CN107141012A - A kind of preparation method of closed pore graphite oxide alkenyl heat-barrier material - Google Patents
A kind of preparation method of closed pore graphite oxide alkenyl heat-barrier material Download PDFInfo
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Abstract
A kind of preparation method of closed pore graphite oxide alkenyl heat-barrier material, is related to a kind of preparation method of heat-barrier material.The present invention is in order to solve that existing Cryogenic tank heat-barrier material weight is big, thermal conductivity factor is high, complex forming technology, high cost the problem of.Preparation method：First, graphene oxide emulsion is prepared；2nd, it is freeze-dried：By graphene oxide 0.5~1.5h of emulsion freeze under the conditions of temperature is 40 DEG C~60 DEG C, then it is freeze-dried 5~7 days, finally dries lyophilized graphene oxide block in the case where temperature is 60 DEG C.The inventive method is to prepare graphene oxide spherical droplets by emulsion method, and then freeze-drying removes the solvent in emulsion：Water and paraxylene, prepare the graphene oxide heat-barrier material with hole-closing structure, reduce graphene oxide heat-barrier material thermal conductivity factor, further improve graphene oxide heat-barrier material heat-proof quality.The present invention is applied to prepare closed pore graphite oxide alkenyl heat-barrier material.
Description
Technical field
The present invention relates to a kind of preparation method of closed pore graphite oxide alkenyl heat-barrier material.
Background technology
Porous heat insulation material has the high and excellent heat-proof quality of light weight, porosity, and porous heat insulation material is heat-insulated
One of most widely used in material system, maximally effective material.Traditional organic foam-thermal insulation, glass fibre and asbestos etc. are led
Hot coefficient is higher, and practical application volume is big, it is necessary to which thicker material can be only achieved effect of heat insulation, and old discarded material is difficult
Degraded is difficult to reclaim, and environmental pollution is big；Organic foam material linear expansion coefficient is bigger than normal simultaneously, easily is influenceed to produce by temperature change and broken
It is bad, it is impossible to applied to temperature environment jumpy.
Cryogenic tank in space industry is the Primary containers for storing cryogenic propellant, tank heat-barrier material and heat-insulated skill
Art can efficiently control the transmission of heat, prevent cryogenic liquid from drastically evaporating, and prevent liquefaction of the air on tank outer wall, reach
The purpose being incubated to cold insulation.It is to realize that composite tank overall structure subtracts to design and develop the efficient heat-barrier material of novel light
Weight, lifts adiabatic efficiency, realizes the key of cryogenic media safe storage.It is existing with foam, aeroge and vacuum insulation interlayer
For the heat-barrier material and heat insulating construction of representative, otherwise weight is big, thermal conductivity factor is high, otherwise complex forming technology, cost are high, it is difficult to
Meet the insulation requirements of composite tank efficient and light weight.The characteristics of organic foam material easy moisture absorption, has a strong impact on heat-insulating efficiency；
Such as with SiO2Aeroge is poor for the cellular insulant moulding process of representative；The condition of high vacuum degree of high-vacuum insulation sandwich material is obtained
Keep relatively difficult for a long time, be widely used more on metallic tank.Therefore, novel light is designed and developed efficiently heat-insulated
Material is to realize composite tank overall structure loss of weight, lifts adiabatic efficiency, realizes the key of cryogenic media safe storage.
The content of the invention
The present invention is in order to solve that existing Cryogenic tank heat-barrier material weight is big, thermal conductivity factor is high, complex forming technology, into
The problem of this is high, proposes a kind of preparation method of closed pore graphite oxide alkenyl heat-barrier material.
A kind of preparation method of closed pore graphite oxide alkenyl heat-barrier material, is specifically realized by the following steps：
First, graphene oxide emulsion is prepared：
Graphene oxide aqueous dispersions are prepared using Hummers methods, by oxirane epoxy under room temperature and stirring condition
Propane block co-polyether, which is stirred at room temperature, to be dissolved in graphene oxide aqueous dispersions, is then added paraxylene, is finally existed
5~30min of high speed shear under 8000~16000r/min speed, obtains graphene oxide emulsion；
The content of graphene oxide is 7~9mg/mL in the graphene oxide aqueous dispersions；The graphene oxide water
The mass ratio of graphene oxide and ethylene oxide propylene oxide block co-polyether in dispersion liquid is 1：(0.5~4)；The oxidation
The volume ratio of graphene aqueous dispersions and paraxylene is 5：(5~7)；The phase of the ethylene oxide propylene oxide block co-polyether
It is 8530 to molecular mass；
2nd, it is freeze-dried：
The graphene oxide emulsion freeze 0.5 for first obtaining step one under the conditions of temperature is -40 DEG C~-60 DEG C~
1.5h, is then to be freeze-dried 5~7 days under the conditions of -60 DEG C in temperature, obtains lyophilized graphene oxide block, then by lyophilized oxygen
Graphite alkene block, which is placed in vacuum drying chamber, to be dried, that is, obtains closed pore graphite oxide alkenyl heat-barrier material；The drying
Temperature be 60 DEG C, dry time is 12~48h.
The inventive method possesses following beneficial effect：
1st, the present invention is to prepare graphene oxide spherical droplets by emulsion method, and then freeze-drying removes molten in emulsion
Agent：Water and paraxylene, prepare the graphene oxide heat-barrier material with hole-closing structure, reduce the heat-insulated material of graphene oxide
The thermal conductivity factor of material, further improves the heat-proof quality of graphene oxide heat-barrier material；
2nd, graphene heat-barrier material is designed as hole-closing structure by the present invention, can effectively reduce graphene heat-barrier material stomata
Interior air thermal convection current effect, and then the heat-proof quality of graphene heat-barrier material is improved, Effective Regulation and the management of heat transfer are realized, is dashed forward
The limitation of the traditional insulation materials such as broken foamed plastics, glass fibre and asbestos；
3rd, graphene heat-barrier material prepared by the present invention can apply the composite Cryogenic tank in space industry exhausted
In heat structure, can also be applied in the insulation of thermal engineering pipeline and equipment, and liquid hydrogen, liquid nitrogen and liquid oxygen conveyance conduit guarantor
The storage and transmission of cold, liquefied natural gas and liquefaction coalbed, the insulation of building construction, refrigerating equipment etc. have important
Scientific value and Practical significance.
4th, the present invention selects ethylene oxide propylene oxide block co-polyether (F68) as a kind of high molecular surfactant,
Can synergistic oxidation graphene as stabilizer improve stability of emulsion, while the high score that it is 8530 that F68, which is relative molecular mass,
Sub- polymer, plays a supporting role in closed-cell insulation material.
5th, paraxylene is used as oil phase, the molecular structure of paraxylene and the hydrophobic side group of graphene oxide in the present invention
Structure is similar, and graphene oxide can be aligned on the surface of paraxylene and water, water, paraxylene and graphene oxide mixing
Liquid forms stable emulsion through high speed shear.Employed in reclaimed water of the present invention, paraxylene and graphene oxide liquid mixture to two
Toluene is as oil phase, and compared with other oil phase materials such as acetophenone, hexamethylene or chloroform, mixed liquor is 16000rpm's
Remain to keep the stabilization of emulsion under speed after high speed shear 10min, will not occur lamination；Acetophenone, hexamethylene or chloroform
Deng preparation emulsion under 16000rpm speed high speed shear 10min can be layered wild effect.
6th, the present invention is freezed graphene oxide emulsion in the environment of -60 DEG C, is then freeze-dried, to two
Toluene oil phase can be reclaimed in freeze drier, repeated and utilized, reduce and prepare the heat-insulated material of closed pore graphite oxide alkenyl
The cost of material.
7th, the inventive method environmental protection, simply, cost is low, repeats, it is easy to control.
8th, the graphene oxide heat-barrier material of hole-closing structure prepared by the present invention, 0.021~0.035g/cm of density3, density
Far smaller than common styrenic foams (30~40g/cm3) heat-barrier material, porosity 95.5~90.2%, thermal conductivity factor is
22.1mW/ (mK), is a kind of efficient and light weight heat-insulating material less than 55mW/ (mK).
Brief description of the drawings：
Fig. 1 is the photo in kind of graphite oxide alkenyl heat-barrier material prepared by embodiment 1；
Fig. 2 is the photo in kind of graphite oxide alkenyl heat-barrier material prepared by embodiment 2；
Fig. 3 is the photo in kind of graphite oxide alkenyl heat-barrier material prepared by embodiment 3；
Fig. 4 is the photo in kind of graphite oxide alkenyl heat-barrier material prepared by embodiment 4；
Fig. 5 is graphene oxide emulsion optical microscope photograph prepared by embodiment 4, and scale is 20 μm in figure；
Fig. 6 is the photo in kind of graphite oxide alkenyl heat-barrier material prepared by embodiment 5；
Fig. 7 is graphene oxide emulsion optical microscope photograph prepared by embodiment 5, and scale is 20 μm in figure；
Fig. 8 is graphite oxide alkenyl heat-barrier material scanning electron microscope (SEM) photograph prepared by embodiment 5.
Embodiment：
Technical solution of the present invention is not limited to act embodiment set forth below, in addition between each embodiment
Any reasonable combination.
Embodiment one：A kind of preparation method of closed pore graphite oxide alkenyl heat-barrier material of present embodiment, the party
Method is carried out according to the following steps：
First, graphene oxide emulsion is prepared：
Graphene oxide aqueous dispersions are prepared using Hummers methods, by oxirane epoxy under room temperature and stirring condition
Propane block co-polyether, which is stirred at room temperature, to be dissolved in graphene oxide aqueous dispersions, is then added paraxylene, is finally existed
5~30min of high speed shear under 8000~16000r/min speed, obtains graphene oxide emulsion；
2nd, it is freeze-dried：
The graphene oxide emulsion freeze 0.5 for first obtaining step one under the conditions of temperature is -40 DEG C~-60 DEG C~
1.5h, is then to be freeze-dried 5~7 days under the conditions of -60 DEG C in temperature, obtains lyophilized graphene oxide block, then by lyophilized oxygen
Graphite alkene block, which is placed in vacuum drying chamber, to be dried, that is, obtains closed pore graphite oxide alkenyl heat-barrier material.
Present embodiment possesses following beneficial effect：
1st, present embodiment is to prepare graphene oxide spherical droplets by emulsion method, and then freeze-drying is removed in emulsion
Solvent：Water and paraxylene, prepare the graphene oxide heat-barrier material with hole-closing structure, reduce graphene oxide every
The thermal conductivity factor of hot material, further improves the heat-proof quality of graphene oxide heat-barrier material；
2nd, graphene heat-barrier material is designed as hole-closing structure by present embodiment, can effectively reduce graphene heat-barrier material
Air thermal convection current is acted in stomata, and then improves the heat-proof quality of graphene heat-barrier material, realizes the Effective Regulation and pipe of heat transfer
Reason, breaks through the limitation of the traditional insulation materials such as foamed plastics, glass fibre and asbestos；
3rd, graphene heat-barrier material prepared by present embodiment can apply the composite low temperature in space industry to store
In case heat insulating construction, it can also be applied in the insulation of thermal engineering pipeline and equipment, and liquid hydrogen, liquid nitrogen and liquid oxygen conveyance conduit
Cold insulation, the storage and transmission of liquefied natural gas and liquefaction coalbed, the insulation of building construction, refrigerating equipment etc. have important
Scientific value and Practical significance.
4th, present embodiment is used as a kind of high-molecular surface active from ethylene oxide propylene oxide block co-polyether (F68)
Agent, can synergistic oxidation graphene as stabilizer improve stability of emulsion, while the height that it is 8530 that F68, which is relative molecular mass,
Molecularly Imprinted Polymer, plays a supporting role in closed-cell insulation material.
5th, paraxylene is used as oil phase, the molecular structure of paraxylene and the hydrophobic side of graphene oxide in present embodiment
Unit structure is similar, and graphene oxide can be aligned on the surface of paraxylene and water, water, paraxylene and graphene oxide
Mixed liquor forms stable emulsion through high speed shear.Adopted in present embodiment reclaimed water, paraxylene and graphene oxide liquid mixture
With paraxylene as oil phase, compared with other oil phase materials such as acetophenone, hexamethylene or chloroform, mixed liquor exists
Remain to keep the stabilization of emulsion under 16000rpm speed after high speed shear 10min, will not occur lamination；Acetophenone, ring
The emulsion of the preparation such as hexane or chloroform high speed shear 10min under 16000rpm speed can be layered wild effect.
6th, present embodiment is freezed graphene oxide emulsion in the environment of -60 DEG C, is then freeze-dried,
Paraxylene oil phase can be reclaimed in freeze drier, repeat utilize, reduce prepare closed pore graphite oxide alkenyl every
The cost of hot material.
7th, present embodiment method environmental protection, simply, cost is low, repeats, it is easy to control.
8th, the graphene oxide heat-barrier material of hole-closing structure prepared by present embodiment, 0.021~0.035g/cm of density3,
Density is far smaller than common styrenic foams (30~40g/cm3) heat-barrier material, porosity 95.5~90.2%, thermal conductivity factor
It is a kind of efficient and light weight heat-insulating material less than 55mW/ (mK) for 22.1mW/ (mK).
Embodiment two：Present embodiment from unlike embodiment one：Graphite oxide described in step one
The content of graphene oxide is 7~9mg/mL in alkene aqueous dispersions.Other steps and parameter are identical with embodiment one.
Embodiment three：Present embodiment from unlike embodiment one or two：Aoxidized described in step one
The mass ratio of graphene oxide and ethylene oxide propylene oxide block co-polyether in graphene aqueous dispersions is 1：(0.5~4).
Other steps and parameter are identical with embodiment one or two.
Embodiment four：Unlike one of present embodiment and embodiment one to three：Described in step one
The volume ratio of graphene oxide aqueous dispersions and paraxylene is 5：(5~7).Other steps and parameter and embodiment one
It is identical to one of three.
Embodiment five：Unlike one of present embodiment and embodiment one to four：Described in step one
The relative molecular mass of ethylene oxide propylene oxide block co-polyether is 8530.Other steps and parameter and embodiment one
It is identical to one of four.
Embodiment six：Unlike one of present embodiment and embodiment one to five：Described in step 2
Dry temperature is 60 DEG C, and the dry time is 12~48h.One of other steps and parameter and embodiment one to five phase
Together.
Beneficial effects of the present invention are verified using following examples：
Embodiment 1：
A kind of preparation method of closed pore graphite oxide alkenyl heat-barrier material, is specifically realized by the following steps：
First, graphene oxide emulsion is prepared：
Graphene oxide aqueous dispersions are prepared using Hummers methods, by oxirane epoxy under room temperature and stirring condition
Propane block co-polyether, which is stirred at room temperature, to be dissolved in graphene oxide aqueous dispersions, is then added paraxylene, is finally existed
High speed shear 10min under 16000 speed, obtains graphene oxide emulsion；
The content of graphene oxide is 8mg/mL in the graphene oxide aqueous dispersions；The graphene oxide moisture dissipates
The mass ratio of graphene oxide and ethylene oxide propylene oxide block co-polyether in liquid is 1:0.5；The graphene oxide water
The volume ratio of dispersion liquid and paraxylene is 5:7；The relative molecular mass of the ethylene oxide propylene oxide block co-polyether is
8530；
2nd, it is freeze-dried：
The graphene oxide emulsion freeze 0.5h for first obtaining step one under the conditions of temperature is -60 DEG C, then in temperature
Spend to be freeze-dried 5 days under the conditions of -60 DEG C, obtain lyophilized graphene oxide block, then lyophilized graphene oxide block is placed in
It is dried in vacuum drying chamber, that is, obtains closed pore graphite oxide alkenyl heat-barrier material；The temperature of the drying is 60 DEG C, is dried
Time be 24h；The photo in kind of graphite oxide alkenyl heat-barrier material prepared by embodiment 1 is as shown in Figure 1；
Embodiment 2：
The present embodiment is as different from Example 1：Graphene oxide in graphene oxide aqueous dispersions described in step one
Mass ratio with ethylene oxide propylene oxide block co-polyether is 1：1；Other are same as Example 1；Oxidation prepared by embodiment 2
The photo in kind of graphene-based heat-barrier material is as shown in Figure 2；
Embodiment 3：
The present embodiment is as different from Example 1：Graphene oxide in graphene oxide aqueous dispersions described in step one
Mass ratio with ethylene oxide propylene oxide block co-polyether is 1：2；Other are same as Example 1；
The photo in kind of graphite oxide alkenyl heat-barrier material prepared by embodiment 3 is as shown in Figure 3；Contrasted by Fig. 1,2 and 3
Show, in graphene oxide closed-cell insulation material prepared by different F68 contents, graphene oxide and F68 mass ratioes are 1:When 2,
It is preferable that the shape for the sample that freeze-drying is obtained is kept, and further relating to F68 can play a part of supporting heat-barrier material structure.
Embodiment 4：
The present embodiment is as different from Example 1：Graphene oxide in graphene oxide aqueous dispersions described in step one
Mass ratio with ethylene oxide propylene oxide block co-polyether is 1：4；Other are same as Example 1.Oxidation prepared by embodiment 4
The photo in kind of graphene-based heat-barrier material is as shown in Figure 4；Graphene oxide emulsion optical microscope photograph prepared by embodiment 4
As shown in figure 5, scale is 20 μm, as shown in Figure 5, a diameter of 6.5 ± 3.8 μm of graphene oxide microemulsion droplets in figure；
Embodiment 5：
The present embodiment is as different from Example 1：Oxirane ring is not added in step one graphene oxide aqueous dispersions
Ethylene Oxide block co-polyether；Other are same as Example 1.
The photo in kind of graphite oxide alkenyl heat-barrier material prepared by embodiment 5 is as shown in Figure 6；Contrasted by Fig. 4 and Fig. 6
Understand, the graphene oxide closed-cell insulation material containing F68 is able to maintain that shape in freeze-drying, play structural support work
With；
Graphene oxide emulsion optical microscope photograph prepared by embodiment 5 is as shown in fig. 7, scale is 20 μm in figure；From
Understood in figure, a diameter of 15.9 ± 7.3 μm of graphene oxide microemulsion droplets；By Fig. 7 and Fig. 5, F68 can make emulsion liquid
Drip diameter to reduce, be conducive to improving stability of emulsion；
Graphite oxide alkenyl heat-barrier material scanning electron microscope (SEM) photograph prepared by embodiment 5 is as shown in Figure 8；As can be known from Fig. 8, aoxidize
Graphene emulsion can form ball-type hole-closing structure, and freeze-drying back aperture size and diameter of droplets in emulsion by freeze-drying
It is close.
Claims (6)
1. a kind of preparation method of closed pore graphite oxide alkenyl heat-barrier material, it is characterised in that：This method is carried out according to the following steps；
First, graphene oxide emulsion is prepared：
Graphene oxide aqueous dispersions are prepared using Hummers methods, by ethylene oxide propylene oxide under room temperature and stirring condition
Block co-polyether, which is stirred at room temperature, to be dissolved in graphene oxide aqueous dispersions, then adds paraxylene, finally 8000~
5~30min of high speed shear under 16000r/min speed, obtains graphene oxide emulsion；
2nd, it is freeze-dried：
First temperature be -40 DEG C~-60 DEG C under the conditions of by step it is a kind of obtain graphene oxide emulsion freeze 0.5~
1.5h, is then to be freeze-dried 5~7 days under the conditions of -60 DEG C in temperature, obtains lyophilized graphene oxide block, then by lyophilized oxygen
Graphite alkene block, which is placed in vacuum drying chamber, to be dried, that is, obtains closed pore graphite oxide alkenyl heat-barrier material.
2. the preparation method of closed pore graphite oxide alkenyl heat-barrier material according to claim 1, it is characterised in that：Step one
The content of graphene oxide is 7~9mg/mL in the graphene oxide aqueous dispersions.
3. the preparation method of closed pore graphite oxide alkenyl heat-barrier material according to claim 1, it is characterised in that：Step one
The mass ratio of graphene oxide and ethylene oxide propylene oxide block co-polyether in the graphene oxide aqueous dispersions is 1：
(0.5~4).
4. the preparation method of closed pore graphite oxide alkenyl heat-barrier material according to claim 1, it is characterised in that：Step one
The volume ratio of the graphene oxide aqueous dispersions and paraxylene is 5：(5~7).
5. the preparation method of closed pore graphite oxide alkenyl heat-barrier material according to claim 1, it is characterised in that：Step one
The relative molecular mass of the ethylene oxide propylene oxide block co-polyether is 8530.
6. the preparation method of closed pore graphite oxide alkenyl heat-barrier material according to claim 1, it is characterised in that：Step 2
The temperature of the drying is 60 DEG C, and the dry time is 12~48h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114668868A (en) * | 2022-03-03 | 2022-06-28 | 苏州捷康人工智能科技有限公司 | Concatenation formula track sterilizer |
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| CN101941693A (en) * | 2010-08-25 | 2011-01-12 | 北京理工大学 | Graphene aerogel and preparation method thereof |
| CN103723718A (en) * | 2014-01-23 | 2014-04-16 | 哈尔滨工业大学 | Preparation method of thermal insulating material having ultralow density, ultrahigh elasticity and ultralow thermal conductivity |
| WO2016042321A1 (en) * | 2014-09-15 | 2016-03-24 | University Of York | Mesoporous materials from nanoparticle enhanced polysaccharides |
| CN105819440A (en) * | 2016-06-08 | 2016-08-03 | 东南大学 | Method for preparing block graphene aerogel |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101941693A (en) * | 2010-08-25 | 2011-01-12 | 北京理工大学 | Graphene aerogel and preparation method thereof |
| CN103723718A (en) * | 2014-01-23 | 2014-04-16 | 哈尔滨工业大学 | Preparation method of thermal insulating material having ultralow density, ultrahigh elasticity and ultralow thermal conductivity |
| WO2016042321A1 (en) * | 2014-09-15 | 2016-03-24 | University Of York | Mesoporous materials from nanoparticle enhanced polysaccharides |
| CN105819440A (en) * | 2016-06-08 | 2016-08-03 | 东南大学 | Method for preparing block graphene aerogel |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114668868A (en) * | 2022-03-03 | 2022-06-28 | 苏州捷康人工智能科技有限公司 | Concatenation formula track sterilizer |
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| CN107141012B (en) | 2020-06-09 |
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