CN102344779A - Method for preparing graphene and inorganic salt high-temperature phase change composite material - Google Patents
Method for preparing graphene and inorganic salt high-temperature phase change composite material Download PDFInfo
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- CN102344779A CN102344779A CN2010102470041A CN201010247004A CN102344779A CN 102344779 A CN102344779 A CN 102344779A CN 2010102470041 A CN2010102470041 A CN 2010102470041A CN 201010247004 A CN201010247004 A CN 201010247004A CN 102344779 A CN102344779 A CN 102344779A
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Abstract
The invention relates to a method for preparing a graphene and inorganic salt high-temperature phase change composite material. The method comprises the following steps of: (1) preparing graphene sol; (2) preparing an inorganic salt solution, adding a surfactant, and mixing uniformly; (3) adding the graphene sol into the inorganic salt solution, and stirring until the graphene sol and the inorganic salt solution are mixed uniformly to obtain a composite material preform; (4) putting the composite material preform into an ultra-low-temperature freezer, quickly freezing to form a solid and taking out; (5) putting the solid-state composite material preform into a vacuum freezing dispersion drying instrument and drying; and (6) taking out after the drying of the composite material preform is finished, and calcining until the moisture is completely removed to obtain a grapheme/inorganic salt phase change composite material. Compared with the prior art, the method has the advantages that: the process is reasonable, easy to operate and low in cost; and the prepared grapheme/inorganic salt phase change composite material has the advantages of high coefficient of heat conductivity, high energy storage density and the like, has excellent performance, can meet different application requirements, and is suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method of matrix material, especially relate to the preparation method of a kind of Graphene and inorganic salt high-temperature phase-change matrix material.
Background technology
Along with growing with each passing day of international energy demand, traditional fossil energy is because of the restriction of storage, environment and output, and clean solar receives much concern.Solar energy thermal-power-generating is the most effective solar utilization technique.In this technology, because the temperature that Salar light-gathering produces is high, selecting reliable high temperature heat transfer accumulation of heat working medium is the key that improves solar energy thermal-power-generating efficient.
Phase-change accumulation energy is comparatively effective energy storage mode at present.And in practical application, below the low temperature, the development of high-temperature heat-storage system was then slower relatively during the transformation temperature of existing phase-change accumulation energy system was in mostly.In solar energy high-temperature phase-change material heat accumulation process, the heat conductivility of system has very big influence to its service efficiency.And the heat conductivility of general phase change material is lower.
The composite phase-change material that with the carbon material is strongthener has excellent heat conductivility.Wherein Graphene has because of it during performances such as very high resistance to compression, heat conduction, conduction are used to the preparation of organic composite phase-change material and use.Show that according to the research report heat conductivility of Graphene is superior to other carbon materials such as carbon nanotube in carbon material family, so well used.But Graphene is reunited easily, and influence how in the Composite Preparation process, to eliminate its reunion is the difficult point in the whole process of preparation.
Summary of the invention
The object of the invention is exactly to provide a kind of energy storage big for the defective that overcomes above-mentioned prior art existence, the preparation method of the Graphene of good heat conductivity and inorganic salt high-temperature phase-change matrix material.
The object of the invention can be realized through following technical scheme:
The preparation method of a kind of Graphene and inorganic salt high-temperature phase-change matrix material is characterized in that, this method may further comprise the steps:
(1) graphite oxide is scattered in the deionized water, the gained mixture is handled, obtain mixed solution with ultrasonic cell pulverization machine; Mixed solution is carried out centrifugal treating, and getting that supernatant obtains with mono-layer graphite oxide alkene is the colloidal sol of disperse phase, to wherein adding Hydrazine Hydrate 80; Shaking up and being placed on temperature is to react 0.5～3h in 20～30 ℃ the water-bath; Controlling rotating speed again is 4000rpm, and the product that obtains is carried out centrifugal treating 5～20min, obtains Graphene colloidal sol;
(2) compound concentration is the inorganic salt solution of 5mg/ml～9mg/ml, to wherein adding tensio-active agent, it is mixed again;
(3) Graphene colloidal sol is mixed with inorganic salt solution and stir, obtain composite preform, place the cryotherapy case freezing rapidly this precast body, take out after treating to be frozen into solids fully;
(4) solids that step (3) is made places vacuum freezing to disperse drying installation to carry out drying; Took out the back at room temperature dry 8～10 days earlier; Place vacuum dryer to be fired to moisture then and remove fully, promptly obtain Graphene and inorganic salt phase change composite material.
The concentration of graphite oxide is 1.0mg/ml～1.2mg/ml in the mixed solution of said step (1).
The weight ratio of Hydrazine Hydrate 80 and mono-layer graphite oxide alkene is (1.0～1.2) in the said step (1): 1.
Inorganic salt in the said step (2) are one or more in muriate, nitrate salt or the carbonate.
The preferred lithium nitrate of inorganic salt, SODIUMNITRATE or saltpetre in the said step (2).
Tensio-active agent in the said step (2) is a sodium lauryl sulphate, and the add-on of tensio-active agent is 0.01～0.05% of an inorganic salt quality.
The Graphene in the composite preform of said step (3) and the weight ratio of inorganic salt are 1: (1～9).
The temperature of cryotherapy case is-120 ℃～-140 ℃ in the said step (3).
The condenser temperature of vacuum freezing drying device is-54 ℃～-45 ℃ in the said step (4), and pressure is 13Pa.
The temperature of vacuum dryer is 100 ℃ in the said step (4), and be 10min time of drying.
Compared with prior art, the present invention selects heat of phase transformation big, and transformation temperature is high; The good comprehensive properties inorganic salt are chosen the Graphene carbon material as strongthener as the fundamental research material, and technology is reasonable; Simple to operate, with low cost, the Graphene that makes/inorganic salt phase change composite material has the thermal conductivity height; Various advantage excellent propertys such as energy storage density is big can satisfy different application requirements, are fit to suitability for industrialized production.
Description of drawings
Fig. 1 is a process flow sheet of the present invention;
The thermal conductivity that Fig. 2 obtains product for embodiment 1 is with the variation of temperature curve;
The thermal conductivity that Fig. 3 obtains product for embodiment 2 is with the variation of temperature curve;
The thermal conductivity that Fig. 4 obtains product for embodiment 3 is with the variation of temperature curve.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is elaborated.
Embodiment 1
The preparation method of a kind of Graphene/inorganic salt high-temperature phase-change matrix material, its technical process is as shown in Figure 1, and this method may further comprise the steps:
According to mass ratio is 5.5: 4.5, takes by weighing 1.10g LiNO respectively with the YP102N electronic balance
3, 0.90g NaNO
3Configuration 8mg/ml mixed nitrate solution 250ml.Get 8mg/ml mixed nitrate solution 10ml, add a certain amount of tensio-active agent sodium lauryl sulphate SDS, stir until mixing.Constant temperature blender with magnetic force stirs 20min, ultra-sonic dispersion 20min.Measure the redox graphene colloidal sol 20ml of 1mg/ml, add in the above-mentioned mixing solutions, stirring is dispersed in until redox graphene colloidal sol and obtains composite preform in the mixing solutions rapidly.
Composite preform is placed the plastics casing that is covered with masking foil, seal, put into cryotherapy case quick freezing, note the maintenance level simultaneously with preservative film.Treat that liquid form mixt is frozen into when solid-state, take out, substitute preservative film with masking foil and seal plastics casing; And cover at masking foil and to stab several pores; Put into the vacuum lyophilization diverting device and carry out vacuum lyophilization, the device condenser temperature is made as-54 ℃ ℃, and pressure is 13Pa.
Dry 8 days, treat that moisture is removed after, take out the temperature vacuum condition calcining down that places 100 ℃, calcining 10min.Obtaining mass ratio is the redox graphene/mixed nitrate high temperature composite phase-change material of 1: 4 (2: 8).Through MDSC test with calculate, the temperature variant curve of thermal conductivity such as Fig. 2 that can this matrix material.
Take by weighing 2.25gKNO with the YP102N electronic balance
3Configuration 9mg/ml KNO
3Solution 250ml; Get 9mg/mlKNO
3Solution 10ml adds a certain amount of tensio-active agent sodium lauryl sulphate SDS, stirs until mixing.Constant temperature blender with magnetic force stirs 20min, ultra-sonic dispersion 20min; Measure the redox graphene colloidal sol 10ml of 1mg/ml, add in the above-mentioned mixing solutions, stirring is dispersed in until redox graphene colloidal sol and obtains composite preform in the mixing solutions rapidly.
Composite preform is placed the plastics casing that is covered with masking foil, seal, put into cryotherapy case quick freezing, note the maintenance level simultaneously with preservative film.Treat that liquid form mixt is frozen into when solid-state, take out, substitute preservative film with masking foil and seal plastics casing; And cover at masking foil and to stab several pores; Put into the vacuum lyophilization diverting device and carry out vacuum lyophilization, the device condenser temperature is made as-50 ℃, and pressure is 13Pa.
Dry 9 days, treat that moisture is removed after, take out the temperature vacuum condition calcining down that places 100 ℃, calcining 10min obtains mass ratio and is redox graphene/saltpetre high temperature composite phase-change material of 1: 9.Through MDSC test with calculate, the temperature variant curve of thermal conductivity such as Fig. 3 that can this matrix material.
Embodiment 3
As shown in Figure 1, a kind of Graphene/inorganic salt high-temperature phase-change matrix material and preparation method thereof, this method may further comprise the steps:
Take by weighing 2.00gKNO with the YPl02N electronic balance
3Configuration 8mg/ml KNO
3Solution 250ml; Get 8mg/mlKNO
3Solution 10ml adds a certain amount of tensio-active agent sodium lauryl sulphate SDS, stirs until mixing; Constant temperature blender with magnetic force stirs 20min, ultra-sonic dispersion 20min; Measure the redox graphene colloidal sol 20ml of 1mg/ml, add in the above-mentioned mixing solutions, stirring is dispersed in until redox graphene colloidal sol and obtains composite preform in the mixing solutions rapidly.
Composite preform is placed the plastics casing that is covered with masking foil, seal, put into cryotherapy case quick freezing, note the maintenance level simultaneously with preservative film; Treat that liquid form mixt is frozen into when solid-state; Take out; Substitute preservative film with masking foil and seal plastics casing, and cover stamp several pores (light Graphene is taken and prevent away the entering of impurity when preventing to vacuumize), put into the vacuum lyophilization diverting device and carry out vacuum lyophilization at masking foil; The device condenser temperature is made as-45 ℃, and pressure is 13Pa;
Dry 10 days, treat that moisture is removed after, take out the temperature vacuum condition calcining down that places 100 ℃, calcining 10min, obtaining mass ratio is the redox graphene/saltpetre high temperature composite phase-change material of 1: 4 (2: 8).Through MDSC test with calculate, the temperature variant curve of thermal conductivity such as Fig. 4 that can this matrix material.
The preparation method of a kind of Graphene and inorganic salt high-temperature phase-change matrix material, this method may further comprise the steps:
(1) graphite oxide is scattered in the deionized water, the concentration of controlled oxidation graphite is 1.0mg/ml, with ultrasonic cell pulverization machine the gained mixture is handled; Mixed solution after centrifugal treating is ultrasonic; Getting that supernatant obtains with mono-layer graphite oxide alkene is the colloidal sol of disperse phase, and to wherein adding Hydrazine Hydrate 80, the weight ratio of Hydrazine Hydrate 80 and mono-layer graphite oxide alkene is 1: 1; Shaking up and being placed on temperature is to react 3h in 20 ℃ the water-bath; Controlling rotating speed again is 4000rpm, and the product that obtains is carried out centrifugal treating 5min, obtains redox graphene colloidal sol;
(2) compound concentration is the sodium chloride solution of 5mg/ml, and again to wherein adding sodium lauryl sulphate, the add-on of controlling this tensio-active agent is 0.01% of a weight sodium chloride, and it is mixed;
(3) weight ratio of control Graphene and sodium-chlor is 1: 1; Graphene colloidal sol is mixed with sodium chloride solution and stirs; Obtain composite preform; The temperature of control cryotherapy case is-120 ℃, places the cryotherapy case freezing rapidly this precast body, takes out after treating to be frozen into solids fully;
(4) condenser temperature of control vacuum freezing drying device is-54 ℃, and pressure is 13Pa, places vacuum freezing to disperse dry instrument to carry out drying solid-state composite preform; Took out the back at room temperature dry 9 days earlier; Place vacuum dryer then, the temperature of control vacuum dryer is 100 ℃, and be 10min time of drying; It is fired to moisture removes fully, promptly obtain Graphene and inorganic salt phase change composite material.
The preparation method of a kind of Graphene and inorganic salt high-temperature phase-change matrix material, this method may further comprise the steps:
(1) graphite oxide is scattered in the deionized water, the concentration of controlled oxidation graphite is 1.2mg/ml, with ultrasonic cell pulverization machine the gained mixture is handled; Mixed solution after centrifugal treating is ultrasonic; Getting that supernatant obtains with mono-layer graphite oxide alkene is the colloidal sol of disperse phase, and to wherein adding Hydrazine Hydrate 80, the weight ratio of Hydrazine Hydrate 80 and mono-layer graphite oxide alkene is 1.2: 1; Shaking up and being placed on temperature is to react 0.5h in 30 ℃ the water-bath; Controlling rotating speed again is 4000rpm, and the product that obtains is carried out centrifugal treating 20min, obtains redox graphene colloidal sol;
(2) compound concentration is the sodium carbonate solution of 9mg/ml, and again to wherein adding sodium lauryl sulphate, the add-on of controlling this tensio-active agent is 0.05% of a yellow soda ash weight, and it is mixed;
(3) weight ratio of control Graphene and yellow soda ash is 1: 9; Graphene colloidal sol is mixed with sodium carbonate solution and stirs; Obtain composite preform; The temperature of control cryotherapy case is-140 ℃, places the cryotherapy case freezing rapidly this precast body, takes out after treating to be frozen into solids fully;
(4) condenser temperature of control vacuum freezing drying device is-45 ℃, and pressure is 13Pa, places vacuum freezing to disperse dry instrument to carry out drying solid-state composite preform; Took out the back at room temperature dry 10 days earlier; Place vacuum dryer then, the temperature of control vacuum dryer is 100 ℃, and be 10min time of drying; It is fired to moisture removes fully, promptly obtain Graphene and inorganic salt phase change composite material.
Claims (10)
1. the preparation method of Graphene and inorganic salt high-temperature phase-change matrix material is characterized in that this method may further comprise the steps:
(1) graphite oxide is scattered in the deionized water, the gained mixture is handled, obtain mixed solution with ultrasonic cell pulverization machine; Mixed solution is carried out centrifugal treating, and getting that supernatant obtains with mono-layer graphite oxide alkene is the colloidal sol of disperse phase, to wherein adding Hydrazine Hydrate 80; Shaking up and being placed on temperature is to react 0.5～3h in 20～30 ℃ the water-bath; Controlling rotating speed again is 4000rpm, and the product that obtains is carried out centrifugal treating 5～20min, obtains Graphene colloidal sol;
(2) compound concentration is the inorganic salt solution of 5mg/ml～9mg/ml, to wherein adding tensio-active agent, it is mixed again;
(3) Graphene colloidal sol is mixed with inorganic salt solution and stir, obtain composite preform, place the cryotherapy case freezing rapidly this precast body, take out after treating to be frozen into solids fully;
(4) solids that step (3) is made places vacuum freezing to disperse drying installation to carry out drying; Took out the back at room temperature dry 8～10 days earlier; Place vacuum dryer to be fired to moisture then and remove fully, promptly obtain Graphene and inorganic salt phase change composite material.
2. the preparation method of a kind of Graphene according to claim 1 and inorganic salt high-temperature phase-change matrix material is characterized in that, the concentration of graphite oxide is 1.0mg/ml～1.2mg/ml in the mixed solution of said step (1).
3. the preparation method of a kind of Graphene according to claim 1 and inorganic salt high-temperature phase-change matrix material is characterized in that, the weight ratio of Hydrazine Hydrate 80 and mono-layer graphite oxide alkene is (1.0～1.2) in the said step (1): 1.
4. the preparation method of a kind of Graphene according to claim 1 and inorganic salt high-temperature phase-change matrix material is characterized in that, the inorganic salt in the said step (2) are one or more in muriate, nitrate salt or the carbonate.
5. according to the preparation method of claim 1 or 4 described a kind of Graphenes and inorganic salt high-temperature phase-change matrix material, it is characterized in that the preferred lithium nitrate of inorganic salt, SODIUMNITRATE or saltpetre in the said step (2).
6. the preparation method of a kind of Graphene according to claim 1 and inorganic salt high-temperature phase-change matrix material; It is characterized in that; Tensio-active agent in the said step (2) is a sodium lauryl sulphate, and the add-on of tensio-active agent is 0.01～0.05wt% of inorganic salt.
7. the preparation method of a kind of Graphene according to claim 1 and inorganic salt high-temperature phase-change matrix material is characterized in that, the Graphene in the composite preform of said step (3) and the weight ratio of inorganic salt are 1: (1～9).
8. the preparation method of a kind of Graphene according to claim 1 and inorganic salt high-temperature phase-change matrix material is characterized in that, the temperature of cryotherapy case is-120 ℃～-140 ℃ in the said step (3).
9. the preparation method of a kind of Graphene according to claim 1 and inorganic salt high-temperature phase-change matrix material is characterized in that, the condenser temperature of vacuum freezing drying device is-54 ℃～-45 ℃ in the said step (4), and pressure is 13Pa.
10. the preparation method of a kind of Graphene according to claim 1 and inorganic salt high-temperature phase-change matrix material is characterized in that, the temperature of vacuum dryer is 100 ℃ in the said step (4), and be 10min time of drying.
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| CN103525373A (en) * | 2012-07-05 | 2014-01-22 | 中国科学院大连化学物理研究所 | Composite amorphous phase-change heat storage material and preparation method thereof |
| CN104845591A (en) * | 2015-03-31 | 2015-08-19 | 戚荣生 | Heat storage phase-change material |
| CN105018041A (en) * | 2015-06-11 | 2015-11-04 | 贵州新碳高科有限责任公司 | Porous graphene film, and phase-changing energy-storing composite material |
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Application publication date: 20120208 |