CN107579254A - A kind of synthetic method of graphene oxide modification mesoporous silicon oxide - Google Patents
A kind of synthetic method of graphene oxide modification mesoporous silicon oxide Download PDFInfo
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- CN107579254A CN107579254A CN201710760483.9A CN201710760483A CN107579254A CN 107579254 A CN107579254 A CN 107579254A CN 201710760483 A CN201710760483 A CN 201710760483A CN 107579254 A CN107579254 A CN 107579254A
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Abstract
The present invention relates to a kind of synthetic method of graphene oxide modification mesoporous silicon oxide, step are as follows：(1) contain 25% the hexadecyltrimethylammonium chloride aqueous solution 31.2g, 0.6g triethanolamine, 192mL deionized waters and 27mL ethanol, stirred 30 minutes at 60 DEG C, obtain solution A；(2) 3g graphite is added in 1000mL large beakers, 3g sodium nitrate and the 100mL concentrated sulfuric acids, ice bath is put into after being stirred at room temperature and is cooled under 0 DEG C of ice bath, 15g potassium permanganate is added slowly with stirring, after 0 DEG C of stirring 90 minutes, 35~40 DEG C of stirring in water bath are transferred to 2 hours；System gradually becomes the sticky sposh of brownish black；150mL water to system was added in 30 minutes and is changed into orange-yellow, after continuously adding 300mL water, the aqueous hydrogen peroxide solutions of 20mL 30% is added and stirs 15 minutes, system is changed into glassy yellow, stands overnight.Preparation method of the present invention is easy to use, and effect is good, and technique is simple, and the product obtained has preferable performance.
Description
Technical field
The present invention relates to a kind of synthetic method of graphene oxide modification mesoporous silicon oxide, belongs to material technology neck
Domain.
Background technology
With the arrival of rare-view set-up, the exploitation of new energy is maked rapid progress.For example mixed even in automobile industry, oil electricity
Pure electronic automotive development is like a raging fire.In electrochemical energy storage field, lithium ion battery turns into because its capacity density is higher to be ground
Study carefully and wide variety of focus.Compared to for all kinds of lithium batteries for comparing shaping on the market, no matter lithium-sulfur cell holds from theory
It is all very advantageous for amount or relative price.Specifically, elemental sulfur has 1675mAhg-1High theoretical specific capacity and
2500Whkg-1High theory compare energy.Using 18650 ferric phosphate lithium cells used in tesla's automobile as contrast, lithium-sulfur cell reason
Its 10 times by capacity, price but for it 1/10. also just because of this, lithium-sulfur cell is likely to the hair as novel high-capacity battery
Open up direction.
In previous report, poromerics such as ZIF etc. has been used for the exploration that lithium-sulphur cell positive electrode carries sulphur body.Its micropore knot
Structure can be as the storage site of sulphur, and its confinement effect can prevent the loss of sulphur in battery charge and discharge process.Mesoporous two
As positive pole load sulphur body, its advantage is embodied in following aspects silica：On the one hand, compared to large pore material, mesoporous material ratio
Surface area is high；Compared to poromerics, mesoporous material pore volume is again big, therefore most of researcher guesses the spy on its aperture
Point will bring the advantage of comprehensive other two kinds of porous materials for it.On the other hand, compared to organometallic skeletal, its stability
It is good, smaller from probability destroyed in test process is synthesized to.
The strategy of sulphur is carried based on porous material, the present invention utilizes graphene oxide pair on the basis of mesoporous silicon oxide
Mesoporous silicon oxide is coated, and is applied as lithium-sulphur cell positive electrode and is carried sulphur body, and its performance improves to some extent.But current lithium
Sulphur battery is many still in development phase, its reason.One side sulphur and the more lithium sulfide electric conductivities of discharging product are equal
Bad, this shows as differing larger between actual specific capacity and theoretical specific capacity.On the other hand it is the more of sulphur reduction process formation
Lithium sulfide dissolution causes shuttle effect, causes its active material to be largely lost in charge and discharge process.In terms of comprehensive, with elemental sulfur
And decay low as lithium-sulfur cell made of positive pole its specific capacity is exceedingly fast.Just because of this, the suitable load sulphur body material of selection will be right
Its performance is produced and greatly improved.
The content of the invention
It is an object of the invention to provide a kind of synthetic method of graphene oxide modification mesoporous silicon oxide, so as to more
Improve it well and prepare effect, obtain the material of more preferable performance.
To achieve these goals, technical scheme is as follows.
A kind of synthetic method of graphene oxide modification mesoporous silicon oxide, step are as follows：
(1) containing 25% the hexadecyltrimethylammonium chloride aqueous solution 31.2g, 0.6g triethanolamine, 192mL deionized waters with
And 27mL ethanol, stirred 30 minutes at 60 DEG C, obtain solution A；36.5mL tetraethyl orthosilicates were added dropwise to solution in 2 minutes
In A, then stirred at 40 DEG C 2 hours and system is gradually bleached；Gained white precipitate is with being centrifuged at a high speed, 18000rpm
30min is run, is then washed with water 2 times, then with containing mass ratio 1:9 concentrated hydrochloric acid and the cleaning agent of ethanol wash 3 times, until precipitation
It is nearly transparent；Washed 3 times with ethanol again, finally dried 12 hours at 60 DEG C, obtain white powder 5g；
(2) 3g graphite, 3g sodium nitrate and the 100mL concentrated sulfuric acids are added in 1000mL large beakers, ice is put into after being stirred at room temperature
Bath is cooled under 0 DEG C of ice bath, and 15g potassium permanganate is added slowly with stirring, and after 0 DEG C is stirred 90 minutes, is transferred to 35~40 DEG C of water
Bath stirring 2 hours；System gradually becomes the sticky sposh of brownish black；150mL water to system was added in 30 minutes and is changed into orange-yellow,
After continuously adding 300mL water, add the aqueous hydrogen peroxide solutions of 20mL 30% and stir 15 minutes, system is changed into glassy yellow, stands
Overnight；After abandoning supernatant, 250mL concentrated hydrochloric acids are added into light brown precipitation:Water=1:10 hydrochloric acid solution, after being sufficiently stirred
Stand, discard clear liquid, be repeated 3 times；It is washed with water until precipitating and is changed into dark-brown, is scattered in 500mL water, with pellicle bag filter
Dialyse 1 week, the various ions in thorough removing system；Weigh 300mg colloidal sol shapes mesoporous silicon oxide and add 100mL hydrochloric acid solutions
And ultrasound is then added dropwise to the ultrasonic disperse 20g graphenes of 2 hours under conditions of stirring, stopped after half an hour to scattered
Stirring, stands overnight；Washing centrifuges precipitation, 5000rpm processing 10min, freezes, can obtain light brown fluffy cotton-shaped graphite
Olefinic oxide modification mesoporous silicon oxide 265mg.
The beneficial effect of the invention is：Preparation method of the present invention is easy to use, and effect is good, and technique is simple, is obtained
Product has preferable performance.
Embodiment
The embodiment of the present invention is described with reference to embodiment, to be better understood from the present invention.
Embodiment
The synthetic method of graphene oxide modification mesoporous silicon oxide in the present embodiment, step are as follows：
(1) containing 25% the hexadecyltrimethylammonium chloride aqueous solution 31.2g, 0.6g triethanolamine, 192mL deionized waters with
And 27mL ethanol, stirred 30 minutes at 60 DEG C, obtain solution A；36.5mL tetraethyl orthosilicates were added dropwise to solution in 2 minutes
In A, then stirred at 40 DEG C 2 hours and system is gradually bleached；Gained white precipitate is with being centrifuged at a high speed, 18000rpm
30min is run, is then washed with water 2 times, then with containing mass ratio 1:9 concentrated hydrochloric acid and the cleaning agent of ethanol wash 3 times, until precipitation
It is nearly transparent；Washed 3 times with ethanol again, finally dried 12 hours at 60 DEG C, obtain white powder 5g；
(2) 3g graphite, 3g sodium nitrate and the 100mL concentrated sulfuric acids are added in 1000mL large beakers, ice is put into after being stirred at room temperature
Bath is cooled under 0 DEG C of ice bath, and 15g potassium permanganate is added slowly with stirring, and after 0 DEG C is stirred 90 minutes, is transferred to 35~40 DEG C of water
Bath stirring 2 hours；System gradually becomes the sticky sposh of brownish black；150mL water to system was added in 30 minutes and is changed into orange-yellow,
After continuously adding 300mL water, add the aqueous hydrogen peroxide solutions of 20mL 30% and stir 15 minutes, system is changed into glassy yellow, stands
Overnight；After abandoning supernatant, 250mL concentrated hydrochloric acids are added into light brown precipitation:Water=1:10 hydrochloric acid solution, after being sufficiently stirred
Stand, discard clear liquid, be repeated 3 times；It is washed with water until precipitating and is changed into dark-brown, is scattered in 500mL water, with pellicle bag filter
Dialyse 1 week, the various ions in thorough removing system；Weigh 300mg colloidal sol shapes mesoporous silicon oxide and add 100mL hydrochloric acid solutions
And ultrasound is then added dropwise to the ultrasonic disperse 20g graphenes of 2 hours under conditions of stirring, stopped after half an hour to scattered
Stirring, stands overnight；Washing centrifuges precipitation, 5000rpm processing 10min, freezes, can obtain light brown fluffy cotton-shaped graphite
Olefinic oxide modification mesoporous silicon oxide 265mg.
It is uninfluenced that the sample intermediary hole silica pattern of synthesis is can be seen that from Electronic Speculum result, and in lamellar graphite
Olefinic oxide superficial growth.Gas adsorption desorption has then been carried out respectively to the sample after GO-CMS and its filling sulphur.From GO-CMS
Adsorption desorption curve it is seen that, it maintains CMS meso-hole structure.And support the adsorption curve after sulphur and almost connect by contrast
Zero is bordering on, we can speculate that sulphur is had been enter among duct accordingly.GO-CMS is fired to obtain rGO-CMS, and by three kinds
Sample assembly battery carries out electro-chemical test.As can be seen that after graphene coated, the decay of CMS systems does not almost occur
Change, and initial charge/discharge capacity is obtained for lifting.And although the rGO-CMS formed after GO is reduced its initial capacity has
Very big lifting, but the increase of its attenuation rate, when circulating for 100, its specific capacity is just similar to CMS.To sum up, GO-CMS exists
Performance is excellent in terms of charge/discharge capacity and attenuation rate.
Described above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications are also considered as
Protection scope of the present invention.
Claims (1)
- A kind of 1. synthetic method of graphene oxide modification mesoporous silicon oxide, it is characterised in that：Step is as follows：(1) containing 25% the hexadecyltrimethylammonium chloride aqueous solution 31.2g, 0.6g triethanolamine, 192mL deionized waters and 27mL ethanol, stirred 30 minutes at 60 DEG C, obtain solution A；36.5mL tetraethyl orthosilicates were added dropwise to solution A in 2 minutes In, then stirred at 40 DEG C 2 hours and system is gradually bleached；Gained white precipitate is with being centrifuged at a high speed, 18000rpm 30min is run, is then washed with water 2 times, then with containing mass ratio 1:9 concentrated hydrochloric acid and the cleaning agent of ethanol wash 3 times, until precipitation It is nearly transparent；Washed 3 times with ethanol again, finally dried 12 hours at 60 DEG C, obtain white powder 5g；(2) 3g graphite, 3g sodium nitrate and the 100mL concentrated sulfuric acids are added in 1000mL large beakers, it is cold to be put into ice bath after being stirred at room temperature To 0 DEG C of ice bath, 15g potassium permanganate is added slowly with stirring, and after 0 DEG C is stirred 90 minutes, is transferred to 35~40 DEG C of water-baths and is stirred Mix 2 hours；System gradually becomes the sticky sposh of brownish black；150mL water to system was added in 30 minutes and is changed into orange-yellow, is continued After adding 300mL water, add the aqueous hydrogen peroxide solutions of 20mL 30% and stir 15 minutes, system is changed into glassy yellow, stands Night；After abandoning supernatant, 250mL concentrated hydrochloric acids are added into light brown precipitation:Water=1:10 hydrochloric acid solution, it is sufficiently stirred rear quiet Put, discard clear liquid, be repeated 3 times；It is washed with water until precipitating and is changed into dark-brown, is scattered in 500mL water, it is saturating with pellicle bag filter Analyse 1 week, the various ions in thorough removing system；Weigh 300mg colloidal sol shapes mesoporous silicon oxide and add 100mL hydrochloric acid solutions simultaneously Ultrasound is then added dropwise to the ultrasonic disperse 20g graphenes of 2 hours under conditions of stirring, stops stirring after half an hour to scattered Mix, stand overnight；Washing centrifuges precipitation, 5000rpm processing 10min, freezes, can obtain light brown fluffy cotton-shaped graphene Modified oxide mesoporous silicon oxide 265mg.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108767270A (en) * | 2018-06-11 | 2018-11-06 | 佛山腾鲤新能源科技有限公司 | A kind of preparation method of fuel-cell catalyst |
| CN111215103A (en) * | 2019-11-27 | 2020-06-02 | 西安交通大学 | Preparation method of graphene modified mesoporous silica supported heteropolyacid catalyst |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104027814A (en) * | 2014-05-29 | 2014-09-10 | 福州大学 | Amino-modified mesoporous silica with dual drug-loading effects |
| CN105203619A (en) * | 2015-10-30 | 2015-12-30 | 黑龙江大学 | Method for detecting p-nitrophenol with graphene/nano silver-nickel alloy as electrode |
-
2017
- 2017-08-30 CN CN201710760483.9A patent/CN107579254A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104027814A (en) * | 2014-05-29 | 2014-09-10 | 福州大学 | Amino-modified mesoporous silica with dual drug-loading effects |
| CN105203619A (en) * | 2015-10-30 | 2015-12-30 | 黑龙江大学 | Method for detecting p-nitrophenol with graphene/nano silver-nickel alloy as electrode |
Non-Patent Citations (1)
| Title |
|---|
| SHIJU ABRAHAM，ET AL.: "Mesoporous silica particle embedded functional graphene oxide as an efficient platform for urea biosensing", 《ANALYTICAL METHODS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108767270A (en) * | 2018-06-11 | 2018-11-06 | 佛山腾鲤新能源科技有限公司 | A kind of preparation method of fuel-cell catalyst |
| CN108767270B (en) * | 2018-06-11 | 2021-01-29 | 山东岱擎新能源科技有限公司 | Preparation method of fuel cell catalyst |
| CN111215103A (en) * | 2019-11-27 | 2020-06-02 | 西安交通大学 | Preparation method of graphene modified mesoporous silica supported heteropolyacid catalyst |
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