A reworkable epoxy resin-based glass material with latent heat storage function
By immobilizing phase change materials in epoxy resin using dynamic ester exchange bonds, the problems of solid-liquid phase change material leakage and the difficulty of reprocessing thermosetting plastics have been solved, realizing latent heat storage performance and reprocessing capability, and expanding the application of epoxy resin.
Patent Information
- Application Number
- CN202310188378.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-03-02
- Publication Date
- 2026-02-06
- Estimated Expiration
- 2043-03-02
AI Technical Summary
Existing solid-liquid phase change materials are prone to leakage, which limits the service life and heat storage capacity of composite phase change materials. Furthermore, thermosetting plastics are difficult to reprocess, resulting in resource waste.
Phase change materials are grafted and fixed into a three-dimensional cross-linked network of epoxy resin using dynamic ester exchange bonds to form a reprocessable epoxy resin glass material with latent heat storage function.
While achieving latent heat storage performance, the material also exhibits good stability at high temperatures and can be reprocessed, reducing resource waste and expanding the application areas of epoxy resin.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to a reworkable epoxy resin glass material with latent heat storage function and a preparation method thereof, in particular to a reworkable epoxy resin glass material with latent heat storage function using ester exchange bond as dynamic covalent bond, and belongs to the technical field of composite materials. BACKGROUND
[0002] Due to the pollution and non-renewable nature of fossil fuels, people have begun to turn their attention to the development of renewable and clean energy. Among various renewable energy sources, such as solar energy, wind energy and tidal energy, they have the disadvantages of intermittency and instability. How to realize energy storage is the key to the development and utilization of renewable and clean energy.
[0003] Phase change materials can maintain a constant temperature during melting or solidification, while storing or releasing a large amount of energy. Using phase change materials for thermal energy storage is a promising method for developing and utilizing renewable and clean energy. At present, the most commonly used phase change energy storage materials are mainly solid-liquid phase change materials. In order to solve the possible leakage problem of solid-liquid phase change materials, people try to make solid-liquid phase change materials into shaped phase change materials and microcapsule phase change materials, and good results have been achieved. The shortcomings of shaped phase change materials and microcapsule phase change materials are that once the support material or microcapsule shell material is damaged due to external factors, leakage will occur, which will affect the service life and heat storage capacity of the composite phase change material. Therefore, more stable solid-solid phase change materials have gradually attracted people's attention.
[0004] At present, people mainly prepare solid-solid phase change materials through the means of constructing supramolecular and chemical cross-linking. Supramolecular phase change materials refer to the way of binding phase change materials in polymer network through physical interaction (hydrogen bond, chain entanglement and physical absorption), which occurs solid-solid phase change behavior after reaching the melting temperature. Liu Z L et al. (Solar Energy Materials and Solar Cells J. 2020, 216, 110678.) prepared supramolecular phase change materials by polyacrylic acid / silica. Due to the restriction of chain segments, polyethylene glycol (PEG) shows solid state. Yin G Z et al. (Composites Communications J. 2021, 27, 10089.) reported a poly (glycerol itaconic acid) supramolecular phase change material. Hydrogen bond force makes PEG show solid-solid phase change characteristics, but this method cannot guarantee the leakage of the material at high temperature (higher than the dissociation temperature of non-covalent bond). Chemical cross-linking is a way to permanently fix phase change materials in cross-linked network through chemical bonding. Swati S et al. (Solar Energy J. 2019, 181, 187-194) used tetraethyl orthosilicate (TEOS) as cross-linking agent to cross-link PEG and hydroxyl-terminated polydimethylsiloxane. Peng et al. (Solar Energy Materials and Solar Cells J. 2016, 145, 238-247) used diphenyl methane diisocyanate as cross-linking agent to prepare PEG cross-linked copolymer with β-cyclodextrin as the skeleton. The phase change material of this structure can still maintain stability under harsh environmental conditions, but due to permanent cross-linking, the material cannot be recycled and reused, which exists certain pollution and waste of resources. Therefore, it is of great significance to find a cross-linked polymer that can be recycled and reprocessed to prepare solid-solid phase change materials.
[0005] Thermosetting plastics is an important polymer material. Common phenolic resin, epoxy resin and unsaturated polyester thermosetting plastics have good dimensional stability, high heat resistance, high hardness and strong anti creep ability, and are widely used in building, household appliances, decoration, chemical industry, automobile, aerospace and other fields. However, thermosetting plastics cannot be melted or dissolved after cross linking and curing, which is difficult to be reprocessed and utilized, resulting in a large amount of waste that cannot be disposed of, thereby limiting the sustainable development and application of thermosetting plastics. Therefore, in 2011, Leibler et al. proposed the concept of reprocessable thermosetting plastics based on dynamic covalent bonds, namely glass-like materials. Since then, glass-like materials based on ester exchange, amino exchange of meta-vinyl amine ester, alkyl exchange, imine exchange, carbamate exchange and borate exchange have been reported. On this basis, solid-solid phase change materials based on glass-like materials have also attracted people's attention. Glass-like solid-solid phase change materials based on carbamate (Chem Eng J. 2022; 450, J Energy Storage. 2021; 36: 102343), disulfide bond (Energy. 2021; 232: 121070) and Diels-Alder reaction (J Mater Chem A. 2019; 7: 21802-11, Chem Eng J. 2022; 448) have been reported. However, the above glass-like solid-solid phase change materials are all based on polyurethane thermosetting plastics. Epoxy resin based thermosetting plastics are widely used high molecular materials, and epoxy resin glass-like materials based on dynamic ester exchange reaction are the first reported glass-like materials. Therefore, giving the epoxy resin glass-like materials based on dynamic ester exchange reaction with latent heat storage performance can greatly expand their application in the fields of new energy development and utilization and improving energy utilization efficiency. SUMMARY
[0006] The purpose of the present application is to provide a reprocessable epoxy resin glass-like material with latent heat storage performance and a preparation method thereof. The preparation method is simple and easy to operate, and the cost is controllable. The epoxy resin glass-like material provided by the present application not only has good latent heat storage capacity and leakage prevention performance, but also has good tensile performance and reprocessing forming characteristics, which can reduce resource waste.
[0007] In order to achieve the above technical purpose, the present application provides an epoxy resin glass-like material based on dynamic ester exchange bond with latent heat storage function, which grafts and fixes the phase change heat storage material in the glass-like material through ester exchange bond.
[0008] As a preferred scheme, the phase change heat storage material is at least one of α, ω-bis-terminal hydroxyl-containing ethylene glycol polymer, and the molecular weight of the polyethylene glycol is not limited. For example, but not limited to: polyethylene glycol 400, polyethylene glycol 2000, polyethylene glycol 4000, polyethylene glycol 8000, polyethylene glycol 10000, polyethylene glycol 20000, etc.
[0009] In order to achieve the above technical purpose, the present application provides a method for preparing a reworkable epoxy resin glass material with latent heat storage function, which is to graft and fix the phase change material in the three-dimensional crosslinked network of the epoxy resin by dynamic covalent bond. The specific preparation process is as follows: mixing bisphenol A diglycidyl ether, succinic anhydride, catalyst and polyethylene glycol and heating to melt, mixing the mixture uniformly by stirring until transparent during this period, then quickly pouring the viscous solution into a mold, curing at a certain temperature, then naturally cooling to room temperature and demolding to obtain a reworkable epoxy resin glass material with latent heat storage function.
[0010] As a preferred scheme, the amount of the phase change material accounts for 35% to 55% of the total mass of the sample. The preferred phase change material can provide more reaction sites for ester exchange, accelerate the topological rearrangement of the network, and is beneficial to the thermal processing and reshaping of the material.
[0011] As a preferred scheme, the mass of the added bisphenol A diglycidyl ether accounts for 34.73% to 50.13% of the total mass of the sample. The preferred bisphenol A diglycidyl ether is mainly used to cooperate with the curing agent to graft and anchor the phase change material in the three-dimensional network by covalent bond, preventing the leakage of the phase change material during use.
[0012] As a preferred scheme, the amount of the added succinic anhydride and bisphenol A diglycidyl ether is added according to the molar ratio of anhydride to epoxy group (0.4 to 0.6). The preferred succinic anhydride mainly serves as a bridge linking bisphenol A diglycidyl ether and the phase change material, and also reacts with bisphenol A diglycidyl ether to form a three-dimensional crosslinked network.
[0013] As a preferred scheme, the catalyst can be at least one of zinc acetate and zinc acetylacetone, and the amount of the catalyst in terms of moles is 10% of the amount of succinic anhydride. The preferred catalyst mainly promotes the ring-opening reaction of the epoxy group and the anhydride, and also controls the ester exchange reaction rate during thermal processing.
[0014] As a preferred scheme, the curing temperature is 100°C to 190°C, and the curing time is 5 to 6 hours. The staged curing is to ensure sufficient contact and mixing between the substances, and to ensure complete curing of the resin. The curing time affects the reaction degree of polyethylene glycol with anhydride and epoxy group.
[0015] The preparation method of the reworkable epoxy resin-based glass material with latent heat storage function provided by the present application is carried out according to the following specific steps:
[0016] 1) Bisphenol A diglycidyl ether, succinic anhydride, catalyst and polyethylene glycol are weighed and placed in a beaker;
[0017] 2) The beaker is heated to 100-150 DEG C and stirred to melt until the mixture is transparent;
[0018] 3) The viscous solution is quickly poured into a preheated mold at 100-150 DEG C, and cured at 100-190 DEG C for 3-6 hours, the curing procedure is: 100-130 DEG C for 1-2 hours, 140-160 DEG C for 1-2 hours, 170-190 DEG C for 1-2 hours, and then naturally cooled to room temperature and demolded to obtain the reworkable epoxy resin-based glass material with latent heat storage function.
[0019] Compared with the prior art, the technical scheme of the present application has the following beneficial technical effects:
[0020] 1) The present application provides a reworkable epoxy resin-based glass material with latent heat storage function, which greatly expands the application field of epoxy resin thermosetting plastics.
[0021] 2) The prepared reworkable epoxy resin-based glass material with latent heat storage function can be processed and reshaped by thermal processing, thereby effectively avoiding the waste of resources caused by the inability of traditional thermosetting plastics epoxy resin to be recycled.
[0022] 3) The softness of polyethylene glycol can compensate for the defects of the glass-like body in flexibility and ductility, so that it can more flexibly cope with various environments. At the same time, after grafting and anchoring polyethylene glycol to the polymer chain of the epoxy resin-based glass material, the thermal stability of polyethylene glycol can be significantly improved, and the temperature range of its application can be expanded. BRIEF DESCRIPTION OF DRAWINGS
[0023] Figure 1 The thermal analysis curve of the reworkable epoxy resin-based glass material with latent heat storage function of Examples 1-5.
[0024] Figure 2 The thermogravimetric curve of the reworkable epoxy resin-based glass material with latent heat storage function of Examples 6-10.
[0025] Figure 3 The stress-strain curve of the reworkable epoxy resin-based glass material with latent heat storage function of Example 11. DETAILED DESCRIPTION
[0026] The following will be described in further detail with polyethylene glycol 10000 as a representative phase change material in combination with specific examples, but these examples do not limit the scope of the present application.
[0027] Example 1.
[0028] Preparation of the reworkable epoxy resin-based glass material with latent heat storage function: 5.25 g of polyethylene glycol 10000, 7.52 g of bisphenol a diglycidyl ether, 1.77 g of succinic anhydride, and 0.47 g of zinc acetylacetone were taken into a 25 ml beaker, which was placed in an oil bath at 150°C and stirred to melt until the mixture became transparent, then the viscous solution was quickly poured into a mold preheated at 150°C, and cured in an oven for 3 hours. In order to ensure complete curing, the curing temperature program was set to 130°C for 1 hour, 160°C for 1 hour, and 190°C for 1 hour. After curing, it was naturally cooled to room temperature and demolded to obtain the reworkable epoxy resin-based glass material with latent heat storage function.
[0029] Heat storage test results: the phase change peak temperature was 39.57°C, and the phase change latent heat was 16 J / g.
[0030] Tensile test results: the tensile strength was 5.3 MPa, and the elongation was 22.6%.
[0031] Stability test: the material was cut into a rectangular strip and placed in a constant temperature oven at 150°C. After 3 hours, it was observed that the shape of the rectangular strip did not change and there was no liquid leakage.
[0032] Reworking test: the material was cut into small particles and placed in a vulcanizing machine at 190°C and a pressure of 10 MPa for 1 hour. The small particle material could be hot pressed into a whole piece of material.
[0033] Example 2.
[0034] Preparation of the reworkable epoxy resin-based glass material with latent heat storage function: 6 g of polyethylene glycol 10000, 6.94 g of bisphenol a diglycidyl ether, 1.61 g of succinic anhydride, and 0.3 g of zinc acetate were taken into a 25 ml beaker, which was placed in an oil bath at 100°C and stirred to melt until the mixture became transparent, then the viscous solution was quickly poured into a mold preheated at 100°C, and cured in an oven for 6 hours. In order to ensure complete curing, the curing temperature program was set to 100°C for 2 hours, 140°C for 2 hours, and 170°C for 2 hours. After curing, it was naturally cooled to room temperature and demolded to obtain the reworkable epoxy resin-based glass material with latent heat storage function.
[0035] Heat storage test results: the phase change peak temperature was 45.04°C, and the phase change latent heat was 27.1 J / g.
[0036] Tensile test result: tensile strength is 9.5 MPa, elongation is 25.7%.
[0037] Stability test: cut the material into rectangular strips, put it into a constant temperature oven at 150°C, after 3 hours, observe that the shape of the rectangular strip does not change and there is no liquid leakage.
[0038] Reprocessing test: cut the material into small particles, and then put it into a vulcanizing machine, heat press at 190°C and 10 MPa pressure for 1 hour, the small particle material can be hot pressed into a whole material.
[0039] Example 3.
[0040] Preparation of reworkable epoxy resin-based glass material with latent heat storage function: take 6.75 g of polyethylene glycol 10000, 6.36 g of bisphenol a diglycidyl ether, 1.49 g of succinic anhydride and 0.39 g of zinc acetylacetone into a 25 ml beaker, put it into an oil bath at 120°C and stir to melt until the mixture is transparent, then quickly pour the viscous solution into a preheated mold at 120°C, solidify in an oven for 6 hours, in order to ensure complete solidification, the solidification temperature program is set to 120°C for 2 hours, 150°C for 2 hours, 180°C for 2 hours, after solidification, naturally cool to room temperature and demold to get a reworkable epoxy resin-based glass material with latent heat storage function.
[0041] Heat storage test result: phase change peak temperature is 45.96°C, phase change latent heat is 37 J / g.
[0042] Tensile test result: tensile strength is 9.78 MPa, elongation is 26.6%.
[0043] Stability test: cut the material into rectangular strips, put it into a constant temperature oven at 150°C, after 3 hours, observe that the shape of the rectangular strip does not change and there is no liquid leakage.
[0044] Reprocessing test: cut the material into small particles, and then put it into a vulcanizing machine, heat press at 190°C and 10 MPa pressure for 1 hour, the small particle material can be hot pressed into a whole material.
[0045] Example 4.
[0046] Preparation of reworkable epoxy resin-based glass material with latent heat storage function: 7.5 g of polyethylene glycol 10000, 5.79 g of bisphenol a diglycidyl ether, 1.36 g of succinic anhydride and 0.36 g of zinc acetylacetone were taken into a 25 ml beaker, which was placed in an oil bath at 120°C and stirred to melt until the mixture became transparent, then the viscous solution was quickly poured into a preheated mold at 120°C, and cured in an oven for 6 hours, in order to ensure complete curing, the curing temperature program was set as 120°C for 2 hours, 150°C for 2 hours, 180°C for 2 hours, and after curing, it was naturally cooled to room temperature and demolded to obtain a reworkable epoxy resin-based glass material with latent heat storage function.
[0047] Heat storage test results: the phase change peak temperature is 46.97°C, and the phase change latent heat is 45.9 J / g.
[0048] Tensile test results: tensile strength is 8.36 MPa, elongation is 17.5%.
[0049] Stability test: cut the material into a rectangular strip and put it into a constant temperature oven at 150°C, after 3 hours, observe that the shape of the rectangular strip does not change and there is no liquid leakage.
[0050] Reworking test: cut the material into small particles, and then put it into a vulcanizing machine, heat and press at 190°C and a pressure of 10 MPa for 1 hour, the small particle material can be hot pressed into a whole piece of material.
[0051] Example 5.
[0052] Preparation of reworkable epoxy resin-based glass material with latent heat storage function: 7.5 g of polyethylene glycol 10000, 5.79 g of bisphenol a diglycidyl ether, 1.36 g of succinic anhydride and 0.36 g of zinc acetylacetone were taken into a 25 ml beaker, which was placed in an oil bath at 120°C and stirred to melt until the mixture became transparent, then the viscous solution was quickly poured into a preheated mold at 120°C, and cured in an oven for 6 hours, in order to ensure complete curing, the curing temperature program was set as 120°C for 2 hours, 150°C for 2 hours, 180°C for 2 hours, and after curing, it was naturally cooled to room temperature and demolded to obtain a reworkable epoxy resin-based glass material with latent heat storage function.
[0053] Heat storage test results: the phase change peak temperature is 46.97°C, and the phase change latent heat is 45.9 J / g.
[0054] Tensile test results: tensile strength is 8.36 MPa, elongation is 17.5%.
[0055] Stability test: cut the material into a rectangular strip and put it into a constant temperature oven at 150°C, after 3 hours, observe that the shape of the rectangular strip does not change and there is no liquid leakage.
[0056] Reprocessing test: The material was cut into small particles and placed in a vulcanizing machine at 190°C and 10 MPa pressure for 1 hour. The small particle material could be hot-pressed into a whole piece of material.
[0057] Example 6.
[0058] Preparation of a reprocessable epoxy resin-based glass material with latent heat storage function: 5.25 g of polyethylene glycol 10000, 7.52 g of bisphenol a diglycidyl ether, 1.77 g of succinic anhydride, and 0.47 g of zinc acetylacetone were taken into a 25 ml beaker, which was placed in an oil bath at 120°C and stirred to melt until the mixture became transparent. Then the viscous solution was quickly poured into a preheated mold at 120°C. The mold was cured in an oven for 5 hours. To ensure complete curing, the curing temperature program was set to 120°C for 1 hour, 150°C for 2 hours, and 180°C for 2 hours. After curing, the mold was naturally cooled to room temperature and demolded to obtain a reprocessable epoxy resin-based glass material with latent heat storage function.
[0059] Heat storage test results: the phase change peak temperature was 39.21°C, and the phase change latent heat was 2.4 J / g.
[0060] Tensile test results: the tensile strength was 5.64 MPa, and the elongation was 23.4%.
[0061] Stability test: the material was cut into a rectangular strip and placed in a constant temperature oven at 150°C. After 3 hours, it was observed that the shape of the rectangular strip did not change and there was no liquid leakage.
[0062] Reprocessing test: The material was cut into small particles and placed in a vulcanizing machine at 190°C and 10 MPa pressure for 1 hour. The small particle material could be hot-pressed into a whole piece of material.
[0063] Example 7.
[0064] Preparation of a reprocessable epoxy resin-based glass material with latent heat storage function: 5.25 g of polyethylene glycol 10000, 7.52 g of bisphenol a diglycidyl ether, 1.77 g of succinic anhydride, and 0.47 g of zinc acetylacetone were taken into a 25 ml beaker, which was placed in an oil bath at 120°C and stirred to melt until the mixture became transparent. Then the viscous solution was quickly poured into a preheated mold at 120°C. The mold was cured in an oven for 5 hours. To ensure complete curing, the curing temperature program was set to 120°C for 1 hour, 150°C for 2 hours, and 180°C for 2 hours. After curing, the mold was naturally cooled to room temperature and demolded to obtain a reprocessable epoxy resin-based glass material with latent heat storage function.
[0065] Heat storage test results: the phase change peak temperature was 47.15°C, and the phase change latent heat was 29.2 J / g.
[0066] Tensile test result: tensile strength is 7.53 MPa, elongation is 23%.
[0067] Stability test: cut the material into rectangular strips, put it into a constant temperature oven at 150°C, after 3 hours, observe that the shape of the rectangular strip does not change and there is no liquid leakage.
[0068] Reprocessing test: cut the material into small particles, and then put it into a vulcanizing machine, heat press at 190°C and 10 MPa pressure for 1 hour, the small particle material can be hot pressed into a whole material.
[0069] Example 8.
[0070] Preparation of reworkable epoxy resin-based glass material with latent heat storage function: take 6.75 g of polyethylene glycol 10000, 6.36 g of bisphenol a diglycidyl ether, 1.49 g of succinic anhydride and 0.39 g of zinc acetylacetone into a 25 ml beaker, put it into an oil bath at 120°C and stir to melt until the mixture is transparent, then quickly pour the viscous solution into a preheated mold at 120°C, and solidify in an oven for 5 hours. In order to ensure complete solidification, the solidification temperature program is set to 120°C for 1 hour, 150°C for 2 hours, and 180°C for 2 hours. After solidification, naturally cool to room temperature and demold to obtain a reworkable epoxy resin-based glass material with latent heat storage function.
[0071] Heat storage test result: phase change peak temperature is 50.17°C, phase change latent heat is 45.7 J / g.
[0072] Tensile test result: tensile strength is 8.88 MPa, elongation is 29.26%.
[0073] Stability test: cut the material into rectangular strips, put it into a constant temperature oven at 150°C, after 3 hours, observe that the shape of the rectangular strip does not change and there is no liquid leakage.
[0074] Reprocessing test: cut the material into small particles, and then put it into a vulcanizing machine, heat press at 190°C and 10 MPa pressure for 1 hour, the small particle material can be hot pressed into a whole material.
[0075] Example 9.
[0076] Preparation of reworkable epoxy resin-based glass material with latent heat storage function: 7.5 g of polyethylene glycol 10000, 5.79 g of bisphenol a diglycidyl ether, 1.36 g of succinic anhydride and 0.36 g of zinc acetylacetone were taken into a 25 ml beaker, which was placed in an oil bath at 120°C and stirred to melt until the mixture became transparent, then the viscous solution was quickly poured into a preheated mold at 120°C, and cured in an oven for 5 hours, in order to ensure complete curing, the curing temperature program was set to 120°C for 1 hour, 150°C for 2 hours, 180°C for 2 hours, and then naturally cooled to room temperature after curing, and then demolded to obtain a reworkable epoxy resin-based glass material with latent heat storage function.
[0077] Heat storage test results: the phase change peak temperature is 51°C, and the phase change latent heat is 51.4 J / g.
[0078] Tensile test results: tensile strength is 8.48 MPa, elongation is 22.1%.
[0079] Stability test: cut the material into a rectangular strip and place it in a constant temperature oven at 150°C, after 3 hours, observe that the rectangular strip shape has not changed and there is no liquid leakage.
[0080] Reworking test: cut the material into small particles, and then place it in a vulcanizing machine, heat and press at 190°C and a pressure of 10 MPa for 1 hour, the small particle material can be hot-pressed into a whole piece of material.
[0081] Example 10.
[0082] Preparation of reworkable epoxy resin-based glass material with latent heat storage function: 7.5 g of polyethylene glycol 10000, 5.79 g of bisphenol a diglycidyl ether, 1.36 g of succinic anhydride and 0.36 g of zinc acetylacetone were taken into a 25 ml beaker, which was placed in an oil bath at 120°C and stirred to melt until the mixture became transparent, then the viscous solution was quickly poured into a preheated mold at 120°C, and cured in an oven for 5 hours, in order to ensure complete curing, the curing temperature program was set to 120°C for 1 hour, 150°C for 2 hours, 180°C for 2 hours, and then naturally cooled to room temperature after curing, and then demolded to obtain a reworkable epoxy resin-based glass material with latent heat storage function.
[0083] Heat storage test results: the phase change peak temperature is 52.6°C, and the phase change latent heat is 63.2 J / g.
[0084] Tensile test results: tensile strength is 7.58 MPa, elongation is 9.5%.
[0085] Stability test: cut the material into a rectangular strip and place it in a constant temperature oven at 150°C, after 3 hours, observe that the rectangular strip shape has not changed and there is no liquid leakage.
[0086] Reprocessing test: The material was cut into small particles and placed in a vulcanizing machine and hot-pressed at 190°C under a pressure of 10 MPa for 1 hour. The small particle material cut into pieces could be hot-pressed into a whole material.
[0087] Example 11.
[0088] Preparation of a reprocessable epoxy resin-based glass material with latent heat storage function: 7.5 g of polyethylene glycol 10000, 5.19 g of bisphenol a diglycidyl ether, 1.83 g of succinic anhydride, and 0.48 g of zinc acetylacetone were taken into a 25 ml beaker, which was placed in an oil bath at 120°C and stirred to melt until the mixture became transparent. Then the viscous solution was quickly poured into a preheated mold at 120°C. The mold was cured in an oven for 6 hours. To ensure complete curing, the curing temperature program was set to 120°C for 2 hours, 150°C for 2 hours, and 180°C for 2 hours. After curing, the mold was naturally cooled to room temperature and demolded to obtain a reprocessable epoxy resin-based glass material with latent heat storage function.
[0089] Heat storage test results: the phase change peak temperature was 49.2°C, and the phase change latent heat was 38.35 J / g.
[0090] Tensile test results: the tensile strength was 9.78 MPa, and the elongation was 29.7%.
[0091] Stability test: the material was cut into a rectangular strip and placed in a constant temperature oven at 150°C. After 3 hours, it was observed that the shape of the rectangular strip did not change and there was no liquid leakage.
[0092] Reprocessing test: The material was cut into small particles and placed in a vulcanizing machine and hot-pressed at 190°C under a pressure of 10 MPa for 1 hour. The small particle material cut into pieces could be hot-pressed into a whole material.
[0093] Example 12.
[0094] Preparation of a reprocessable epoxy resin-based glass material with latent heat storage function: 7.5 g of polyethylene glycol 10000, 5.19 g of bisphenol a diglycidyl ether, 1.83 g of succinic anhydride, and 0.48 g of zinc acetylacetone were taken into a 25 ml beaker, which was placed in an oil bath at 120°C and stirred to melt until the mixture became transparent. Then the viscous solution was quickly poured into a preheated mold at 120°C. The mold was cured in an oven for 6 hours. To ensure complete curing, the curing temperature program was set to 120°C for 2 hours, 150°C for 2 hours, and 180°C for 2 hours. After curing, the mold was naturally cooled to room temperature and demolded to obtain a reprocessable epoxy resin-based glass material with latent heat storage function.
[0095] Heat storage test results: the phase change peak temperature was 49.2°C, and the phase change latent heat was 38.35 J / g.
[0096] Tensile test results: tensile strength of 9.58 MPa, elongation of 25.4%.
[0097] Stability test: cut the material into rectangular strips, put into a constant temperature oven at 150°C, after 3 hours, observe that the shape of the rectangular strips has not changed and there is no liquid leakage.
[0098] Reprocessing test: cut the material into small particles, and then put them into a vulcanizing machine and heat press at 190°C under a pressure of 10 MPa for 1 hour. The small particle materials can be heat pressed into a whole piece of material.
Claims
1. A reprocessable epoxy resin glass material with latent heat storage function, characterized in that: The glass-like material is composed of an epoxy resin cross-linked framework grafted with a phase change thermal storage material, and can be further processed by hot pressing. The phase change thermal storage material is at least one type of polyethylene glycol containing α,ω-di-terminated hydroxyl groups. The reprocessable epoxy resin glass-like material with latent heat storage function is prepared as follows: Bisphenol A diglycidyl ether, succinic anhydride, catalyst, and polyethylene glycol are mixed and stirred at 100℃~150℃ until the mixture becomes transparent. Then, the viscous solution is quickly poured into a mold preheated at 100℃~150℃ and cured. After naturally cooling to room temperature, it is demolded to obtain the final product. The amount of polyethylene glycol is 35% to 55% of the total sample mass, the amount of bisphenol A diglycidyl ether is 31.13% to 50.13% of the total sample mass, the molar ratio of succinic anhydride to bisphenol A diglycidyl ether is 0.4 to 0.6, the molar amount of catalyst is 5% to 20% of the molar amount of succinic anhydride, and the catalyst is at least one of zinc acetate or zinc acetylacetonate; the curing procedure is curing at 100℃ to 130℃ for 1 to 2 hours, curing at 140℃ to 160℃ for 1 to 2 hours, and curing at 170℃ to 190℃ for 1 to 2 hours.
Citation Information
Patent Citations
Method for preparing polyethylene glycol and epoxy resin formed composite phase-change materials
CN101230256A