CN109943026B - Supercritical water degradation polyester gradient phase change heat storage material and preparation method thereof - Google Patents
Supercritical water degradation polyester gradient phase change heat storage material and preparation method thereof Download PDFInfo
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- CN109943026B CN109943026B CN201910110592.5A CN201910110592A CN109943026B CN 109943026 B CN109943026 B CN 109943026B CN 201910110592 A CN201910110592 A CN 201910110592A CN 109943026 B CN109943026 B CN 109943026B
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Abstract
The invention relates to a variable material and the technical field of heat storage thereof, in particular to a supercritical water degradation polyester gradient phase change heat storage material and a preparation method thereof. The invention adopts a supercritical water method to carry out multistage degradation on polyester to obtain low molecular weight polyester with various molecular weights or melting points, and a gradient phase change heat storage material is formed by the low molecular weight polyester with various molecular weights or melting points, and the phase change heat storage material has a plurality of solid-liquid phase change points.
Description
Technical Field
The invention relates to a gradient phase change heat storage material and a preparation method thereof, in particular to a composite phase change material with multiple phase change points, which is formed by two or more groups of phase change materials with different solid-liquid phase change points, and belongs to the technical field of phase change materials and heat storage thereof.
Background
The phase-change heat storage realizes isothermal heat storage by utilizing the heat absorption and release of the material at the melting point, and has higher efficiency compared with a sensible heat storage mode.
Solar sunlight intensity is different in different seasons, different regions and different time of day, the temperature generated by the solar heat storage material is different, if a single phase change material is used for absorbing heat, the temperature value in each time interval can be difficult to approach to a phase change point to the maximum extent, therefore, the phase change material is difficult to work at the phase change point, more times of heat storage can be completed in a low-efficiency sensible heat mode, if a composite phase change material with a plurality of phase change points is adopted, each phase change component can approach to a phase change working state to the maximum extent, the sensible heat occupation ratio is reduced to the maximum extent, and the heat storage is realized at the highest efficiency.
Chinese patent CN106221676A discloses a phase change heat storage material with multiple phase change points and a preparation process thereof, and the principle is that phase change materials with multiple phase change points are mixed to form a graded phase change material with multiple phase change temperatures; chinese patent CN106634856A discloses a two-gradient phase-change heat storage material and a preparation method thereof, the invention aims to achieve the purpose of performance complementation by compounding two phase-change materials with different performances, and the patent does not mention that the phase-change heat exchange is completed at each temperature point by different phase-change temperatures. Chinese patent CN106675525A discloses a "phase change cold storage material with two phase change points and its preparation method", the purpose of the invention is to make its working temperature always between two phase change temperatures by the composite material with two phase change points, the patent does not mention that the phase change heat exchange is completed at each temperature point by different phase change temperatures.
The phase-change materials with different phase-change points adopted in the patent are heterogeneous inorganic composite phase-change materials with different phase-change points, and due to the fact that the materials are heterogeneous, the problem of microscopic cracks caused by incompatibility exists, the cracks can block conduction of heat flow, and heat conductivity is reduced. Heterogeneous phase change materials are mixed together, and due to different molecular structures, crystallization can be influenced, and thus supercooling degree is influenced. This requires that either a plurality of different nucleating agents are selected corresponding to a plurality of phase change materials or the selected nucleating agents have a nucleating effect on a plurality of heterogeneous phase change materials when selecting the nucleating agents, which reduces the range of phase change material selection.
The phase change point of the phase change material adopted in the patent is fixed and invariable, and a user cannot freely select the phase change material according to needs. In fact, it is very difficult to find the phase-change material according to the specified phase-change temperature, and the phase-change temperature of the phase-change material cannot be changed generally, so if the phase-change temperature point of the material, that is, the melting point of the material, can be changed by control, the phase-change temperature required by the user can be met more accurately.
On the other hand, chinese patent CN105509528A discloses a "multi-level gradient phase change regenerator", which is a structure with multiple phase change points obtained by structural design, specifically, the phase change layers with multiple levels of different phase change temperatures are arranged from top to bottom in sequence, so as to realize the heat exchange between the heat exchange medium and each level of phase change layer in sequence, and thus, when the fluid heat exchange medium is used for heat exchange in the heat exchange process, the temperature of the fluid heat exchange medium is continuously changed, and the fluid heat exchange medium is just subjected to efficient phase change heat exchange with the multiple layers of phase change heat storage layers with different phase change temperatures; chinese patent CN108413796A discloses a "temperature gradient energy storage heat exchanger", which also uses a structure of stacking a plurality of heat storage sandwich plates to realize gradient heat exchange. Chinese patent CN106940148A discloses a 'gradient fractal lattice sandwich reinforced phase change heat sink', which has the principle that phase change sandwich is sequentially arranged into an array according to a gradient changing mode to improve the heat exchange efficiency, and the basic structure is also laminated according to the heat flow direction; none of the above patents modifies the phase change material and thereby changes the phase change point.
Chinese patent CN200810058354 discloses a process for degrading plastics by supercritical xylene, which adopts supercritical xylene to degrade polyethylene and the like into oil products, and aims to degrade waste plastics into oil products. Chinese patent CN200910081359 discloses a waste polyester depolymerization method, which adopts supercritical methanol and 280 ℃ of 220-. The Chinese patent CN1189537C adopts supercritical water at 380-450 ℃ to degrade polyethylene into oil, and the Chinese patent CN1247742C adopts supercritical water at 380-450 ℃ to degrade polypropylene into oil.
The molecular weight of the polyester polymer is generally 2-3 ten thousand, the polyester polymer belongs to crystalline plastics, the melting point is about 255-260 ℃, and the degraded monomer dimethyl phthalate can be used as a raw material of polyester. The theoretical enthalpy of crystallization is 140 KJ/kg.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a supercritical water degradation polyester gradient phase change heat storage material and a preparation method thereof. The invention adopts a supercritical water method to carry out multistage degradation on polyester to obtain low molecular weight polyester with various molecular weights or melting points, and a gradient phase change heat storage material is formed by the low molecular weight polyester with various molecular weights or melting points, and the phase change heat storage material has a plurality of solid-liquid phase change points.
In order to achieve the purpose, the invention adopts the following technical scheme: the utility model provides a supercritical water degradation polyester gradient phase change heat-retaining material which characterized in that: comprising two or more different molecular weight polyesters.
According to above supercritical water degradation polyester gradient phase change heat storage material which characterized in that: the molecular weight of the polyester is 1000-8000.
According to above supercritical water degradation polyester gradient phase change heat storage material which characterized in that: the polyester material is two or more than two of the polyester with the molecular weight of 1200, the molecular weight of 2500, the molecular weight of 5500 and the molecular weight of 5500.
According to above supercritical water degradation polyester gradient phase change heat storage material which characterized in that: the particle size of the polyester is 3-5 mm.
The invention also discloses a preparation method of the supercritical water degradation polyester gradient phase change heat storage material, which is characterized by comprising the following steps: adding polyester into a reaction kettle, adding water into the reaction kettle, sealing and heating at 370-420 ℃ for 5-30 minutes to react to obtain polyester with different molecular weights;
two or more than two polyesters are combined into a gradient phase change heat storage material, a heat conducting agent, an antioxidant and an auxiliary setting agent are added, the mixture is dispersed for 5 to 20 minutes in a reaction kettle at the temperature of 150-170 ℃, and the mixture is taken out, cooled and crushed into particles with the particle size of 3 to 5 mm.
The preparation method of the supercritical water degradation polyester gradient phase change heat storage material is characterized by comprising the following steps: the heat conducting agent is one or more of graphite powder, foamed aluminum and carbon powder, and the addition amount is 1-10%.
The preparation method of the supercritical water degradation polyester gradient phase change heat storage material is characterized by comprising the following steps: the antioxidant is one or more of phenothiazine, salicylate and BHA, and the addition amount is 0.5-2%.
The preparation method of the supercritical water degradation polyester gradient phase change heat storage material is characterized by comprising the following steps: the auxiliary setting agent is one or more of attapulgite, perlite, foamed aluminum and expanded graphite, and the addition amount is 1-10%.
A preparation method of a supercritical water degradation polyester gradient phase change heat storage material is characterized by comprising the following steps: the polyester gradient phase change heat storage material is prepared according to the preparation method of the supercritical water degradation polyester gradient phase change heat storage material.
The invention has the beneficial effects that:
because the multi-gradient phase-change material contains a plurality of phase-change points, each temperature in the heat storage process is provided with the corresponding heat storage material close to the phase-change points, so that the heat transfer and storage processes are close to phase-change heat exchange to the maximum extent, and high-efficiency heat transfer and storage are achieved.
Meanwhile, as the plurality of phase change materials with the same quality and different phase change points have good compatibility, the heat insulation crack caused by phase separation is reduced to the greatest extent, and the heat conduction performance of the materials is improved.
Because a plurality of homogeneous phase change materials with different phase change points are uniformly dispersed and mixed and at least one group of solid components always exists, the molecular material with high phase change temperature forms a solid phase continuous or discrete net shape similar to sponge, namely the material can also form a shape-stabilized material, and the leakage or loss of the liquid phase component with low melting point is slowed down.
Because the molecular structures of a plurality of phase change materials with the same homogeneous phase change point and different phase change points are the same, the high-melting-point component is used as the self-induced crystallization nucleation of the geomelting-point component, so that the material can reduce or omit the nucleating agent, namely the material can perform the self-nucleation.
Polyesters are relatively easy to hydrolyze and degrade more readily than other low molecular weight polymers.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention.
Detailed Description
In the invention, the percentage is weight percentage.
Homogeneity is the same substance, and its molecular structure is the same, but the molecular weight is different.
The embodiments of the present invention will be further described with reference to the accompanying drawings, wherein the flow of the embodiments is shown in the drawings, and the embodiments described below are exemplary and intended to explain the present invention and should not be construed as limiting the invention, and any modification, equivalent replacement or improvement made within the spirit and principle of the present invention shall be included in the scope of the claims of the present invention, and all technical solutions not described in detail are known in the art.
As shown in figure 1, 100kg of polyester is added into a reaction kettle according to the required phase transition temperature range, 30-50 kg of water is added into the reaction kettle at the temperature of 370-420 ℃, and the reaction is carried out for 5-30 minutes by sealing and heating, so as to obtain the low molecular weight polyester with the molecular weight of 1000-8000. By controlling the reaction temperature and the reaction time, polyesters with different molecular weights and different molecular weight distributions can be obtained.
The low molecular weight polyester having the desired molecular weight can be obtained by purifying the low molecular weight polyester, and the purification process, preferably the purification process, can be omitted.
Two or more low molecular weight polyesters with melting points form a gradient phase change heat storage material, 2-10% of heat conducting agent, 0.5-2% of antioxidant and 1-10% of auxiliary setting agent are added and dispersed in a reaction kettle at the temperature of 150-170 ℃ for 5-20 minutes, and the mixture is taken out, cooled and crushed into 3-5mm particles, so that the supercritical water degradation polyester gradient phase change heat storage material can be obtained.
The heat conducting agent is one or more of graphite powder, foamed aluminum and carbon powder, and preferably foamed aluminum is selected. The addition amount is 1-10%.
The antioxidant is one or more of phenothiazine, salicylate and BHA, and is preferably salicylate. The addition amount is 0.5-2%.
The auxiliary setting agent is one or more of attapulgite, perlite, foamed aluminum and expanded graphite, and the attapulgite is preferred. The addition amount is 1-10%.
The first embodiment is as follows:
adding 100kg of polyester into a reaction kettle, adding 50kg of water into the reaction kettle at the temperature of 400 ℃, sealing, heating and reacting for 30 minutes, removing water and drying to obtain the low molecular weight polyester with the molecular weight of 1200 and the melting point of 61 ℃.
Adding 100kg of polyester into a reaction kettle, adding 40kg of water into the reaction kettle at 385 ℃, sealing and heating for reaction for 20 minutes, removing water and drying to obtain the low molecular weight polyester with the molecular weight of 2500 and the melting point of 77 ℃.
Adding 100kg of polylactic acid into a reaction kettle, adding 30kg of water into the reaction kettle at the temperature of 375 ℃, sealing, heating and reacting for 10 minutes, removing water and drying to obtain the low molecular weight polyester with the molecular weight of 5500 and the melting point of 86 ℃.
The three low molecular weight polyesters with melting points are combined into a gradient phase change heat storage material according to equal proportion, 2% of foamed aluminum, 0.5% of salicylate and 3% of expanded graphite are added into a reaction kettle at 100 ℃ for dispersion for 15 minutes, and the mixture is taken out, cooled and crushed into particles of 3-5mm, so that the supercritical water degradation polyester gradient phase change heat storage material can be obtained.
The use temperature is not more than 80 ℃.
Actually measured phase change temperature is 60-85 ℃, and average phase change enthalpy is 109 KJ/kg.
Example two:
adding 100kg of polyester into a reaction kettle, adding 50kg of water into the reaction kettle at the temperature of 400 ℃, sealing, heating and reacting for 30 minutes, removing water and drying to obtain the low molecular weight polyester with the molecular weight of 1200 and the melting point of 61 ℃.
Adding 100kg of polyester into a reaction kettle, adding 40kg of water into the reaction kettle at 385 ℃, sealing and heating for reaction for 20 minutes, removing water and drying to obtain the low molecular weight polyester with the molecular weight of 2500 and the melting point of 77 ℃.
Adding 100kg of polylactic acid into a reaction kettle, adding 30kg of water into the reaction kettle at the temperature of 375 ℃, sealing, heating and reacting for 10 minutes, removing water and drying to obtain the low molecular weight polyester with the molecular weight of 5500 and the melting point of 86 ℃.
The three low molecular weight polyesters with melting points are combined into a gradient phase change heat storage material according to equal proportion, 5 percent of carbon powder, 0.5 percent of phenothiazine and 3 percent of attapulgite are added into a reaction kettle at 100 ℃ for dispersing for 15 minutes, and the gradient phase change heat storage material is taken out, cooled and crushed into particles with the particle size of 3-5mm, thus obtaining the hydrothermal degradation polylactic acid gradient phase change heat storage material.
The use temperature is not more than 80 ℃.
Actually measured phase change temperature is 61-86 ℃, and average phase change enthalpy is 110 KJ/kg.
Example three:
adding 100kg of polyester into a reaction kettle, adding 50kg of water into the reaction kettle at the temperature of 400 ℃, sealing, heating and reacting for 30 minutes, removing water and drying to obtain the low molecular weight polyester with the molecular weight of 1200 and the melting point of 61 ℃.
Adding 100kg of polyester into a reaction kettle, adding 40kg of water into the reaction kettle at 385 ℃, sealing and heating for reaction for 20 minutes, removing water and drying to obtain the low molecular weight polyester with the molecular weight of 2500 and the melting point of 77 ℃.
100kg of polyester is added into a reaction kettle, 30kg of water is added into the reaction kettle at the temperature of 375 ℃, the reaction kettle is sealed and heated for 10 minutes, and the low molecular weight polyester with the molecular weight of 5500 and the melting point of 86 ℃ is obtained after dehydration and drying.
The three low molecular weight polyesters with melting points form a gradient phase change heat storage material according to the ratio of 1:2:3, 8% of graphite powder, 2% of BHA and 6% of perlite are added into a reaction kettle at 100 ℃ for dispersing for 15 minutes, and the mixture is taken out, cooled and crushed into particles of 3-5mm, so that the hydrothermal degradation polylactic acid gradient phase change heat storage material can be obtained.
The use temperature is not more than 80 ℃.
Actually measured phase change temperature is 60-86 ℃, and average phase change enthalpy is 108 KJ/kg.
The invention compounds the phase-change materials with various melting points, and compared with various heterogeneous composite phase-change materials, the heterogeneous composite phase-change materials have the same molecular structure, better compatibility and easy uniform mixing into a homogeneous dispersion form, can form a homogeneous crystal alloy form similar to that of a metal alloy, and have the advantages that all the components are fully dissolved mutually, the phase domains are fine, solid-phase homogeneous particles which are close to each other and have high melting points can become a nucleating agent of a liquid phase component with a low melting point, and the crystallization supercooling degree is reduced to the maximum extent.
When in use, if the component with the temperature not exceeding the highest melting point in the components of the gradient phase-change material is used, namely at least one component is always kept in a solid phase, the homogeneous solid particles are uniformly mixed in the liquid phase, a compatible thickening effect is achieved on the liquid phase, and a stabilizing and shaping agent required by the phase-change material can be reduced or omitted.
Most homogeneous metals, inorganic non-metals cannot have multiple melting points, with crystalline polymers being an exception. The crystalline polymers with different molecular weights have the same molecular structure, different molecular weights and different melting points in a certain range, and by utilizing the characteristic, the gradient phase-change material with the characteristics can be obtained by compounding the homogeneous polymers with different molecular weights.
In order to obtain polymers of different molecular weights, the molecular weight of the final product can be controlled during polymerization. The above method is troublesome if a plurality of polymers having different molecular weights are to be obtained.
The ready-made polymer is degraded, and oligomers with different molecular weights are obtained by controlling the degradation process, so that the method is a good method for obtaining homogeneous polymers with different molecular weights. The oligomers formed during the degradation process are generally not of a single molecular weight but are normally distributed in the composition. By controlling the degradation conditions, the molecular weight distribution can be adjusted, and from the viewpoint of cost, oligomers with a broad molecular weight distribution more closely meet the gradient requirements of the gradient phase change material, which makes the gradient cells finer, so that, in the degradation operation, measures advantageous for a broad molecular weight distribution are preferred.
The conventional polyester polymer in the nature has high phase-change temperature and is difficult to be used as a phase-change heat storage material, and the method reduces the molecular weight of the polyester polymer and the phase-change temperature of the polyester polymer, so that the polyester polymer can be suitable for the fields of solar devices and the like, and the purpose of practicability of the polyester polymer is realized. And the polyester is relatively easy to hydrolyze, is easier to degrade, and has small influence on the environment even if being used in large quantity.
Claims (6)
1. The utility model provides a supercritical water degradation polyester gradient phase change heat-retaining material which characterized in that: comprises two or more than two polyesters with different molecular weights, and the polyester material is two or more than two polyesters with the molecular weight of 1200, the molecular weight of 2500 and the molecular weight of 5500.
2. The supercritical water-degradable polyester gradient phase-change heat storage material of claim 1, which is characterized in that: the particle size of the polyester is 3-5 mm.
3. A preparation method of a supercritical water degradation polyester gradient phase change heat storage material is characterized by comprising the following steps: adding polyester into a reaction kettle, adding water into the reaction kettle, heating at 370-420 ℃, sealing, and reacting for 5-30 minutes to obtain polyester with different molecular weights, wherein the polyester material is two or more than two of the polyester with the molecular weight of 1200, the polyester with the molecular weight of 2500 and the polyester with the molecular weight of 5500;
two or more than two polyesters are combined into a gradient phase change heat storage material, a heat conducting agent, an antioxidant and an auxiliary setting agent are added, the mixture is dispersed for 5 to 20 minutes in a reaction kettle at the temperature of 150-170 ℃, and the mixture is taken out, cooled and crushed into particles with the particle size of 3 to 5 mm.
4. The preparation method of the supercritical water degradation polyester gradient phase change heat storage material as claimed in claim 3, wherein: the heat conducting agent is one or more of graphite powder, foamed aluminum and carbon powder, and the addition amount is 1-10%.
5. The preparation method of the supercritical water degradation polyester gradient phase change heat storage material as claimed in claim 3, wherein: the antioxidant is one or more of phenothiazine, salicylate and BHA, and the addition amount is 0.5-2%.
6. The preparation method of the supercritical water degradation polyester gradient phase change heat storage material as claimed in claim 3, wherein: the auxiliary setting agent is one or more of attapulgite, perlite, foamed aluminum and expanded graphite, and the addition amount is 1-10%.
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Denomination of invention: A gradient phase change heat storage material for supercritical water degraded polyester and its preparation method Effective date of registration: 20220516 Granted publication date: 20210608 Pledgee: Wuhan rural commercial bank Limited by Share Ltd. Yangluo Economic Development Zone Branch Pledgor: WUHAN BLOOMING LOW CARBON INDUSTRY CO.,LTD. Registration number: Y2022420000118 |
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Date of cancellation: 20230412 Granted publication date: 20210608 Pledgee: Wuhan rural commercial bank Limited by Share Ltd. Yangluo Economic Development Zone Branch Pledgor: WUHAN BLOOMING LOW CARBON INDUSTRY CO.,LTD. Registration number: Y2022420000118 |
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Denomination of invention: A Supercritical Water Degradation Polyester Gradient Phase Change Thermal Storage Material and Its Preparation Method Effective date of registration: 20230414 Granted publication date: 20210608 Pledgee: Wuhan rural commercial bank Limited by Share Ltd. Yangluo Economic Development Zone Branch Pledgor: WUHAN BLOOMING LOW CARBON INDUSTRY CO.,LTD. Registration number: Y2023420000160 |