CN110819311A - Method for preparing hydrated salt/paraffin/cellulose sponge composite phase change material by inverse emulsion method - Google Patents
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- C09K5/02—Materials undergoing a change of physical state when used
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- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
Abstract
The invention relates to a method for preparing a hydrated salt/paraffin/cellulose sponge composite phase-change material by an inverse emulsion method. The method comprises the following steps: preparing a reverse emulsion of the paraffin-coated hydrated salt, preparing oleophilic cellulose sponge, and preparing a hydrated salt/paraffin/cellulose sponge composite phase-change material. The method can reduce supercooling degree of the hydrated salt and improve thermal stability of the hydrated salt.
Description
Technical Field
The invention belongs to the field of phase-change material preparation methods, and particularly relates to a method for preparing a hydrous salt/paraffin/cellulose sponge composite phase-change material by using an inverse emulsion method.
Background
The phase change material refers to a substance that changes a phase state of a substance according to a change in temperature and releases and absorbs heat during a phase transition process to provide latent heat, and is classified into an organic phase change material and an inorganic phase change material. Compared with organic phase change materials, inorganic hydrated salt phase change materials have a series of advantages of high enthalpy value, high heat storage density, high heat conductivity, incombustibility, low price and the like, and are widely applied to the field of heat storage.
The Chinese patent with the application number of 2018112773140 discloses a segmented heat storage composite phase change material and a preparation method thereof. The organic phase-change material is used for emulsifying the hydrated salt phase-change material to obtain the segmented heat storage phase-change material, so that the problem of volatilization of free water generated after the hydrated salt is melted is solved to a certain extent. Although the phase change heat storage material prepared by the technology has excellent phase change performance, the phase change material with the segmented phase change point has uneven heat absorption temperature section, is not beneficial to daily use, and the organic phase change material has overlarge specific gravity and lower content of hydrated salt, and is not beneficial to exerting the excellent heat storage performance of the hydrated salt.
However, hydrated salt phase change materials also have some inherent drawbacks:
1. the hydrous salt phase-change material has a supercooling problem in the process of temperature reduction and crystallization and cannot be crystallized in a required temperature range.
2. The salt hydrate phase-change material reduces the phase change enthalpy value due to the volatilization of moisture after a plurality of heating and cooling cycles.
3. The hydrous salt phase-change material has a problem of leakage after melting.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing a hydrated salt/paraffin/cellulose sponge composite phase-change material by an inverse emulsion method, so as to overcome the defects of low thermal stability of the hydrated salt phase-change material, supercooling in the process of cooling crystallization and the like in the prior art.
The invention provides a method for preparing a hydrated salt/paraffin/cellulose sponge composite phase-change material by an inverse emulsion method, which comprises the following steps:
(1) taking molten hydrated salt as a water phase and molten paraffin as an oil phase, adding an emulsifier, and stirring to obtain paraffin-coated hydrated salt reverse emulsion; wherein the mass ratio of the hydrated salt to the paraffin is 1: 1-4: 1, and the emulsifier accounts for 1-5% of the mass of the hydrated salt;
(2) mixing cellulose with a cross-linking agent and a hydrophobic modifier, stirring, freezing, freeze-drying, and then cross-linking to obtain oleophilic type cellulose sponge, wherein the mass ratio of the cellulose to the hydrophobic modifier is 1: 0.5-1: 6;
(3) and (3) soaking the oleophilic cellulose sponge in the step (2) into the emulsion of the paraffin-coated hydrated salt in the step (1) to obtain the hydrated salt/paraffin/cellulose sponge composite phase-change material.
The melting temperature in the step (1) is 40-70 ℃.
The stirring in the step (1) is mechanical stirring, the stirring speed is 2000-10000 rpm, and the stirring time is 1-5 min.
The hydrated salt in the step (1) comprises sodium sulfate decahydrate, sodium carbonate decahydrate, disodium hydrogen phosphate dodecahydrate, sodium acetate trihydrate, calcium chloride hexahydrate, magnesium chloride hexahydrate or eutectic salt.
The eutectic salt comprises 66.6 wt% of CaCl2·6H2O+33.4wt％MgCl2·6H2O、60wt％ Na2HPO4·12H2O+40wt％Na2SO4·10H2O、75wt％Na2HPO4·12H2O+25wt％Na2CO3·10H2And one or more of O.
The paraffin in the step (1) comprises one or more of hexadecane, octadecane, eicosane and docosane.
The emulsifier in the step (1) comprises one or more of Span20, Tween20, Span60, Tween60, Span80 and Tween 80.
The cellulose in the step (2) comprises one or more of carboxymethyl cellulose, bacterial cellulose, microcrystalline cellulose, cellulose nanocrystal, cellulose micro/nanowire, wood pulp cellulose, straw cellulose and bamboo cellulose.
And (3) the crosslinking agent and the hydrophobic modifier in the step (2) are vinyl silanes, and the vinyl silanes comprise one or more of vinyl triethoxysilane, vinyl trimethoxysilane and vinyl tris (β -methoxyethoxy) silane.
And (3) stirring in the step (2) at the temperature of 20-40 ℃ for 1-3 h.
The freeze-drying temperature in the step (2) is-60 to-30 ℃, and the freeze-drying time is 24 to 48 hours.
And (3) in the step (2), the crosslinking temperature is 90-110 ℃, and the crosslinking time is 20-60 min.
In the step (3), the dipping temperature is 40-70 ℃, and the dipping time is 0.5-2 h.
The invention also provides the hydrated salt/paraffin/cellulose sponge composite phase-change material prepared by the method.
The invention also provides application of the hydrated salt/paraffin/cellulose sponge composite phase change material prepared by the method.
The invention aims to emulsify the hydrated salt by paraffin with similar melting point through an emulsion method, thereby reducing the supercooling degree of the hydrated salt, improving the thermal stability of the hydrated salt, and then filling the hydrated salt into cellulose sponge to obtain the composite phase change material which can keep a solid state above the melting point. The present invention emulsifies the hydrated salt into paraffin by using the advanced crystallization of low undercooling paraffin to provide a confined space for the hydrated salt and using paraffin crystals as nucleating agents to promote the crystallization of the hydrated salt. Meanwhile, paraffin covers the surface of the hydrated salt when melted, so that the paraffin has an oil sealing effect on the hydrated salt, and the volatilization of water in the hydrated salt can be greatly improved, thereby improving the thermal stability of the hydrated salt.
Advantageous effects
(1) In the invention, as the paraffin is an organic phase-change material and also has phase-change enthalpy, the addition of the paraffin does not reduce the integral enthalpy of the integral composite phase-change material.
(2) The advanced crystallization of the paraffin in the invention effectively promotes the crystallization of the hydrated salt and reduces the supercooling degree of the hydrated salt.
(3) The paraffin wax sealing agent plays a role in oil sealing for the hydrated salt when the paraffin wax is melted, and improves the thermal stability of the hydrated salt.
Drawings
FIG. 1 shows DSC curves of an emulsion (HPC) prepared according to example 1 of the present invention and the corresponding pure mixed salt and pure paraffin wax.
FIG. 2 is a scanning electron micrograph of the emulsion (HPC) prepared in example 1 according to the present invention.
FIG. 3 is a TG thermal stability curve for emulsions (HPC) prepared in accordance with example 1 of the present invention, pure hydrated salts, pure paraffin wax and Shape Stable Phase Change Materials (SSPCMs) after adsorption to cellulose sponges.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The raw material cellulose nanowire aqueous solution (solid content of 2.0 wt%) in the examples was provided by trichodiamond biotechnology limited of Tianjin; the organic phase change material paraffin, hydrated salt and emulsifier are all purchased from national medicine group chemical reagents, Inc.
Example 1
(1) Weighing 50g of 2 wt% cellulose nanowire aqueous solution, adjusting the pH value to 4, adding 2g of vinyltrimethoxysilane, and stirring for 3h at normal temperature to obtain uniform cellulose nanowire-silane mixed suspension. Pouring the mixed suspension into a glass watch glass, putting into liquid nitrogen for freezing for 20min, taking out, putting into a freeze dryer for freeze drying at-50 ℃ for 48h, then putting into an oven, and drying and crosslinking at 110 ℃ for 1h to obtain the oleophilic type cellulose sponge.
(2) 20g of disodium hydrogen phosphate dodecahydrate, 10g of eicosane and 1g of Span80 were weighed, heated to 60 ℃ to melt, and stirred at 10000rpm for 5min under high-speed shearing to obtain a uniform emulsion. The sponge prepared in step (1) was dipped into the emulsion and kept in an oven at 60 ℃ for 1 h. And (3) taking out the sponge to obtain the hydrated salt/paraffin/cellulose composite phase-change material with stable shape, wherein the loading rate of the hydrated salt and the paraffin in the composite phase-change material is 92.7%.
FIG. 1 shows that: the pure hydrated salt has very high supercooling degree, the paraffin has almost no supercooling degree, and after the pure hydrated salt and the paraffin are compounded, the supercooling degree of the hydrated salt is greatly reduced due to the action of a nucleating agent of the paraffin. Meanwhile, the endothermic peak after the two are compounded still keeps a single peak.
FIG. 2 shows that: the SEM image of the compounded emulsion can obviously show the appearance of the emulsion drops of the hydrated salt coated by the paraffin.
FIG. 3 shows: the pure hydrated salt has poor thermal stability and starts to decompose from 30 ℃. And after the hydrated salt is emulsified by the paraffin, the stability of the hydrated salt is also improved since the paraffin is very stable, and hardly decomposed until 70 ℃. The emulsion after being adsorbed by the cellulose can also keep good stability before 70 ℃.
Example 2
(1) Oleophilic cellulose sponge was prepared according to example 1 by replacing "vinyltrimethoxysilane" with "vinyltriethoxysilane" in example 1, the remainder being the same as in example 1.
(2) 30g of sodium sulfate decahydrate, 10g of octadecane and 1.5g of Span60 are weighed, heated to 60 ℃ for melting, and stirred for 5min under the condition of high-speed shearing at 5000rpm to obtain uniform emulsion. The sponge prepared in step (1) was dipped into the emulsion and kept in an oven at 60 ℃ for 1 h. And (3) taking out the sponge to obtain the hydrated salt/paraffin/cellulose composite phase-change material with a stable shape, wherein the loading rate of the hydrated salt and the paraffin in the composite phase-change material is 91.5%.
Example 3
(1) Oleophilic cellulose sponge was prepared as in example 1 except that "vinyltrimethoxysilane" in example 1 was changed to "vinyltris (β -methoxyethoxy) silane" in accordance with example 1.
(2) 40g of 60% disodium hydrogen phosphate dodecahydrate + 40% sodium sulfate decahydrate, 10g of docosane and 2g of span60 were weighed, heated to 60 ℃ to melt, and stirred at 10000rpm for 5min under high-speed shearing to obtain a uniform emulsion. The sponge prepared in step (1) was dipped into the emulsion and kept in an oven at 60 ℃ for 1 h. And (3) taking out the sponge to obtain the hydrated salt/paraffin/cellulose composite phase-change material with a stable shape, wherein the loading rate of the hydrated salt and the paraffin in the composite phase-change material is 91.7%.
And (3) performance testing: the melting temperature and enthalpy values are read from DSC curves measured with a differential scanning calorimeter (NETZSCH DSC214, Germany). The temperature at which supercooling is improved is the difference between the crystallization temperature of the hydrated salt emulsified with paraffin and the crystallization temperature of pure hydrated salt. The decomposition temperature was read from the thermogravimetric curve of a thermogravimetric analyzer (TGA, NETZSCH 209F3, Germany).
The performance data for examples 1-3 are shown in Table 1.
TABLE 1 thermal Performance data for the examples
| Melting temperature (. degree.C.) | Melting enthalpy (J/g) | Supercooling improvement (. degree.C.) | Onset decomposition temperature (. degree. C.) | |
| Example 1 | 36.7 | 227.3 | 14.6 | 71.7 |
| Example 2 | 26.5 | 216.9 | 13.3 | 72.1 |
| Example 3 | 27.1 | 215.5 | 13.8 | 71.9 |
Claims (10)
1. A method for preparing a hydrated salt/paraffin/cellulose sponge composite phase-change material by an inverse emulsion method comprises the following steps:
(1) taking molten hydrated salt as a water phase and molten paraffin as an oil phase, adding an emulsifier, and stirring to obtain paraffin-coated hydrated salt reverse emulsion; wherein the mass ratio of the hydrated salt to the paraffin is 1: 1-4: 1, and the emulsifier accounts for 1-5% of the mass of the hydrated salt;
(2) mixing cellulose with a cross-linking agent and a hydrophobic modifier, stirring, freezing, freeze-drying, and then cross-linking to obtain oleophilic type cellulose sponge, wherein the mass ratio of the cellulose to the cross-linking agent to the hydrophobic modifier is 1: 0.5-1: 6;
(3) and (3) soaking the oleophilic cellulose sponge in the step (2) into the reverse emulsion of the paraffin-coated hydrated salt in the step (1) to obtain the hydrated salt/paraffin/cellulose sponge composite phase-change material.
2. The method according to claim 1, wherein the melting temperature in the step (1) is 40-70 ℃; the stirring time is 1-5 min.
3. The method of claim 1, wherein the hydrated salt in step (1) comprises sodium sulfate decahydrate, sodium carbonate decahydrate, disodium hydrogen phosphate dodecahydrate, sodium acetate trihydrate, calcium chloride hexahydrate, magnesium chloride hexahydrate, or a eutectic salt.
4. The method of claim 3, wherein the eutectic salt comprises 66.6 wt% CaCl2·6H2O+33.4wt％MgCl2·6H2O、60wt％Na2HPO4·12H2O+40wt％Na2SO4·10H2O、75wt％Na2HPO4·12H2O+25wt％Na2CO3·10H2And one or more of O.
5. The method as claimed in claim 1, wherein the paraffin wax in the step (1) comprises one or more of hexadecane, octadecane, eicosane and docosane; the emulsifier comprises one or more of Span20, Tween20, Span60, Tween60, Span80 and Tween 80.
6. The method as claimed in claim 1, wherein the cellulose in step (2) comprises one or more of carboxymethyl cellulose, bacterial cellulose, microcrystalline cellulose, cellulose nanocrystals, cellulose micro/nanowires, wood pulp cellulose, straw cellulose and bamboo cellulose, and the cross-linking agent and the hydrophobic modifier are vinylsilanes, wherein the vinylsilanes comprise one or more of vinyltriethoxysilane, vinyltrimethoxysilane and vinyltris (β -methoxyethoxy) silane.
7. The method according to claim 1, wherein the stirring temperature in the step (2) is 20-40 ℃, and the stirring time is 1-3 h; the freeze drying temperature is-60 to-30 ℃, and the freeze drying time is 24 to 48 hours; the crosslinking temperature is 90-110 ℃, and the crosslinking time is 20-60 min.
8. The method of claim 1, wherein the dipping temperature in the step (3) is 40-70 ℃ and the dipping time is 0.5-2 h.
9. A hydrated salt/paraffin/cellulose sponge composite phase change material prepared by the method of claim 1.
10. Use of the hydrated salt/paraffin/cellulose sponge composite phase change material prepared by the method of claim 1.
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| CN112321887A (en) * | 2020-09-29 | 2021-02-05 | 浙江理工大学 | Preparation method of mechanical flexible cellulose aerogel with gradient change of wettability |
| CN112552553A (en) * | 2020-12-09 | 2021-03-26 | 桂林理工大学 | Composite foam porous material and preparation method and application thereof |
| CN113337252A (en) * | 2021-05-31 | 2021-09-03 | 苏州大学 | Cellulose-based flexible heat storage composite material and preparation method thereof |
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| CN112552553A (en) * | 2020-12-09 | 2021-03-26 | 桂林理工大学 | Composite foam porous material and preparation method and application thereof |
| CN112552553B (en) * | 2020-12-09 | 2022-06-17 | 桂林理工大学 | Composite foam porous material and preparation method and application thereof |
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