CN109233014A - A kind of preparation method of butadiene rubber-graphene oxide composite material - Google Patents
A kind of preparation method of butadiene rubber-graphene oxide composite material Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of butadiene rubber-graphene oxide composite material, belong to technical field of polymer composite materials.The present invention first will be added esters of silicon acis and react after graphene oxide and fatty acid ultrasonic disperse, presoma is made, it is spray-dried after again mixing presoma and gelatin dispersion liquid, gelatin-presoma complex microsphere is made, again by further temperature reaction after gelatin-presoma complex microsphere charing, modified graphene oxide microballoon is made, then by itself and butadiene rubber, coal tar, stearic acid, zinc oxide, antioxidant and promotor, which are added in mixer, to be kneaded, after parking, it is added in open mill, and sulphur is added, it is transferred in vulcanizer and vulcanizes after mixing, it is cooling, discharging, up to butadiene rubber-graphene oxide composite material.Gained butadiene rubber-graphene oxide composite material graphene oxide of the invention has excellent reinforcing effect to butadiene rubber.
Description
Technical field
The invention discloses a kind of preparation methods of butadiene rubber-graphene oxide composite material, and it is compound to belong to macromolecule
Field of material technology.
Background technique
Since carbon nanotube and graphene are found, chemistry, physics, material science, electronic technology just it have been widely used in
Equal numerous areas.Graphene and carbon nanotube have special nanostructure, assign both carbon materials excellent physical mechanical
Performance is widely used as nanofiller to improve the electricity of nanocomposite, mechanics, calorifics, optics etc. performance.Stone
The potential application foreground of black alkene and carbon nanotube in various fields has attracted the extensive concern of researcher.
Carbon nano tube compound material research has been carried out more than 20 years, has made significant headway, but carbon nanotube is multiple
Two large problems are remained in the preparation process of condensation material:
(1) the dispersion of carbon nanotube, i.e. carbon nanotube are easy to happen agglomeration in process；
(2) carbon nanotube high production cost is difficult to large-scale production.Graphene is that one kind is made of carbon atom with sp2 hybridized orbit
The two-dimensional material of hexangle type honeycomb lattice, only one carbon atom of thickness, carbon nanotube can be regarded as by the seamless volume of graphene
Made of song.Although graphene is identical with the chemical composition of carbon nanotube, the topological structure of carbon nanotube and graphene and
Surface topography difference is very big, therefore they possess respective unique performance.Carbon nanotube is compared, the main advantage of graphene is
The presoma of graphene is graphite, abundance, cheap, is conducive to low cost and prepares high-quality graphene, makes nano combined material
Material industrialization is possibly realized, while possessing some performances different from carbon nanotube, such as dispersed.
The research of graphene carbon nanotube polymer composite is concentrated mainly on plastic substrate at present, for example, asphalt mixtures modified by epoxy resin
Rouge, PMMA, PC, PU, PA, PP etc..Researcher carries out function to graphene and carbon nanotube by the method for physics and chemistry
Change and be modified to improve their dispersibilities in the base, but these treatment processes are often to its surface state and draw ratio etc.
Generate certain influence.It is compound that Nobile etc. is prepared for polyethylene/MWNTs with melt-blending process on miniature double rod screw extruder
Material, MWNTs is well dispersed in PE and promotes nonisothermal crystallization.Lv etc. uses molecular mechanics and molecular dynamics simulation
Study influence of the chemisorption to the Graphene polymer composite interfacial bond property of functionalization, simulation results
Show that graphene surface functional group is more, the combination of graphene and polymeric matrix can and shearing force it is bigger, the analog result and
PMMA/TrG composite material experimental result is consistent.About the dispersion application study of graphene or carbon nanotube in rubber material
It is seldom, on the one hand important reason is that the viscosity of rubber matrix is high, be on the other hand that the surface of rubber can be low, make nano material
It is difficult to disperse wherein, nanofiller is easy to reunite and cannot give full play to its effect.We conducted polymolecularity height to lead thus
Dispersion performance research of the electrical graphene in rubber material, as a result obtains the graphene rubber material of fine dispersion, right
The mechanics of rubber material, electric property studies have shown that the dispersibility of graphene is higher than carbon nanotube, and the two can be
Collaboration dispersion is carried out in rubber matrix.It is traditional at present when carrying out blending and modifying to butadiene rubber with graphene oxide, because of suitable fourth
Rubber only have carbon, protium composition, between graphene oxide only only have Van der Waals force and weak π-π interaction force, two
Interaction force is weaker between person, causes graphene oxide that can not further promote the reinforcing effect of butadiene rubber, therefore also
It need to be studied.
Summary of the invention
The present invention solves the technical problem of: blending and modifying is carried out to butadiene rubber with graphene oxide for tradition
When, because butadiene rubber only has carbon, protium composition, only only have Van der Waals force and weak π-π mutual between graphene oxide
Active force, interaction force is weaker between the two, causes graphene oxide that can not further mention the reinforcing effect of butadiene rubber
The drawbacks of rising, provides a kind of preparation method of butadiene rubber-graphene oxide composite material.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
(1) according to parts by weight, 20~30 parts of graphene oxides are successively taken, 80~120 parts of fatty acid, 20~30 parts of esters of silicon acis,
After graphene oxide and fatty acid ultrasonic disperse, will first add esters of silicon acis, it is still aging after heating stirring reaction, then through from
Heart separation, washing and drying, obtain presoma；
(2) after being in mass ratio 1:1~1:3 mixing and ball milling for presoma and gelatin dispersion liquid, spray drying obtains gelatin-forerunner
Bluk recombination microballoon；
(3) the slowly heating charing under inert gas shielding state by gelatin-presoma complex microsphere, is further warming up to
1480~1500 DEG C, cooling after pyroreaction, discharging obtains modified graphene oxide microballoon；
(4) according to parts by weight, 10~20 parts of modified graphene oxide microballoons are successively taken, 80~120 parts of butadiene rubbers, 4~6 parts
Coal tar, 2~4 parts of stearic acid, 3~5 parts of zinc oxide, 1~3 part of antioxidant, 1~3 part of promotor, 3~5 parts of sulphur will first change
Property graphene oxide microballoon, butadiene rubber, coal tar, stearic acid, zinc oxide, antioxidant and promotor be added in mixer and mix
Refining after parking, is added in open mill, and sulphur is added, is transferred in vulcanizer and vulcanizes after mixing, and cooling, discharging is to get along fourth rubber
Glue-graphene oxide composite material.
Step (1) fatty acid is any one in ricinoleic acid, arachidonic acid or linolenic acid.
Step (1) esters of silicon acis is any one in methyl orthosilicate, ethyl orthosilicate or positive silicic acid propyl ester.
Step (2) the gelatin dispersion liquid process for preparation are as follows: by gelatin and water be in mass ratio 1:5~1:10 mix after it is quiet
Swelling, then heated stirring and dissolving are set, gelatin dispersion liquid is obtained.
Step (3) inert gas is any one in nitrogen, argon gas or helium.
Step (3) the slow heating charcoal, which is turned to, is warming up to 450~500 DEG C with 0.3~0.5 DEG C/min rate program, protects
3~5h of temperature charing.
Step (4) coal tar is any one in coalite tar or medium temperature coal tar.
Step (4) antioxidant is antioxidant 1010, any one in antioxidant 1076 or irgasfos 168.
Step (4) promotor is any one in Vulcanization accelerator TMTD, captax or promotor ZDMC.
The beneficial effects of the present invention are:
Technical solution of the present invention makes the structure of its single sheet change from the physical structure of graphene oxide, to improve
Mechanical snap power between graphene oxide and butadiene rubber linear molecule makes graphene oxide so that the two be made to be firmly combined
The reinforcing effect of butadiene rubber is further promoted, the technical scheme is that by following means to graphene oxide physics structure
It makes and is changed: firstly, technical solution of the present invention is using in the carboxyl and graphene oxide structure in fatty acid molecule structure
Hydroxyl dehydration occurs, and using esters of silicon acis as dehydrating agent, absorb the moisture of generation and hydrolyze esters of silicon acis, hydrolysis production
Graphene absorption can be oxidized after raw silica at once, the reunion of silica is avoided and further grows up, thus aoxidizing
Graphene-structured surface forms nano silica bulge-structure, then coats one layer of gelatin again in silica surface, thus
Graphene oxide-silica-gelatin MULTILAYER COMPOSITE micro-sphere structure is formed, in subsequent slow heating carbonization process, due to bright
Char shrinkage occurs for glue, to be conducive to silicon dioxide intermediate layer as temperature is further promoted in the ready-made pleated structure in surface
Carbon-silico-carbo chemical bond is formed between internal layer graphene oxide and outside pleated structure, reinforces siliceous ingredient as intermediate
Layer makes to form firm connection between layer and layer structure, and when being blended with rubber molecule, the presence of pleated structure, which has, to be conducive to linearly
Protrusion or angular surface winding of the rubber molecular chain on pleated structure surface is affiliated to, so that mechanical snap is formed, and siliceous ingredient
Be reinforced be conducive to improve mechanical snap stability, avoid surface texture from failing in loading process, to make graphite oxide
Alkene further promotes the reinforcing effect of butadiene rubber.
Specific embodiment
According to parts by weight, 20~30 parts of graphene oxides are successively taken, 80~120 parts of fatty acid, 20~30 parts of esters of silicon acis,
First graphene oxide and fatty acid are poured into three-necked flask, in supersonic frequency be 55~60kHz under the conditions of ultrasonic disperse 45~
After 60min, then esters of silicon acis is added into three-necked flask, three-necked flask is then moved into digital display and is tested the speed constant temperature blender with magnetic force, in
Temperature is 85~90 DEG C, under the conditions of revolving speed is 600~800r/min, after heating stirring reacts 3~5h, stops stirring and heating,
Still aging 6~8h, then material in three-necked flask is transferred in centrifuge, under the conditions of revolving speed is 8000~12000r/min from
The heart separates 15~20min, collects lower sediment thing, and wash gained lower sediment thing 3~5 times with dehydrated alcohol, then will washing
Lower sediment thing afterwards is transferred in baking oven, is dried under the conditions of being 105~110 DEG C in temperature to constant weight, is obtained presoma；In mass ratio
Presoma and gelatin dispersion liquid are added in ball grinder for 1:1~1:3, and are that oxidation is added in 10:1~30:1 by ball material mass ratio
Zirconium ball milling pearl, after 4~6h of ball milling mixing, discharging obtains ball milling material, then gained ball milling material is delivered to spray drying by screw pump
In device, control feed rate is 15~30g/min, is 110~120 DEG C in inlet air temperature, leaving air temp is 65~70 DEG C of conditions
Lower spray drying obtains gelatin-presoma complex microsphere；Gained gelatin-presoma complex microsphere is transferred in retort again, and with
400~500mL/min rate is passed through inert gas shielding into furnace, then with the slow temperature programming of 0.3~0.5 DEG C/min rate
To 450~500 DEG C, after 3~5h of heat preservation charing, continue with the further temperature programming of 10~15 DEG C/min rate to 1480~1500
DEG C, it after 3~5h of pyroreaction, cools to room temperature with the furnace, discharges, obtain modified graphene oxide microballoon；According to parts by weight, successively
Take 10~20 parts of modified graphene oxide microballoons, 80~120 parts of butadiene rubbers, 4~6 parts of coal tar, 2~4 parts of stearic acid, 3~5
Part zinc oxide, 1~3 part of antioxidant, 1~3 part of promotor, 3~5 parts of sulphur, first by modified graphene oxide microballoon, along fourth rubber
It is kneaded under the conditions of being 72~75 DEG C in temperature in glue, coal tar, stearic acid, zinc oxide, antioxidant and promotor addition mixer
After 15~20min, standing parks 8~10h, then material in mixer is transferred in open mill, and sulphur is added, in temperature be 48
Under the conditions of~50 DEG C, be kneaded 8~10min, then material in open mill be transferred in vulcanizing press, in pressure be 10~20MPa,
Temperature is 10~20min of hot-press vulcanization under the conditions of 155~160 DEG C, cooling, is discharged compound to get butadiene rubber-graphene oxide
Material.The fatty acid is any one in ricinoleic acid, arachidonic acid or linolenic acid.The esters of silicon acis is positive silicic acid first
Any one in ester, ethyl orthosilicate or positive silicic acid propyl ester.The gelatin dispersion liquid process for preparation are as follows: gelatin and water are pressed into matter
Amount obtains gelatin dispersion liquid than being to stand swelling, then heated stirring and dissolving after 1:5~1:10 is mixed.The inert gas is nitrogen
Any one in gas, argon gas or helium.The coal tar is any one in coalite tar or medium temperature coal tar.It is described
Antioxidant is antioxidant 1010, any one in antioxidant 1076 or irgasfos 168.The promotor is Vulcanization accelerator TMTD, promotees
Into any one in agent M or promotor ZDMC.
According to parts by weight, 30 parts of graphene oxides, 120 parts of fatty acid, 30 parts of esters of silicon acis, first by graphite oxide are successively taken
Alkene and fatty acid pour into three-necked flask, under the conditions of supersonic frequency is 60kHz after ultrasonic disperse 60min, then to three-necked flask
Three-necked flask is then moved to digital display and tested the speed constant temperature blender with magnetic force by middle addition esters of silicon acis, is 90 DEG C in temperature, revolving speed is
Under the conditions of 800r/min, after heating stirring reacts 5h, stop stirring and heating, still aging 8h, then by material in three-necked flask
It is transferred in centrifuge, is centrifugated 20min under the conditions of revolving speed is 12000r/min, collect lower sediment thing, and with anhydrous second
Alcohol washing gained lower sediment thing 5 times, then the lower sediment thing after washing is transferred in baking oven, under the conditions of temperature is 110 DEG C
Drying obtains presoma to constant weight；Presoma and gelatin dispersion liquid are added in ball grinder for 1:3 in mass ratio, and press ball material matter
Ratio is measured as 30:1 addition zirconium oxide ball milling pearl, after ball milling mixing 6h, discharging obtains ball milling material, then gained ball milling material is passed through screw rod
Pump is delivered in spray dryer, and control feed rate is 30g/min, is 120 DEG C in inlet air temperature, leaving air temp is 70 DEG C of items
It is spray-dried under part, obtains gelatin-presoma complex microsphere；Gained gelatin-presoma complex microsphere is transferred in retort again, and
Inert gas shielding is passed through into furnace with 500mL/min rate, then with the slow temperature programming of 0.5 DEG C/min rate to 500 DEG C,
After heat preservation charing 5h, continues with the further temperature programming of 15 DEG C/min rate to 1500 DEG C, after pyroreaction 5h, cool to the furnace
Room temperature, discharging, obtains modified graphene oxide microballoon；According to parts by weight, 20 parts of modified graphene oxide microballoons are successively taken, 120
Part butadiene rubber, 6 parts of coal tar, 4 parts of stearic acid, 5 parts of zinc oxide, 3 parts of antioxidant, 3 parts of promotors, 5 parts of sulphur will be first modified
Graphene oxide microballoon, butadiene rubber, coal tar, stearic acid, zinc oxide, antioxidant and promotor are added in mixer in temperature
After being kneaded 20min under the conditions of being 75 DEG C, standing parks 10h, then material in mixer is transferred in open mill, and sulphur is added,
Under the conditions of temperature is 50 DEG C, is kneaded 10min, then material in open mill is transferred in vulcanizing press, in pressure be 20MPa,
Temperature is hot-press vulcanization 20min under the conditions of 160 DEG C, cooling, is discharged to get butadiene rubber-graphene oxide composite material.It is described
Fatty acid is ricinoleic acid.The esters of silicon acis is methyl orthosilicate.The gelatin dispersion liquid process for preparation are as follows: press gelatin and water
Mass ratio is standing swelling after 1:10 mixing, then heated stirring and dissolving, obtains gelatin dispersion liquid.The inert gas is nitrogen.
The coal tar is coalite tar.The antioxidant is antioxidant 1010.The promotor is Vulcanization accelerator TMTD.
According to parts by weight, 30 parts of graphene oxides, 120 parts of fatty acid, 30 parts of esters of silicon acis, first by graphite oxide are successively taken
Alkene and fatty acid pour into three-necked flask, under the conditions of supersonic frequency is 60kHz after ultrasonic disperse 60min, then to three-necked flask
Three-necked flask is then moved to digital display and tested the speed constant temperature blender with magnetic force by middle addition esters of silicon acis, is 90 DEG C in temperature, revolving speed is
Under the conditions of 800r/min, after heating stirring reacts 5h, stop stirring and heating, still aging 8h, then by material in three-necked flask
It is transferred in centrifuge, is centrifugated 20min under the conditions of revolving speed is 12000r/min, collect lower sediment thing, and with anhydrous second
Alcohol washing gained lower sediment thing 5 times, then the lower sediment thing after washing is transferred in baking oven, under the conditions of temperature is 110 DEG C
Drying obtains presoma to constant weight；Presoma and gelatin dispersion liquid are added in ball grinder for 1:3 in mass ratio, and press ball material matter
Ratio is measured as 30:1 addition zirconium oxide ball milling pearl, after ball milling mixing 6h, discharging obtains ball milling material, then gained ball milling material is passed through screw rod
Pump is delivered in spray dryer, and control feed rate is 30g/min, is 120 DEG C in inlet air temperature, leaving air temp is 70 DEG C of items
It is spray-dried under part, obtains gelatin-presoma complex microsphere；Gained gelatin-presoma complex microsphere is transferred in retort again, and
Inert gas shielding is passed through into furnace with 500mL/min rate, then with the slow temperature programming of 0.5 DEG C/min rate to 500 DEG C,
After heat preservation charing 5h, continues with the further temperature programming of 15 DEG C/min rate to 1500 DEG C, after pyroreaction 5h, cool to the furnace
Room temperature, discharging, obtains modified graphene oxide microballoon；According to parts by weight, 20 parts of modified graphene oxide microballoons are successively taken, 120
Part butadiene rubber, 6 parts of coal tar, 4 parts of stearic acid, 5 parts of zinc oxide, 3 parts of antioxidant, 3 parts of promotors, 5 parts of sulphur will be first modified
Graphene oxide microballoon, butadiene rubber, coal tar, stearic acid, zinc oxide, antioxidant and promotor are added in mixer in temperature
After being kneaded 20min under the conditions of being 75 DEG C, standing parks 10h, then material in mixer is transferred in open mill, and sulphur is added,
Under the conditions of temperature is 50 DEG C, is kneaded 10min, then material in open mill is transferred in vulcanizing press, in pressure be 20MPa,
Temperature is hot-press vulcanization 20min under the conditions of 160 DEG C, cooling, is discharged to get butadiene rubber-graphene oxide composite material.It is described
Fatty acid is ricinoleic acid.The esters of silicon acis is methyl orthosilicate.The gelatin dispersion liquid process for preparation are as follows: press gelatin and water
Mass ratio is standing swelling after 1:10 mixing, then heated stirring and dissolving, obtains gelatin dispersion liquid.The inert gas is nitrogen.
The coal tar is coalite tar.The antioxidant is antioxidant 1010.The promotor is Vulcanization accelerator TMTD.
According to parts by weight, 30 parts of graphene oxides, 120 parts of fatty acid, 30 parts of esters of silicon acis, first by graphite oxide are successively taken
Alkene and fatty acid pour into three-necked flask, under the conditions of supersonic frequency is 60kHz after ultrasonic disperse 60min, then to three-necked flask
Three-necked flask is then moved to digital display and tested the speed constant temperature blender with magnetic force by middle addition esters of silicon acis, is 90 DEG C in temperature, revolving speed is
Under the conditions of 800r/min, after heating stirring reacts 5h, stop stirring and heating, still aging 8h, then by material in three-necked flask
It is transferred in centrifuge, is centrifugated 20min under the conditions of revolving speed is 12000r/min, collect lower sediment thing, and with anhydrous second
Alcohol washing gained lower sediment thing 5 times, then the lower sediment thing after washing is transferred in baking oven, under the conditions of temperature is 110 DEG C
Drying obtains presoma to constant weight；Presoma and gelatin dispersion liquid are added in ball grinder for 1:3 in mass ratio, and press ball material matter
Ratio is measured as 30:1 addition zirconium oxide ball milling pearl, after ball milling mixing 6h, discharging obtains ball milling material, then gained ball milling material is passed through screw rod
Pump is delivered in spray dryer, and control feed rate is 30g/min, is 120 DEG C in inlet air temperature, leaving air temp is 70 DEG C of items
It is spray-dried under part, obtains gelatin-presoma complex microsphere；Gained gelatin-presoma complex microsphere is transferred in retort again, and
Inert gas shielding is passed through into furnace with 500mL/min rate, then with the slow temperature programming of 0.5 DEG C/min rate to 500 DEG C,
After heat preservation charing 5h, continues with the further temperature programming of 15 DEG C/min rate to 1500 DEG C, after pyroreaction 5h, cool to the furnace
Room temperature, discharging, obtains modified graphene oxide microballoon；According to parts by weight, 20 parts of modified graphene oxide microballoons are successively taken, 120
Part butadiene rubber, 6 parts of coal tar, 4 parts of stearic acid, 5 parts of zinc oxide, 3 parts of antioxidant, 3 parts of promotors, 5 parts of sulphur will be first modified
Graphene oxide microballoon, butadiene rubber, coal tar, stearic acid, zinc oxide, antioxidant and promotor are added in mixer in temperature
After being kneaded 20min under the conditions of being 75 DEG C, standing parks 10h, then material in mixer is transferred in open mill, and sulphur is added,
Under the conditions of temperature is 50 DEG C, is kneaded 10min, then material in open mill is transferred in vulcanizing press, in pressure be 20MPa,
Temperature is hot-press vulcanization 20min under the conditions of 160 DEG C, cooling, is discharged to get butadiene rubber-graphene oxide composite material.It is described
Fatty acid is ricinoleic acid.The esters of silicon acis is methyl orthosilicate.The gelatin dispersion liquid process for preparation are as follows: press gelatin and water
Mass ratio is standing swelling after 1:10 mixing, then heated stirring and dissolving, obtains gelatin dispersion liquid.The inert gas is nitrogen.
The coal tar is coalite tar.The antioxidant is antioxidant 1010.The promotor is Vulcanization accelerator TMTD.
1 to 3 gained butadiene rubber of example-graphene oxide composite material is subjected to performance detection, specific detection method is such as
Under:
The tensile strength of sample is tested according to GB/T528；Hardness is tested according to GB/T531.Specific testing result is such as
Shown in table 1:
Table 1: performance detection table
| Detection content | Example 1 | Example 2 | Example 3 |
| Tensile strength/MPa | 8.22 | 4.23 | 4.86 |
| Hardness/HA | 72 | 50 | 59 |
By 1 testing result of table it is found that present invention gained butadiene rubber-graphene oxide composite material graphene oxide is to along fourth
Rubber has excellent reinforcing effect.
Claims (9)
1. a kind of preparation method of butadiene rubber-graphene oxide composite material, it is characterised in that specific preparation step are as follows:
(1) according to parts by weight, 20~30 parts of graphene oxides are successively taken, 80~120 parts of fatty acid, 20~30 parts of esters of silicon acis,
After graphene oxide and fatty acid ultrasonic disperse, will first add esters of silicon acis, it is still aging after heating stirring reaction, then through from
Heart separation, washing and drying, obtain presoma；
(2) after being in mass ratio 1:1~1:3 mixing and ball milling for presoma and gelatin dispersion liquid, spray drying obtains gelatin-forerunner
Bluk recombination microballoon；
(3) the slowly heating charing under inert gas shielding state by gelatin-presoma complex microsphere, is further warming up to
1480~1500 DEG C, cooling after pyroreaction, discharging obtains modified graphene oxide microballoon；
(4) according to parts by weight, 10~20 parts of modified graphene oxide microballoons are successively taken, 80~120 parts of butadiene rubbers, 4~6 parts
Coal tar, 2~4 parts of stearic acid, 3~5 parts of zinc oxide, 1~3 part of antioxidant, 1~3 part of promotor, 3~5 parts of sulphur will first change
Property graphene oxide microballoon, butadiene rubber, coal tar, stearic acid, zinc oxide, antioxidant and promotor be added in mixer and mix
Refining after parking, is added in open mill, and sulphur is added, is transferred in vulcanizer and vulcanizes after mixing, and cooling, discharging is to get along fourth rubber
Glue-graphene oxide composite material.
2. a kind of preparation method of butadiene rubber-graphene oxide composite material according to claim 1, it is characterised in that
Step (1) fatty acid is any one in ricinoleic acid, arachidonic acid or linolenic acid.
3. a kind of preparation method of butadiene rubber-graphene oxide composite material according to claim 1, it is characterised in that
Step (1) esters of silicon acis is any one in methyl orthosilicate, ethyl orthosilicate or positive silicic acid propyl ester.
4. a kind of preparation method of butadiene rubber-graphene oxide composite material according to claim 1, it is characterised in that
Step (2) the gelatin dispersion liquid process for preparation are as follows: by gelatin and water be in mass ratio 1:5~1:10 mix after stand be swollen,
Heated stirring and dissolving again obtains gelatin dispersion liquid.
5. a kind of preparation method of butadiene rubber-graphene oxide composite material according to claim 1, it is characterised in that
Step (3) inert gas is any one in nitrogen, argon gas or helium.
6. a kind of preparation method of butadiene rubber-graphene oxide composite material according to claim 1, it is characterised in that
Step (3) the slow heating charcoal, which is turned to, is warming up to 450~500 DEG C with 0.3~0.5 DEG C/min rate program, and heat preservation charing 3~
5h。
7. a kind of preparation method of butadiene rubber-graphene oxide composite material according to claim 1, it is characterised in that
Step (4) coal tar is any one in coalite tar or medium temperature coal tar.
8. a kind of preparation method of butadiene rubber-graphene oxide composite material according to claim 1, it is characterised in that
Step (4) antioxidant is antioxidant 1010, any one in antioxidant 1076 or irgasfos 168.
9. a kind of preparation method of butadiene rubber-graphene oxide composite material according to claim 1, it is characterised in that
Step (4) promotor is any one in Vulcanization accelerator TMTD, captax or promotor ZDMC.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109834271A (en) * | 2019-02-25 | 2019-06-04 | 俞小峰 | A kind of preparation method of aluminum electrolytic tank long-acting special impermeabilisation brick |
| CN110655689A (en) * | 2019-10-22 | 2020-01-07 | 戴章 | Graphene nanocomposite with heat resistance |
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