CN109943044B - Polylactic acid gradient phase change heat storage material and preparation method thereof - Google Patents
Polylactic acid gradient phase change heat storage material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a gradient phase-change heat storage material and a preparation method thereof, belonging to the technical field of phase-change materials and heat storage thereof. The invention adopts a biodegradation imitating method to carry out multi-stage degradation on polylactic acid to obtain low molecular weight polylactic acid with various molecular weights or melting points, and a gradient phase change heat storage material is formed by the low molecular weight polylactic acid, 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 adopting 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 CN201080010934 discloses a chemical recycling polylactic acid by an alcoholysis method, which degrades polylactic acid into lactic acid under the conditions of an alkali catalyst, a lactate ester solvent and 80-180 ℃ and aims to recycle waste polylactic acid. Chinese patent CN201610407510 discloses a method for recovering polylactic acid waste, which degrades polylactic acid into lactic acid and calcium lactate under the conditions of lactide solvent and 170-220 ℃, and aims at recovering waste polylactic acid. Chinese patent CN201810529672 discloses a method for efficiently recycling waste colored polylactic acid, which degrades polylactic acid into alkyl lactate under the conditions of alkali catalyst, organic alcohol such as methanol and the like, 50-180 ℃ and 0.5-5 hours, and aims to recycle the waste polylactic acid.
The above patents all aim to recover polylactic acid as a small molecule monomer by means of a catalyst, a solvent, a high temperature, and a long time. Or the polypropylene is degraded into propylene monomer by adopting a method of ultraviolet ray and biological fermentation, and the method is also used for recovering waste plastics.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a polylactic acid gradient phase change heat storage material and a preparation method thereof. The invention adopts a biodegradation imitating method to carry out multi-stage degradation on polylactic acid to obtain low molecular weight polylactic acid with various molecular weights or melting points, and a gradient phase change heat storage material is formed by the low molecular weight polylactic acid, 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: a polylactic acid gradient phase change heat storage material is characterized in that: comprises two or more polylactic acids with different molecular weights.
According to polylactic acid gradient phase change heat storage material as above, its characterized in that: the molecular weight of the polylactic acid is 3000-40000.
According to polylactic acid gradient phase change heat storage material as above, its characterized in that: the polylactic acid has any two or more of 3500, 8500, 25000 and 35000.
A preparation method of polylactic acid gradient phase change heat storage material is characterized by comprising the following steps: the method comprises the following steps: adding polylactic acid into the multilayer vibration ultraviolet vibration irradiation box, wherein the temperature is 25-40 ℃, the ultraviolet intensity is 10-1000 uW/cm2, the irradiation time is 1-10 hours, injecting fermentation liquor for fermentation for 1-10 days, and obtaining polylactic acid with different molecular weights and different molecular weight distributions by controlling the reaction conditions; two or more than two kinds of polylactic acid with different molecular weight are combined into a gradient phase change heat storage material, 1-10% of heat conducting agent and 1-10% of auxiliary setting agent are added, dispersed for 5-20 minutes in an internal mixer at the temperature of 150-.
The preparation method of the polylactic acid gradient phase change heat storage material is characterized by comprising the following steps: the fermentation liquor is one of 2-5% of fusarium candidum, penicillium and humus.
The preparation method of the polylactic acid 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.
The preparation method of the polylactic acid gradient phase change heat storage material is characterized by comprising the following steps: the auxiliary shaping agent is one or more of attapulgite, perlite, foamed aluminum and expanded graphite.
The preparation method of the polylactic acid gradient phase change heat storage material is characterized by comprising the following steps: the multi-layer vibration ultraviolet vibration irradiation box is in a grid shape, an ultraviolet lamp array for controlling irradiation intensity is arranged above each interlayer, and each interlayer is heated and vibrated.
The preparation method of the polylactic acid gradient phase change heat storage material is characterized by comprising the following steps: the polylactic acid gradient phase change heat storage material is prepared by the preparation method.
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 per se also forms a shape-stabilized material, and the leakage or loss of the liquid phase component with low melting point is slowed down. Due to the fact that the molecular structures of the plurality of phase change materials with the same homogeneous phase change points and different phase change points are the same, the nucleating agent can be reduced or omitted, and the material can perform self-nucleation. Compared with other low molecular weight polymers, the polylactic acid belongs to biodegradable materials and has better environmental protection property.
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, according to the required phase transition temperature range, 100kg of polylactic acid is added into the multilayer vibration ultraviolet vibration irradiation box, the temperature is 25-40 ℃, the ultraviolet intensity is 10-1000 uW/cm2, the irradiation time is 1-10 hours, and then fermentation liquor is injected for fermentation for 1-10 days, so that low molecular weight polylactic acid with the molecular weight of 3000-40000 is obtained. By controlling the reaction conditions, polylactic acid with different molecular weights and different molecular weight distributions can be obtained. The fermentation liquor is one of 2-5% fusarium candidum, penicillium and humus, and the degradation speed of the fermentation liquor is improved.
The low molecular weight polylactic acid having a desired molecular weight can be obtained by purifying the low molecular weight polylactic acid, and a purification process, preferably a purification process, can be omitted.
The method comprises the steps of forming a gradient phase change heat storage material by two or more low molecular weight polylactic acids with melting points, adding 2-10% of a heat conducting agent and 1-10% of an auxiliary setting agent, dispersing in an internal mixer at the temperature of 150-.
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 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%.
In the present invention, the polylactic acid is homogeneous, and at least two molecular weights or melting points of the low molecular weight polylactic acid are selected. The proportion can be selected according to the heat storage amount of the required phase change point, and preferably is evenly distributed. The molecular weight of the low molecular weight polylactic acid is 3000-40000, the corresponding melting point is 69-130 ℃, and the phase change enthalpy is 81-96 kj/kg.
The invention also discloses a multilayer vibration ultraviolet vibration irradiation box, wherein the irradiation box is in a grid shape, an ultraviolet lamp array capable of controlling irradiation intensity is arranged above each interlayer, each interlayer can be heated and vibrated, polylactic acid is added into the multilayer vibration ultraviolet irradiation box to be irradiated according to the set ultraviolet intensity, heating temperature and irradiation time, then ultraviolet rays are closed, fermentation liquor is injected, and fermentation is carried out for a certain time at a certain temperature, so that low molecular weight polylactic acid with the molecular weight of 3000-40000 is obtained. The low molecular weight polylactic acid with the required molecular weight can be obtained by purifying the low molecular weight polylactic acid. The fermentation liquor is one of 2-5% fusarium candidum, penicillium and humus, and the degradation speed of the fermentation liquor is improved.
The first embodiment is as follows:
adding 100kg of polylactic acid into a multilayer vibration ultraviolet vibration irradiation box, controlling the temperature at 40 ℃, the ultraviolet intensity at 500uW/cm2, irradiating for 9 hours, injecting 5% fusarium candida fermentation liquor, fermenting for 8 days, removing water, and drying to obtain the low molecular weight polylactic acid with the molecular weight of 3500 and the melting point of 71 ℃.
Adding 100kg of polylactic acid into a multilayer vibration ultraviolet vibration irradiation box, controlling the temperature at 32 ℃, the ultraviolet intensity at 200uW/cm2, irradiating for 5 hours, then injecting 3.5% of penicillium fermentation liquor, fermenting for 4 days, removing water and drying to obtain the low molecular weight polylactic acid with the molecular weight of 8500 and the melting point of 87 ℃.
Adding 100kg of polylactic acid into a multilayer vibration ultraviolet vibration irradiation box, wherein the temperature is 27 ℃, the ultraviolet intensity is 100uW/cm2, the irradiation time is 2 hours, then injecting 2% of humic acid bacteria fermentation liquor for fermentation for 2 days, removing water and drying to obtain the low molecular weight polylactic acid with the molecular weight of 25000 and the melting point of 110 ℃.
The three low-molecular-weight polylactic acids 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 120 ℃ internal mixer to be dispersed for 15 minutes, and the mixture is taken out, cooled and crushed into particles with the particle size 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 105 ℃.
Actually measured phase transition temperature is 70-112 ℃, and average phase transition enthalpy is 89 KJ/kg.
Example two:
adding 100kg of polylactic acid into a multilayer vibration ultraviolet vibration irradiation box, controlling the temperature at 32 ℃, the ultraviolet intensity at 200uW/cm2, irradiating for 5 hours, injecting 4% of penicillium fermentation liquor, fermenting for 4 days, removing water, and drying to obtain the low molecular weight polylactic acid with the molecular weight of 8500 and the melting point of 87 ℃.
Adding 100kg of polylactic acid into a multilayer vibration ultraviolet vibration irradiation box, wherein the temperature is 27 ℃, the ultraviolet intensity is 100uW/cm2, the irradiation time is 2 hours, then injecting 3% of humic acid bacteria fermentation liquor for fermentation for 2 days, removing water and drying to obtain the low molecular weight polylactic acid with the molecular weight of 25000 and the melting point of 110 ℃.
Adding 100kg of polylactic acid into a multilayer vibration ultraviolet vibration irradiation box, wherein the temperature is 27 ℃, the ultraviolet intensity is 100uW/cm2, the irradiation time is 1 hour, then injecting 2.5% fusarium candida fermentation liquor for fermentation for 1 day, removing water and drying to obtain the low molecular weight polylactic acid with the molecular weight of 35000 and the melting point of 122 ℃.
And (2) forming the gradient phase change heat storage material by the three low-molecular-weight polylactic acids with the melting points according to equal proportion, adding 5% of carbon powder, 0.5% of phenothiazine and 3% of attapulgite, adding the mixture into a 130 ℃ internal mixer for dispersing for 15 minutes, taking out, cooling and crushing the mixture 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 120 ℃.
Actually measured phase transition temperature is 86-119 ℃, and average phase transition enthalpy is 95 KJ/kg.
Example three:
adding 100kg of polylactic acid into a multilayer vibration ultraviolet vibration irradiation box, irradiating for 5 hours at the temperature of 32 ℃, with the ultraviolet intensity of 200uW/cm2, injecting 4.5% of humic acid bacteria fermentation liquor, fermenting for 4 days, removing water and drying to obtain the low molecular weight polylactic acid with the molecular weight of 8500 and the melting point of 87 ℃.
Adding 100kg of polylactic acid into a multilayer vibration ultraviolet vibration irradiation box, wherein the temperature is 27 ℃, the ultraviolet intensity is 100uW/cm2, the irradiation time is 2 hours, then injecting 3.5% fusarium candida fermentation liquor for fermentation for 2 days, removing water and drying to obtain the low molecular weight polylactic acid with the molecular weight of 25000 and the melting point of 110 ℃.
Adding 100kg of polylactic acid into a multilayer vibration ultraviolet vibration irradiation box, wherein the temperature is 27 ℃, the ultraviolet intensity is 100uW/cm2, the irradiation time is 1 hour, then injecting 2% of penicillium fermentation liquor, fermenting for 1 day, removing water and drying to obtain the low molecular weight polylactic acid with the molecular weight of 35000 and the melting point of 122 ℃.
The three low-molecular-weight polylactic acid 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 an internal mixer at 130 ℃ 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 120 ℃.
The actually measured phase transition temperature is 86-119 ℃, and the average phase transition enthalpy is 97 KJ/kg.
The invention is a phase-change material composite with various melting points, compared with various heterogeneous composite phase-change materials, the various homogeneous composite phase-change materials have the same molecular structure and better compatibility with each other, are easy to be uniformly mixed into a homogeneous dispersion form, can form a homogeneous crystal alloy form similar to that of a metal alloy, are fully mutually soluble and have small phase domains, and 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, thereby reducing the crystallization supercooling degree 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 polylactic acid polymer has a molecular weight of 7-10 ten thousand generally, belongs to crystalline plastics, has a melting point of about 175 ℃, can be used for biodegradable plastics, can be used as a raw material of polylactic acid, and is low in strength and not large in application at present. The present invention degrades the ready-made polymer to obtain oligomer with different molecular weight through controlling the degradation process, and is one excellent method of obtaining homogeneous polymer with different molecular weight. 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 invention adopts a biological-like fermentation method to degrade the ready-made polylactic acid, and obtains the polylactic acid with different molecular weights by controlling the degradation process. The invention creates a higher-degree natural biodegradation environment, and carries out rapid and controllable molecular weight grading degradation on the polylactic acid to obtain various low molecular weight polylactic acids for gradient phase change materials.
Claims (6)
1. A preparation method of polylactic acid gradient phase change heat storage material is characterized by comprising the following steps: the method comprises the following steps: adding polylactic acid into a multilayer vibration ultraviolet vibration irradiation box, wherein the temperature is 25-40 ℃, the ultraviolet intensity is 10-1000 uW/cm2, the irradiation time is 1-10 hours, and injecting fermentation liquor for fermentation for 1-10 days to obtain polylactic acid with different molecular weights and different molecular weight distributions; adding 1-10% of heat-conducting agent and 1-10% of auxiliary setting agent into the two or more polylactic acids, dispersing for 5-20 minutes in an internal mixer at the temperature of 150-.
2. The preparation method of the polylactic acid gradient phase change heat storage material according to claim 1, wherein the preparation method comprises the following steps: the fermentation liquor is one of 2-5% of fusarium candidum, penicillium and humus.
3. The preparation method of the polylactic acid gradient phase change heat storage material according to claim 1, wherein the preparation method comprises the following steps: the heat conducting agent is one or more of graphite powder, foamed aluminum and carbon powder.
4. The preparation method of the polylactic acid gradient phase change heat storage material according to claim 1, wherein the preparation method comprises the following steps: the auxiliary shaping agent is one or more of attapulgite, perlite, foamed aluminum and expanded graphite.
5. The preparation method of the polylactic acid gradient phase change heat storage material according to claim 1, wherein the preparation method comprises the following steps: the multi-layer vibration ultraviolet vibration irradiation box is in a grid shape, an ultraviolet lamp array for controlling irradiation intensity is arranged above each interlayer, and each interlayer is heated and vibrated.
6. The polylactic acid gradient phase-change heat storage material obtained by the method of claim 1, which is characterized in that: the heat conducting agent comprises two or more polylactic acids with different molecular weights, the polylactic acid is a combination of any two or more of 3500 molecular weight, 8500 molecular weight, 25000 molecular weight and 35000 molecular weight, and also comprises 1-10% of heat conducting agent and 1-10% of auxiliary setting agent.
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| CN101058719A (en) * | 2006-11-22 | 2007-10-24 | 电子科技大学 | Composite phase-change material and preparation method thereof |
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| CN105085872A (en) * | 2014-05-08 | 2015-11-25 | 中国石油化工股份有限公司 | In-situ generated polylactic acid compound and preparation method therefor |
| CN105778465A (en) * | 2016-03-29 | 2016-07-20 | 西安理工大学 | Polyethylene glycol-porous expanded graphite material and preparation method thereof |
| CN106221676A (en) * | 2016-07-29 | 2016-12-14 | 贺迈新能源科技（上海）有限公司 | The phase change heat storage material of many transformation temperatures and preparation technology thereof |
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| CN101058719A (en) * | 2006-11-22 | 2007-10-24 | 电子科技大学 | Composite phase-change material and preparation method thereof |
| CN103073733A (en) * | 2013-01-06 | 2013-05-01 | 嘉兴天源药业有限公司 | Method adopting temperature inductivity characteristic of phase-change high polymer material to prepare biodegradable particles |
| CN105085872A (en) * | 2014-05-08 | 2015-11-25 | 中国石油化工股份有限公司 | In-situ generated polylactic acid compound and preparation method therefor |
| CN105778465A (en) * | 2016-03-29 | 2016-07-20 | 西安理工大学 | Polyethylene glycol-porous expanded graphite material and preparation method thereof |
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Denomination of invention: A polylactic acid 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 |
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