It is controllable, it is widely used in the treatment of radioactive nucleus waste liquid.It is right137Cs+/90Sr2+For, conventional inorganic ion exchanger mainly has
Clay, zeolite, ammonium phosphomolybdate (ammonium molybdophosphate, AMP), cobalt hexacyanoferrate potassium (potassium
Cobalt hexacyanoferrete, KCoCF), and crystalline hydrate silicon sodium titanate (Crystalline
Sillicotitanate, CST) etc..CST has extremely strong chemical stability, heat endurance and irradiation stability, and to Cs+/Sr2+It is that ion-exchange treatment contains Cs with high selectivity+/Sr2+Radioactive wastewater most it is competitive it is inorganic from
Sub- exchanger.
Although general-purpose oil product company of the U.S.(UOP)CST has been commercially produced in nineteen ninety-five and in global several laboratories
Carry out obtaining immense success except caesium test in high activity liquid waste, but the mesh such as specific synthesis technique, the composition structure of material about CST
Before still fall within American National secret, the rare report of periodical literature.The synthesis of current CST is general with organic silicon source(Such as orthosilicic acid four
Ethyl ester, ethanol silicon etc.)And organic titanium source(Such as isopropyl titanate)Sol-gel is initially formed, then CST is prepared with hydro-thermal method.Use
Organic silicon source/titanium source high cost, environmental problem is seriously polluted, and contains dephasign using the CST samples obtained by the preparation of this method.Therefore
The research tendency of the technology should how prepare the CST pure materials without dephasign using green material, so as to more efficiently
Treatment contains Cs+/Sr2+Radioactive nucleus waste liquid.
The content of the invention
To solve the above problems, the invention provides a kind of method for synthesizing nanometer CST.The method is with Na2Si2O3·
9H2O and NaOH is silicon source, with TiCl4Ethanol solution be titanium source, successfully prepared not using collosol and gel-hydrothermal synthesis method
Nanometer CST crystal containing dephasign, solves CST and prepares the problem containing dephasign.
To achieve these goals, the technical scheme taken of the present invention is:
A kind of utilization inorganic raw material synthesizes the method for nano hydrated silicon metal sodium titanate, and silicon source and titanium source, bag are prepared with inorganic matter
Preparation silicon source, tri- processes of titanium source and CST are included, is comprised the following steps that:
S1, weigh appropriate Na2Si2O3·9H2O solids and NaOH solids, in being dissolved in ultra-pure water under room temperature and magnetic agitation,
Certain density silicon liquid is obtained, as the silicon source for preparing CST;
S2, by appropriate TiCl4Solution is slowly dropped in absolute ethyl alcohol under magnetic stirring, obtains certain density homogeneous transparent
Yellow solution, i.e. TiCl4Ethanol solution, as the titanium source for preparing CST;
S3, under magnetic stirring, by Si:Ti=0.98:1(The ratio between amount of material)Ratio, the yellow solution that will be obtained in S2 delays
Slowly it is added in the silicon liquid that S1 is prepared, obtains uniform sol-gel, and adjust pH to 12.5 ~ 12.7;
S4, the collosol and gel that will be prepared are placed in the autoclave that interior village is polytetrafluoroethylene (PTFE), baking oven are put into, in constant temperature
After spending lower crystallization for a period of time, removal of impurity Na is removed in the product filtering that will be obtained+, and extremely filtered with ultra-pure water and absolute ethanol washing
The pH value of liquid is about 8 ~ 9, and the product of washing is placed in dries a period of time in baking oven, obtain CST white crystals.
In above-mentioned S2 steps, TiCl4Ethanol solution mass concentration be 0.346g/ml.
The present invention synthesis CST there is extremely strong chemical stability, heat endurance and irradiation stability, can as it is inorganic from
Sub- exchanger, treatment contains Cs+/Sr2+Radioactive wastewater.
Compared with prior art, the invention has the advantages that:
The synthesis of current CST generally uses organic silicon source/titanium source, high cost, and environmental pollution is serious.The present invention uses low cost
Inorganic silicon source/the titanium source of safety non-pollution(Na2Si2O3·9H2O and NaOH/TiCl4Ethanol solution), using sol-gel water
Thermal synthesis method successfully prepares CST white powder crystal.Through X-ray diffractometer(XRD, X-ray diffraction), sweep
Retouch electron microscope(SEM, Scanning electron microscope), transmission electron microscope(TEM,
Transmission electron microscope)Deng analysis means of testing analysis, the CST prepared by the present invention is pure thing
Matter, without any impurity, and particle diameter is up to nanoscale, and this is at home and abroad there is not yet research.The present invention successfully solves CST preparations
Problem containing dephasign, this achievement helps speed up the development of CST functional materials, is it containing Cs+/Sr2+Radioactive nucleus give up
Application in liquid treatment disposal is laid a good foundation.
Brief description of the drawings
Fig. 1 is the preparation flow of the method that a kind of utilization inorganic raw material of the invention synthesizes nano hydrated silicon metal sodium titanate
Figure.
Fig. 2 is to have synthesized the X-ray diffraction of CST in embodiment 2(XRD)Figure.
Fig. 3 is to have synthesized the SEM of CST in embodiment 2(SEM)Figure.
Fig. 4 is to have synthesized the transmission electron microscope of CST in embodiment 2(TEM)Figure.
Specific embodiment
Example given below is intended so that the invention will be further described, but is not to be construed as to present invention protection model
The limitation enclosed, person skilled in art according to the content of the invention described above is made to the present invention some nonessential improvement and
Adjustment, still falls within protection scope of the present invention.
Synthesize preparation flow such as Fig. 1 institutes of nano hydrated silicon metal sodium titanate in following each embodiments using inorganic raw material
Show.
Embodiment 1:
25.3571g Na are weighed first2Si2O3·9H2O solids and 9g NaOH solids, are dissolved in super under room temperature and magnetic agitation
In pure water, 500mL solution is configured to, obtains the silicon liquid that silicon concentration is 5g/L.Then under magnetic stirring, in fume hood, will
5mL TiCl4Solution is slowly dropped in 20mL absolute ethyl alcohols, obtains the yellow solution of homogeneous transparent, i.e. TiCl4-CH3CH2OH。
The silicon liquid 50mL that prior process is obtained is taken again, is added in the pressure vessel being made up of polytetrafluoroethylene (PTFE), take TiCl4-CH3CH2OH
5mL.By TiCl4-CH3CH2OH is added in silicon liquid, and stirring is not stopped, obtains uniform sol-gel, and adjust pH to 12.5 ~
12.7.The pressure vessel is put into autoclave again, good seal, places into the baking oven that temperature is 170 DEG C and heat 7 days.7
After it, removal of impurity Na is removed in the white solid that taking-up is obtained, filtering+, and with the pH value of ultra-pure water and absolute ethanol washing to filtrate
About 8 ~ 9.The product of washing is placed in dries a period of time in baking oven, obtain CST white powder crystal.Gained CST crystal is not for
Pure material containing any dephasign.
Embodiment 2:
30.4285g Na are weighed first2Si2O3·9H2O solids and 9g NaOH solids, are dissolved in super under room temperature and magnetic agitation
In pure water, 500mL solution is configured to, obtains the silicon liquid that silicon concentration is 6g/L.Then under magnetic stirring, in fume hood, will
5mL TiCl4Solution is slowly dropped in 20mL absolute ethyl alcohols, obtains the yellow solution of homogeneous transparent, i.e. TiCl4-CH3CH2OH。
The silicon liquid 50mL that prior process is obtained is taken again, is added in the pressure vessel being made up of polytetrafluoroethylene (PTFE), take TiCl4-CH3CH2OH
6mL.By TiCl4-CH3CH2OH is added in silicon liquid, and stirring is not stopped, obtains uniform sol-gel, and adjust pH to 12.5 ~
12.7.The pressure vessel is put into autoclave again, good seal, places into the baking oven that temperature is 170 DEG C and heat 7 days.7
After it, removal of impurity Na is removed in the white solid that taking-up is obtained, filtering+, and with the pH value of ultra-pure water and absolute ethanol washing to filtrate
About 8 ~ 9.The product of washing is placed in dries a period of time in baking oven, obtain CST white powder crystal.Gained CST crystal is not for
Pure material containing any dephasign.
Fig. 2 is the X-ray diffraction for having synthesized CST in this(XRD)Figure, as can be seen from the figure baseline is shallower, does not have
Any amorphous characteristic, shows that the CST crystal is synthesized well.Fig. 3 is its SEM(SEM)Figure, from
Can be seen that the material of preparation is fully crystallized in figure, particle is minimum, in square, show that the CST crystal can be to accomplish nanometer
Level.Fig. 4 is its transmission electron microscope(TEM)Figure, the crystal is in layered laminate as can be seen from Figure, and its cross section is four directions
Type.
Embodiment 3:
35.4999g Na are weighed first2Si2O3·9H2O solids and 9g NaOH solids, are dissolved in super under room temperature and magnetic agitation
In pure water, 500mL solution is configured to, obtains the silicon liquid that silicon concentration is 7g/L.Then under magnetic stirring, in fume hood, will
5mL TiCl4Solution is slowly dropped in 20mL absolute ethyl alcohols, obtains the yellow solution of homogeneous transparent, i.e. TiCl4-CH3CH2OH。
The silicon liquid 50mL that prior process is obtained is taken again, is added in the pressure vessel being made up of polytetrafluoroethylene (PTFE), take TiCl4-CH3CH2OH
7mL.By TiCl4-CH3CH2OH is added in silicon liquid, and stirring is not stopped, obtains uniform sol-gel, and adjust pH to 12.5 ~
12.7.The pressure vessel is put into autoclave again, good seal, places into the baking oven that temperature is 170 DEG C and heat 7 days.7
After it, removal of impurity Na is removed in the white solid that taking-up is obtained, filtering+, and with the pH value of ultra-pure water and absolute ethanol washing to filtrate
About 8 ~ 9.The product of washing is placed in dries a period of time in baking oven, obtain CST white powder crystal.Gained CST crystal is not for
Pure material containing any dephasign.
Embodiment 4:
25.3571g Na are weighed first2Si2O3·9H2O solids and 9g NaOH solids, are dissolved in super under room temperature and magnetic agitation
In pure water, 500mL solution is configured to, obtains the silicon liquid that silicon concentration is 5g/L.Then under magnetic stirring, in fume hood, will
5mL TiCl4Solution is slowly dropped in 20mL absolute ethyl alcohols, obtains the yellow solution of homogeneous transparent, i.e. TiCl4-CH3CH2OH。
The silicon liquid 50mL that prior process is obtained is taken again, is added in the pressure vessel being made up of polytetrafluoroethylene (PTFE), take TiCl4-CH3CH2OH
5mL.By TiCl4-CH3CH2OH is added in silicon liquid, and stirring is not stopped, obtains uniform sol-gel, and adjust pH to 12.5 ~
12.7.The pressure vessel is put into autoclave again, good seal, places into the baking oven that temperature is 180 DEG C and heat 7 days.7
After it, removal of impurity Na is removed in the white solid that taking-up is obtained, filtering+, and with the pH value of ultra-pure water and absolute ethanol washing to filtrate
About 8 ~ 9.The product of washing is placed in dries a period of time in baking oven, obtain CST white powder crystal.Gained CST crystal is not for
Pure material containing any dephasign.
Embodiment 5:
25.3571g Na are weighed first2Si2O3·9H2O solids and 9g NaOH solids, are dissolved in super under room temperature and magnetic agitation
In pure water, 500mL solution is configured to, obtains the silicon liquid that silicon concentration is 5g/L.Then under magnetic stirring, in fume hood, will
5mL TiCl4Solution is slowly dropped in 20mL absolute ethyl alcohols, obtains the yellow solution of homogeneous transparent, i.e. TiCl4-CH3CH2OH。
The silicon liquid 50mL that prior process is obtained is taken again, is added in the pressure vessel being made up of polytetrafluoroethylene (PTFE), take TiCl4-CH3CH2OH
5mL.By TiCl4-CH3CH2OH is added in silicon liquid, and stirring is not stopped, obtains uniform sol-gel, and adjust pH to 12.5 ~
12.7.The pressure vessel is put into autoclave again, good seal, places into the baking oven that temperature is 190 DEG C and heat 7 days.7
After it, removal of impurity Na is removed in the white solid that taking-up is obtained, filtering+, and with the pH value of ultra-pure water and absolute ethanol washing to filtrate
About 8 ~ 9.The product of washing is placed in dries a period of time in baking oven, obtain CST white powder crystal.Gained CST crystal is not for
Pure material containing any dephasign.
Embodiment 6:
25.3571g Na are weighed first2Si2O3·9H2O solids and 9g NaOH solids, are dissolved in super under room temperature and magnetic agitation
In pure water, 500mL solution is configured to, obtains the silicon liquid that silicon concentration is 5g/L.Then under magnetic stirring, in fume hood, will
5mL TiCl4Solution is slowly dropped in 20mL absolute ethyl alcohols, obtains the yellow solution of homogeneous transparent, i.e. TiCl4-CH3CH2OH。
The silicon liquid 50mL that prior process is obtained is taken again, is added in the pressure vessel being made up of polytetrafluoroethylene (PTFE), take TiCl4-CH3CH2OH
5mL.By TiCl4-CH3CH2OH is added in silicon liquid, and stirring is not stopped, obtains uniform sol-gel, and adjust pH to 12.5 ~
12.7.The pressure vessel is put into autoclave again, good seal, places into the baking oven that temperature is 200 DEG C and heat 7 days.7
After it, removal of impurity Na is removed in the white solid that taking-up is obtained, filtering+, and with the pH value of ultra-pure water and absolute ethanol washing to filtrate
About 8 ~ 9.The product of washing is placed in dries a period of time in baking oven, obtain CST white powder crystal.Gained CST crystal is not for
Pure material containing any dephasign.
Embodiment 7:
25.3571g Na are weighed first2Si2O3·9H2O solids and 9g NaOH solids, are dissolved in super under room temperature and magnetic agitation
In pure water, 500mL solution is configured to, obtains the silicon liquid that silicon concentration is 5g/L.Then under magnetic stirring, in fume hood, will
5mL TiCl4Solution is slowly dropped in 20mL absolute ethyl alcohols, obtains the yellow solution of homogeneous transparent, i.e. TiCl4-CH3CH2OH。
The silicon liquid 50mL that prior process is obtained is taken again, is added in the pressure vessel being made up of polytetrafluoroethylene (PTFE), take TiCl4-CH3CH2OH
5mL.By TiCl4-CH3CH2OH is added in silicon liquid, and stirring is not stopped, obtains uniform sol-gel, and adjust pH to 12.5 ~
12.7.The pressure vessel is put into autoclave again, good seal, places into the baking oven that temperature is 210 DEG C and heat 7 days.7
After it, removal of impurity Na is removed in the white solid that taking-up is obtained, filtering+, and with the pH value of ultra-pure water and absolute ethanol washing to filtrate
About 8 ~ 9.The product of washing is placed in dries a period of time in baking oven, obtain CST white powder crystal.Gained CST crystal is not for
Pure material containing any dephasign.
Claims (4)
1. a kind of method that utilization inorganic raw material synthesizes nano hydrated silicon metal sodium titanate, it is characterised in that comprise the following steps that:
S1, by Na2Si2O3·9H2O solids and NaOH solids, in being dissolved in ultra-pure water under room temperature and magnetic agitation, as preparation
The silicon source of CST;
S2, by TiCl4Solution is slowly dropped in absolute ethyl alcohol under magnetic stirring, used as the titanium source for preparing CST;
S3, under magnetic stirring, by the ratio between the amount Si of material:Ti=0.98:1 ratio, the solution that will be obtained in S2 is slowly added to
To in the silicon source described in S1, uniform sol-gel is obtained, and adjust pH value;
S4, the sol-gel that will be prepared at a constant temperature crystallization for a period of time after, products therefrom filtering, remove removal of impurity Na+,
And wash, dry, obtain CST white crystals.
2. the method that utilization inorganic raw material according to claim 1 synthesizes nano hydrated silicon metal sodium titanate, its feature exists
In, in S2 steps, TiCl4Ethanol solution mass concentration be 0.346g/ml.
3. the method that utilization inorganic raw material according to claim 1 synthesizes nano hydrated silicon metal sodium titanate, its feature exists
In, in S3 steps, regulation pH value to 12.5 ~ 12.7.
4. the method that utilization inorganic raw material according to claim 1 synthesizes nano hydrated silicon metal sodium titanate, its feature exists
In in S4 steps, it is 8 ~ 9 to use ultra-pure water and absolute ethanol washing to filtrate pH value;Crystallization temperature is 170 DEG C ~ 210 DEG C, is done
Dry temperature is 60 ± 10 DEG C.
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Cited By (2)
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CN108622901A (en) * | 2018-04-28 | 2018-10-09 | 哈尔滨工程大学 | A kind of preparation method of morphology controllable oxygen murmanite nano material |
CN114047274A (en) * | 2021-09-22 | 2022-02-15 | 四川轻化工大学 | Separation and extraction system for nuclides in radioactive sample |
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CN102092725A (en) * | 2010-12-01 | 2011-06-15 | 西南科技大学 | Method for producing hydrate crystal silicon sodium titanate from waste strontium-barium glass |
CN102976311A (en) * | 2012-12-24 | 2013-03-20 | 武汉大学 | Two-dimensional lamellae carbon nano fluorescent material |
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2017
- 2017-02-17 CN CN201710086483.5A patent/CN106882813A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102092725A (en) * | 2010-12-01 | 2011-06-15 | 西南科技大学 | Method for producing hydrate crystal silicon sodium titanate from waste strontium-barium glass |
CN102976311A (en) * | 2012-12-24 | 2013-03-20 | 武汉大学 | Two-dimensional lamellae carbon nano fluorescent material |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108622901A (en) * | 2018-04-28 | 2018-10-09 | 哈尔滨工程大学 | A kind of preparation method of morphology controllable oxygen murmanite nano material |
CN114047274A (en) * | 2021-09-22 | 2022-02-15 | 四川轻化工大学 | Separation and extraction system for nuclides in radioactive sample |
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