CN108455589A - A kind of graphene oxide prepares reaction kettle - Google Patents
A kind of graphene oxide prepares reaction kettle Download PDFInfo
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- CN108455589A CN108455589A CN201810568855.2A CN201810568855A CN108455589A CN 108455589 A CN108455589 A CN 108455589A CN 201810568855 A CN201810568855 A CN 201810568855A CN 108455589 A CN108455589 A CN 108455589A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 180
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 70
- 238000003756 stirring Methods 0.000 claims abstract description 76
- 239000000376 reactant Substances 0.000 claims abstract description 51
- 230000009514 concussion Effects 0.000 claims abstract description 43
- 238000003801 milling Methods 0.000 claims description 21
- 238000009527 percussion Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 9
- 230000033001 locomotion Effects 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000010079 rubber tapping Methods 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 19
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 229910002804 graphite Inorganic materials 0.000 description 19
- 239000010439 graphite Substances 0.000 description 19
- 239000000203 mixture Substances 0.000 description 10
- 230000036632 reaction speed Effects 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 239000003921 oil Substances 0.000 description 6
- 239000013618 particulate matter Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 230000001020 rhythmical effect Effects 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- -1 graphite Alkene Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000033764 rhythmic process Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000010729 system oil Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention belongs to graphene oxides to prepare manufacturing technology field, and specifically a kind of graphene oxide prepares reaction kettle；Including shell, reaction container, commissioning pipe, collecting pipe, pillar, stirring module, concussion module and support spring；Reaction container is located at enclosure interior, and reaction container is used for reactant reaction；Commissioning pipe is located at reaction container top, and collecting pipe is located at reaction container lower end；Pillar is located at reaction container center；Stirring module is located on reaction container, and stirring module upper end is fixed on shell, and stirring module stirs and stirs module for reactant and provides power for concussion module；Concussion module is located at outside reaction container, and concussion module-external is connect with housing into rotation, and concussion module, which is used to tap reaction container, to be shaken；Support spring is located between concussion module and reaction container, and support spring is used to support reaction container；The present invention can be such that the raw material for preparing graphene oxide quickly fully reacts, and improve the preparation efficiency of graphene oxide.
Description
Technical field
The invention belongs to technical field of preparation of graphene oxide, specifically a kind of graphene oxide prepares reaction kettle.
Background technology
Graphene oxide thin slice is product of the powdered graphite after chemical oxidation and stripping, and graphene oxide is single original
Sublayer can expand to some tens of pm on lateral dimension at any time.Graphene oxide is usually with the potassium permanganate in the concentrated sulfuric acid
With powdered graphite is oxidized react after, obtain brown edge have derivative carboxylic acid group and in the plane be mainly phenolic hydroxyl group and
The graphite flake of epoxy group, it is graphene oxide that this graphene layers can be vigorously stirred stripping through ultrasound or high shear, and
Stable, sundown single-layer graphene oxide suspension is formed in water；Drying processing can be obtained graphene oxide；
Prepare and be generally stirred using magnetic stirring apparatus during graphene oxide, but prepare graphene oxide still take compared with
It is long, two days are needed at the soonest, and preparation efficiency is low；
Also occur the technical solution of some graphene oxide preparation facilities in the prior art, such as application No. is
A Chinese patent of CN201710855441 discloses a kind of integrated device and preparation method thereof preparing graphene oxide, packet
Include that " jacketed reactor for preparing the integrated device of graphene oxide is placed on magnetic stirring apparatus, and supersonic signal generator is placed in folder
Cover the top of reactor；The outer layer chuck of jacketed reactor is provided with inlet tube and outlet, and Subcooling water circulating system follows
Ring oil bath system is connected to inlet tube by corresponding outlet line respectively, and Subcooling water circulating system outlet line is provided with
Cooling water outlet switching valve, recycle oil bath system outlet line are provided with heating oil outlet switching valve；Low-temperature cooling water cyclic system
System, recycle oil bath system are connected to outlet, Subcooling water circulating system return piping by corresponding inlet line respectively
It is provided with return water switching valve, recycle oil bath system oil return pipeline is provided with oil return switching valve." technical solution by ultrasound, stirring
And oxidation process carries out in a reactor, but be only deposited in existing equipment supersonic signal generator and magnetic stirring apparatus
The ultrasound and agitating function for coming together to realize the device, to improve the preparation efficiency of graphene oxide, but the equipment mechanism is huge
It is big and complicated, using having inconvenience more.
In consideration of it, a kind of graphene oxide of the present invention prepares reaction kettle, prepared by graphene oxide of the present invention
Reaction kettle is simple in structure, and equipment volume is small, easy to use, and has stirring to the reactant for preparing graphene oxide preparation, rolls
With the effect of concussion, the reaction speed of reactant is accelerated, improves the preparation efficiency of graphene oxide.
Invention content
In order to make up for the deficiencies of the prior art, the present invention proposes a kind of graphene oxide and prepares reaction kettle, master of the present invention
It is used for the preparation of graphene oxide.Graphene oxide of the present invention prepares that reaction kettle is simple in structure, and equipment volume is small, uses
It is convenient；Meanwhile graphene oxide of the present invention prepares reaction kettle and makes graphene oxide in preparation process, reactant reaction
Object can be sufficiently stirred, rolled and be shaken so that prepare graphene oxide reactant can fast reaction, improve reaction
The reaction speed of object, to improve the preparation efficiency of graphene oxide.
The technical solution adopted by the present invention to solve the technical problems is：It is prepared by a kind of graphene oxide of the present invention
Reaction kettle, including shell, reaction container, commissioning pipe, collecting pipe, pillar, stirring module, concussion module and support spring；It is described anti-
Answer bucket position in enclosure interior, reaction container is used for reactant reaction；The commissioning pipe is located at reaction container top, and commissioning pipe is for launching
Reactant；The collecting pipe is located at reaction container lower end, and collecting pipe is used to collect the mixed solution after reaction；The pillar is located at anti-
Answer bucket central, pillar lower part is provided with heating rod, and heating rod is heated for reactant；The stirring module is located on reaction container,
Stirring module upper end is fixed on shell, and stirring module lower part is located in reaction container, stirring module for reactant stirring and
Stirring module provides power for concussion module；The concussion module is located at outside reaction container, shakes module-external and housing into rotation
Connection, concussion module top and reaction container elastic connection, concussion module, which is used to tap reaction container, to be shaken；The support spring position
Between concussion module and reaction container, support spring is used to support reaction container.
The stirring module includes motor, drive shaft, crank, bulb and stirring blade, and the motor is located at upper part of the housing,
The lower end of motor is connect with drive shaft upper end；The crank is fixedly connected with drive shaft lower end, and crank connects with the rotation of bulb upper end
It connects, crank-motion drives ball joint-rotating to swing；The bulb lower end is resisted against on pillar, and bulb is rotatablely connected with pillar, bulb
The regular swing around while rotation of rotation driving stirring blade；The stirring blade is fixed on bulb, stirring
The lower end of blade is not contacted with the bucket bottom of reaction container, and stirring blade is stirred for reactant.When work, motor drives driving shaft rotation
Dynamic, drive shaft drives bulb rotation and revolution by crank, that is, making bulb, regular inclination is put around while rotation
Dynamic rotation, bulb drive stirring blade regular swing rotary around while rotation, can preferably stir mixture
Mix uniformly, be unlikely to make mixture only by a centre of gyration rotation and so that particulate matter is all collected at the swirl center of rotation,
It can avoid reactant precipitation in this way so that stirring thing can be sufficiently stirred by stirring blade, improve the reaction efficiency of reactant.
The lower end of the stirring blade is provided with milling roller, and milling roller is rotatablely connected with stirring blade, and stirring blade is put
When moving to bottom, milling roller rolls the reactant of precipitation against the bucket bottom of reaction container, milling roller when against reaction container bucket bottom.
When work, stirring blade rotation simultaneously regular is swung around so that and milling roller is rhythmical to be resisted against on reaction container bucket bottom,
Also around drive shaft turns when being resisted against reaction container bucket bottom due to milling roller so that milling roller can will be deposited in reaction container bucket
The particulate matter at bottom pulverizes so that reactant reaction is more abundant, while also improving the reaction speed of reactant, promotes oxidation
Efficiency prepared by graphene.
The concussion module includes fixing barrel, stamp, resetting spring and turning barrel；The fixing barrel is sheathed on outside reaction container
Side, fixing barrel top and reaction container elastic connection, the lower end of fixing barrel is fixedly connected with the casing, on the bucket wall and bucket bottom of fixing barrel
It is evenly equipped with multiple mounting grooves；The stamp is provided with multiple, and stamp passes through the mounting groove of fixing barrel, stamp and fixing barrel
It is slidably connected；The resetting spring is located in mounting groove and reseting spring sleeve is on stamp, and resetting spring is used for stamp
Reset after percussion；The turning barrel is located on the outside of fixing barrel, and turning barrel upper end is fixedly connected with drive shaft, and turning barrel follows driving shaft rotation
Dynamic, turning barrel outer wall is connect with housing into rotation, the curved wall of turning barrel and the wall thickness consecutive variations at bucket bottom, is squeezed always at the heavy wall of turning barrel
Stamp end makes stamp resist the outer barrel wall of reaction container, detaches with stamp end at the thin-walled of turning barrel and does not contact always,
Turning barrel rotation driving stamp intermittent drumming reaction bucket outer surface.When work, drive shaft turns drive turning barrel rotation, turning barrel to turn
Dynamic that stamp is driven to do percussion movement to reaction container in fixing barrel, resetting spring resets stamp, the bucket bottom of reaction container and side
Wall will generate acutely concussion so that graphite and other mixtures in reactant are not easy to be attached on reaction container inner wall, especially
Be by some external moistenings and it is internal be also that dry graphite powder shakes off from the bucket wall of reaction container, be conducive to the suitable of reactant reaction
Profit carries out so that reaction is more abundant, improves reaction speed when prepared by graphene oxide；Meanwhile the violent shake of reaction container
It is dynamic, the graphite oxide in reaction later stage can be made to be removed into graphene oxide by concussion so that small amounts graphene has been generated at this time,
The efficiency for being conducive to be removed graphite oxide with ultrasonic wave, to improve the efficiency of graphene oxide preparation.
The percussion end of the stamp is provided with striking head, and striking head is fixedly connected with stamp；The striking head includes
Fixed plate, elasticity tap bar one, elasticity taps bar two and elasticity taps bar three；The elasticity taps bar one and grows in its natural state
Degree be shorter than elasticity tap bar two, elasticity tap bar two be shorter in length than in its natural state elasticity tap bar three, elasticity tap bar one,
Elasticity taps bar two and elasticity taps the length of bar three and can be compressed as equal length, and elasticity taps bar one, elasticity taps bar
Two is identical with the elasticity percussion structure of bar three, and elastic percussion bar one, elasticity tap bar two and elastic percussion bar three is vertically fixed
In striking head；It includes bar one, spring one and bar two that the elasticity, which taps bar three, and one end of the spring one is connect with bar one, bullet
The other end of spring one is fixedly connected with bar two, and the variation of one length of spring changes elasticity and taps three overall length of bar.When work, tap
Stick is tapped to reaction container outer wall, and because being provided with striking head on stamp, elasticity taps bar one, elasticity taps bar two and elasticity taps
The length of bar three is different, and elasticity taps the bucket wall of the first drumming reaction bucket of bar three, and later, elasticity taps bar three and compressed, and elasticity is struck
The bucket wall of two drumming reaction bucket of bar is hit, followed by, elasticity taps bar two and compressed, and elasticity taps the continuation of bar three and compressed, elasticity
One drumming reaction bucket of bar is tapped, i.e., when stamp drumming reaction bucket, striking head on stamp can continuous quick drumming reaction
Bucket three times, improves the frequency of stamp drumming reaction bucket, enhances the effect of reaction container concussion so that reactant is more not easy
It is attached on the bucket wall of reaction container, while more graphite oxides being made, at graphene oxide, to improve oxidation by concussion stripping
The preparation efficiency of graphene.
The beneficial effects of the invention are as follows：
1. a kind of graphene oxide of the present invention prepares reaction kettle, graphene oxide of the present invention prepares reaction kettle
Simple in structure, equipment volume is small, easy to use；The present invention passes through reaction container, pillar, stirring module, concussion module and support bullet
Spring cooperates with each other so for preparing the raw material of graphene oxide can be fast after being sufficiently stirred, rolling and acutely shake
Fast fully reaction, and can be during generating reaction product graphite oxide, it is graphite oxide that can remove partial oxidation of graphite
Alkene improves the preparation efficiency of graphene oxide；Meanwhile shaking module and sharing a motor with stirring module, save equipment
Production cost.
2. a kind of graphene oxide of the present invention prepares reaction kettle, the present invention passes through reaction container, pillar and stirring mould
Block cooperates with each other, pillar support stirring module, stir the stirring blade of module in reaction container while rotation to four
Week regular wallowing motion rotation so that the reactant of stirring will not avoid only in the centre of gyration rotation of a position
Bulk and granular reactant are collected at the swirl center of rotation, avoid reactant from precipitating so that reactant is able to abundant
Stirring, accelerates the reaction speed of reactant, improves the preparation efficiency of graphene oxide.
3. a kind of graphene oxide of the present invention prepares reaction kettle, the present invention passes through reaction container, support spring and shake
Cooperating with each other for module is swung, support spring supports reaction container, drives stamp to be moved back and forth in fixing barrel by turning barrel
Carry out drumming reaction bucket, and striking head is set on stamp, continuous quickly drumming reaction bucket three times, and draws multiple striking heads together
Resonance is played, the frequency of stamp drumming reaction bucket is improved, enhances the effect of reaction container concussion so that reactant is more not easy
It is attached on the bucket wall of reaction container, while more graphite oxides being made, at graphene oxide, to improve oxidation by concussion stripping
The preparation efficiency of graphene.
Description of the drawings
The invention will be further described below in conjunction with the accompanying drawings.
Fig. 1 is that the graphene oxide of the present invention prepares reaction kettle structural schematic diagram；
Fig. 2 is the striking head structural schematic diagram of the present invention；
Fig. 3 is the turning barrel structural schematic diagram of the present invention；
Fig. 4 is the A-A sectional views about Fig. 4；
In figure：Shell 1, commissioning pipe 3, collecting pipe 4, pillar 5, heating rod 51, stirring module 6, motor 61, drives reaction container 2
Moving axis 62, crank 63, bulb 64, stirring blade 65, milling roller 66, concussion module 7, fixing barrel 71, stamp 72, resetting spring
73, turning barrel 74, striking head 75, fixed plate 751, elasticity tap bar 1, elasticity taps bar 2 753, elasticity taps bar 3 754,
Support spring 8.
Specific implementation mode
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention be easy to understand, tie below
Specific implementation mode is closed, the present invention is further explained.
As shown in Figs 1-4, a kind of graphene oxide prepares reaction kettle, including shell 1, reaction container 2, commissioning pipe 3, receipts
Collector 4, pillar 5, stirring module 6, concussion module 7 and support spring 8；The reaction container 2 is located inside shell 1, and reaction container 2 is used
In reactant reaction；The commissioning pipe 3 is located at 2 top of reaction container, and commissioning pipe 3 is for launching reactant；The collecting pipe 4 is located at
2 lower end of reaction container, collecting pipe 4 are used to collect the mixed solution after reaction；The pillar 5 is located at the center of reaction container 2, under pillar 5
Portion is provided with heating rod 51, and heating rod 51 is heated for reactant；The stirring module 6 is located on reaction container 2, stirs module 6
Upper end is fixed on shell 1, and 6 lower part of stirring module is located in reaction container 2, and stirring module 6 is stirred and stirred for reactant
Module 6 is that concussion module 7 provides power；The concussion module 7 is located at outside reaction container 2,1 turn of concussion module 7 outside and shell
Dynamic connection, concussion 7 top of module and 2 elastic connection of reaction container, concussion module 7, which is used to tap reaction container 2, to be shaken；The support
Spring 8 is located between concussion module 7 and reaction container 2, and support spring 8 is used to support reaction container 2.
The stirring module 6 includes motor 61, drive shaft 62, crank 63, bulb 64 and stirring blade 65, the motor 61
Positioned at 1 top of shell, the lower end of motor 61 is connect with 62 upper end of drive shaft；The crank 63 is fixed with 62 lower end of drive shaft to be connected
It connects, crank 63 is rotatablely connected with 64 upper end of bulb, and the movement of crank 63 drives 64 rotary oscillation of bulb；64 lower end of the bulb against
On pillar 5, bulb 64 is rotatablely connected with pillar 5, and the rotation of bulb 64 driving stirring blade 65 has around while rotation
The swing of rule；The stirring blade 65 is fixed on bulb 64, and the lower end of stirring blade 65 does not connect with the bucket bottom of reaction container 2
It touches, stirring blade 65 is stirred for reactant.When work, motor 61 drives drive shaft 62 to rotate, and drive shaft 62 passes through crank 63
Drive 64 rotation of bulb and revolution, that is, make bulb 64 regular wallowing motion rotation around, bulb 64 while rotation
The regular swing rotary around while rotation of stirring blade 65 is driven, can preferably be stirred the mixture for uniformly, no
It is avoidable in this way as making mixture only so that particulate matter is all collected at the swirl center of rotation by the rotation of centre of gyration
Reactant precipitates so that stirring thing can be sufficiently stirred by stirring blade 65, improve the reaction efficiency of reactant.
The lower end of the stirring blade 65 is provided with milling roller 66, and milling roller 66 is rotatablely connected with stirring blade 65, and is stirred
When mixing blade 65 and swinging to bottom, milling roller 66 is against the bucket bottom of reaction container 2, and milling roller 66 is when against 2 barrels of bottoms of reaction container
Roll the reactant of precipitation.When work, the rotation of stirring blade 65 simultaneously regular is swung around so that milling roller 66 has rhythm
Be resisted against on 2 barrels of bottoms of reaction container, also rotate, make around drive shaft 62 when being resisted against 2 barrels of bottoms of reaction container due to milling roller 66
The particulate matter for being deposited in 2 barrels of bottoms of reaction container can be pulverized by obtaining milling roller 66 so that reactant reaction is more abundant, while also carrying
The high reaction speed of reactant, promotes the efficiency of graphene oxide preparation.
The concussion module 7 includes fixing barrel 71, stamp 72, resetting spring 73 and turning barrel 74；71 sets of the fixing barrel
Set on 2 outside of reaction container, 71 top of fixing barrel and 2 elastic connection of reaction container, the lower end of fixing barrel 71 are fixedly connected with shell 1,
It is evenly equipped with multiple mounting grooves 711 on the bucket wall of fixing barrel 71 and bucket bottom；The stamp 72 is provided with multiple, and stamp 72 passes through
The mounting groove 711 of fixing barrel 71, stamp 72 are slidably connected with fixing barrel 71；The resetting spring 73 is located in mounting groove 711
And 73 sets of resetting spring is on stamp 72, resetting spring 73 is for the reset after the percussion of stamp 72；The turning barrel 74
In 71 outside of fixing barrel, 74 upper end of turning barrel is fixedly connected with drive shaft 62, and turning barrel 74 follows drive shaft 62 to rotate, 74 outer wall of turning barrel
It is rotatablely connected with shell 1, the curved wall of turning barrel 74 and the wall thickness consecutive variations at bucket bottom, stamp is squeezed always at the heavy wall of turning barrel 74
72 ends make stamp 72 resist the outer barrel wall of reaction container 2, detach with 72 end of stamp at the thin-walled of turning barrel 74 and do not connect always
It touches, 72 intermittent 2 outer surface of drumming reaction bucket of the rotation driving stamp of turning barrel 74.When work, the rotation of drive shaft 62 drives turning barrel
74 rotations, the rotation of turning barrel 74 drive stamp 72 to do percussion movement to reaction container 2 in fixing barrel 71, and the reset of resetting spring 73 is struck
Stick 72 is hit, bucket bottom and the side wall of reaction container 2 will generate acutely concussion so that graphite and other mixtures in reactant are not easy
It is attached on 2 inner wall of reaction container, especially that some external moistenings are internal is also dry graphite powder from the bucket wall of reaction container 2
It shakes off, is conducive to being smoothed out for reactant reaction so that reaction is more abundant, improves reaction when prepared by graphene oxide
Speed；Meanwhile the strenuous vibration of reaction container 2, the graphite oxide in reaction later stage can be made to be removed into graphene oxide by concussion so that
Small amounts graphene has been generated at this time, is conducive to the efficiency that graphite oxide is removed with ultrasonic wave, to improve graphite oxide
Efficiency prepared by alkene.
The percussion end of the stamp 72 is provided with striking head 75, and striking head 75 is fixedly connected with stamp 72；It is described to strike
Tap the head 75 include fixed plate 751, elasticity tap bar 1, elasticity tap bar 2 753 and elasticity tap bar 3 754；The elasticity
It taps bar 1 and is shorter in length than elasticity percussion bar 2 753 in its natural state, elasticity taps bar 2 753 and grows in its natural state
Degree is shorter than elasticity and taps bar 3 754, and elasticity taps bar 1, elasticity taps bar 2 753 and elasticity taps the length of bar 3 754
It can be compressed as equal length, and elasticity taps bar 1, elasticity taps bar 2 753 and elasticity taps the structure phase of bar 3 754
Together, elasticity taps bar 1, elasticity taps bar 2 753 and elasticity taps bar 3 754 and is perpendicularly fixed at fixed plate 751；It is described
It includes bar one, spring one and bar two that elasticity, which taps bar 3 754, and one end of the spring one connect with bar one, spring one it is another
End is fixedly connected with bar two, and the variation of one length of spring changes elasticity and taps 3 754 overall length of bar.When work, stamp 72 to
2 outer wall of reaction container taps, and because being provided with striking head 75 on stamp 72, elasticity taps bar 1, elasticity taps 2 753 and of bar
The length that elasticity taps bar 3 754 is different, and the bucket wall of 3 754 first drumming reaction bucket 2 of elasticity percussion bar, later, elasticity taps bar
3 754 are compressed, and elasticity taps the bucket wall of 2 753 drumming reaction bucket 2 of bar, and followed by, elasticity taps bar 2 753 and compressed, bullet
Property tap bar 3 754 continuation compressed, elasticity tap one 752 drumming reaction bucket 2 of bar, i.e., when 72 drumming reaction bucket 2 of stamp,
Striking head 75 on stamp 72 continuously three times, can improve the frequency of 72 drumming reaction bucket 2 of stamp by quick drumming reaction bucket 2
Rate enhances the effect of the concussion of reaction container 2 so that reactant is more not easy to be attached on the bucket wall of reaction container 2, while making more
More graphite oxides, at graphene oxide, improves the preparation efficiency of graphene oxide by concussion stripping.
Concrete operations flow is as follows：
In use, being fed intake into reaction container 2 with commissioning pipe 3, reaction container 2 is given by the heating rod 51 of 5 lower part of pillar later
Inside rise to required temperature；Start motor 61, make motor 61 that drive shaft 62 be driven to rotate, drive shaft 62 drives bulb by crank 63
64 rotations and revolution, that is, making bulb 64, regular swing rotary, bulb 64 drive stirring blade around while rotation
The 65 regular swings around while rotation, can stir the mixture for well uniformly, be unlikely to make mixture only by
One centre of gyration rotates and so that particulate matter is all collected at the swirl center of rotation, can avoid reactant precipitation in this way so that
Stirring thing can be sufficiently stirred by stirring blade 65, improve the reaction efficiency of reactant；When stirring blade 65 stirs, paddle
Piece 65 is rotated and regular is swung around so that milling roller 66 is rhythmical to be resisted against on 2 barrels of bottoms of reaction container, due to rolling
Roller 66 is also rotated around drive shaft 62 when being resisted against 2 barrels of bottoms of reaction container so that milling roller 66 can will be deposited in 2 barrels of reaction container
The particulate matter at bottom pulverizes so that reactant reaction is more abundant, while also improving the reaction speed of reactant, promotes oxidation
Efficiency prepared by graphene；After motor 61 drives drive shaft 62 to rotate, the rotation of drive shaft 62 also will drive turning barrel 74 to rotate, and turn
74 rotation of bucket drives stamp 72 to do percussion movement to reaction container 2 in fixing barrel 71, and resetting spring 73 resets stamp 72, instead
The bucket bottom and side wall for answering bucket 2 will generate acutely concussion so that graphite powder and other mixtures in reactant are not easy to be attached to
On 2 inner wall of reaction container, especially that some external moistenings are internal is also that dry graphite powder shakes off from the bucket wall of reaction container 2,
Be conducive to being smoothed out for reactant reaction so that reaction is more abundant, improves reaction speed when prepared by graphene oxide；
Meanwhile the strenuous vibration of reaction container 2, the graphite oxide in reaction later stage can be made to be removed into graphene oxide by concussion so that at this time
Small amounts graphene has been generated, has been conducive to the efficiency for removing graphite oxide with ultrasonic wave, to improve graphene oxide system
Standby efficiency；In tapping board drumming reaction 2 outer wall of bucket, because being provided with striking head 75 on stamp 72, elasticity taps bar one
752, elasticity taps bar 2 753 and the elastic length for tapping bar 3 754 is different, and elasticity taps 3 754 elder generation's drumming reaction bucket 2 of bar
Bucket wall, later, elasticity tap bar 3 754 and are compressed, and elasticity taps the bucket wall of 2 753 drumming reaction bucket 2 of bar, followed by, elasticity
It taps bar 2 753 to be compressed, elasticity taps the continuation of bar 3 754 and compressed, and elasticity taps one 752 drumming reaction bucket 2 of bar, i.e., ought strike
When hitting 72 drumming reaction bucket 2 of stick, the striking head 75 on stamp 72 continuously three times, can improve percussion by quick drumming reaction bucket 2
The frequency of 72 drumming reaction bucket 2 of stick enhances the effect of the concussion of reaction container 2 so that reactant is more not easy to be attached to reaction container 2
Bucket wall on, while make more graphite oxides by concussion stripping at graphene oxide, improve the preparation of graphene oxide
Efficiency；After the completion of graphene to be oxidized prepares in reaction kettle mixed solution reaction, mixed solution is taken out with collecting pipe 4, is continued
Carry out next step operation.
The basic principles, main features and advantages of the invention have been shown and described above.The technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe the originals of the present invention
Reason, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes and improvements
It all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its equivalent circle
It is fixed.
Claims (5)
1. a kind of graphene oxide prepares reaction kettle, it is characterised in that：Including shell (1), reaction container (2), commissioning pipe (3), receive
Collector (4), pillar (5), stirring module (6), concussion module (7) and support spring (8)；The reaction container (2) is located at shell (1)
Inside, reaction container (2) are used for reactant reaction；The commissioning pipe (3) is located at reaction container (2) top, and commissioning pipe (3) is for launching
Reactant；The collecting pipe (4) is located at reaction container (2) lower end, and collecting pipe (4) is used to collect the mixed solution after reaction；It is described
Pillar (5) is located at reaction container (2) center, and pillar (5) lower part is provided with heating rod (51), and heating rod (51) adds for reactant
Heat；The stirring module (6) is located on reaction container (2), and stirring module (6) stirs and stirs module (6) for reactant and is
It shakes module (7) and power is provided；The concussion module (7) is located at reaction container (2) outside, shakes module (7) top and reaction container
(2) elastic connection, concussion module (7), which is used to tap reaction container (2), to be shaken；The support spring (8) is located at concussion module (7)
Between reaction container (2), support spring (8) is used to support reaction container (2).
2. a kind of graphene oxide according to claim 1 prepares reaction kettle, it is characterised in that：The stirring module (6)
Including motor (61), drive shaft (62), crank (63), bulb (64) and stirring blade (65), the motor (61) is located at shell
(1) lower end on top, motor (61) is connect with drive shaft (62) upper end；The crank (63) is fixed with drive shaft (62) lower end to be connected
It connects, crank (63) is rotatablely connected with bulb (64) upper end, and crank (63) movement drives bulb (64) rotary oscillation；The bulb
(64) lower end is resisted against on pillar (5), and bulb (64) is rotatablely connected with pillar (5), bulb (64) rotation driving stirring blade
(65) the regular swing around while rotation；The stirring blade (65) is fixed on bulb (64), stirring blade
(65) lower end is not contacted with the bucket bottom of reaction container (2), and stirring blade (65) is stirred for reactant.
3. a kind of graphene oxide according to claim 2 prepares reaction kettle, it is characterised in that：The stirring blade (65)
Lower end be provided with milling roller (66), milling roller (66) is rotatablely connected with stirring blade (65), and stirring blade (65) is swung to
When bottom, against the bucket bottom of reaction container (2), it is heavy that milling roller (66) rolls milling roller (66) when against reaction container (2) bucket bottom
The reactant in shallow lake.
4. a kind of graphene oxide according to claim 2 prepares reaction kettle, it is characterised in that：The concussion module (7)
Including fixing barrel (71), stamp (72), resetting spring (73) and turning barrel (74)；The fixing barrel (71) is sheathed on reaction container
(2) outside, fixing barrel (71) top and reaction container (2) elastic connection, the lower end of fixing barrel (71) are fixedly connected with shell (1),
Multiple mounting grooves (711) are evenly equipped on the bucket wall of fixing barrel (71) and bucket bottom；The stamp (72) is provided with multiple, stamp
(72) mounting groove (711) of fixing barrel (71), stamp (72) is passed through to be slidably connected with fixing barrel (71)；The resetting spring
(73) it is located in mounting groove (711) and resetting spring (73) set is on stamp (72) that resetting spring (73) is used for stamp
(72) reset after tapping；The turning barrel (74) is located on the outside of fixing barrel (71), and turning barrel (74) upper end is fixed with drive shaft (62)
Connection, turning barrel (74) outer wall are rotatablely connected with shell (1), the curved wall of turning barrel (74) and the wall thickness consecutive variations at bucket bottom, turning barrel
(74) outer barrel wall that stamp (72) end makes stamp (72) resist reaction container (2), turning barrel (74) are squeezed at heavy wall always
Thin-walled at do not contacted with the separation of stamp (72) end always, turning barrel (74) rotation driving stamp (72) is intermittent tap it is anti-
Answer bucket (2) outer surface.
5. a kind of graphene oxide according to claim 4 prepares reaction kettle, it is characterised in that：The stamp (72)
It taps end and is provided with striking head (75), striking head (75) is fixedly connected with stamp (72)；The striking head (75) includes tapping
Head (751), elasticity tap bar one (752), elasticity taps bar two (753) and elasticity taps bar three (754)；The elasticity taps bar
One (752) are shorter in length than elasticity and tap bar two (753) in its natural state, and elasticity taps bar two (753) and grows in its natural state
Degree is shorter than elasticity and taps bar three (754), and elasticity taps bar one (752), elasticity taps bar two (753) and elasticity taps bar three
(754) length can be compressed as equal length, and elasticity taps bar one (752), elasticity taps bar two (753) and elasticity percussion
The structure of bar three (754) is identical, and elasticity percussion bar one (752), elasticity tap bar two (753) and elasticity taps bar three (754)
It is perpendicularly fixed at striking head (751)；It includes bar one, spring one and bar two that the elasticity, which taps bar three (754), the spring one
One end is connect with bar one, and the other end of spring one is fixedly connected with bar two, and the variation of one length of spring changes elasticity and taps bar three
(754) overall length.
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| CN111994903A (en) * | 2020-08-28 | 2020-11-27 | 西安近代化学研究所 | Synthetic method of 3-aminopropyltriethoxysilane modified graphene oxide |
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Application publication date: 20180828 |