CN109266311A - A kind of preparation method of clay-based composite energy-storage material - Google Patents
A kind of preparation method of clay-based composite energy-storage material Download PDFInfo
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- CN109266311A CN109266311A CN201811054042.8A CN201811054042A CN109266311A CN 109266311 A CN109266311 A CN 109266311A CN 201811054042 A CN201811054042 A CN 201811054042A CN 109266311 A CN109266311 A CN 109266311A
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Abstract
The invention discloses a kind of preparation methods of clay-based composite energy-storage material, the specific steps are prepare vegetable-fibre slurry and clay slurry respectively, then the two is mixed in a certain ratio, and a certain amount of water is further added and adjusts mixed slurry concentration, freezed after mixing evenly.Vacuum freeze drying is carried out again obtains corresponding recessed soil/plant fiber composite aerogel.Phase-change material is injected into aeroge hole by vacuum impregnation technology, both a kind of recessed soil matrix composite energy-storage material.Gained phase-change material loading of the invention is reused up to 3000% or so of aeroge sole mass without obvious leakage phenomenon.
Description
Technical field
The invention belongs to clay field of deep, are related to the preparation method of clay-based gel, and in particular to a kind of clay-based
The preparation method of composite energy-storage material.
Background technique
Phase-change material (phase change material, PCM), which refers to, issues anger in fixed temperature (phase transition temperature)
The material of phase, liquid phase or solid phase variation, same time store heat or release thermal energy along with thermal energy is absorbed to release heat
Amount, so as to adjust and control the temperature of operation source or the environment temperature of material peripheral.Though inorganic phase-changing material phase transformation is latent
It is hot big, but its crystallization water is volatile, and heat accumulation is poorly reversible, there is supercooling and separates with serious phase.Organic phase change material performance is steady
Fixed, good reversibility, phase transition temperature is suitable for latent heat of phase change height, and nontoxic non-corrosive, but thermal coefficient is small, density is smaller,
Inflammable in the presence of high temperature or strong oxidizer, decomposition, security performance are poor.Organic-inorganic composite phase-change material can not only solve
Its leakage and etching problem in use process can also improve the disadvantage of single phase transformation material thermal conductivity difference to a certain extent.
Eastern (CN1303182C) of Tongji University is using light porous haydite as matrix, internal adsorption storage phase-change material, outside cladding
Polymer matrix composite film, material heat exchange efficiency obtained is high, and stability is good；Beijing Yu Tian phase-change accumulation energy Science and Technology Ltd.
Du rabbit put down (CN105950120A) using expanded graphite as be formed carrier storage phase-change material, solve degree of supercooling with mutually separate
The problem of.There is leakage phenomenon when undergoing phase transition in the above phase-change material, seriously affect energy-storage property.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of preparation methods of clay-based energy storage material, by with gas
Gel increases uptake as phase-change material carrier, to effectively inhibit leakage phenomenon of the phase-change material when undergoing phase transition.
The present invention is achieved by the following technical solutions:
A kind of preparation method of clay-based composite energy-storage material, includes the following steps:
It is configured to vegetable-fibre slurry and clay slurry Step 1: plant fiber and clay are respectively placed in deionized water,
Step 2: vegetable-fibre slurry and clay slurry in proportion are mixed and added into carboxymethylcellulose sodium solution, stir evenly
Low-temperature quick-freezing obtains solid afterwards；
Step 3: step 2 obtained solid frozen dried is obtained clay/plant fiber composite aerogel；
Step 4: aeroge obtained by step 3 is placed in a vacuum drying oven together with phase-change material, it is being higher than phase-change material
Vacuum impregnation 1h or more takes out cooling under conditions of 15 DEG C -30 DEG C of phase transition temperature, obtains clay-based composite energy-storage material.
Further improvement of the present invention scheme are as follows:
Vegetable-fibre slurry concentration described in step 1 is 1wt% ~ 2wt%, and recessed soil slurry concentration is 2wt% ~ 5wt%, and carboxymethyl is fine
Tieing up plain sodium solution concentration is 2wt%.
Vegetable-fibre slurry described in step 2, clay slurry mass ratio be 1:1 ~ 5, carboxymethylcellulose sodium solution
Additional amount is the 2% ~ 8% of clay stock quality.
Quick freezing temperature described in step 2 is -18 DEG C ~ -80 DEG C.
Freeze-drying is that for 24 hours ~ 72h is dried in vacuo at -20 DEG C ~ -70 DEG C described in step 3.
Vacuum-impregnated vacuum degree described in step 4 is 10 ~ 60kPa
Further improvement project of the invention are as follows:
Plant fiber described in step 1 is wood fibre, bamboo fiber or grass fiber.
Clay described in step 1 is bentonite or recessed soil.
Phase-change material described in step 4 is one of paraffin wax, atoleine, palmitinic acid, lauric acid, stearic acid
Or two or more mixing.
The invention has the benefit that
The present invention is auxiliary material by main material, plant fiber of fibrous type clay mine, common to construct pore structure airsetting glue frame abundant
Frame structure；Clay is good with plant fiber compatibility and is natural monodimension nanometer material, the compound good machine of imparting aeroge of the two
Tool performance and abundant pore structure, carrying phase-change accumulation energy substance is more, and composite material is compared former phase-change material latent heat of phase change and obtained
It improves, i.e., energy-storage property significantly improves.
Gained phase-change material loading of the invention is up to 3000% or so of aeroge sole mass, present invention gained phase transformation
Material does not have drop after reaching phase-change material phase transition temperature, and being maintained at standing in phase transition temperature is not in that apparent sinking is existing
As showing to reuse without obvious leakage phenomenon also without obvious leakage phenomenon without layering after air-setting.The present invention prepares work
Skill is simple, raw materials used cheap and green non-poisonous.
Detailed description of the invention
Fig. 1 is the SEM electron microscope of clay-based composite energy-storage material made from embodiment 1.
Specific embodiment
Embodiment 1
It taking 1g Original Pulp (fibre diameter 0.5mm ~ 3mm), 99g deionized water is added, impregnate 30min, refiner is homogenized 10 times,
Each 3min obtains the vegetable-fibre slurry of 1wt%；The recessed soil of 5g is taken, 95g deionized water, beater 10000rpm mashing is added
The recessed soil paste material of 5wt% is made in 30min；The recessed soil paste material of 4g, 5wt% are taken, 4g, 1wt% vegetable-fibre slurry are added thereto,
0.2g, 2wt% carboxymethylcellulose sodium solution, high speed, which is beaten, to be uniformly mixed；The sample mixed is poured into mold at -80 DEG C
Lower progress is quick-frozen；The sample freezed is subjected to frozen dried, freeze-drying is that vacuum drying 72h is carried out at -20 DEG C, is obtained recessed
Soil/plant fiber gas composite aerogel.Aerogel material is immersed in the paraffin wax being stored at 80 DEG C, 60kPa is placed into
2h under vacuum environment takes out cooling, finally obtains clay-based composite energy-storage material.Gained sample phase-change material adsorbance is carrier
The 2951.6% of quality, phase transition temperature are 53 DEG C, and latent heat of phase change 151.5J/g, more single wax phase change latent heat improves
24.2%, and without obvious leakage phenomenon.
Embodiment 2
It taking 2g Original Pulp (fibre diameter 0.5mm ~ 3mm), 98g deionized water is added, impregnate 30min, refiner is homogenized 10 times,
Each 3min obtains the vegetable-fibre slurry of 2wt%；The recessed soil of 5g is taken, 95g deionized water, beater 10000rpm mashing is added
The recessed soil paste material of 5wt% is made in 30min；Take the recessed soil paste material of 4g, 5wt%, thereto be added 8g, 2wt% vegetable-fibre slurry and
0.08g, 2wt% carboxymethylcellulose sodium solution, high speed, which is beaten, to be uniformly mixed；The sample mixed is poured into mold at -80 DEG C
Lower progress is quick-frozen；The sample freezed is subjected to frozen dried, freeze-drying is that vacuum drying 45h is carried out at -40 DEG C, is obtained recessed
Soil/plant fiber gas composite aerogel.Aerogel material is immersed and is stored in the lauric acid mixed at 80 DEG C and tristearin
In acid solution, it is placed into 2h under vacuum environment, cooling is taken out, finally obtains clay-based composite energy-storage material.Gained sample phase transformation
Adsorption capacities of materials is the 3101.9% of carrier quality, and phase transition temperature is 53.3 DEG C, latent heat of phase change 142.5J/g, compared with without compound
Phase-change material improve 16.8%, and ne-leakage phenomenon.
Embodiment 3
It taking 2g Original Pulp (fibre diameter 0.5mm ~ 3mm), 98g deionized water is added, impregnate 30min, refiner is homogenized 10 times,
Each 3min obtains the vegetable-fibre slurry of 2wt%；5g bentonite is taken, 95g deionized water, beater 10000rpm mashing is added
The bentonite slurry of 5wt% is made in 30min；The bentonite slurry of 4g, 5wt% are taken, 2.5g, 2wt% plant fiber are added thereto
Slurry, 0.24g, 2wt% carboxymethylcellulose sodium solution, high speed, which is beaten, to be uniformly mixed；The sample mixed is poured into mold
It is carried out at -30 DEG C quick-frozen；The sample freezed is subjected to frozen dried, freeze-drying is to be dried in vacuo at -70 DEG C for 24 hours,
Obtain bentonite/plant fiber gas composite aerogel.Aerogel material is immersed in the paraffin wax being stored at 80 DEG C, juxtaposition
Enter 2h under vacuum environment, takes out cooling, finally obtain clay-based composite energy-storage material.Gained sample phase-change material adsorbance is to carry
The 3411.6% of weight, phase transition temperature are 53 DEG C, latent heat of phase change 134.1J/g, and more single paraffin improves 9.9%, without obvious
Leakage.
Embodiment 4
It taking 2g bamboo fiber (fibre diameter 0.5mm ~ 3mm), 98g deionized water is added, impregnate 30min, refiner is homogenized 10 times,
Each 3min obtains the vegetable-fibre slurry of 2wt%；5g bentonite is taken, 98g deionized water, beater 10000rpm mashing is added
The bentonite slurry of 2wt% is made in 30min；The bentonite slurry of 2g, 5wt% are taken, 10g, 2wt% plant fiber pulp are added thereto
Material, 0.16g, 2wt% carboxymethylcellulose sodium solution, high speed, which is beaten, to be uniformly mixed；By the sample mixed pour into mold-
It is carried out at 30 DEG C quick-frozen；The sample freezed is subjected to frozen dried, freeze-drying is to be dried in vacuo at -70 DEG C for 24 hours, is obtained
Bentonite/plant fiber gas composite aerogel.Aerogel material is immersed in the palmitinic acid being stored at 75 DEG C, vacuum is placed into
2h under environment takes out cooling, finally obtains clay-based composite energy-storage material.Gained sample phase-change material adsorbance is carrier quality
2781%, phase transition temperature is 64.5 DEG C, latent heat of phase change 141.7J/g, and more single palmitinic acid improves 13%, without obvious leakage.
Claims (9)
1. a kind of preparation method of clay-based composite energy-storage material, which comprises the steps of:
It is configured to vegetable-fibre slurry and clay slurry Step 1: plant fiber and clay are respectively placed in deionized water,
Step 2: vegetable-fibre slurry and clay slurry in proportion are mixed and added into carboxymethylcellulose sodium solution, stir evenly
Low-temperature quick-freezing obtains solid afterwards；
Step 3: step 2 obtained solid frozen dried is obtained clay/plant fiber composite aerogel；
Step 4: aeroge obtained by step 3 is placed in a vacuum drying oven together with phase-change material, it is being higher than phase-change material
Vacuum impregnation 1h or more takes out cooling under conditions of 15 DEG C ~ 30 DEG C of phase transition temperature, obtains clay-based composite energy-storage material.
2. a kind of preparation method of clay-based composite energy-storage material according to claim 1, it is characterised in that: in step 1
The vegetable-fibre slurry concentration is 1wt% ~ 2wt%, and clay slurry concentration is 2wt% ~ 5wt%, and carboxymethylcellulose sodium solution is dense
Degree is 2wt%.
3. a kind of preparation method of clay-based composite energy-storage material according to claim 1, feature exist: institute in step 2
State vegetable-fibre slurry, clay slurry mass ratio be 1:1 ~ 5, carboxymethylcellulose sodium solution additional amount be clay slurry matter
The 2% ~ 8% of amount.
4. a kind of preparation method of clay-based composite energy-storage material according to claim 1, it is characterised in that: in step 2
The quick freezing temperature is -18 DEG C ~ -80 DEG C.
5. a kind of preparation method of clay-based composite energy-storage material according to claim 1, it is characterised in that: step 3 institute
Stating freeze-drying is that for 24 hours ~ 72h is dried in vacuo at -20 DEG C ~ -70 DEG C.
6. a kind of preparation method of clay-based composite energy-storage material according to claim 1, it is characterised in that: in step 1
The plant fiber is wood fibre, bamboo fiber or grass fiber.
7. a kind of preparation method of clay-based composite energy-storage material according to claim 1, it is characterised in that: in step 1
The clay is bentonite or recessed soil.
8. a kind of preparation method of clay-based composite energy-storage material according to claim 1, it is characterised in that: in step 4
The phase-change material is the mixing of one or more of paraffin wax, atoleine, palmitinic acid, lauric acid, stearic acid.
9. a kind of preparation method of clay-based composite energy-storage material according to claim 1, it is characterised in that: in step 4
The vacuum-impregnated vacuum degree is -40 ~ -100kPa.
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Cited By (3)
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| CN110499145A (en) * | 2019-08-26 | 2019-11-26 | 张立强 | Aeroge adsorbs phase-change accumulation energy powder, preparation method and applications |
| CN112940689A (en) * | 2021-02-05 | 2021-06-11 | 浙江海洋大学 | Composite phase change material for diving suit and preparation method thereof |
| CN113150365A (en) * | 2021-05-27 | 2021-07-23 | 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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| CN112940689A (en) * | 2021-02-05 | 2021-06-11 | 浙江海洋大学 | Composite phase change material for diving suit and preparation method thereof |
| CN113150365A (en) * | 2021-05-27 | 2021-07-23 | 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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