CN105854803A - Preparation method of graphene capable of serving as adsorbent - Google Patents
Preparation method of graphene capable of serving as adsorbent Download PDFInfo
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- CN105854803A CN105854803A CN201610327292.9A CN201610327292A CN105854803A CN 105854803 A CN105854803 A CN 105854803A CN 201610327292 A CN201610327292 A CN 201610327292A CN 105854803 A CN105854803 A CN 105854803A
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- graphene
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- temperature
- argon gas
- quartz boat
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
Abstract
The invention discloses a preparation method of graphene capable of serving as an adsorbent. The preparation method comprises the following steps: uniformly laying graphite oxides in a quartz boat, and covering another quartz boat in a semi-closed state; placing in the center of a quartz tube; extending the quartz tube into a tube furnace; introducing an argon gas as a protective gas, starting temperature programming 15 min later; enabling the furnace temperature to rise to 200-1000 DEG C at a temperature rise rate of 10 DEG C/min; keeping the temperature for 1 h; and then naturally cooling to the room temperature to obtain graphene. The preparation method is simple to operate, environment-friendly and short in production period; the prepared graphene has excellent thermal stability, high specific surface area and excellent adsorption effects on pollutants in water.
Description
Technical field
It is contemplated that invent the preparation method that a kind of simple preparation can be used as the Graphene of adsorbent.
Background technology
Absorption method is simple and convenient to operate and the advantage such as with low cost owing to having design, is currently to remove in water
One of pollutant most common method.At present conventional adsorbent species include charcoal class, humic acids, mineral substance,
High score subclass etc..Nano material is due to its bigger specific surface area, having obtained the most widely in absorption
Research.Wherein, carbon nanomaterial Graphene, is preferable sorbing material.Existing graphene preparation method has
Micromechanics stripping method, epitaxial growth method, chemical vapour deposition technique etc., the quality of graphene prepared is higher but exists
Production cost is high, preparation process complicated, production cycle length and be difficult to the problems such as extensive preparation, should in reality
There is many limitation in.
To this end, the present invention first with thermal reduction graphite oxide with graphite oxide for raw material directly in inert gas
Self reduction generates Graphene, and while simple to operate, with short production cycle, production cost is relatively low.
Summary of the invention
The object of the invention is for solving the problems of the prior art, it is provided that a kind of simple, with short production cycle and low
The preparation of cost can be used as the preparation method of the Graphene of adsorbent.
For realizing object above, the technical solution adopted in the present invention is:
(1) graphite oxide on uniform spreading in quartz boat, covers another quartz boat semiclosed；It is put into stone
English pipe central authorities, stretch into quartz ampoule in tube furnace；
(2) in the quartz ampoule of tube furnace, it is passed through argon gas as protective gas, and heats；Described heating-up temperature
Being 200 DEG C～1000 DEG C, heating rate is 10 DEG C/min；
(3), after having heated up, keep furnace temperature 1h, make fully oxidized reduction, fully expand stripping, the coldest
But Graphene is obtained.
Above technical scheme principle is: there is also a lot of oxygen-containing functional group in graphite oxide in addition to carbon,
In an inert atmosphere, in the environment of isolation air, heat treatment step makes carbon therein and oxygen interact, and sends out
Raw redox reaction, produces CO, CO of little molecule2Deng gas molecule, while the effusion of these little molecules
Graphene sheet layer is strutted so that the microstructure of material tends to the Graphene of the two-dimensional structure of monolayer, cruelly
Expose more surface area.
The beneficial effects of the present invention is:
The present invention provide preparation method technique is simple, with short production cycle and low cost, production process does not produce it
Its any harmful side product, has simple, economy, advantages of environment protection；The present invention is used to provide
Graphene prepared by method possesses good heat endurance and high-specific surface area, and specific surface area is up to 477m2/g,
Pore volume can reach 1.13cm3/ g, has good adsorption capacity to antibiotic pollutant in water.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of the Graphene prepared by the present invention.
Fig. 2 is the adsorption isothermal curve at different temperatures of the Graphene prepared by the present invention and adsorption capacity analysis result.
Detailed description of the invention
The following examples are to further illustrate the present invention rather than limit the scope of the present invention.
Embodiment 1
In a quartz boat, graphite oxide on uniform spreading, covers another quartz boat semiclosed；Push it into stone
English pipe central authorities, stretch into quartz ampoule in tube furnace.It is passed through argon gas as protective gas, wait after inspection air-tightness
15min, then starts temperature programming, with the heating rate of 10 DEG C/min, makes furnace temperature rise to 200 DEG C, and protects
Holding temperature 1h, naturally cool to thereafter less than 60 DEG C and stop logical argon gas, sampling obtains Graphene.BET tests
The specific surface area of result display Graphene is 272.8m2/g。
10mg Graphene adsorbent is joined in the ciprofloxacin solution of 40mL variable concentrations, put into 25 DEG C
Constant-temperature table vibration 24h, prepares Langmuir adsorption isothermal curve, is balanced adsorbance, and display is to ring
Third husky star adsorption effect is good.
Embodiment 2
The present embodiment and the difference of embodiment 1, be only to change furnace temperature temperature: make furnace temperature rise to 400 DEG C.
Particularly as follows: in a quartz boat graphite oxide on uniform spreading, cover another quartz boat semiclosed；Will
It pushes quartz ampoule central authorities, is stretched in tube furnace by quartz ampoule.It is passed through argon gas as protective gas, checks airtight
Wait 15min after property, then start temperature programming, with the heating rate of 10 DEG C/min, make furnace temperature rise to 400 DEG C,
And keep temperature 1h, and naturally cooling to thereafter less than 60 DEG C and stop logical argon gas, sampling obtains Graphene.BET
The specific surface area of test result display Graphene is 318.6m2/g。
10mg Graphene adsorbent is joined in the ciprofloxacin solution of 40mL variable concentrations, put into 25 DEG C
Constant-temperature table vibration 24h, prepares Langmuir adsorption isothermal curve, is balanced adsorbance, and display is to ring
Third husky star adsorption effect is good.
Embodiment 3
The present embodiment and the difference of embodiment 1, be only to change furnace temperature temperature: make furnace temperature rise to 600 DEG C.
Particularly as follows: in a quartz boat graphite oxide on uniform spreading, cover another quartz boat semiclosed；Will
It pushes quartz ampoule central authorities, is stretched in tube furnace by quartz ampoule.It is passed through argon gas as protective gas, checks airtight
Wait 15min after property, then start temperature programming, with the heating rate of 10 DEG C/min, make furnace temperature rise to 600 DEG C,
And keep temperature 1h, and naturally cooling to thereafter less than 60 DEG C and stop logical argon gas, sampling obtains Graphene.
10mg Graphene adsorbent is joined in the ciprofloxacin solution of 40mL variable concentrations, put into 25 DEG C
Constant-temperature table vibration 24h, prepares Langmuir adsorption isothermal curve, is balanced adsorbance, and display is to ring
Third husky star adsorption effect is good.The specific surface area of BET test result display Graphene is 399.0m2/g。
Embodiment 4
The present embodiment and the difference of embodiment 1, be only to change furnace temperature temperature: make furnace temperature rise to 800 DEG C.
Particularly as follows: in a quartz boat graphite oxide on uniform spreading, cover another quartz boat semiclosed；Will
It pushes quartz ampoule central authorities, is stretched in tube furnace by quartz ampoule.It is passed through argon gas as protective gas, checks airtight
Wait 15min after property, then start temperature programming, with the heating rate of 10 DEG C/min, make furnace temperature rise to 800 DEG C,
And keep temperature 1h, and naturally cooling to thereafter less than 60 DEG C and stop logical argon gas, sampling obtains Graphene.
10mg Graphene adsorbent is joined in the ciprofloxacin solution of 40mL variable concentrations, put into 25 DEG C
Constant-temperature table vibration 24h, prepares Langmuir adsorption isothermal curve, is balanced adsorbance, and display is to ring
Third husky star adsorption effect is good.The specific surface area of BET test result display Graphene is 442.5m2/g。
Embodiment 5 (optimum)
The present embodiment and the difference of embodiment 1, be only to change furnace temperature temperature: make furnace temperature rise to 1000 DEG C.
Particularly as follows: in a quartz boat graphite oxide on uniform spreading, cover another quartz boat semiclosed；Will
It pushes quartz ampoule central authorities, is stretched in tube furnace by quartz ampoule.It is passed through argon gas as protective gas, checks airtight
Wait 15min after property, then start temperature programming, with the heating rate of 10 DEG C/min, make furnace temperature rise to
1000 DEG C, and keep temperature 1h, naturally cooling to thereafter less than 60 DEG C and stop logical argon gas, sampling obtains graphite
Alkene.The specific surface area of BET test result display Graphene is 477.0m2/g。
10mg Graphene adsorbent is joined in the ciprofloxacin solution of 40mL variable concentrations, put into 15 DEG C,
25 DEG C and 40 DEG C of constant-temperature table vibration 24h, prepare Langmuir adsorption isothermal curve, as in figure 2 it is shown, be
The Graphene of embodiment 5 adsorption isothermal curve at different temperatures and adsorption capacity analysis result, display is to ring
Third husky star adsorption effect is good.
The Graphene that the present embodiment prepares has good heat endurance, has high-specific surface area and to antibiotic etc.
Pollutant has good absorption property.The Qm that the adsorption isothermal curve of Fig. 2 is drawn reaches, more than 300, to say
Bright absorption property is good.
To sum up, Graphene prepared by each embodiment is carried out IR Characterization as it is shown in figure 1, along be heat-treated temperature
The raising of degree, oxygen-containing functional group content reduces, and C/O gradually steps up.
As it is shown in figure 1, be the infrared spectrogram of the grapheme material of five embodiment gained.Abscissa is wave number,
Ordinate is light transmittance, and this is a kind of survey observing material functional group kind and qualitative observation functional group relative amount
Method for testing.Along with the rising of heat treatment temperature, each peak intensity of infrared spectrum weakens, and oxygen-containing functional group is described
Quantity reduces relatively, and the relative amount of oxygen reduces, and illustrates that redox is more thorough.The effusion of more little molecules carries
For more active forces making graphene sheet layer strut, the knot increased with the raising of heat treatment temperature with specific surface area
The most consistent.
Claims (4)
1. the preparation method of a Graphene, it is characterised in that step is: put into graphite oxide at quartz boat
Cover another quartz
Boat is semiclosed, puts in tube furnace；With argon gas as protective gas, temperature programming, 10 DEG C/min of heating rate,
Make furnace temperature rise to 200 DEG C～1000 DEG C, and keep temperature 1h, naturally cool to thereafter room temperature, it is thus achieved that Graphene.
The preparation method of Graphene the most according to claim 1, it is characterised in that: with argon gas for protection
Gas, flow is less than 0.3L/min, and before starting temperature programming, the time is no less than 15min.
The preparation method of Graphene the most according to claim 1, it is characterised in that: make grapheme material
Naturally cool to less than 60 DEG C and stop logical argon gas.
The preparation method of Graphene the most according to claim 1, it is characterised in that: the Graphene tool prepared
There is good heat endurance, there is high-specific surface area and the pollutants such as antibiotic are had good absorption property.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011147A (en) * | 2012-12-27 | 2013-04-03 | 中南大学 | Method for preparing graphene through thermal reduction |
| CN104925785A (en) * | 2015-03-13 | 2015-09-23 | 宁波南车新能源科技有限公司 | Preparation methods of porous graphene and supercapacitor with porous graphene |
-
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- 2016-05-17 CN CN201610327292.9A patent/CN105854803A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011147A (en) * | 2012-12-27 | 2013-04-03 | 中南大学 | Method for preparing graphene through thermal reduction |
| CN104925785A (en) * | 2015-03-13 | 2015-09-23 | 宁波南车新能源科技有限公司 | Preparation methods of porous graphene and supercapacitor with porous graphene |
Non-Patent Citations (4)
| Title |
|---|
| ALEXANDR V. DOLBINA ET AL.: "The effect of the thermal reduction temperature on the structure andsorption capacity of reduced graphene oxide materials", 《APPLIED SURFACE SCIENCE》 * |
| HYE-MI JU ET AL.: "Structures of thermally and chemically reduced graphene", 《MATERIALS LETTERS》 * |
| 朱璇等: "石墨烯对环丙沙星的吸附性能研究", 《2014年第12届全国水处理化学大会暨学术研讨会论文摘要集》 * |
| 祁振等: "石墨烯对四环素的吸附热力学及动力学研究", 《山东大学学报(工学版)》 * |
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