CN102827584A - High-phase-change thermoset phase change material and preparation method thereof - Google Patents
High-phase-change thermoset phase change material and preparation method thereof Download PDFInfo
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- CN102827584A CN102827584A CN2012103153279A CN201210315327A CN102827584A CN 102827584 A CN102827584 A CN 102827584A CN 2012103153279 A CN2012103153279 A CN 2012103153279A CN 201210315327 A CN201210315327 A CN 201210315327A CN 102827584 A CN102827584 A CN 102827584A
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Abstract
The invention discloses a high-phase-change thermoset phase change material. The high-phase-change thermoset phase change material is prepared form expandable graphite of which the expansion multiplying power is 100-500mL/g and erythritol which is adsorbed into gaps of the expandable graphite, wherein the weight of the expandable graphite accounts for 10-20 percent of the total weight, and the balance is erythritol. The method comprises the following steps of: heating erythritol in an oil bath of 125-135 DEG C according to a certain proportion till the erythritol is fully molten for later use; putting expandable graphite into a vacuum drying oven; drying at the temperature of 65-75 DEG C under the vacuum degree of -0.09MPa for 8-12 hours; taking out, and putting into a muffle furnace of which the temperature is 700-800 DEG C for calcining for 30-90 seconds to form expansion graphite with a microcellular structure for later use; stirring the two kinds of materials in the oil bath for 1-1.5 hours; and naturally cooling to obtain a product. The high-phase-change thermoset phase change material is simple in structure; and according to the porous adsorption characteristic of the expansion graphite and the high-phase-change potential heat value of the erythritol, the product has higher phase change potential heat value than a phase change material prepared in the prior art.
Description
Technical field
The present invention relates to a kind of functional composite material technical field, relate to a kind of high heat of phase transformation typing phase change material and preparation method thereof specifically.
Background technology
Phase change material is meant with temperature variation and changes the material that form also can provide latent heat.Utilize the latent heat of phase change material can carry out the storage or the release of energy; To make the facility of various raising energy utilization rates; Phase change material commonly used is the solid-liquid phase change material; Be that its phase transition process is to be become liquid state or become solid-state journey by liquid state by solid-state, at this moment phase change material will absorb or discharge a large amount of latent heat.The application of phase change material aspect peak load shifting, novel energy-saving construction timber, waste heat recovery and the air-conditioning technical of sun power utilization, aerospace, thermal load more and more widely.Because its related device is simple, volume is little, flexible design, easy to use and be easy to characteristics such as management and popular.
In numerous latent heat storage materials, use the more materials such as paraffin, lipid acid, inorganic hydrated salt, glycitols that mainly contain.Wherein, sugar alcohol be one type very important in warm phase-change heat-storage material, it can provide the multiple phase change material of fusing point 100 deg.c, its advantage is that latent heat density is than higher.Yet present a kind of problem of ubiquity; The solid-liquid phase change material leaks after in phase transition process, producing liquid easily, generally adopts to this problem at present phase change material is carried out micro encapsulation, discloses a kind of glycitols typing phase-change material micro-capsule like Chinese patent CN102492397; Its latent heat of phase change value is about 230J/g; But because the restriction of micro encapsulation rate can not be given full play to the high latent heat density of sugar alcohol, and the micro encapsulation cost is very high, is difficult to realize suitability for industrialized production.
Summary of the invention
To the objective of the invention is the deficiency in order solving the problems of the technologies described above, a kind of high heat of phase transformation typing phase change material to be provided, the present invention is with low cost, nontoxic non-corrosiveness, and the latent heat of phase change value is big, good stability.
The present invention is in order to solve the deficiency of above-mentioned technology; The technical scheme that is adopted is: a kind of high heat of phase transformation typing phase change material; The expansible black lead that by expansion multiplying power is 100-500 mL/g is processed with the erythritol that is adsorbed in the expansible black lead space; Wherein, the weight of expansible black lead accounts for the 10-20% of gross weight, and all the other are erythritol;
A kind of high heat of phase transformation typing phase change material, its preparation method is:
Step 1, raw-material choosing
Take by weighing the expansible black lead that erythritol and expansion multiplying power are 100-500 mL/g respectively, and the weight of erythritol accounts for the 80-90% of erythritol and expansible black lead particle gross weight;
Step 2, the erythritol that step 1 is taken by weighing are placed in the beaker, in 125～135 ℃ oil bath, heat, and it is subsequent use to form melt;
Step 3, the expansion multiplying power that step 1 is taken by weighing are that the expansible black lead of 100-500 mL/g is put into vacuum drying oven; Temperature be 65～75 ℃, vacuum tightness for the condition of-0.09MPa under dry 8～12 hours; Taking out then and placing temperature is retort furnace roasting 30～90s of 700～800 ℃; Formation has the expanded graphite of microvoid structure, and is subsequent use;
Step 4, the swollen purulence graphite of step 2 preparation is put into the erythritol melt of step 1 preparation, in 125～135 ℃ oil bath, stir l～1.5 hour after, obtain product behind the naturally cooling.
The expansible black lead that uses among the present invention is a kind of loose porous vermiform material that is obtained through graphite intercalation, washing and drying, high temperature puffing by natural flake graphite; After the processing of high temperature expansionization; The original plane layer of graphite obviously splits and produces nonaffine deformation, forms netted pass expansion of structure graphite.With the erythritol is that phase change material, expanded graphite are supporting structure; Utilize the porous characterization of adsorption of expanded graphite and the high latent heat of phase change of erythritol; Prepared the typing phase change material of the high latent heat of phase change value of the present invention, the phase change material of this method preparation has higher latent heat of phase change value than the typing phase change material of prior art for preparing.
Beneficial effect: the present invention compared with prior art has the following advantages:
1, the present invention adopts expansible black lead and erythritol to process, and is with low cost, nontoxic non-corrosiveness;
2, the present invention utilizes the high latent heat of phase change value of the porous characterization of adsorption and the erythritol of expanded graphite; The liquid that this phase change material is produced when solid-liquid transforms is difficult for leaking; Realize regularization simultaneously; Because erythritol belongs to high latent heat phase change material, be heat storage phase-changing material with the erythritol, being the phase change material that makes like this of body material with the expanded graphite has higher latent heat of phase change value than the phase change material of prior art for preparing.
Embodiment
A kind of high heat of phase transformation typing phase change material is that the expansible black lead of 100-500 mL/g is processed with the erythritol that is adsorbed in the expansible black lead space by expansion multiplying power, and wherein, the weight of expansible black lead accounts for the 10-20% of gross weight, and all the other are erythritol;
A kind of high heat of phase transformation typing phase change material, its preparation method may further comprise the steps:
Step 1, raw-material choosing
Take by weighing the expansible black lead that erythritol and expansion multiplying power are 100-500 mL/g respectively, and the weight of erythritol accounts for the 80-90% of erythritol and expansible black lead particle gross weight;
Step 2, the erythritol that step 1 is taken by weighing are placed in the beaker, in 125～135 ℃ oil bath, heat, and it is subsequent use to form melt;
Step 3, the expansion multiplying power that step 1 is taken by weighing are that the expansible black lead of 100-500 mL/g is put into vacuum drying oven; Temperature be 65～75 ℃, vacuum tightness for the condition of-0.09MPa under dry 8～12 hours; Taking out then and placing temperature is retort furnace roasting 30～90s of 700～800 ℃; Formation has the expanded graphite of microvoid structure, and is subsequent use;
Step 4, the swollen purulence graphite of step 2 preparation is put into the erythritol melt of step 1 preparation, in 125～135 ℃ oil bath, stir l～1.5 hour after, obtain product behind the naturally cooling.
EXAMPLE l:
At first, take by weighing the 45g erythritol and be placed in the beaker, in 130 ℃ oil bath, be heated to complete melted state, form melt;
Secondly; Taking by weighing the 5g expansion multiplying power is the expansible black lead particle of 200 mL/g; Put into vacuum drying oven, temperature be 70 ℃, vacuum tightness for the condition of-0.09MPa under after dry 10 hours, taking out and placing temperature is 750 ℃ retort furnace thermal treatment 60s; Make the expansible black lead grain expansion, prepare expanded graphite with microvoid structure;
At last, above-mentioned swollen purulence graphite is put into the erythritol melt, in 130 ℃ oil bath, stir, adsorb after 1 hour, obtain product behind the naturally cooling.
Experiment shows has the heat setting type phase change material latent heat of phase change value of this kind proportioning preparation can reach 308.2J/g, is that peak 238.0 J/g of Chinese patent CN102492397 exceed about 29.5% than Comparative Examples.
Embodiment 2:
At first, take by weighing the 28g erythritol and be placed in the beaker, in 135 ℃ oil bath, be heated to complete melted state, form melt;
Secondly; Taking by weighing the 5g expansion multiplying power is the expansible black lead particle of 500 mL/g; Put into vacuum drying oven, temperature be 70 ℃, vacuum tightness for the condition of-0.09MPa under after dry 12 hours, taking out and placing temperature is 800 ℃ retort furnace thermal treatment 80s; Make the expansible black lead grain expansion, prepare expanded graphite with microvoid structure;
At last, above-mentioned swollen purulence graphite is put into the erythritol melt, in 135 ℃ oil bath, stir, adsorb after 1.5 hours, obtain product behind the naturally cooling.
Experiment shows has the heat setting type phase change material latent heat of phase change value of this kind proportioning preparation can reach 289.0J/g, is that peak 238.0 J/g of Chinese patent CN102492397 exceed about 21.4% than Comparative Examples.
Embodiment 3:
At first, take by weighing the 20g erythritol and be placed in the beaker, in 125 ℃ oil bath, be heated to complete melted state, form melt;
Secondly; Taking by weighing the 5g expansion multiplying power is the expansible black lead particle of 100 mL/g; Put into vacuum drying oven, temperature be 70 ℃, vacuum tightness for the condition of-0.09MPa under after dry 8 hours, taking out and placing temperature is 700 ℃ retort furnace thermal treatment 50s; Make the expansible black lead grain expansion, prepare expanded graphite with microvoid structure;
At last, above-mentioned swollen purulence graphite is put into the erythritol melt, in 125 ℃ oil bath, stir, adsorb after 1.5 hours, obtain product behind the naturally cooling.
Experiment shows has the heat setting type phase change material latent heat of phase change value of this kind proportioning preparation can reach 271.1J/g, is that peak 238.0 J/g of Chinese patent CN102492397 exceed about 13.9% than Comparative Examples.
Embodiment 4
At first, take by weighing the 20g erythritol and be placed in the beaker, in 125 ℃ oil bath, be heated to complete melted state, form melt;
Secondly; Taking by weighing the 5g expansion multiplying power is the expansible black lead particle of 300 mL/g; Put into vacuum drying oven, temperature be 75 ℃, vacuum tightness for the condition of-0.09MPa under after dry 10 hours, taking out and placing temperature is 800 ℃ retort furnace thermal treatment 30s; Make the expansible black lead grain expansion, prepare expanded graphite with microvoid structure;
At last, above-mentioned swollen purulence graphite is put into the erythritol melt, in 125 ℃ oil bath, stir, adsorb after 0.5 hour, obtain product behind the naturally cooling.
Embodiment 5
At first, take by weighing the 45g erythritol and be placed in the beaker, in 130 ℃ oil bath, be heated to complete melted state, form melt;
Secondly; Taking by weighing the 5g expansion multiplying power is the expansible black lead particle of 500 mL/g; Put into vacuum drying oven, temperature be 65 ℃, vacuum tightness for the condition of-0.09MPa under after dry 12 hours, taking out and placing temperature is 700 ℃ retort furnace thermal treatment 90s; Make the expansible black lead grain expansion, prepare expanded graphite with microvoid structure;
At last, above-mentioned swollen purulence graphite is put into the erythritol melt, in 125 ℃ oil bath, stir, adsorb after 1.5 hours, obtain product behind the naturally cooling.
The present invention is simple in structure, and is with low cost, nontoxic non-corrosiveness; Utilize expanded graphite porous characterization of adsorption and the high latent heat of phase change value of erythritol; The liquid that this phase change material is produced when solid-liquid transforms is difficult for leaking, and realizes regularization simultaneously, and erythritol belongs to high latent heat phase change material; With the erythritol is heat storage phase-changing material, and being the phase change material that makes like this of body material with the expanded graphite has higher latent heat of phase change value than the phase change material of prior art for preparing.
Claims (2)
1. one kind high heat of phase transformation typing phase change material; It is characterized in that: the expansible black lead that by expansion multiplying power is 100-500 mL/g is processed with the erythritol that is adsorbed in the expansible black lead space; Wherein, the weight of expansible black lead accounts for the 10-20% of gross weight, and all the other are erythritol.
2. a kind of high heat of phase transformation typing phase change material as claimed in claim 1 is characterized in that this preparation methods may further comprise the steps:
Step 1, raw-material choosing
Take by weighing the expansible black lead that erythritol and expansion multiplying power are 100-500 mL/g respectively, and the weight of erythritol accounts for the 80-90% of erythritol and expansible black lead particle gross weight;
Step 2, the erythritol that step 1 is taken by weighing are placed in the beaker, in 125～135 ℃ oil bath, heat, and it is subsequent use to form melt;
Step 3, the expansion multiplying power that step 1 is taken by weighing are that the expansible black lead of 100-500 mL/g is put into vacuum drying oven; Being 65～75 ℃, vacuum tightness in temperature is under the condition of-0.09 MPa dry 8～12 hours; Taking out then and placing temperature is retort furnace roasting 30～90s of 700～800 ℃; Formation has the expanded graphite of microvoid structure, and is subsequent use;
Step 4, the swollen purulence graphite of step 2 preparation is put into the erythritol melt of step 1 preparation, in 125～135 ℃ oil bath, stir l～1.5 hour after, obtain product behind the naturally cooling.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104001458A (en) * | 2014-06-16 | 2014-08-27 | 深圳市优能橡塑制品股份有限公司 | Phase-change thermoregulation microcapsule and preparing method thereof |
| CN104774594A (en) * | 2015-04-10 | 2015-07-15 | 哈尔滨工业大学 | Preparation method of phase-change composite material with high heat conductivity and high density |
| CN104830281A (en) * | 2015-05-07 | 2015-08-12 | 长沙理工大学 | Intermediate-temperature composite shape-stabilized phase-change heat storage material and preparation method thereof |
| CN104830280A (en) * | 2015-05-07 | 2015-08-12 | 长沙理工大学 | Shape-stabilized phase change material for passive thermal protection and preparation method thereof |
| CN105331334A (en) * | 2015-10-19 | 2016-02-17 | 哈尔滨工业大学 | Preparation method of short carbon fiber/meso-erythritol phase change composite material |
| CN103289655B (en) * | 2013-07-03 | 2016-03-02 | 西北大学 | Expanded graphite composite heat storage material and its preparation method and application |
| CN107603571A (en) * | 2017-09-26 | 2018-01-19 | 华北电力大学 | Shape the preparation of expanded graphite-based antierythrite medium temperature composite phase-change heat-storage material |
| CN108084973A (en) * | 2018-02-05 | 2018-05-29 | 天津天爱环保技术开发有限公司 | A kind of heat accumulation phase change composite material, preparation method and applications |
| CN110157384A (en) * | 2019-04-30 | 2019-08-23 | 国电南瑞科技股份有限公司 | A kind of anti-oxidant composite phase-change heat-storage material of high thermal conductivity and preparation method thereof |
| CN110484216A (en) * | 2019-08-26 | 2019-11-22 | 张立强 | Graphite adsorbs phase-change accumulation energy powder, preparation method and applications |
| CN111040737A (en) * | 2019-12-16 | 2020-04-21 | 中国科学院青海盐湖研究所 | Shaped phase-change energy storage material and preparation method thereof |
| CN113801639A (en) * | 2021-09-13 | 2021-12-17 | 华南理工大学 | Phase-change energy storage material and preparation method thereof |
| CN114686179A (en) * | 2021-12-27 | 2022-07-01 | 江苏金合能源科技有限公司 | Semi-shaped composite organic phase change material and preparation method thereof |
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Cited By (15)
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| CN103289655B (en) * | 2013-07-03 | 2016-03-02 | 西北大学 | Expanded graphite composite heat storage material and its preparation method and application |
| CN104001458B (en) * | 2014-06-16 | 2016-05-25 | 傅伟 | A kind of Microencapsulated Phase Change Materials and preparation method thereof |
| CN104001458A (en) * | 2014-06-16 | 2014-08-27 | 深圳市优能橡塑制品股份有限公司 | Phase-change thermoregulation microcapsule and preparing method thereof |
| CN104774594A (en) * | 2015-04-10 | 2015-07-15 | 哈尔滨工业大学 | Preparation method of phase-change composite material with high heat conductivity and high density |
| CN104830280A (en) * | 2015-05-07 | 2015-08-12 | 长沙理工大学 | Shape-stabilized phase change material for passive thermal protection and preparation method thereof |
| CN104830281A (en) * | 2015-05-07 | 2015-08-12 | 长沙理工大学 | Intermediate-temperature composite shape-stabilized phase-change heat storage material and preparation method thereof |
| CN104830281B (en) * | 2015-05-07 | 2017-12-05 | 长沙理工大学 | Intermediate-temperature composite shape-stabilized phase-change heat storage material and preparation method thereof |
| CN105331334A (en) * | 2015-10-19 | 2016-02-17 | 哈尔滨工业大学 | Preparation method of short carbon fiber/meso-erythritol phase change composite material |
| CN107603571A (en) * | 2017-09-26 | 2018-01-19 | 华北电力大学 | Shape the preparation of expanded graphite-based antierythrite medium temperature composite phase-change heat-storage material |
| CN108084973A (en) * | 2018-02-05 | 2018-05-29 | 天津天爱环保技术开发有限公司 | A kind of heat accumulation phase change composite material, preparation method and applications |
| CN110157384A (en) * | 2019-04-30 | 2019-08-23 | 国电南瑞科技股份有限公司 | A kind of anti-oxidant composite phase-change heat-storage material of high thermal conductivity and preparation method thereof |
| CN110484216A (en) * | 2019-08-26 | 2019-11-22 | 张立强 | Graphite adsorbs phase-change accumulation energy powder, preparation method and applications |
| CN111040737A (en) * | 2019-12-16 | 2020-04-21 | 中国科学院青海盐湖研究所 | Shaped phase-change energy storage material and preparation method thereof |
| CN113801639A (en) * | 2021-09-13 | 2021-12-17 | 华南理工大学 | Phase-change energy storage material and preparation method thereof |
| CN114686179A (en) * | 2021-12-27 | 2022-07-01 | 江苏金合能源科技有限公司 | Semi-shaped composite organic phase change material and preparation method thereof |
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Application publication date: 20121219 |