CN102344778A - Preparation method of high-temperature phase-change composite material - Google Patents

Preparation method of high-temperature phase-change composite material Download PDF

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Publication number
CN102344778A
CN102344778A CN2010102469896A CN201010246989A CN102344778A CN 102344778 A CN102344778 A CN 102344778A CN 2010102469896 A CN2010102469896 A CN 2010102469896A CN 201010246989 A CN201010246989 A CN 201010246989A CN 102344778 A CN102344778 A CN 102344778A
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temperature phase
preparation
matrix material
inorganic
change matrix
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CN2010102469896A
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张东
曾亮
张震雷
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Tongji University
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Tongji University
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Abstract

The invention relates to a preparation method of a high-temperature phase-change composite material, which comprises the following steps: adding two inorganic salts into deionized water, fully stirring till the mixture is completely dissolved so as to obtain an inorganic mixed salt saturated solution, slowly and dropwisely adding the solution into a carbon material, continuously stirring to obtain a carbon material/inorganic salt mixed solution, performing ultrasonic treatment to obtain a mixed solution with uniformly-dispersed carbon materials, putting the mixed solution in a drying oven, completely drying the water, taking out and grinding to obtain a product. Compared with the prior art, the invention has a reasonable process, simple operations, and low cost; the prepared porous graphite carbon/nanotube/inorganic salt high-temperature phase-change composite material has excellent performance, can meet different application requirements, and is applicable to industrial production.

Description

A kind of preparation method of high-temperature phase-change matrix material
Technical field
The present invention relates to a kind of preparation method of matrix material, especially relate to a kind of porous graphite/carbon nanotube/inorganic salt high-temperature phase-change composite material and preparation method thereof.
Background technology
Fast development along with whole world industry; Problems such as fossil energy exhaustion and environmental pollution are more and more outstanding; Particularly the mankind increase demands for energy day by day now; Produce and life in to the serious waste phenomenon of the energy; Can not effectively utilize the energy (like sun power) of occurring in nature again; Phase change material can store the energy or the natural energy resources of these wastes as a kind of energy storage material; Needs according to different discharge; Make the energy obtain reasonable use, its Application Areas mainly comprises solar energy thermal-power-generating; Industry thermal utilization and waste heat recovery; Power peak regulation; Building energy conservation; Agricultural greenhouse; Aerospace equipment etc.To solar energy thermal-power-generating, the demand of aspects such as high temperature industrial furnace regenerator, high-temperature phase-change energy storage material becomes the type material that comes into one's own day by day.The inorganic salts phase change material has the fusing point height, and volume change is little in the phase transition process, and latent heat of phase change is big, and advantages such as low price are to use maximum high-temperature phase-change energy storage materials at present.Yet the inorganic salts high-temperature phase-change energy storage material generally has shortcomings such as heat transfer property is low, corrodes container easily like muriate, and some carbonate decomposes easily, and viscosity is big when liquid, and volume change is big etc. during the fluorochemical phase transformation, in application, has received very big restriction.So improve the thermal conductivity of phase-changing energy storage material, solve the key that problems such as itself and instrument consistency become the phase change material widespread use.
Summary of the invention
The object of the invention is exactly the preparation method that a kind of technology high-temperature phase-change matrix material reasonable, simple to operate is provided for the defective that overcomes above-mentioned prior art existence.
The object of the invention can be realized through following technical scheme:
A kind of preparation method of high-temperature phase-change matrix material is characterized in that, this method may further comprise the steps:
(1) two kinds of inorganic salt is joined fully stirring in the deionized water, it is dissolved fully, obtain inorganic mixing salt saturated solution;
(2) take by weighing carbon material, be placed in the furnace pot of clean dry;
(3) inorganic mixed-salt aqueous solution is slowly splashed in the carbon material, and constantly stir, obtain carbon material/inorganic salt mixing solutions, carry out supersound process then, obtain the finely dispersed mixing solutions of carbon material;
(4) mixing solutions is placed loft drier, with the moisture complete drying, taking-up promptly obtains product after grinding.
Inorganic salt in the said step (1) comprise nitrate, muriate or carbonate.
Two kinds of preferred SODIUMNITRATE of inorganic salt in the said step (1) and lithium nitrate.
The weight ratio of two kinds of inorganic salt in the said step (1) is 1: 9~9: 1.
The concentration of the inorganic mixing salt saturated solution in the said step (1) is 10~60wt%.
Carbon material in the said step (2) is porous graphite or carbon nanotube.
The amount of the carbon material in the said step (3) be inorganic mixing salt 1~99wt%.
The time of the supersound process in the said step (3) is 5~20min.
The loft drier temperature is 40~100 ℃ in the said step (4), and be 24~48h time of drying.
Compared with prior art; Porous graphite/carbon nanotube that the present invention prepares/inorganic salt high-temperature phase-change matrix material and preparation method thereof technology is reasonable; Simple to operate; It is poor to have solved inorganic salt high temperature phase change material (pcm) heat conductivility; The problem of easy corrosion container etc.; The phase change composite material excellent property that makes can satisfy different application requirements, is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is the process flow sheet of embodiment 1;
The thermal conductivity that Fig. 2 obtains product for embodiment 1 is with the variation of temperature curve;
Fig. 3 is the process flow sheet of embodiment 2;
The thermal conductivity that Fig. 4 obtains product for embodiment 2 is with the variation of temperature curve;
The thermal conductivity that Fig. 5 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 porous graphite/inorganic salt high-temperature phase-change matrix material, its technical process as shown in Figure 1, this method may further comprise the steps:
(1) respectively takes by weighing the NaNO of 30g at 4.5: 5.5 by mass ratio 3(13.5g) and LiNO 3(17.5g), add the deionized water of 50mL, be stirred well to dissolving fully, be mixed with concentration and be 37.5% NaNO 3-LiNO 3(4.5-5.5) saturated solution is labeled as A.
(2) will clean and the exsiccant furnace pot places on the electronic balance after the zero clearing accurately weighing 0.5g porous graphite.
(3) get A solution 13.3g (containing mixing salt quality 5g) in the step (1), slowly be added drop-wise in the porous graphite, and constantly stir, inorganic salt solution is fully absorbed by porous graphite, obtain porous graphite/NaNO after the supersound process 3-LiNO 3(4.5-5.5) mixing solutions.
(4) with porous graphite/NaNO 3-LiNO 3(4.5-5.5) mixing solutions places 70 ℃ of loft drier 24h, evaporates fully until moisture, obtains porous graphite (inorganic salt quality 10%)/NaNO after take out grinding 3-LiNO 3(4.5-5.5) high-temperature phase-change matrix material.Through MDSC test with calculate, the temperature variant curve of thermal conductivity such as Fig. 2 that can this matrix material.
Embodiment 2
The preparation method of a kind of carbon nanotube/inorganic salt high-temperature phase-change matrix material, its technical process as shown in Figure 3, this method may further comprise the steps:
(1) respectively takes by weighing the NaNO of 30g at 4.5: 5.5 by mass ratio 3(13.5g) and LiNO 3(17.5g), add the deionized water of 50mL, be stirred well to dissolving fully, be mixed with concentration and be 37.5% NaNO 3-LiNO 3(4.5-5.5) saturated solution is labeled as B.
(2) will clean and the exsiccant furnace pot places on the electronic balance after the zero clearing accurately weighing 1.5g carbon nanotube.
(3) get B solution 13.3g (containing mixing salt quality 5g) in the step (1), slowly be added drop-wise in the carbon nanotube, and constantly stir, make inorganic salt solution fully and carbon nanotube compound, obtain carbon nanotube/NaNO after the supersound process 3-LiNO 3(4.5-5.5) mixing solutions.
(4) with carbon nanotube/NaNO 3-LiNO 3(4.5-5.5) mixing solutions places 70 ℃ of loft drier 24h, evaporates fully until moisture, obtains carbon nanotube (inorganic salt quality 30%)/NaNO after take out grinding 3-LiNO 3(4.5-5.5) high-temperature phase-change matrix material.Through MDSC test with calculate, the temperature variant curve of thermal conductivity such as Fig. 4 that can this matrix material.
Embodiment 3
The preparation method of a kind of porous graphite/inorganic salt high-temperature phase-change matrix material, this method may further comprise the steps:
(1) respectively takes by weighing the NaNO of 30g at 4.5: 5.5 by mass ratio 3(13.5g) and LiNO 3(17.5g), add the deionized water of 50mL, be stirred well to dissolving fully, be mixed with concentration and be 37.5% NaNO 3-LiNO 3(4.5-5.5) saturated solution is labeled as C.
(2) will clean and the exsiccant furnace pot places on the electronic balance after the zero clearing accurately weighing 0.35g porous graphite.
(3) get C solution 1.35g (containing mixing salt quality 0.5g) in the step (1), slowly be added drop-wise in the porous graphite, and constantly stir, make inorganic salt solution fully and porous graphite compound, obtain porous graphite/NaNO after the supersound process 3-LiNO 3(4.5-5.5) mixing solutions.
(4) with porous graphite/NaNO 3-LiNO 3(4.5-5.5) mixing solutions places 70 ℃ of loft drier 24h, evaporates fully until moisture, obtains porous graphite (inorganic salt quality 70%)/NaNO after take out grinding 3-LiNO 3(4.5-5.5) high-temperature phase-change matrix material.Through MDSC test with calculate, the temperature variant curve of thermal conductivity such as Fig. 5 that can this matrix material.
Embodiment 4
A kind of preparation method of high-temperature phase-change matrix material, this method may further comprise the steps:
(1) with sodium-chlor and Repone K by weight being to join in the deionized water after mixing at 1: 9 fully to stir, it is dissolved fully, obtaining sodium-chlor-Repone K mixing salt concentration is the saturated solution of 10wt%;
(2) take by weighing the 0.01g porous graphite, in the furnace pot with its clean dry;
(3) 10g sodium-chlor-Repone K mixing salt solution (containing mixing salt 1g) is slowly splashed in the porous graphite, and constantly stir, obtain porous graphite/inorganic salt mixing solutions, carry out supersound process 5min then, obtain the finely dispersed mixing solutions of porous graphite;
(4) mixing solutions is placed loft drier, control loft drier temperature is 40 ℃, time of drying be 48h with the moisture complete drying, take out and promptly obtain the high-temperature phase-change matrix material after grinding.
Embodiment 5
A kind of preparation method of high-temperature phase-change matrix material, this method may further comprise the steps:
(1) with yellow soda ash and salt of wormwood by weight being to join in the deionized water after mixing at 9: 1 fully to stir, it is dissolved fully, obtaining yellow soda ash-salt of wormwood mixing salt concentration is the saturated solution of 60wt%;
(2) take by weighing the 0.59g carbon nanotube, in the furnace pot with its clean dry;
(3) 1g yellow soda ash-salt of wormwood mixing salt solution (containing mixing salt 0.6g) is slowly splashed in the carbon nanotube; And constantly stir; Obtain carbon nanotube/inorganic salt mixing solutions, carry out supersound process 20min then, obtain the finely dispersed mixing solutions of carbon nanotube;
(4) mixing solutions is placed loft drier, control loft drier temperature is 100 ℃, time of drying be 24h with the moisture complete drying, take out and promptly obtain the high-temperature phase-change matrix material after grinding.

Claims (9)

1. the preparation method of a high-temperature phase-change matrix material is characterized in that, this method may further comprise the steps:
(1) two kinds of inorganic salt is joined fully stirring in the deionized water, it is dissolved fully, obtain inorganic mixing salt saturated solution;
(2) take by weighing carbon material, be placed in the furnace pot of clean dry;
(3) inorganic mixed-salt aqueous solution is slowly splashed in the carbon material, and constantly stir, obtain carbon material/inorganic salt mixing solutions, carry out supersound process then, obtain the finely dispersed mixing solutions of carbon material;
(4) mixing solutions is placed loft drier, with the moisture complete drying, taking-up promptly obtains product after grinding.
2. the preparation method of a kind of high-temperature phase-change matrix material according to claim 1 is characterized in that, the inorganic salt in the said step (1) comprise nitrate, muriate or carbonate.
3. the preparation method of a kind of high-temperature phase-change matrix material according to claim 1 and 2 is characterized in that, two kinds of preferred SODIUMNITRATE of inorganic salt in the said step (1) and lithium nitrate.
4. the preparation method of a kind of high-temperature phase-change matrix material according to claim 1 is characterized in that, the weight ratio of two kinds of inorganic salt in the said step (1) is 1: 9~9: 1.
5. the preparation method of a kind of high-temperature phase-change matrix material according to claim 1 is characterized in that, the concentration of the inorganic mixing salt saturated solution in the said step (1) is 10~60wt%.
6. the preparation method of a kind of high-temperature phase-change matrix material according to claim 1 is characterized in that, the carbon material in the said step (2) is porous graphite or carbon nanotube.
7. the preparation method of a kind of high-temperature phase-change matrix material according to claim 1 is characterized in that, the amount of the carbon material in the said step (3) be inorganic mixing salt 1~99wt%.
8. the preparation method of a kind of high-temperature phase-change matrix material according to claim 1 is characterized in that, the time of the supersound process in the said step (3) is 5~20min.
9. the preparation method of a kind of high-temperature phase-change matrix material according to claim 1 is characterized in that, the loft drier temperature is 40~100 ℃ in the said step (4), and be 24~48h time of drying.
CN2010102469896A 2010-08-06 2010-08-06 Preparation method of high-temperature phase-change composite material Pending CN102344778A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103773317A (en) * 2012-10-24 2014-05-07 深圳市润麒麟科技发展有限公司 Multi-layer carbon nanotube composite phase-change energy-storage material and preparation method thereof
CN104357020A (en) * 2014-11-28 2015-02-18 巴彦淖尔市卓越建筑材料有限公司 Nanometer modified inorganic room-temperature phase change heat storage material and preparation method thereof
CN105623619A (en) * 2016-02-02 2016-06-01 小墨热管理材料技术(深圳)有限公司 Flexible heat conduction/heat storage double-function composite material, method for manufacturing same and application of flexible heat conduction/heat storage double-function composite material
CN106047303A (en) * 2016-06-30 2016-10-26 郭舒洋 Preparation method of high-heat-conductivity composite heat storage material
CN109560296A (en) * 2017-09-27 2019-04-02 清远道动新材料科技有限公司 Perovskite type catalyst and its preparation method and application, zinc air secondary cell

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张焘等: "《膨胀石墨、石墨烯改善无机盐相变材料热物性能》", 《无机盐工业》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103773317A (en) * 2012-10-24 2014-05-07 深圳市润麒麟科技发展有限公司 Multi-layer carbon nanotube composite phase-change energy-storage material and preparation method thereof
CN104357020A (en) * 2014-11-28 2015-02-18 巴彦淖尔市卓越建筑材料有限公司 Nanometer modified inorganic room-temperature phase change heat storage material and preparation method thereof
CN104357020B (en) * 2014-11-28 2017-08-25 巴彦淖尔市卓越建筑材料有限公司 A kind of nano modified inorganic room temperature phase-change heat accumulating and preparation method thereof
CN105623619A (en) * 2016-02-02 2016-06-01 小墨热管理材料技术(深圳)有限公司 Flexible heat conduction/heat storage double-function composite material, method for manufacturing same and application of flexible heat conduction/heat storage double-function composite material
CN105623619B (en) * 2016-02-02 2019-09-10 小墨热管理材料技术(深圳)有限公司 A kind of flexibility is thermally conductive/the difunctional composite material and preparation method of heat accumulation and purposes
CN106047303A (en) * 2016-06-30 2016-10-26 郭舒洋 Preparation method of high-heat-conductivity composite heat storage material
CN109560296A (en) * 2017-09-27 2019-04-02 清远道动新材料科技有限公司 Perovskite type catalyst and its preparation method and application, zinc air secondary cell

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