CN107522464A - The preparation method of wide warm graphene composite material - Google Patents
The preparation method of wide warm graphene composite material Download PDFInfo
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- CN107522464A CN107522464A CN201710940960.XA CN201710940960A CN107522464A CN 107522464 A CN107522464 A CN 107522464A CN 201710940960 A CN201710940960 A CN 201710940960A CN 107522464 A CN107522464 A CN 107522464A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The invention discloses the raw material such as preparation method, the technology utilization DDQ, potassium hydrogen persulfate, glass fibre, two myristoyl phosphatidylinositols, terpinyl acetate, graphene, pyrovinic acid, trifluoro methylsulfonimide of wide warm graphene composite material wide warm graphene composite material is obtained by grinding the process optimizations such as spray drying, high temperature banburying, granulation, hydrogen shield heat treatment shaping.The wide temperature graphene composite material being prepared, its is ageing-resistant, is suitable for wide temperature range, has preferable application prospect.
Description
Technical field
The present invention relates to this technical field of material, the preparation method of wide warm graphene composite material is related specifically to.
Background technology
Graphene is commonly described as the plane sheets of monoatomic thickness of the dense accumulation in honeycomb crystal lattice, but these lists
The part that the plane sheets of atomic thickness merge typically as material, it is typically included in the defective material of tool in the lattice
Material.For example, the unit of pentagon and hexagon forms defect.If there is isolated pentagon shaped cells, then the plain bending
Coning shape.Similarly, isolated hexagon makes the sheet material turn into saddle.When graphene is prepared by known methods,
These and other defects generally be present.The unique electric charge engineering properties of graphene causes the interest being used for it in various applications.
For example, electrochemical energy storage has been received in electronic car and in the rechargeable energy system from interval wind and solar energy source
Potential application very big concern.
With growing scientific and technological level, the demand of material heat resistance increasingly increases, how the temperature of reinforcing material
Accommodation is the focus place of current precision instrument system.The broader temperature range between curie point and ultralow temperature, use
In the magnetic material of different field, irreplaceable effect is played with its excellent performance.In order to reach effective temperature control characteristic
Purpose, people are often through material mixture ratio and doping, intense adjustment technical process is changed, to obtain expected performance.Originally grind
Study carefully the preparation for being directed to the wide adiabator of optimized development, be not only adjusted from raw material ratio, be have also been made in preparation technology big
Amplitude modification, the wide adiabator heatproof conformability of preparation is superior, it is expected meeting the needs of industry.
The content of the invention
In order to solve the above technical problems, the present invention provides the preparation method of wide warm graphene composite material, the technology utilization
DDQ, potassium hydrogen persulfate, glass fibre, two myristoyl phosphatidylinositols, terpinyl acetate, graphene,
It is fixed that the raw materials such as pyrovinic acid, trifluoro methylsulfonimide are heat-treated by grinding spray drying, high temperature banburying, granulation, hydrogen shield
The process optimizations such as type obtain wide warm graphene composite material.The wide temperature graphene composite material being prepared, its is ageing-resistant, can fit
Wide temperature range is answered, there is preferable application prospect.
The purpose of the present invention can be achieved through the following technical solutions：
The preparation method of wide warm graphene composite material, comprises the following steps：
(1) DDQ 1-3 parts, potassium hydrogen persulfate 2-3 parts, glass fibre 10-15 parts add suitable quantity of water, grinding
2-3h obtains 1000 mesh slurries, and spray drying obtains powder；
(2) by the slurry powder of step (1) and two myristoyl phosphatidylinositols 1-4 parts, terpinyl acetate 2-7 parts,
In graphene 9-13 parts, pyrovinic acid 4-6 parts stirring mixture input banbury, trifluoro methylsulfonimide 2-5 parts are added, also
3-5h, 800 revs/min of rotating speed are kneaded in originality atmosphere, reaction temperature is 760-800 DEG C, is subsequently cooled to 330 DEG C, obtains
To banburying mixture；
(3) by the banburying mixture spray injection drying machine of step (2), it is dried to powder；
(4) by the powdered rubber of step (3) according to molal weight than 25:1 mixes with deionized water, is injected after stirring
Comminutor is granulated；
(5) obtained be granulated of step (4) is put into cartridge type hydrogen protective heat treatment furnace, at 300 DEG C, under conditions of 2-3h
Sizing heat treatment is carried out, it is to be cooled to after room temperature with stove natural cooling, hydrogen is closed, is got product.
Preferably, the spray dryer EAT in the step (1) is 320 DEG C, 270 DEG C of leaving air temp.
Preferably, the reducibility gas in the step (2) is carbon dioxide.
Preferably, the spray dryer EAT in the step (3) is 220 DEG C, 160 DEG C of leaving air temp, constant flow pump
It is 95 revs/min to turn degree.
Preferably, the granulation parameter in the step (4) is 180 DEG C, 750 revs/min.
Compared with prior art, its advantage is the present invention：
(1) preparation method of wide temperature graphene composite material of the invention utilize DDQ, potassium hydrogen persulfate,
The originals such as glass fibre, two myristoyl phosphatidylinositols, terpinyl acetate, graphene, pyrovinic acid, trifluoro methylsulfonimide
Material obtains wide warm graphene by process optimizations such as grinding spray drying, high temperature banburying, granulation, hydrogen shield heat treatment shapings and answered
Condensation material.The wide temperature graphene composite material being prepared, its is ageing-resistant, is suitable for wide temperature range, has preferably application
Prospect.
(2) wide temperature graphene composite material raw material of the invention be easy to get, technique it is simple, suitable for heavy industrialization utilization,
It is practical.
Embodiment
The technical scheme of invention is described in detail with reference to specific embodiment.
Embodiment 1
(1) 10 parts of 1 part of DDQ, 2 parts of potassium hydrogen persulfate, glass fibre addition suitable quantity of water, grinding 2h are obtained
1000 mesh slurries, spray drying obtain powder, and wherein spray dryer EAT is 320 DEG C, 270 DEG C of leaving air temp；
(2) by the slurry powder of step (1) and 1 part of two myristoyl phosphatidylinositols, 2 parts of terpinyl acetate, graphite
In 4 parts of 9 parts of alkene, pyrovinic acid stirring mixture input banburies, 2 parts of trifluoro methylsulfonimide is added, in carbon dioxide atmosphere
Middle mixing 3h, 800 revs/min of rotating speed, reaction temperature are 760 DEG C, are subsequently cooled to 330 DEG C, obtain banburying mixture；
(3) by the banburying mixture spray injection drying machine of step (2), powder is dried to, spray dryer EAT is
220 DEG C, 160 DEG C of leaving air temp, it is 95 revs/min that constant flow pump, which turns degree,；
(4) by the powdered rubber of step (3) according to molal weight than 25:1 mixes with deionized water, is injected after stirring
Comminutor is granulated, and it is 180 DEG C, 750 revs/min to be granulated parameter；
(5) obtained be granulated of step (4) is put into cartridge type hydrogen protective heat treatment furnace, at 300 DEG C, entered under conditions of 2h
Row sizing heat treatment, it is to be cooled to after room temperature with stove natural cooling, hydrogen is closed, is got product.
The performance test results of the obtained warm graphene composite material of width are as shown in table 1.
Embodiment 2
(1) 12 parts of 2 parts of DDQ, 2 parts of potassium hydrogen persulfate, glass fibre addition suitable quantity of water, grinding 2.2h are obtained
To 1000 mesh slurries, spray drying obtains powder, and wherein spray dryer EAT is 320 DEG C, 270 DEG C of leaving air temp；
(2) by the slurry powder of step (1) and 2 parts of two myristoyl phosphatidylinositols, 3 parts of terpinyl acetate, graphite
In 5 parts of 10 parts of alkene, pyrovinic acid stirring mixture input banburies, 3 parts of trifluoro methylsulfonimide is added, in carbon dioxide atmosphere
Middle mixing 4h, 800 revs/min of rotating speed, reaction temperature are 770 DEG C, are subsequently cooled to 330 DEG C, obtain banburying mixture；
(3) by the banburying mixture spray injection drying machine of step (2), powder is dried to, spray dryer EAT is
220 DEG C, 160 DEG C of leaving air temp, it is 95 revs/min that constant flow pump, which turns degree,；
(4) by the powdered rubber of step (3) according to molal weight than 25:1 mixes with deionized water, is injected after stirring
Comminutor is granulated, and it is 180 DEG C, 750 revs/min to be granulated parameter；
(5) obtained be granulated of step (4) is put into cartridge type hydrogen protective heat treatment furnace, at 300 DEG C, under conditions of 2.2h
Sizing heat treatment is carried out, it is to be cooled to after room temperature with stove natural cooling, hydrogen is closed, is got product.
The performance test results of the obtained warm graphene composite material of width are as shown in table 1.
Embodiment 3
(1) 14 parts of 3 parts of DDQ, 2 parts of potassium hydrogen persulfate, glass fibre addition suitable quantity of water, grinding 2.7h are obtained
To 1000 mesh slurries, spray drying obtains powder, and wherein spray dryer EAT is 320 DEG C, 270 DEG C of leaving air temp；
(2) by the slurry powder of step (1) and 3 parts of two myristoyl phosphatidylinositols, 5 parts of terpinyl acetate, graphite
In 5 parts of 12 parts of alkene, pyrovinic acid stirring mixture input banburies, 4 parts of trifluoro methylsulfonimide is added, in carbon dioxide atmosphere
Middle mixing 4.5h, 800 revs/min of rotating speed, reaction temperature are 780 DEG C, are subsequently cooled to 330 DEG C, obtain banburying mixture；
(3) by the banburying mixture spray injection drying machine of step (2), powder is dried to, spray dryer EAT is
220 DEG C, 160 DEG C of leaving air temp, it is 95 revs/min that constant flow pump, which turns degree,；
(4) by the powdered rubber of step (3) according to molal weight than 25:1 mixes with deionized water, is injected after stirring
Comminutor is granulated, and it is 180 DEG C, 750 revs/min to be granulated parameter；
(5) obtained be granulated of step (4) is put into cartridge type hydrogen protective heat treatment furnace, at 300 DEG C, under conditions of 2.6h
Sizing heat treatment is carried out, it is to be cooled to after room temperature with stove natural cooling, hydrogen is closed, is got product.
The performance test results of the obtained warm graphene composite material of width are as shown in table 1.
Embodiment 4
(1) 15 parts of 3 parts of DDQ, 3 parts of potassium hydrogen persulfate, glass fibre addition suitable quantity of water, grinding 3h are obtained
1000 mesh slurries, spray drying obtain powder, and wherein spray dryer EAT is 320 DEG C, 270 DEG C of leaving air temp；
(2) by the slurry powder of step (1) and 4 parts of two myristoyl phosphatidylinositols, 7 parts of terpinyl acetate, graphite
In 6 parts of 13 parts of alkene, pyrovinic acid stirring mixture input banburies, 5 parts of trifluoro methylsulfonimide is added, in carbon dioxide atmosphere
Middle mixing 5h, 800 revs/min of rotating speed, reaction temperature are 800 DEG C, are subsequently cooled to 330 DEG C, obtain banburying mixture；
(3) by the banburying mixture spray injection drying machine of step (2), powder is dried to, spray dryer EAT is
220 DEG C, 160 DEG C of leaving air temp, it is 95 revs/min that constant flow pump, which turns degree,；
(4) by the powdered rubber of step (3) according to molal weight than 25:1 mixes with deionized water, is injected after stirring
Comminutor is granulated, and it is 180 DEG C, 750 revs/min to be granulated parameter；
(5) obtained be granulated of step (4) is put into cartridge type hydrogen protective heat treatment furnace, at 300 DEG C, entered under conditions of 3h
Row sizing heat treatment, it is to be cooled to after room temperature with stove natural cooling, hydrogen is closed, is got product.
The performance test results of the obtained warm graphene composite material of width are as shown in table 1.
Comparative example 1
(1) 10 parts of 1 part of DDQ, 2 parts of potassium hydrogen persulfate, glass fibre addition suitable quantity of water, grinding 2h are obtained
1000 mesh slurries, spray drying obtain powder, and wherein spray dryer EAT is 320 DEG C, 270 DEG C of leaving air temp；
(2) by the slurry powder of step (1) and 1 part of two myristoyl phosphatidylinositols, 2 parts of terpinyl acetate, graphite
In 4 parts of 9 parts of alkene, pyrovinic acid stirring mixture input banburies, 2 parts of trifluoro methylsulfonimide is added, in carbon dioxide atmosphere
Middle mixing 3h, 800 revs/min of rotating speed, reaction temperature are 760 DEG C, are subsequently cooled to 330 DEG C, obtain banburying mixture；
(3) by the banburying mixture of step (2) according to molal weight than 25:1 mixes with deionized water, is noted after stirring
Enter comminutor granulation, it is 180 DEG C, 750 revs/min to be granulated parameter；
(4) obtained be granulated of step (3) is put into cartridge type hydrogen protective heat treatment furnace, at 300 DEG C, entered under conditions of 2h
Row sizing heat treatment, it is to be cooled to after room temperature with stove natural cooling, hydrogen is closed, is got product.
The performance test results of the obtained warm graphene composite material of width are as shown in table 1.
Comparative example 2
(1) 15 parts of 3 parts of DDQ, 3 parts of potassium hydrogen persulfate, glass fibre addition suitable quantity of water, grinding 3h are obtained
1000 mesh slurries, spray drying obtain powder, and wherein spray dryer EAT is 320 DEG C, 270 DEG C of leaving air temp；
(2) by the slurry powder of step (1) and 4 parts of two myristoyl phosphatidylinositols, 7 parts of terpinyl acetate, graphite
In 6 parts of 13 parts of alkene, pyrovinic acid stirring mixture input banburies, 5 parts of trifluoro methylsulfonimide is added, in carbon dioxide atmosphere
Middle mixing 5h, 800 revs/min of rotating speed, reaction temperature are 800 DEG C, are subsequently cooled to 330 DEG C, obtain banburying mixture；
(3) by the banburying mixture spray injection drying machine of step (2), powder is dried to, spray dryer EAT is
220 DEG C, 160 DEG C of leaving air temp, it is 95 revs/min that constant flow pump, which turns degree,；
(4) by the powdered rubber of step (3) according to molal weight than 25:1 mixes with deionized water, is injected after stirring
Comminutor is granulated, and it is 180 DEG C, 750 revs/min to be granulated parameter；
(5) after the obtained granulation of step (4) being naturally cooled into room temperature, get product.
The performance test results of the obtained warm graphene composite material of width are as shown in table 1.
It is strong that the wide temperature graphene composite materials of embodiment 1-4 and comparative example 1-2 obtained are subjected to notch shock respectively
This several degree, thermal conductivity factor, wear-resisting weather-proof performance tests.
Table 1
The preparation method of the wide temperature graphene composite material of the present invention utilizes DDQ, potassium hydrogen persulfate, glass
The raw materials such as glass fiber, two myristoyl phosphatidylinositols, terpinyl acetate, graphene, pyrovinic acid, trifluoro methylsulfonimide
It is compound that wide warm graphene is obtained by process optimizations such as grinding spray drying, high temperature banburying, granulation, hydrogen shield heat treatment shapings
Material.The wide temperature graphene composite material being prepared, its is ageing-resistant, is suitable for wide temperature range, before having preferably application
Scape.The wide temperature graphene composite material raw material of the present invention is easy to get, technique is simple, is used suitable for heavy industrialization, practical.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
The equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, it is included within the scope of the present invention.
Claims (5)
1. the preparation method of wide warm graphene composite material, it is characterised in that comprise the following steps：
(1) DDQ 1-3 parts, potassium hydrogen persulfate 2-3 parts, glass fibre 10-15 parts add suitable quantity of water, grind 2-3h
1000 mesh slurries are obtained, spray drying obtains powder；
(2) by the slurry powder of step (1) and two myristoyl phosphatidylinositols 1-4 parts, terpinyl acetate 2-7 parts, graphite
In alkene 9-13 parts, pyrovinic acid 4-6 parts stirring mixture input banbury, trifluoro methylsulfonimide 2-5 parts are added, in reproducibility
3-5h, 800 revs/min of rotating speed are kneaded in atmosphere, reaction temperature is 760-800 DEG C, is subsequently cooled to 330 DEG C, obtains close
Refine mixture；
(3) by the banburying mixture spray injection drying machine of step (2), it is dried to powder；
(4) by the powdered rubber of step (3) according to molal weight than 25:1 mixes with deionized water, injects and is granulated after stirring
Machine is granulated；
(5) obtained be granulated of step (4) is put into cartridge type hydrogen protective heat treatment furnace, at 300 DEG C, carried out under conditions of 2-3h
Sizing heat treatment, it is to be cooled to after room temperature with stove natural cooling, hydrogen is closed, is got product.
2. the preparation method of the warm graphene composite material of width according to claim 1, it is characterised in that the step (1)
In spray dryer EAT be 320 DEG C, 270 DEG C of leaving air temp.
3. the preparation method of the warm graphene composite material of width according to claim 1, it is characterised in that the step (2)
In reducibility gas be carbon dioxide.
4. the preparation method of the warm graphene composite material of width according to claim 1, it is characterised in that the step (3)
In spray dryer EAT be 220 DEG C, 160 DEG C of leaving air temp, constant flow pump turn degree be 95 revs/min.
5. the preparation method of the warm graphene composite material of width according to claim 1, it is characterised in that the step (4)
In granulation parameter be 180 DEG C, 750 revs/min.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660695A (en) * | 2012-04-17 | 2012-09-12 | 重庆材料研究院 | Copper wire and method for preparing shielding copper wire mesh |
| CN106189229A (en) * | 2016-08-20 | 2016-12-07 | 张伟 | Graphene conductive heat conduction thin-film material of doping metals alloy and preparation method thereof |
| CN106206064A (en) * | 2016-08-24 | 2016-12-07 | 张伟 | Ultracapacitor High-performance graphene electrode material and preparation method thereof |
| CN106280448A (en) * | 2016-08-20 | 2017-01-04 | 张伟 | A kind of Graphene composite cable material and preparation method thereof |
| CN106915961A (en) * | 2017-02-24 | 2017-07-04 | 华南理工大学 | A kind of Graphene zirconium oxide composite material and preparation method thereof |
-
2017
- 2017-10-11 CN CN201710940960.XA patent/CN107522464A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660695A (en) * | 2012-04-17 | 2012-09-12 | 重庆材料研究院 | Copper wire and method for preparing shielding copper wire mesh |
| CN106189229A (en) * | 2016-08-20 | 2016-12-07 | 张伟 | Graphene conductive heat conduction thin-film material of doping metals alloy and preparation method thereof |
| CN106280448A (en) * | 2016-08-20 | 2017-01-04 | 张伟 | A kind of Graphene composite cable material and preparation method thereof |
| CN106206064A (en) * | 2016-08-24 | 2016-12-07 | 张伟 | Ultracapacitor High-performance graphene electrode material and preparation method thereof |
| CN106915961A (en) * | 2017-02-24 | 2017-07-04 | 华南理工大学 | A kind of Graphene zirconium oxide composite material and preparation method thereof |
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