CN105776875B - One kind mixes cobalt glass microballoon and its preparation method and application - Google Patents
One kind mixes cobalt glass microballoon and its preparation method and application Download PDFInfo
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- CN105776875B CN105776875B CN201610184565.9A CN201610184565A CN105776875B CN 105776875 B CN105776875 B CN 105776875B CN 201610184565 A CN201610184565 A CN 201610184565A CN 105776875 B CN105776875 B CN 105776875B
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- Prior art keywords
- cobalt
- glass microballoon
- mixing
- xerogel
- cobalt glass
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
- C01B3/0084—Solid storage mediums characterised by their shape, e.g. pellets, sintered shaped bodies, sheets, porous compacts, spongy metals, hollow particles, solids with cavities, layered solids
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/02—Compositions for glass with special properties for coloured glass
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
Abstract
The present invention provides one kind to mix cobalt glass microballoon and its preparation method and application.The present invention mix cobalt glass microballoon and preparation method thereof can produce with it is photic release hydrogen effect mix cobalt glass microballoon, component is the alkali borosilicate glass containing cobalt oxide.The preparation method of the present invention is dry gel method.Cobalt glass microballoon is mixed by mixing cobalt xerogel particles and being formed in vertical high level cadre's gel furnace by processes such as heat absorption, encapsulation, foaming, refining, coolings, dry gel method has many advantages, such as easy to operate, yield and high yield rate.The present invention's mixes cobalt glass microballoon and can absorb visible ray, the express passway of gas molecule is formed after illumination at room temperature, so as to fulfill the controlled release of hydrogen in ball.This, which mixes cobalt glass microballoon, can be subjected to the loading and release of multiple gas, be a kind of high power capacity, hydrogen storage material efficiently, economic, safe, have good application prospect in hydrogen energy source stores and transports.
Description
Technical field
The invention belongs to hydrogen energy source storage arts, and in particular to one kind mixes cobalt glass microballoon and its preparation method and application.
Background technology
Hydrogen Energy is a kind of green, regenerative resource, important role will be played the part of in the energy resource supply of human future.Hydrogen Energy
One of the problem to be solved that efficiently uses be to establish a kind of suitable supply-conveying-storage-consumption system.It establishes a kind of
High weight ratio and volume ratio and safe hydrogen storage system are an important links.The storage of hydrogen should meet：(1) it is high
Energy density, (2) safety, low energy consumption and controllable for the loading and release of (3) gas,（4）Repeated loading and release are amenable to,
(5) it is inexpensive.
Glass microsphere is that a kind of have very much should because having many advantages, such as that efficient, safe, light, economical, convenient, compressive resistance is high
With the hydrogen storage vessel of prospect.Draw ratio（The ratio between diameter and wall thickness）For 50 ~ 200 glass microsphere, the weight efficiency height of hydrogen storage
Up to 14 wt.% ~ 21wt.%, the blowing pressure is up to 62.1MPa ~ 150MPa.Hydrogen storage is existed based on hydrogen in glass microsphere at present
Infiltration rate and temperature in glass microsphere spherical shell is closely related.In high temperature（300°C~400°C）Under, hydrogen is in glass microsphere ball
Infiltration rate in shell greatly increases, thus hydrogen can spread the spherical shell for penetrating glass microsphere quickly.At room temperature, infiltration speed
Rate reduces the several orders of magnitude, thus hydrogen is limited in glass microsphere, until glass microsphere is reheated to certain temperature,
Hydrogen is just released.This traditional inflation and delivery mode under high-temperature and high-pressure conditions because carrying out, and pressure is room temperature in ball
Under more than twice, glass microsphere is made to be in larger tension state, thus the compressive resistance of glass microsphere is required it is big, also can shadow
Ring the service life of glass microsphere.In addition, traditional thermal diffusion method danger is larger, energy consumption is higher.
At present, preparing the main method of glass microsphere has flame method, sessile drop method, Hoppe methods and dry gel method etc..Flame method
Balling-up efficiency is low, and ball-formation quality is poor, thus compressive resistance is not high.And sessile drop method needs glass forming substance to be dissolved in water that this is severe
The range of choice that requirement limits glass ingredient is carved, so as to limit the promotion of glass microsphere multiple performance.Although Hoppe methods exist
Introducing portion doped chemical, the inflation of macromolecular gaseous diffusion process etc. have advantage, but the sintering process of the method is micro- to glass
The refinement of ball is insufficient, and the compressive resistance of gained glass microsphere is not as good as sessile drop method and dry gel method.In addition, the work of this method
Skill poor controllability, yield and yield rate are very low, and the technical difficulty of research and development is big, of high cost, the period is long.It is micro- that dry gel method prepares glass
Ball not only simple, yield and high yield rate, can significantly expand the diameter and wall thickness of glass microsphere, and eliminate other methods pair
The limitation of glass ingredient selection can introduce doping of a variety of required elements realizations to glass microsphere, specific so as to assign it
Function improves its performance.
It mixes in the shell of cobalt glass microballoon containing specific functionality ion, inside and outside connection can be formed under illumination condition
Gas diffusion paths, realize the controllable quick release of hydrogen at room temperature, which is known as " photic to release hydrogen " effect.Photic hydrogen of releasing is kept away
Exempted from traditional gas diffusion there are the problem of.It is efficient with balling-up that cobalt glass microballoon is mixed obtained by dry gel method, sphericity is high,
The advantages that performances such as diameter, wall thickness and compressive resistance, gas retaining are adjustable.At present, being prepared using dry gel method has photic release
There is not been reported for the cobalt glass microballoon of mixing of hydrogen effect.
Invention content
The invention solves a technical problem be to provide one kind and mix cobalt glass microballoon, the invention solves another
Technical problem is to provide a kind of preparation method for mixing cobalt glass microballoon, the invention solves another technical problem be to provide one
Kind mixes the application of cobalt glass microballoon.
The present invention's mixes cobalt glass microballoon, its main feature is that, the component for mixing cobalt glass microballoon is as follows：
SiO2 ：Mass percent is 65.1% ~ 68.8%；
B2O3：Mass percent is 15.6% ~ 16.5%；
CoO：Mass percent is 0.2% ~ 5.5%；
Li2O：Mass percent is 6.5% ~ 6.9%；
Na2O：Mass percent is 5.9% ~ 6.2%；
K2O：Mass percent is 0.5%；
Al 2O3：Mass percent is 0.9%；
The sum of said components are 100%.
The preparation method for mixing cobalt glass microballoon of the present invention, includes the following steps：
A. it is 2 hours dry at 100 °C that cobalt xerogel block will be mixed；
B. the cobalt xerogel block of mixing in step a is poured into the agate mortar of vibrating screen and is ground, the amplitude of vibrating screen
For 1.1mm ~ 1.2mm, 0.1s is divided between time of vibration, vibration time is 6min ~ 8min；It is 180 μm, 160 μm, 125 μ with aperture
The sieve sequence of m sieves the cobalt xerogel particles of mixing after grinding, and the amplitude of vibrating screen is 0.8mm ~ 0.9mm, during vibration
Between between be divided into 0.1s ~ 0.2s, vibration time is 5min ~ 7min；The cobalt xerogel particles of mixing of each particle size range are respectively sealed in
In vial, storage is in dry environments；
C. the cobalt xerogel particles of mixing of gained in step b is taken to be dried 3 hours at 105 °C；
D. the heat-conducting gas of 1.0atm is passed through into vertical high-temperature xerogel stove, then rises to in-furnace temperature from room temperature
1500°C ~1550°C。
E. the cobalt xerogel particles of mixing in step c are poured into the charging buccal funnel of vertical high-temperature xerogel stove, rotation leakage
Struggle against bottom screw charging；Mix cobalt xerogel particles be made after absorbing heat, encapsulating, foam, refine molten state to mix cobalt glass micro-
Ball；The cobalt glass microballoon of mixing of molten state is made after cooling zone cures, cools down and mixes cobalt glass microballoon；In the sample disc of collecting region
Cobalt glass microballoon is mixed in collection, is obtained required.
The particle size range for mixing cobalt xerogel particles described in step c is 125 μm ~ 159 μm or 160 μm ~ 179 μm.
The heating rate of vertical high-temperature xerogel stove described in step d is 15 °C/min；Heat-conducting gas is mixed for helium argon
Gas, the partial pressure of helium is 75% ~ 95%.
The controllable quick release mixed cobalt glass microballoon and can be applied to hydrogen in hydrogen energy source transport and field of storage of the present invention,
Include the following steps：
A. to mix cobalt glass microballoon inflation：Cobalt glass microballoon will be mixed to be placed in air charging system, be passed through into plenum chamber
The hydrogen of 1.7MPa, inflation room temperature rise to 350 °C, and keep 12h with 10 °C/min rates；Hydrogen gas pressure is increased to again
3.4MPa keeps 12h；Hydrogen gas pressure is finally increased into 5.2MPa, keeps 12h；Then natural cooling plenum chamber takes to room temperature
Go out after inflation and mix cobalt glass microballoon；
B. the controlled release for mixing gas in cobalt glass microballoon after inflating：Cobalt glass microballoon of mixing after inflation is placed on
In the sample room of four-electrode spectrum residual gas analysis system, the continuous spectrum light source for being 0.40W ~ 1.11W with luminous power penetrates sample
Cobalt glass microballoon is mixed after chamber window irradiation inflation, the hydrogen mixed in the cobalt glass microballoon release after control inflation.
Cobalt glass microballoon and its preparation method and application of mixing of the present invention has the following advantages that：
1. cobalt glass microballoon its spherical shell mixed prepared by the present invention includes functional property metal ion, cobalt glass microballoon is mixed
The express passway of gas molecule can be formed after absorption visible ray, realizes the controllable quick release to gas in ball.In addition, mix cobalt glass
The sphericity of glass microballoon is high, and compressive resistance is higher, and gas retaining is good.
2. the present invention mixes cobalt glass microballoon using dry gel method preparation, there is the advantages of balling-up is efficient, simple for process.
Further, it is also possible to the melting temperature of cobalt glass microballoon, viscosity, surface are mixed in the component regulation and control that cobalt xerogel particles are mixed by changing
The properties such as power, and then its surface roughness, sphericity, evenness of wall thickness, compressive resistance, gas retaining and photic hydrogen of releasing is controlled to ring
Answer the multiple performances such as speed.
For example, improve SiO2Content or introduce Al2O3The chemical stability and mechanical strength of glass can be improved；It adds in
B2O3The chemical stability and mechanical performance of glass can be improved, at the same reduce the melting temperature of glass, viscosity, surface tension and
Tendency towards devitrification etc.；Improve Li2O、Na2O、K2The content of O can reduce melting temperature, viscosity and the tendency towards devitrification of glass, but simultaneously
Also chemical durability of glass and mechanical strength can be reduced；CoO concentration can be according to needed for practical application it is photic release hydrogen response speed
Degree is adjusted in the range of mass percent is 0.2% ~ 5.5%.
3. prepared by the present invention mix cobalt glass microballoon be applied to it is photic release hydrogen, have low energy consumption, efficiently, it is safety, controllable
The advantages of, there is potential application value in terms of hydrogen energy source storage and transport.
Specific embodiment
With reference to specific embodiment, the present invention will be described in detail.
Following embodiment is merely to illustrate the present invention, and not limitation of the present invention.Related person skilled in the art exists
It in the case of not departing from the spirit and scope of the present invention, can also make a variety of changes, replace and modification, therefore equal technology
Scheme also belongs to scope of the invention.
Embodiment 1
The present embodiment includes the following steps：
（1）Select 6.9Li2O·6.2Na2O·0.5K2O·0.9Al2O3·0.2CoO·16.5B2O3·68.8SiO2
(wt.%) cobalt xerogel block of mixing is raw material, 2 hours dry at 100 °C, is then ground and sieves.It is ground in vibrating screen
Mill, amplitude 1.2mm, time interval 0.1s, milling time 8min.Successively aperture is used as 160 μm and 125 μm of sieve
Cobalt xerogel particles of mixing after grinding are sieved, amplitude 0.9mm, time interval 0.2s, sieving time 7min；
（2）Take step（1）The cobalt xerogel particles of mixing that the particle size range of middle gained is 125 μm ~ 159 μm dry 3 at 105 °C
Hour；
（3）It is passed through helium argon mixture gas into vertical high-temperature xerogel stove, total gas pressure 1.0atm, wherein, point of helium
Press is 95%；With the rate in-furnace temperature of 15 °C/min 1550 °C are risen to from room temperature.
（4）Take step（2）Middle gained mixes cobalt xerogel particles from vertical high-temperature xerogel stove feed inlet pan feeding, from cooling zone
Collection tray is after cooling to mix cobalt glass microballoon；
（5）Take step（4）The cobalt glass microballoon of mixing of middle gained is placed in air charging system, and 1.7MPa is passed through into plenum chamber
Hydrogen, inflation room temperature be warming up to 350 °C, and keep 12h with 10 °C/min rates；Hydrogen gas pressure is increased to again
3.4MPa keeps 12h；Hydrogen gas pressure is finally increased into 5.2MPa, keeps 12h；Then natural cooling inflates room temperature to room
Temperature is taken out and mixes cobalt glass microballoon after inflation；Cobalt glass microballoon of mixing after inflation is placed on four-electrode spectrum residual gas analysis
In the sample room of system, the continuous spectrum light source for being 1.11W with luminous power mixes cobalt glass through after Sample Cell windows irradiation inflation
Microballoon, the release of hydrogen in control ball.
The cobalt glass microballoon of mixing prepared is blue-tinted transparent, and geometric parameter test is shown, a diameter of 350 μm ~ 450 μm,
Wall thickness is 1.5 μm ~ 3.5 μm；Four-electrode spectrum residual gas analysis system testing is shown, is mixed cobalt glass microballoon and is released at once once illumination
Hydrogen is released, closes light source, the release of gas stops at once, and such release and stopping release process can be followed repeatedly
Ring, until gas discharges completely in ball.
Embodiment 2
The step of embodiment 2 is with embodiment 1 is essentially identical, and the main distinction is to select 6.7Li2O·6.1Na2O·
0.5K2O·
0.9Al2O3·2.3CoO·16.2B2O3·67.3SiO2(wt.%) cobalt xerogel block is mixed for raw material.Process of lapping
The amplitude of vibrating screen is 1.1mm, time interval 0.1s, vibration time 7min.The aperture of sieve used in screening process is 180
μm and 160 μm, the amplitude of vibrating screen is 0.8mm, time interval 0.1s, vibration time 5min；Gained mixes cobalt xerogel grain
The size range of son is 160 μm ~ 179 μm；The total gas pressure for mixing heat-conducting gas in cobalt glass microballoon preparation process is 1.0atm,
In, the partial pressure of helium is 80%, and in-furnace temperature is 1550 °C；The photic power for releasing light source used in hydrogen process is 0.84W.
The cobalt glass microballoon of mixing prepared is blue-tinted transparent, and geometric parameter test is shown, a diameter of 400 μm ~ 500 μm,
Wall thickness is 1 μm ~ 3 μm.
Embodiment 3
The step of embodiment 3 is with embodiment 1 is essentially identical, and the main distinction is selection glass formula 6.5Li2O·
5.9Na2O·0.5K2O·
0.9Al2O3·5.5CoO·15.6B2O3·65.1SiO2(wt.%) corresponding cobalt xerogel of mixing is ground and sieves
Point.The amplitude of process of lapping vibrating screen is 1.1mm, time interval 0.1s, vibration time 6min.Sieve used in screening process
Aperture is 180 μm and 160 μm, and the amplitude of vibrating screen is 0.8mm, time interval 0.2s, vibration time 6min；Gained mixes cobalt
Xerogel particles size range is 160 μm ~ 179 μm；The total gas pressure for mixing furnace gas in cobalt glass microballoon preparation process is
1.0atm, wherein, the partial pressure of helium is 75%, and in-furnace temperature is 1500 °C；It is photic release light source used in hydrogen process power be
0.40W。
The cobalt glass microballoon of mixing prepared is blue-tinted transparent, and geometric parameter test is shown, a diameter of 375 μm ~ 475 μm,
Wall thickness is 2 μm ~ 3 μm.
Claims (4)
1. one kind mixes cobalt glass microballoon, which is characterized in that the component for mixing cobalt glass microballoon is as follows：
SiO2 ：Mass percent is 65.1% ~ 68.8%；
B2O3：Mass percent is 15.6% ~ 16.5%；
CoO：Mass percent is 0.2% ~ 5.5%；
Li2O：Mass percent is 6.5% ~ 6.9%；
Na2O：Mass percent is 5.9% ~ 6.2%；
K2O：Mass percent is 0.5%；
Al 2O3：Mass percent is 0.9%；
The sum of said components are 100%.
2. a kind of preparation method for mixing cobalt glass microballoon, which is characterized in that include the following steps：
A. it is 2 hours dry at 100 °C that cobalt xerogel block will be mixed；
B. the cobalt xerogel block of mixing in step a is poured into the agate mortar of vibrating screen and is ground, the amplitude of vibrating screen is
1.1mm ~ 1.2mm, 0.1s is divided between time of vibration, and vibration time is 6min ~ 8min；It it is 180 μm, 160 μm, 125 μm with aperture
Sieve sequence the cobalt xerogel particles of mixing after grinding are sieved, the amplitude of vibrating screen is 0.8mm ~ 0.9mm, during vibration
Between between be divided into 0.1s ~ 0.2s, vibration time is 5min ~ 7min；The cobalt xerogel particles of mixing of each particle size range are respectively sealed in
In vial, storage is in dry environments；
C. the cobalt xerogel particles of mixing of gained in step b is taken to be dried 3 hours at 105 °C；
D. the heat-conducting gas of 1.0atm is passed through into vertical high-temperature xerogel stove, in-furnace temperature is then risen to 1500 ° from room temperature
C ~1550°C；
E. the cobalt xerogel particles of mixing in step c are poured into the charging buccal funnel of vertical high-temperature xerogel stove, rotatable hopper bottom
Portion's screw feed；That mixes that cobalt xerogel particles are made molten state after absorbing heat, encapsulating, foam, refine mixes cobalt glass microballoon；It is molten
The cobalt glass microballoon of mixing for melting state is made after cooling zone cures, cools down and mixes cobalt glass microballoon；It is collected in the sample disc of collecting region
Cobalt glass microballoon is mixed, is obtained required.
3. the preparation method according to claim 2 for mixing cobalt glass microballoon, which is characterized in that mix cobalt described in step c
The particle size range of xerogel particles is 125 μm ~ 159 μm or 160 μm ~ 179 μm.
4. the preparation method according to claim 2 for mixing cobalt glass microballoon, which is characterized in that vertical described in step d
The heating rate of high temperature xerogel stove is 15 °C/min；Heat-conducting gas is helium argon mixture gas, and the partial pressure of helium is 75% ~ 95%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610184565.9A CN105776875B (en) | 2016-03-29 | 2016-03-29 | One kind mixes cobalt glass microballoon and its preparation method and application |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610184565.9A CN105776875B (en) | 2016-03-29 | 2016-03-29 | One kind mixes cobalt glass microballoon and its preparation method and application |
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| Publication Number | Publication Date |
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| CN105776875A CN105776875A (en) | 2016-07-20 |
| CN105776875B true CN105776875B (en) | 2018-07-03 |
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| CN201610184565.9A Expired - Fee Related CN105776875B (en) | 2016-03-29 | 2016-03-29 | One kind mixes cobalt glass microballoon and its preparation method and application |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106588521A (en) * | 2016-12-31 | 2017-04-26 | 中国科学技术大学 | Free state hydrogen sensitized emulsion explosive and preparation method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101039871A (en) * | 2004-09-21 | 2007-09-19 | 华盛顿萨凡纳河有限公司 | Hollow porous-wall glass microspheres for hydrogen storage |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1160212A1 (en) * | 2000-05-31 | 2001-12-05 | Asahi Glass Co., Ltd. | Hollow glass microspheres and method for producing the same |
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2016
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101039871A (en) * | 2004-09-21 | 2007-09-19 | 华盛顿萨凡纳河有限公司 | Hollow porous-wall glass microspheres for hydrogen storage |
Non-Patent Citations (2)
| Title |
|---|
| 《Effect of Co loading on the hydrogen storage characteristics of hollow glass microspheres 》;Sridhar Dalai等;《international journal of hydrogen energy》;20140117;第39卷;第22-28页 * |
| 《Influence of titanium doping on the structure and properties of hollow glass microspheres for inertial confinement fusion 》;Fang Li等;《Journal of Non-Crystalline Solids》;20160123;第436卷;第3304-3312页 * |
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