CN109399628A - A kind of preparation facilities of low layer number graphene oxide - Google Patents
A kind of preparation facilities of low layer number graphene oxide Download PDFInfo
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- CN109399628A CN109399628A CN201811492027.1A CN201811492027A CN109399628A CN 109399628 A CN109399628 A CN 109399628A CN 201811492027 A CN201811492027 A CN 201811492027A CN 109399628 A CN109399628 A CN 109399628A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
The present invention provides a kind of preparation facilities of low layer number graphene oxide.Described device includes that hydrogel forms unit, low temperature drying unit and transport mechanism, and hydrogel forms unit and receives graphene oxide raw material and water, and stock dispersion is formed to graphene oxide hydrogel in water；Low temperature drying unit has control temperature unit, pressure control unit and a cold dry chamber, and temperature control and pressure control unit do intracavitary temperature and pressure control for cold respectively as not higher than -50 DEG C and lower than 1 atmospheric pressure and control is cold does intracavitary temperature change no more than ± 4 DEG C and pressure change is no more than ± 100Pa；The speed adjusting gear that transport mechanism has the transmission parts for running through cold dry chamber and can adjust transmission parts travel speed, transmission parts, which receive graphene oxide hydrogel, simultaneously makes it after entire cold dry chamber, to obtain the graphene oxide after number of plies reduction from discharge port.The device of the invention can promote its structure and quality while dry graphene oxide raw material.
Description
Technical field
The present invention relates to the production technical fields of graphene oxide, it relates in particular to which one kind is able to produce dry and layer
The device of the lower graphene oxide of number.
Background technique
It is poor generally, due to the thermal stability of graphite oxide, it often just will appear pyrolysis phenomenon during the drying process, and by
Graphite oxide after heat drying is easy to be agglomerated into lump, is unfavorable for subsequent dispersion.
Summary of the invention
It is an object of the invention to solve at least one in deficiencies of the prior art.For example, of the invention
The first purpose is to provide a kind of new equipment dry for graphene oxide.
To achieve the goals above, the present invention provides a kind of preparation facilities of low layer number graphene oxide, the preparations
Device includes that hydrogel forms unit, low temperature drying unit and transport mechanism, wherein the hydrogel, which forms unit, has dispersion
Slot, the dispersion slot can receive graphene oxide and water with first number of plies, and graphene oxide is dispersed in water, with
Form graphene oxide hydrogel；The low temperature drying unit has control temperature unit, pressure control unit and cold dry chamber, wherein described
Cold dry chamber is made of shell and has feed inlet, discharge port and cavity, and the control temperature unit is used for the intracorporal temperature of the chamber
Control is not higher than -50 DEG C and the entire intracorporal temperature change of chamber of control is no more than ± 4 DEG C, and the pressure control unit is used for will be described
The intracorporal pressure control of chamber is lower than 1 atmospheric pressure and the entire intracorporal pressure change of chamber of control is no more than ± 100Pa；The biography
The speed adjusting gear for sending mechanism that there are the transmission parts for running through the cold dry chamber and transmission parts travel speed can be adjusted, the biography
Send part for receiving the graphene oxide hydrogel of the hydrogel formation unit formation and making the graphene oxide hydrogel
After entire cold dry chamber, to obtain the graphene oxide with second number of plies from the discharge port, second number of plies is less than institute
State first number of plies.
Compared with prior art, the beneficial effect comprise that (1) handles graphene oxide with the device of the invention,
Freezing dry process will not destroy the structure of oxidized graphite flake layer, preferably preservation functional group, it is freeze-dried after oxidation stone
Ink is not susceptible to agglomeration；(2) after freeze-dried graphene oxide layer interlamellar spacing is greater than the drying of other drying means
Graphene oxide product, have superior dispersion performance, the less number of plies and bigger specific surface area.
Specific embodiment
Hereinafter, the preparation that the low layer number graphene oxide that the present invention will be described in detail is carried out in conjunction with exemplary embodiment is filled
It sets.
In an exemplary embodiment of the present invention, the preparation facilities of low layer number graphene oxide can be formed by hydrogel
Unit, low temperature drying unit and transport mechanism are constituted.
The hydrogel, which forms unit, has dispersion slot.Dispersion slot can receive graphene oxide with first number of plies and
Water, and graphene oxide is dispersed in water, to form graphene oxide hydrogel.For example, dispersion slot can have groove body, set
It sets the feed opening above groove body and the discharge port of groove body side or bottom is set.Wherein, feed opening is for being added conduct
Raw material has the first number of plies graphene oxide and water.Here, first number of plies can be ten several layers to tens of layers, for example,
20~30 layers.Discharge port is for being discharged graphene oxide hydrogel.It can be further provided in addition, the hydrogel forms unit
Ultrasonic generating mechanism.The ultrasound generating mechanism can emit ultrasonic wave to the dispersion slot, in the water in dispersion slot
Graphene oxide forms ultrasonic vibration, to be conducive to strengthen dispersion effect.
The graphene oxide with first number of plies can be dispersed in water by dispersion slot, and form graphene oxide water
Gel.As containing oxygen-containing functional group in the graphene oxide of raw material.For example, the graphene oxide with first number of plies can
By being prepared using Bronsted acid intercalated graphite.In dispersion process, dispersion effect is further preferably strengthened by ultrasonic disperse
Fruit, thus make hydrone well into the lamellar structure to graphene oxide perhaps in fold or with graphene oxide table
The functional groups in face form graphene oxide hydrogel at hydrated ion.Graphene oxide hydrogel have its own
Structure of water molecules are combined in the lamella or fold of graphene oxide.The solid content of graphene oxide hydrogel can be
0.1~50wt%.
The low temperature drying unit has control temperature unit, pressure control unit and cold dry chamber.Wherein, the cold dry chamber is enclosed by shell
At and with feed inlet, discharge port and the cavity for determining length.The cavity of cold dry chamber can be U-shaped or with annular jaggy,
To save space.However, present exemplary embodiment is not limited to this, the cavity of cold dry chamber can also S-type or linear type.Feed inlet
The front-end and back-end of cavity are separately positioned on along the direction of travel of material with discharge port, and are each provided with openable and closable valve
Cavity and the external world to be separated.The control temperature unit can be the refrigeration for connecting and having constant temperature control function with cold dry chamber
The control of the chamber of cold dry chamber intracorporal temperature not higher than -50 DEG C and can be controlled the chamber of entire cold dry chamber by machine, the refrigeration machine
Intracorporal temperature change is no more than ± 4 DEG C.Also, the pressure control unit can be to connect and with constant pressure control function with cold dry chamber
The vacuum pump of energy, the vacuum pump can be by the intracorporal pressure controls of the chamber of the cold dry chamber for lower than 1 atmospheric pressure and control
The entire intracorporal pressure change of chamber is no more than ± 100Pa.
Further, the control temperature unit can be by the intracorporal temperature control of the chamber is within the scope of -55~-65 DEG C and control is whole
A intracorporal temperature change of chamber is no more than ± 2 DEG C, and the pressure control unit can by the control of the chamber intracorporal pressure 10~
The 100Pa and entire intracorporal pressure change of chamber of control is no more than ± 10Pa, has both metastable low temperature to help to obtain
And the atmosphere of metastable vacuum degree.
By the coordinative role of control temperature unit and pressure control unit, hydrone can be made to become ice molecule, by volume expansion,
Further widen the lamellar structure of graphite；And ice can sublimate volatilization under low-temp low-pressure, and temperature is low, and " entropy " value is low, can
So that the structure that graphene oxide is softened is maintained, make graphene oxide composite material good dispersion, the large specific surface area of preparation.
Moreover, by relative constant cryogenic temperature (for example, the intracorporal temperature of chamber for being not higher than -50 DEG C and the entire cold dry chamber of control becomes
Change and be no more than ± 4 DEG C) and relative constant vacuum degree (for example, lower than 1 atmospheric pressure and controlling the entire intracorporal pressure change of chamber
No more than ± 100Pa), be conducive to the rate of set for making hydrone and degree is relatively stable, therefore, to graphene oxide layer
" strutting " effect stability；And be conducive to make ice molecule sublimate speed and degree it is relatively stable, therefore, be also beneficial to certain journey
Degree avoids local defect caused by the local stress because of graphene oxide layer.It further says, passes through control temperature unit and pressure control
Unit is temperature within the scope of -55~-65 DEG C for the control climate of cold dry chamber and the entire intracorporal temperature change of chamber of control does not surpass
± 2 DEG C and pressure control are crossed in 10~100Pa and the entire intracorporal pressure change of chamber of control is no more than ± 10Pa, more added with
Further stablize conducive to the rate of set and degree for making hydrone, thus to " strutting " effect stability of graphene oxide layer；And
And be conducive to make ice molecule sublimate speed and degree is further stablized, to be also beneficial to further avoid because of graphene oxide
Local defect caused by the local stress of layer.
The tune that the transport mechanism has the transmission parts for running through the cold dry chamber and can adjust transmission parts travel speed
Fast mechanism.The transmission parts can receive the hydrogel and form the graphene oxide hydrogel that unit is formed, and make the oxygen
Graphite alkene hydrogel is advanced finally to obtain from the discharge outlet of the cold dry chamber with second number of plies by entire cold dry chamber
Graphene oxide.The transmission parts can be conveyer belt.The speed adjusting gear can control conveyer belt with pre-set velocity at the uniform velocity
Pass through cold dry chamber.Second number of plies is less than first number of plies.Second number of plies can have compared to first number of plies to significantly decrease.This
In, second number of plies can be the 1/3~1/6 of first number of plies.For example, second number of plies can be 5~7 layers.
In another exemplary embodiment of the invention, the preparation facilities of low layer number graphene oxide can be with above-mentioned
It further comprise buffer area on the basis of the structure of exemplary embodiment.Specifically, buffer area can be connect with discharge port, with
Just it is suitably heated up to the graphene oxide entered in buffer area from discharge port, to enable the graphene oxide as product
Enough adapt to room temperature environment or subsequent treatment process.For example, the length of buffer area can be 1.5~4 meters, but the present exemplary embodiment
It is without being limited thereto.
In another exemplary embodiment of the invention, the preparation facilities of low layer number graphene oxide can be with above-mentioned
On the basis of the structure of exemplary embodiment, pretreating zone is further wrapped.Specifically, pretreating zone can be with the feed inlet
It connects and itself is run through by the transmission parts.Pretreating zone has cooling component, so as to enter in it to by transmission parts
Graphene oxide hydrogel carry out cooling processing appropriate so that the temperature of graphene oxide hydrogel reduces.For example, pre- place
Temperature in reason area can be stably held in the 1/6~3/5 of the intracorporal temperature of the chamber.It, can be to oxygen by the setting of pretreating zone
Graphite alkene is cooled down for the first time, convenient for control temperature-fall period, and is conducive to operation.For example, the length of pretreating zone can be 1.5
~4 meters, but present exemplary embodiment is not limited to this.
In an exemplary embodiment of the present invention, the preparation facilities can pass through the length of the cavity of the cold dry chamber of coordinated control
Degree, the cold speed for doing intracavitary temperature and pressure and transmission parts have the oxygen of second number of plies to obtain described in drying completely
Graphite alkene.Specifically, when designing preparation facilities of the invention, can first according to above-mentioned related request determine it is cold do it is intracavitary
Temperature and pressure then determine the speed of service of cavity length and transmission parts according to requirements such as places, to ensure to pass through transmission parts
Cryogenic freezing can sufficiently be completed by the graphene oxide hydrogel of cold dry chamber and dry process of sublimating by conveying and running.Example
Such as, the cavity length of cold dry chamber can be 10~20 meters, but present exemplary embodiment is not limited to this.
In conclusion the present invention can during drying further " strutting " graphene oxide layer, meanwhile, low
The lower graphene oxide composite material of temperature maintains lower entropy, is conducive to its graphene oxide layer microstructure " strutted "
It keeps, so as to obtain the graphene oxide product of higher quality.For example, graphene obtained by method of the invention is not only
With complete microstructure, and the number of plies of graphene oxide can be made to be reduced to original 1/3~1/6, for example, the number of plies from
20~30 layers can be reduced to 5~7 layers；Increase the specific surface area of graphene oxide, for example, specific surface area from 100~
200m2/ g increases to 200~400m2/g。
Although having been combined exemplary embodiment above and describing the present invention, those of ordinary skill in the art should
It is clear, in the case where not departing from spirit and scope of the claims, above-described embodiment can be carry out various modifications.
Claims (8)
1. a kind of preparation facilities of low layer number graphene oxide, which is characterized in that the preparation facilities includes that hydrogel forms list
Member, low temperature drying unit and transport mechanism, wherein
The hydrogel, which forms unit, has a dispersion slot, the dispersion slot can receive graphene oxide with first number of plies and
Water, and graphene oxide is dispersed in water, to form graphene oxide hydrogel；
The low temperature drying unit have control temperature unit, pressure control unit and cold dry chamber, wherein the cold dry chamber be made of shell and
With feed inlet, discharge port and cavity, the control temperature unit be used for the control of the chamber intracorporal temperature as not higher than -50 DEG C and
The intracorporal temperature change of entire chamber is controlled no more than ± 4 DEG C, the pressure control unit, which is used to control the intracorporal pressure of the chamber, is
Lower than 1 atmospheric pressure and the entire intracorporal pressure change of chamber of control is no more than ± 100Pa；
The governor that the transport mechanism has the transmission parts for running through the cold dry chamber and can adjust transmission parts travel speed
Structure, the transmission parts are used to receive the hydrogel and form the graphene oxide hydrogel of unit formation and make the graphite oxide
Alkene hydrogel is after entire cold dry chamber, to obtain the graphene oxide with second number of plies, the second layer from the discharge port
Number is less than first number of plies.
2. the preparation facilities of low layer number graphene oxide according to claim 1, which is characterized in that the preparation facilities is also
Including the buffer area connecting with the discharge port, the buffer area can carry out the graphene oxide entered in it from discharge port
Heating.
3. the preparation facilities of low layer number graphene oxide according to claim 1, which is characterized in that the preparation facilities is also
Including connecting with the feed inlet and by the perforative pretreating zone of the transmission parts, the pretreating zone can be to entering in it
Graphene oxide hydrogel carries out cooling processing, so that the temperature of graphene oxide hydrogel is reduced and kept in the cavity
Temperature 1/6~3/5.
4. the preparation facilities of low layer number graphene oxide according to claim 1, which is characterized in that the preparation facilities is logical
The length of the cavity of the cold dry chamber of coordinated control, the cold speed for doing intracavitary temperature and pressure and transmission parts are crossed to obtain drying
The complete graphene oxide with second number of plies.
5. the preparation facilities of low layer number graphene oxide according to claim 1, which is characterized in that the control temperature unit will
It is described that the intracorporal temperature control of chamber is within the scope of -55~-65 DEG C and the entire intracorporal temperature change of chamber of control is no more than ± 2 DEG C.
6. the preparation facilities of low layer number graphene oxide according to claim 1, which is characterized in that the pressure control unit will
It is described that the intracorporal pressure control of chamber is in 10~100Pa and the entire intracorporal pressure change of chamber of control is no more than ± 10Pa.
7. the preparation facilities of low layer number graphene oxide according to claim 1, which is characterized in that the chamber of the cold dry chamber
Body is U-shaped or the annular of notch.
8. the preparation facilities of low layer number graphene oxide according to claim 1, which is characterized in that the hydrogel is formed
Unit also has ultrasonic generating mechanism, and the ultrasound generating mechanism emits ultrasonic wave to the dispersion slot, in dispersion slot
Water in graphene oxide formed ultrasonic vibration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811492027.1A CN109399628B (en) | 2018-12-07 | 2018-12-07 | Preparation facilities of low number of layers oxidation graphite alkene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811492027.1A CN109399628B (en) | 2018-12-07 | 2018-12-07 | Preparation facilities of low number of layers oxidation graphite alkene |
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| Publication Number | Publication Date |
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| CN109399628A true CN109399628A (en) | 2019-03-01 |
| CN109399628B CN109399628B (en) | 2021-03-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201811492027.1A Active CN109399628B (en) | 2018-12-07 | 2018-12-07 | Preparation facilities of low number of layers oxidation graphite alkene |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102849731A (en) * | 2012-09-07 | 2013-01-02 | 中国科学技术大学 | Nitrogen-doped graphene hydrogel, preparation method and applications thereof |
| CN103058179A (en) * | 2013-01-21 | 2013-04-24 | 张家港市东大工业技术研究院 | Method for preparing spongy graphene oxide by using freeze-drying method |
| CN103224228A (en) * | 2013-04-07 | 2013-07-31 | 怀化学院 | Selectively reduced graphene oxide and preparation method |
-
2018
- 2018-12-07 CN CN201811492027.1A patent/CN109399628B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102849731A (en) * | 2012-09-07 | 2013-01-02 | 中国科学技术大学 | Nitrogen-doped graphene hydrogel, preparation method and applications thereof |
| CN103058179A (en) * | 2013-01-21 | 2013-04-24 | 张家港市东大工业技术研究院 | Method for preparing spongy graphene oxide by using freeze-drying method |
| CN103224228A (en) * | 2013-04-07 | 2013-07-31 | 怀化学院 | Selectively reduced graphene oxide and preparation method |
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| CN109399628B (en) | 2021-03-26 |
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