CN106044761B - Prepare the high shear force abrasive rubber mill and its preparation method and application of graphene - Google Patents
Prepare the high shear force abrasive rubber mill and its preparation method and application of graphene Download PDFInfo
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Abstract
A kind of high shear force abrasive rubber mill and its preparation method and application preparing graphene, driving mechanism including upper millstone, lower millstone and driving upper millstone rotation, the upper millstone is that upper mill body bottom portion is connected and fixed abrasive rubber upper millstone, and the lower millstone is that lower mill bodies top is connected and fixed abrasive rubber lower millstone.The abrasive rubber upper millstone is that synthetic rubber and/or natural rubber are prepared, and the abrasive rubber lower millstone is that synthetic rubber and/or natural rubber are prepared.The upper and lower mill frictional force of abrasive rubber of the invention is big, it is high-efficient to remove graphite, and gained graphene thickness is thin, the upper and lower mill of abrasive rubber is based on pure shear shear force, impact force is small, the destruction caused by graphite lattice can be effectively avoided, graphene-structured defect is reduced, graphene quality obtained is high.
Description
Technical field
The present invention relates to technical field of graphene preparation more particularly to a kind of high shear force abrasive rubbers for preparing graphene
Mill and its preparation method and application.
Background technique
Graphene causes the extensive concern of countries in the world scientist by its unique property, becomes research in recent years
Hot spot.The preparation method of graphene mainly has mechanical stripping method, graphite oxide-reduction method, chemical vapour deposition technique, extension at present
Growth method etc. is capable of the method for large-scale production graphene, mainly graphite oxide-reduction method at present, but graphite oxide-is also
During redox, the electronic structure and perfection of crystal of graphene are easy to be broken by strong oxidizer former method
It is bad, cause the structure of graphene to have the defects that more, and lead to its part electricity, thermal property loss；Therefore there is an urgent need to
Develop a kind of low cost, high quality, prepare with scale graphene method.
It is compared with other methods, mechanical stripping method is simplest method, is easy to get the graphene of high quality, machinery stripping
There are huge potentiality from method, the maximum feature that Mechanical Method prepares graphene is exactly not carry out oxygen to graphite in stripping process
Change effect, avoids poisonous and hazardous chemical reagent and the destruction to graphene crystal required for chemical method, therefore can
The graphene of acquisition high quality, preparation method simple process, process are easily controllable；But existing mechanical stripping graphite preparation
Graphene efficiency is lower, for example, traditional ball-grinding machine for preparing graphene, mainly using stainless shot, zirconium pearl, ceramic bead etc.
Material is situated between as mill, and graphite is ground in machinery rotation, there are the contact surface between pearl and pearl is smaller, imitates to the removing of graphite
Fruit is bad, secondly, existing ball-grinding machine while also being brought very big to graphite other than providing the shearing force of removing graphite
Impact force, graphite flake unavoidably receive the intense impact of abrading-ball, cause some faults of construction；Pure shear can be thus provided
The grinding method of power is taken seriously, and Chinese patent 201410567235, which discloses to mill, removes the side that graphite device prepares graphene
Method, using horizontal contact surface is formed between upper and lower mill, upper and lower mill is at it close to one end covering one in the face that contacts with each other
Layer wear-resistant ceramic or wear-resistant plastic layer, are rotated by upper lower millstone, grind graphite flake layer in parallel, to make graphene to protect
The mode for holding the original lamella size of graphite is stripped out, and reduces burr and fault of construction, the more general ball-milling method of the method
It improves to some extent, reduces the impact force to graphite, it is advantageous to high-quality graphene is prepared, but the device mill is by ceramic or resistance to
It grinds plastic layer to constitute, enough frictional force is not provided, it is still limited to graphite removing, in view of this, it is necessary to existing skill
The method that grinding method in art prepares graphene is improved, and the milling device for seeking sufficiently large frictional force is necessary, with
It solves the above problems.It is had not been reported with abrasive rubber production mill removing preparing graphite alkene.
Summary of the invention
The technical problems to be solved by the present invention are: solving the above-mentioned problems of the prior art, and provide a kind of prepare
High shear force abrasive rubber mill of graphene and its preparation method and application, the upper and lower contact surface layer of abrasive rubber layer of mill
Frictional force is big, and removing graphite is high-efficient, and gained graphene thickness is thin, the upper and lower mill of abrasive rubber based on pure shear shear force,
Impact force is small, can effectively avoid the destruction caused by graphite lattice, reduces graphene-structured defect, graphene quality obtained
It is high.
The technical solution adopted by the present invention is that:
A kind of high shear force abrasive rubber mill preparing graphene, including upper millstone, lower millstone and driving upper millstone turn
Dynamic driving mechanism, the upper millstone are that upper mill body bottom portion is connected and fixed abrasive rubber upper millstone, and the lower millstone is lower mill
Bodies top is connected and fixed abrasive rubber lower millstone.
In above-mentioned technical proposal, the upper mill ontology and lower mill ontology are metal component.
In above-mentioned technical proposal, the abrasive rubber upper millstone is that synthetic rubber and/or natural rubber are prepared, institute
Stating abrasive rubber lower millstone is that synthetic rubber and/or natural rubber are prepared.
In above-mentioned technical proposal, the bottom surface of the abrasive rubber upper millstone and the top surface of abrasive rubber lower millstone are with recessed
Flute profile grinds line.
A kind of preparation method for the high shear force abrasive rubber mill preparing graphene, comprising:
1, the upper mill ontology of metal and the lower mill ontology of metal are prepared with metal machining common process；
2, abrasive rubber upper millstone and abrasive rubber lower millstone are prepared using abrasive rubber, by the upper and lower mill ontology of metal
Be fixed on be carved with tongue shape mill line metal die in, casting or molding abrasive rubber, solidify, demoulding, can be obtained with above and below
Grind the upper and lower mill with groove type mill line of bulk adhesive together；
3, upper and lower mill is mounted in milling device；
4, motor, speed reducer and transmission mechanism are installed, i.e. composition grinding mill.
In above-mentioned technical proposal, the abrasive rubber is prepared using synthetic rubber and/or natural rubber.
In above-mentioned technical proposal, the synthetic rubber includes one of following or a variety of: polyurethane rubber, butylbenzene rubber
Glue, butadiene rubber, butyl rubber, neoprene, polysulfide rubber, lactoprene, chlorosulfonated polyethylene rubber, silicon rubber
Glue, fluorubber, nitrile rubber, isoprene rubber, EP rubbers.
In above-mentioned technical proposal, using polyurethane wear resistant rubber system for abrasive rubber upper millstone and abrasive rubber lower millstone
Method is as follows:
Polyurethane elastomer can be in wider hardness range elasticity with higher and intensity, excellent wearability, oil resistant
Property, fatigue durability and anti-vibration resistance, the title with " abrasive rubber ", due to rubber friction coefficient all than steel, rock, plastics,
Grinding wheel, ceramics are big, that is, the shearing force for providing removing graphite is big, are suitable for the mill material of removing graphite, specific production method is such as
Under:
(1) polytetramethylene glycol is dehydrated:
In the there-necked flask for being equipped with blender, thermometer, vacuum adapter, suitable polytetramethylene glycol is added, rises
Temperature after being dehydrated the h of 2 h~3 under the MPa vacuum degree of 0.08 MPa~0.09, is cooled to 40 to 100 DEG C~140 DEG C
DEG C~60 DEG C, for use；
(2) performed polymer synthesizes:
Suitable dewatered polytetramethylene glycol and toluene di-isocyanate(TDI) is added by formula ratio in there-necked flask
(TDI), polytetramethylene glycol: TDI=1:0.18-0.28(mass ratio), it is warming up to 80-85 DEG C after mixing evenly, keeps
This temperature makes it react 2h, deaeration 15-30 min, discharging, closed preservation；
(3) preparation of upper and lower mill:
Upper and lower mill mold is preheated to 80-100 DEG C, the glue consumption of mill product is calculated, by the performed polymer liter of metering
Temperature is to 80 DEG C~90 DEG C, vacuum defoamation 15 min~40 min；Then, the 3,3- bis- chloro- 4 that will be measured and melt,
4- diaminodiphenyl-methane (MOCA) is added in above-mentioned performed polymer, and MOCA inventory is by polytetramethylene glycol: MOCA=
1:0.16-0.25(mass ratio) meter, it quickly stirs evenly, is poured into rapidly to be coated with release agent and be preheated and is carved with tongue shape mill
It in the mold of line, is put into blast dry oven at once, the after cure h of 3 h~10 at a temperature of 100 DEG C~110 DEG C,
Reaction is set to tend to be complete；Cooling and mould unloading is to get the upper and lower mill of abrasive rubber together with upper and lower mill bulk adhesive.
In above-mentioned technical proposal, abrasive rubber upper millstone and abrasive rubber are mixed with using natural rubber and synthetic rubber
The method of lower millstone is as follows:
1) it is formulated: mass ratio, rubber 100: natural rubber 46-50, butadiene rubber 50-54, promotor 1-2, vulcanization
Agent 1-2, zinc oxide 4-6, anti-aging agent 2-3, appropriate softening agent, abrasion furnace blacks 50-58；
2) manufacture craft mainly by plasticating, ingredient, mixing, calendering, molding, vulcanization routine operation form, pass through above-mentioned behaviour
Make to obtain and grinds the upper and lower mill of abrasive rubber together with bulk adhesive above and below.
Abrasive rubber and upper and lower mill ontology during rubber system is standby, when casting just automatically with the upper and lower mill ontology of metal
Bonding, does not need other fixation.
The method for preparing graphene using high shear force abrasive rubber mill of the invention is as follows:
By the upper and lower mill product of the abrasive rubber made, installation is fixed on grinding mill, can carry out graphene preparation
It mills operation；A certain amount of neopelex, sodium carboxymethylcellulose, OP-10 compounding dispersing agent and one are weighed first
The deionized water of fixed number amount, is uniformly mixed, the concentration 0.4-1.0mg/ml of dispersing agent, be added a certain amount of crystalline flake graphite or
Expanded graphite, expansible graphite, the concentration 20-40mg/ml of graphite, are uniformly mixed, and then start grinding mill, slowly gradually
Graphite suspension is added, after graphite suspension adds, graphite suspension is re-started and is milled for the second time, repetitive cycling operation,
After milling 6-30 hours, stop operation；Material is taken out, is centrifuged, centrifugal rotational speed is set as 4000-9000 revs/min,
Time 5-30 minute, the unstripped graphite of removal centrifugation bottom of the tube return to raw material of milling next time, obtain graphite dispersing solution,
It can directly apply, or be dried to obtain graphene powder, through detecting, graphene number of plies is less than 10 layers.
The principle of the present invention:
Graphite has layer structure, and in layer, carbon atom arrangement is at hexagon, with Covalent bonding together between atom, in conjunction with
Power is very strong, forms the reticular structure of plane, between the layers, is combined by weaker Van der Waals force, easily sliding and
Removing, therefore under suitable extruding and rubbing action, graphite, which shows as pole, will be completely dissociated, and the size of frictional force is to removing stone
Black effect generates different influences, and the big removing graphite effect of frictional force is high, on the contrary then low, the size source of milling device frictional force
Material in the surface of upper and lower mill contact, different materials have different frictional force, and unlike material friction pair material rubs
Wipe coefficient: steel-steel 0.1, wear-resistant plastic such as polyamide (nylon66 fiber) 0.12-0.25, polytetrafluoroethylene (PTFE) 0.04, ceramic material
Material about 0.2, the coefficient of friction of polyurethane rubber is 0.9, nitrile rubber 1.5, the third rubber of second 1.2, fluorubber 0.85；So far
The mill material majority of existing milling device is steel, followed by stone material and grinding wheel, and plastic applications are less, and rubber, which there are no, answers
With；It is well known that ordinary rubber coefficient of friction is all than steel, rock, plastics such as polytetrafluoroethylene (PTFE) and nylon, grinding wheel, ceramics
Deng big；Graphite has excellent greasy property, itself has self-lubrication, is difficult to remove graphite system without enough shearing forces
Standby graphene.The present invention feature big using the coefficient of friction of rubber, provides powerful shearing force, using abrasive rubber as raw material system
Standby upper and lower mill, is rotated by upper lower millstone, grinds graphite flake layer in parallel, and circumferential sufficiently large frictional force is provided, so that tool
There is the graphite of weak interlayer structure under the action of mill generates powerful shearing force field, realizes graphite layers removing, gained graphene
Thickness compares book；Since rubber friction power is big, removing graphite efficiency it is higher than the mill that other materials make, and due to mill with
Based on pure shear shear force, impact force very little can be effectively prevented from and hit the destruction caused by graphite lattice, reduce graphene-structured
High-quality graphene can be made in defect.
Using caused by above-mentioned technical proposal of the present invention the utility model has the advantages that
1, the present invention makees mill removing graphite using abrasive rubber, and mill is based on pure shear shear force, impact force very little, reduces
Graphene-structured defect, can be made high-quality graphene；
2, the present invention does not need oxidation-reduction method and prepares a large amount of inorganic acid and oxidant needed for graphene, to environment without dirt
Dye；
3, preparation process is simple, and equipment is few, normal temperature and pressure, small investment, is suitable for scale industrial production；
4, since rubber friction power is big, removing graphite efficiency is more high-efficient than the mill that other materials make, can be with high efficiency
Produce graphene；
5, production cost is low, is conducive to downstream product development.
Detailed description of the invention
Fig. 1 is schematic structural view of the invention.
Appended drawing reference: 1-lower mill ontology, 2-abrasive rubber lower millstones, 3-abrasive rubber upper millstones, 4-upper mills are originally
Body, 5-charge pipes, 6-rotation axis.
Specific embodiment:
Referring to Fig. 1, the high shear force abrasive rubber mill for preparing graphene of the invention, including upper millstone, lower millstone and
The driving mechanism of upper millstone rotation is driven, the upper millstone is that upper mill body bottom portion is connected and fixed abrasive rubber upper millstone, described
Lower millstone is that lower mill bodies top is connected and fixed abrasive rubber lower millstone, and the upper mill ontology and lower mill ontology are metal component,
The abrasive rubber upper millstone is that synthetic rubber and/or natural rubber are prepared, and the abrasive rubber lower millstone is synthesis
Rubber and/or natural rubber are prepared, and the bottom surface of the abrasive rubber upper millstone and the top surface of abrasive rubber lower millstone have
Groove type grinds line.
A kind of preparation method for the high shear force abrasive rubber mill preparing graphene, comprising:
1, the upper mill ontology of metal and the lower mill ontology of metal are prepared with metal machining common process；
2, abrasive rubber upper millstone and abrasive rubber lower millstone are prepared using abrasive rubber, by the upper and lower mill ontology of metal
Be fixed on be carved with tongue shape mill line metal die in, casting or molding abrasive rubber, solidify, demoulding, can be obtained with above and below
Grind the upper and lower mill with groove type mill line of bulk adhesive together；
3, upper and lower mill is mounted in milling device；
4, motor, speed reducer and transmission mechanism are installed, i.e. composition grinding mill；
The abrasive rubber is prepared using synthetic rubber and/or natural rubber, under the synthetic rubber includes
It one of states or a variety of: polyurethane rubber, butadiene-styrene rubber, butadiene rubber, butyl rubber, neoprene, polysulfide rubber, poly- third
Olefin(e) acid ester rubber, chlorosulfonated polyethylene rubber, silicon rubber, fluorubber, nitrile rubber, isoprene rubber, EP rubbers.Using poly- ammonia
The method that ester abrasive rubber prepares upper and lower mill is as follows:
Polyurethane elastomer can be in wider hardness range elasticity with higher and intensity, excellent wearability, oil resistant
Property, fatigue durability and anti-vibration resistance, the title with " abrasive rubber ", due to rubber friction coefficient all than steel, rock, plastics,
Grinding wheel, ceramics are big, that is, the shearing force for providing removing graphite is big, are suitable for the millstone device of removing graphite, specific production method is such as
Under:
(1) polytetramethylene glycol is dehydrated:
In the there-necked flask for being equipped with blender, thermometer, vacuum adapter, suitable polytetramethylene glycol is added, rises
Temperature after being dehydrated the h of 2 h~3 under the MPa vacuum degree of 0.08 MPa~0.09, is cooled to 40 to 100 DEG C~140 DEG C
DEG C~60 DEG C, for use；
(2) performed polymer synthesizes:
Suitable dewatered polytetramethylene glycol and toluene di-isocyanate(TDI) is added by formula ratio in there-necked flask
(TDI), polytetramethylene glycol: TDI=1:0.18-0.28(mass ratio), it is warming up to 80-85 DEG C after mixing evenly, keeps
This temperature makes it react 2h, deaeration 15-30 min, discharging, closed preservation；
(3) preparation of upper and lower mill:
Mill mold is preheated to 80-100 DEG C, the glue consumption of mill product is calculated, the performed polymer of metering is warming up to
80 DEG C~90 DEG C, vacuum defoamation 15 min~40 min；Then, the chloro- 4,4- bis- of 3,3- bis- that will be measured and melt
Aminodiphenylmethane (MOCA) is added in above-mentioned performed polymer, and MOCA inventory presses polytetramethylene glycol: MOCA=1:
0.16-0.25(mass ratio) meter, it quickly stirs evenly, is poured into rapidly to be coated with release agent and be preheated and is carved with tongue shape mill line
Mold in, be put into blast dry oven at once, the after cure h of 3 h~10, makes at a temperature of 100 DEG C~110 DEG C
Reaction tends to be complete；Cooling and mould unloading is to get the upper and lower mill of abrasive rubber.
The method for being mixed with upper millstone and lower millstone using natural rubber and synthetic rubber is as follows:
1. formula: mass ratio, rubber 100: natural rubber 46-50, butadiene rubber 50-54, promotor 1-2, vulcanization
Agent 1-2, zinc oxide 4-6, anti-aging agent 2-3, appropriate softening agent, abrasion furnace blacks 50-58；
2. manufacture craft mainly by plasticating, ingredient, mixing, calendering, molding, vulcanization routine operation form, pass through above-mentioned behaviour
Work can obtain the upper and lower mill of abrasive rubber.
The method for preparing graphene using high shear force abrasive rubber mill of the invention is as follows:
By the upper and lower mill product of the abrasive rubber made, installation is fixed on grinding mill, can carry out preparing graphene
It mills operation；A certain amount of neopelex, sodium carboxymethylcellulose, OP-10 compounding dispersing agent and one are weighed first
The deionized water of fixed number amount, is uniformly mixed, the concentration 0.4-1.0mg/ml of dispersing agent, be added a certain amount of crystalline flake graphite or
Expanded graphite, expansible graphite, the concentration 20-40mg/ml of graphite, are uniformly mixed, and then start mill machine, slowly gradually
Graphite suspension is added, after graphite suspension adds, graphite suspension is re-started into second of mill, repetitive cycling operates,
After mill 6-30 hours, stop operation；Material is taken out, is centrifuged, centrifugal rotational speed is set as 4000-9000 revs/min,
Time 5-30 minute, the unstripped graphite of removal centrifugation bottom of the tube return and make mill raw material next time, obtains graphite dispersing solution,
It can directly apply, or be dried to obtain graphene powder, through detecting, graphene number of plies is less than 10 layers.
Raw material: raw material is commercially available technical grade product.
Embodiment 1: using polyurethane wear resistant rubber system for upper and lower mill:
(1), polytetramethylene glycol is dehydrated:
In the there-necked flask for being equipped with blender, thermometer, vacuum adapter, suitable polytetramethylene glycol is added, rises
Temperature to 100 DEG C, 120 DEG C or 140 DEG C, be dehydrated at 0.08 Mpa, 0.085Mpa or 0.09 MPa vacuum degree 2 h, 2.5h or
After 3 h, 40 DEG C, 50 DEG C or 60 DEG C are cooled to, for use；
(2), performed polymer synthesizes:
Appropriate dewatered polytetramethylene glycol and TDI, polytetramethylene two is added by formula ratio in there-necked flask
Alcohol: TDI=1:0.2-0.26(mass ratio), it is warming up to 80 DEG C, 82 DEG C or 85 DEG C after mixing evenly, this temperature is kept to keep it anti-
2h, deaeration 15-30 min are answered, is discharged, closed preservation；
(3), the preparation of upper and lower mill:
Mill mold is preheated to 80 DEG C, 90 DEG C or 100 DEG C, the glue consumption of mill product is calculated, by the pre-polymerization of metering
Body is warming up to 80 DEG C, 85 DEG C or 90 DEG C, vacuum defoamation 15 min~40 min；Then, the MOCA that will be measured and melt
It is added in above-mentioned performed polymer, MOCA inventory is by polytetramethylene glycol: MOCA=1:0.18-0.21(mass ratio) based on, fastly
Speed stirs evenly, and is poured into is coated in release agent and the warmed-up mold for being carved with tongue shape mill line rapidly, be put into air blast at once
In drying oven, 3 h, 5h of after cure or 10 h at a temperature of 100 DEG C, 105 DEG C or 110 DEG C tend to reaction completely,
Cooling and mould unloading is to get the upper and lower mill of abrasive rubber together with upper and lower mill bulk adhesive.
Embodiment 2: abrasive rubber mill is mixed with using natural rubber and synthetic rubber:
Natural rubber and butadiene rubber and various auxiliary agents can be bought in the market；
(1), it is formulated: mass ratio, rubber 100: natural rubber 48, butadiene rubber 52, promotor 1.5, vulcanizing agent 1.5,
Zinc oxide 5, anti-aging agent 2.5, appropriate softening agent, abrasion furnace blacks 55；Manufacture craft by plasticate, ingredient, mixing, calendering, molding,
Vulcanize routine operation to carry out；
(2), it plasticates and ingredient: routinely operating；
(3), be kneaded: natural rubber and butadiene rubber are used in combination, and carry out on mixer, strict control charging sequence and row
Glue temperature will sufficiently turn refining after charging, and thin logical number is no less than 8 times；
(4), roll, form: calendering hole routine operation is molded on molding machine and carries out；
(5), vulcanize: being operated in vulcanizer；
Pass through the available upper and lower mill of abrasive rubber together with upper and lower mill bulk adhesive of aforesaid operations.
Embodiment 3: graphene is prepared using polyurethane wear resistant rubber mill of the present invention
Upper and lower mill made from above-described embodiment 1 is installed on grinding mill, by natural flake graphite 20-40g, go from
Sub- appropriate amount of water makes graphite suspension concentration 2-4%, and neopelex, sodium carboxymethylcellulose, OP-10 compounding is added
Dispersing agent makes neopelex concentration reach 0.5%, stirs 20 minutes, is added to the charging hopper on grinding mill top
In, funnel is configured with blender, and start grinding mill, starts to feed, and regulate charging rate, after the completion of first pass is milled,
Repetitive operation is milled 18 hours, after milling, is centrifuged, centrifugal rotational speed 4000-9000rpm ∕ min, time 5min-
30min, the unstripped graphite of removal centrifugation bottom of the tube, obtains graphene dispersing solution, and through detecting, concentration is 4.2mg ∕ ml, graphite
The alkene number of plies is less than 10 layers.
Embodiment 4: the abrasive rubber mill that application natural rubber of the present invention and synthetic rubber are made by mixing prepares graphene:
Upper and lower mill prepared by above-described embodiment 2 is installed on grinding mill, other operating conditions are obtained with embodiment 3
Graphene dispersing solution, concentration are 3.8mg ∕ ml, and graphene number of plies is less than 10 layers.
Comparative example:
Change mill into an equal amount of stone mill, other operating conditions are milled 32 hours with embodiment 3, are post-processed and real
It is identical to apply example 3, obtains graphene dispersing solution, through detecting, concentration is 0.6mg ∕ ml.
Claims (5)
1. a kind of preparation method for the high shear force abrasive rubber mill for preparing graphene, it is characterised in that: include:
(1), the upper mill ontology of metal and the lower mill ontology of metal are prepared with metal machining common process；
(2), abrasive rubber upper millstone and abrasive rubber lower millstone are prepared using abrasive rubber, the upper and lower mill ontology of metal is consolidated
It is scheduled in the metal die for being carved with tongue shape mill line, casting or molding abrasive rubber solidify, and demoulding can be obtained and grind above and below
The upper and lower abrasive rubber mill with groove type mill line of bulk adhesive together.
2. the preparation method of the high shear force abrasive rubber mill according to claim 1 for preparing graphene, feature exist
In: the abrasive rubber is prepared using synthetic rubber and/or natural rubber.
3. the preparation method of the high shear force abrasive rubber mill according to claim 2 for preparing graphene, feature exist
In: the synthetic rubber includes one of following or a variety of: polyurethane rubber, butadiene-styrene rubber, butadiene rubber, butyl rubber
Glue, neoprene, polysulfide rubber, lactoprene, chlorosulfonated polyethylene rubber, silicon rubber, fluorubber, nitrile rubber,
Isoprene rubber, EP rubbers.
4. preparing the preparation method of the high shear force abrasive rubber mill of graphene, feature according to claim 3
Be: the method for preparing abrasive rubber upper millstone and abrasive rubber lower millstone using polyurethane rubber is as follows:
(1) polytetramethylene glycol is dehydrated:
In the there-necked flask for being equipped with blender, thermometer, vacuum adapter, suitable polytetramethylene glycol is added, is warming up to
100 DEG C~140 DEG C, after the h of 2 h~3 is dehydrated under the MPa vacuum degree of 0.08 MPa~0.09, it is cooled to 40 DEG C~60
DEG C, for use；
(2) performed polymer synthesizes:
Suitable dewatered polytetramethylene glycol and toluene di-isocyanate(TDI) (TDI) is added by formula ratio in there-necked flask,
Polytetramethylene glycol: TDI=1:0.18-0.28 mass ratio is warming up to 80-85 DEG C after mixing evenly, this temperature is kept to make it
React 2h, deaeration 15-30 min, discharging, closed preservation；
(3) preparation of upper and lower mill:
Upper and lower mill mold is preheated to 80-100 DEG C, the glue consumption of mill product is calculated, the performed polymer of metering is warming up to
80 DEG C~90 DEG C, vacuum defoamation 15 min~40 min；Then, chloro- 4, the 4- diamino of 3,3- bis- that will be measured and melt
Diphenyl methane (MOCA) is added in above-mentioned performed polymer, and MOCA inventory presses polytetramethylene glycol: MOCA=1:0.16-
0.25 mass ratio meter, quickly stirs evenly, and is poured into is coated with release agent and the warmed-up mold for being carved with tongue shape mill line rapidly
In, it is put into blast dry oven at once, the after cure h of 3 h~10 at a temperature of 100 DEG C~110 DEG C, tends to reaction
Completely；Cooling and mould unloading is to get the upper and lower mill of abrasive rubber together with upper and lower mill bulk adhesive.
5. the preparation method of the high shear force abrasive rubber mill according to claim 3 for preparing graphene, feature exist
In: the method for being mixed with abrasive rubber upper millstone and abrasive rubber lower millstone using natural rubber and synthetic rubber is as follows:
1. formula: mass ratio, rubber 100: natural rubber 46-50, butadiene rubber 50-54, promotor 1-2, vulcanizing agent 1-2, oxygen
Change zinc 4-6, anti-aging agent 2-3, appropriate softening agent, abrasion furnace blacks 50-58；
2. manufacture craft is by plasticating, ingredient, mixing, calendering, molding, vulcanization routine operation form, can by aforesaid operations
It obtains and grinds the upper and lower mill of abrasive rubber together with bulk adhesive above and below.
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| US8753740B2 (en) * | 2009-12-07 | 2014-06-17 | Nanotek Instruments, Inc. | Submicron-scale graphitic fibrils, methods for producing same and compositions containing same |
| CN101817516A (en) * | 2010-05-21 | 2010-09-01 | 哈尔滨工业大学 | Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping |
| CN202741204U (en) * | 2012-07-06 | 2013-02-20 | 四川省川宏精细化工有限公司 | Improved grinding stripping device |
| CN103285970B (en) * | 2013-06-14 | 2015-04-08 | 深圳市基泰智能设备有限公司 | Graphene processing machine |
| CN104401971B (en) * | 2014-10-23 | 2016-06-29 | 江阴碳谷科技有限公司 | A kind of Graphene grinds stripping off device, Graphene production system and production method |
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2016
- 2016-08-01 CN CN201610616503.0A patent/CN106044761B/en active Active
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