CN109266311B - Preparation method of clay-based composite energy storage material - Google Patents
Preparation method of clay-based composite energy storage material Download PDFInfo
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- CN109266311B CN109266311B CN201811054042.8A CN201811054042A CN109266311B CN 109266311 B CN109266311 B CN 109266311B CN 201811054042 A CN201811054042 A CN 201811054042A CN 109266311 B CN109266311 B CN 109266311B
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
Abstract
The invention discloses a preparation method of a clay-based composite energy storage material, which comprises the specific steps of respectively preparing plant fiber slurry and clay slurry, mixing the plant fiber slurry and the clay slurry according to a certain proportion, further adding a certain amount of water to adjust the concentration of the mixed slurry, and freezing after uniformly stirring. And then carrying out vacuum freeze drying to obtain the corresponding attapulgite/plant fiber composite aerogel. And injecting the phase change material into the pores of the aerogel by a vacuum impregnation method to obtain the attapulgite-based composite energy storage material. The loading amount of the phase-change material obtained by the invention can reach about 3000% of the self mass of the aerogel, and the phase-change material is repeatedly used without obvious leakage phenomenon.
Description
Technical Field
The invention belongs to the field of clay deep processing, relates to a preparation method of clay-based gel, and particularly relates to a preparation method of a clay-based composite energy storage material.
Background
A Phase Change Material (PCM) is a material that changes a gas phase, a liquid phase, or a solid phase at a fixed temperature (phase change temperature), and can adjust and control the temperature of a working source or the ambient temperature around the material by storing heat or releasing heat with the absorption of heat energy at the same time. Although the inorganic phase-change material has large phase-change latent heat, the crystal water is easy to volatilize, the heat storage reversibility is poor, and supercooling and severe phase separation exist. The organic phase change material has stable performance, good reversibility, proper phase change temperature, high phase change latent heat, no toxicity and no corrosiveness, but has small heat conductivity coefficient, small density, flammability and decomposition in the presence of high temperature or strong oxidant, and poor safety performance. The organic-inorganic composite phase change material can not only solve the problems of leakage and corrosion in the using process, but also improve the defect of poor thermal conductivity of a single phase change material to a certain extent. The Zhangdong (CN 1303182C) of the university of Tongji takes light porous ceramsite as a matrix, phase-change materials are adsorbed and stored inside the matrix, and polymer matrix composite films are coated outside the matrix, so that the prepared material has high heat exchange efficiency and good stability; dulepine (CN 105950120A) of Beijing Yutian phase change energy storage technology Limited stores phase change materials by taking expanded graphite as a shaping carrier, thereby solving the problems of supercooling degree and phase separation. The phase-change materials have leakage phenomenon when phase change occurs, and the energy storage performance is seriously influenced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a clay-based energy storage material, which increases the absorption capacity by taking aerogel as a phase change material carrier, thereby effectively inhibiting the leakage phenomenon of the phase change material during phase change.
The invention is realized by the following technical scheme:
a preparation method of a clay-based composite energy storage material comprises the following steps:
step one, plant fiber and clay are respectively placed in deionized water to prepare plant fiber slurry and clay slurry,
step two, mixing the plant fiber slurry and the clay slurry in proportion, adding a sodium carboxymethyl cellulose solution, uniformly stirring, and quickly freezing at low temperature to obtain a solid;
step three, performing freeze-drying treatment on the solid obtained in the step two to obtain the clay/plant fiber composite aerogel;
and step four, placing the aerogel obtained in the step three and the phase-change material in a vacuum drying oven, and carrying out vacuum impregnation for more than 1h at the phase-change temperature of 15-30 ℃ higher than that of the phase-change material, taking out and cooling to obtain the clay-based composite energy storage material.
The invention further improves the scheme as follows:
in the first step, the concentration of the plant fiber slurry is 1wt% -2 wt%, the concentration of the attapulgite slurry is 2wt% -5 wt%, and the concentration of the sodium carboxymethyl cellulose solution is 2 wt%.
In the second step, the mass ratio of the plant fiber slurry to the clay slurry is 1: 1-5, and the addition amount of the sodium carboxymethyl cellulose solution is 2% -8% of the mass of the clay slurry.
And in the second step, the quick-freezing temperature is minus 18 ℃ to minus 80 ℃.
And step three, the freeze-drying is carried out for 24-72 h under the temperature of minus 20-minus 70 ℃.
Fourthly, the vacuum degree of the vacuum impregnation is 10-60 kPa
The invention further improves the scheme as follows:
in the step one, the plant fiber is wood fiber, bamboo fiber or grass fiber.
In the first step, the clay is bentonite or attapulgite.
In the fourth step, the phase-change material is one or a mixture of more than two of section paraffin, liquid paraffin, palmitic acid, lauric acid and stearic acid.
The invention has the beneficial effects that:
the aerogel framework structure with rich pore structures is constructed by taking fiber clay minerals as main materials and plant fibers as auxiliary materials; the clay and the plant fiber have good affinity and are natural one-dimensional nano materials, the combination of the clay and the plant fiber endows the aerogel with good mechanical property and rich pore structure, the bearing phase-change energy storage substances are more, and the phase-change latent heat of the composite material is improved compared with that of the original phase-change material, namely the energy storage property is obviously improved.
The loading capacity of the phase-change material obtained by the invention can reach about 3000% of the self mass of the aerogel, no liquid drop exists after the phase-change material reaches the phase-change temperature of the phase-change material, no obvious sinking phenomenon can occur when the phase-change material is kept standing at the phase-change temperature, no layering exists after the phase-change material is solidified at normal temperature, no obvious leakage phenomenon is shown, and no obvious leakage phenomenon exists after the phase-change material is repeatedly used. The invention has simple preparation process, and the used raw materials are cheap, green and nontoxic.
Drawings
Fig. 1 is an SEM electron micrograph of the clay-based composite energy storage material prepared in example 1.
Detailed Description
Example 1
Taking 1g of primary wood pulp (the fiber diameter is 0.5 mm-3 mm), adding 99g of deionized water, soaking for 30min, and homogenizing for 3min each time for 10 times by a homogenizer to obtain 1wt% of plant fiber slurry; taking 5g of attapulgite, adding 95g of deionized water, and pulping for 30min at 10000rpm of a pulping machine to obtain 5wt% of attapulgite slurry; 4g of attapulgite slurry with the weight percent of 4g and 5 percent is taken, 4g of plant fiber slurry with the weight percent of 1 percent and 0.2g of sodium carboxymethyl cellulose solution with the weight percent of 2 percent are added into the attapulgite slurry, and the mixture is pulped at a high speed and mixed evenly; pouring the mixed sample into a mould to carry out quick freezing at-80 ℃; and (3) carrying out freeze-drying treatment on the frozen sample, wherein the freeze-drying is carried out for 72h under the temperature of minus 20 ℃ to obtain the attapulgite/plant fiber gas composite aerogel. And (3) immersing the aerogel material into the sliced paraffin preserved at the temperature of 80 ℃, placing the sliced paraffin in a vacuum environment of 60kPa for 2h, taking out the sliced paraffin and cooling the sliced paraffin, and finally obtaining the clay-based composite energy storage material. The adsorption capacity of the phase-change material of the obtained sample is 2951.6% of the mass of the carrier, the phase-change temperature is 53 ℃, the phase-change latent heat is 151.5J/g, the phase-change latent heat is improved by 24.2% compared with that of single paraffin, and no obvious leakage phenomenon exists.
Example 2
Taking 2g of primary wood pulp (the fiber diameter is 0.5 mm-3 mm), adding 98g of deionized water, soaking for 30min, and homogenizing for 3min each time for 10 times by a homogenizer to obtain 2wt% of plant fiber slurry; taking 5g of attapulgite, adding 95g of deionized water, and pulping for 30min at 10000rpm of a pulping machine to obtain 5wt% of attapulgite slurry; taking 4g and 5wt% of attapulgite slurry, adding 8g and 2wt% of plant fiber slurry and 0.08g and 2wt% of sodium carboxymethyl cellulose solution, pulping at high speed and mixing uniformly; pouring the mixed sample into a mould to carry out quick freezing at-80 ℃; and (3) carrying out freeze-drying treatment on the frozen sample, wherein the freeze-drying is carried out for 45 hours at the temperature of minus 40 ℃ to obtain the attapulgite/plant fiber gas composite aerogel. And (3) immersing the aerogel material into a mixed lauric acid and stearic acid solution stored at 80 ℃, placing the aerogel material in a vacuum environment for 2h, taking out the aerogel material and cooling to finally obtain the clay-based composite energy storage material. The adsorption capacity of the obtained sample phase-change material is 3101.9% of the mass of the carrier, the phase-change temperature is 53.3 ℃, the latent heat of phase change is 142.5J/g, the adsorption capacity is improved by 16.8% compared with that of the non-compounded phase-change material, and the leakage phenomenon is avoided.
Example 3
Taking 2g of primary wood pulp (the fiber diameter is 0.5 mm-3 mm), adding 98g of deionized water, soaking for 30min, and homogenizing for 3min each time for 10 times by a homogenizer to obtain 2wt% of plant fiber slurry; taking 5g of bentonite, adding 95g of deionized water, and pulping for 30min at 10000rpm of a pulping machine to prepare bentonite slurry with the concentration of 5 wt%; taking 4g and 5wt% of bentonite slurry, adding 2.5g and 2wt% of plant fiber slurry, 0.24g and 2wt% of sodium carboxymethyl cellulose solution, pulping at high speed and mixing uniformly; pouring the mixed sample into a mould to carry out quick freezing at-30 ℃; and (3) carrying out freeze-drying treatment on the frozen sample, wherein the freeze-drying is carried out for 24 hours at the temperature of-70 ℃ to obtain the bentonite/plant fiber gas composite aerogel. And (3) immersing the aerogel material into the sliced paraffin preserved at the temperature of 80 ℃, placing the sliced paraffin in a vacuum environment for 2 hours, taking out the sliced paraffin and cooling the sliced paraffin, and finally obtaining the clay-based composite energy storage material. The adsorption capacity of the phase-change material of the obtained sample is 3411.6% of the mass of the carrier, the phase-change temperature is 53 ℃, the phase-change latent heat is 134.1J/g, the phase-change latent heat is improved by 9.9% compared with single paraffin, and no obvious leakage exists.
Example 4
Taking 2g of bamboo fibers (the fiber diameter is 0.5 mm-3 mm), adding 98g of deionized water, soaking for 30min, homogenizing for 3min each time for 10 times to obtain 2wt% of plant fiber slurry; taking 5g of bentonite, adding 98g of deionized water, and pulping for 30min at 10000rpm of a pulping machine to prepare 2wt% of bentonite slurry; taking 2g and 5wt% of bentonite slurry, adding 10g and 2wt% of plant fiber slurry and 0.16g and 2wt% of sodium carboxymethyl cellulose solution, pulping at high speed and mixing uniformly; pouring the mixed sample into a mould to carry out quick freezing at-30 ℃; and (3) carrying out freeze-drying treatment on the frozen sample, wherein the freeze-drying is carried out for 24 hours at the temperature of-70 ℃ to obtain the bentonite/plant fiber gas composite aerogel. And (3) immersing the aerogel material into palmitic acid stored at the temperature of 75 ℃, placing the aerogel material in a vacuum environment for 2 hours, taking out the aerogel material and cooling to finally obtain the clay-based composite energy storage material. The adsorption capacity of the phase-change material of the obtained sample is 2781% of the mass of the carrier, the phase-change temperature is 64.5 ℃, the phase-change latent heat is 141.7J/g, the phase-change latent heat is improved by 13% compared with single palmitic acid, and no obvious leakage exists.
Claims (5)
1. The preparation method of the clay-based composite energy storage material is characterized by comprising the following steps:
step one, plant fiber and clay are respectively placed in deionized water to prepare plant fiber slurry and clay slurry,
step two, mixing the plant fiber slurry and the clay slurry in proportion, adding a sodium carboxymethyl cellulose solution, uniformly stirring, and quickly freezing at low temperature to obtain a solid;
step three, performing freeze-drying treatment on the solid obtained in the step two to obtain the clay/plant fiber composite aerogel;
step four, placing the aerogel obtained in the step three and the phase-change material in a vacuum drying oven, and carrying out vacuum impregnation for more than 1h at the phase-change temperature of the phase-change material of 15-30 ℃, taking out and cooling to obtain the clay-based composite energy storage material;
in the first step, the plant fiber is wood fiber, bamboo fiber or grass fiber; in the first step, the clay is bentonite or attapulgite; in the first step, the concentration of the plant fiber slurry is 1-2 wt%, and the concentration of the clay slurry is 2-5 wt%; in the second step, the mass ratio of the plant fiber slurry to the clay slurry is 1: 1-5, the addition amount of the sodium carboxymethyl cellulose solution is 2% -8% of the mass of the clay slurry, and the concentration of the sodium carboxymethyl cellulose solution is 2 wt%.
2. The method for preparing the clay-based composite energy storage material according to claim 1, wherein the method comprises the following steps: and in the second step, the quick-freezing temperature is minus 18 ℃ to minus 80 ℃.
3. The method for preparing the clay-based composite energy storage material according to claim 1, wherein the method comprises the following steps: and step three, the freeze-drying is carried out for 24-72 h under the temperature of minus 20-minus 70 ℃.
4. The method for preparing the clay-based composite energy storage material according to claim 1, wherein the method comprises the following steps: in the fourth step, the phase-change material is one or a mixture of more than two of section paraffin, liquid paraffin, palmitic acid, lauric acid and stearic acid.
5. The method for preparing the clay-based composite energy storage material according to claim 1, wherein the method comprises the following steps: the vacuum degree of the vacuum impregnation in the fourth step is-40 to-100 kPa.
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| CN112940689B (en) * | 2021-02-05 | 2022-10-04 | 浙江海洋大学 | Composite phase change material for diving suit and preparation method thereof |
| CN113150365B (en) * | 2021-05-27 | 2023-01-13 | 淮阴工学院 | Preparation of melamine aerogel and fiber type clay reinforced melamine composite aerogel by normal pressure drying method |
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| CN105315482A (en) * | 2015-12-02 | 2016-02-10 | 南京林业大学 | Anisotropic nano-cellulose/montmorillonite composite aerogel and preparation method thereof |
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| CN105315482A (en) * | 2015-12-02 | 2016-02-10 | 南京林业大学 | Anisotropic nano-cellulose/montmorillonite composite aerogel and preparation method thereof |
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