CN1587339A - Porous graphite base phase change energy storage composite material and its preparing method - Google Patents
Porous graphite base phase change energy storage composite material and its preparing method Download PDFInfo
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- CN1587339A CN1587339A CN 200410052870 CN200410052870A CN1587339A CN 1587339 A CN1587339 A CN 1587339A CN 200410052870 CN200410052870 CN 200410052870 CN 200410052870 A CN200410052870 A CN 200410052870A CN 1587339 A CN1587339 A CN 1587339A
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Abstract
The present invention relates to one kind of composite porous graphite base phase change energy-storing material and its preparation process. The composite phase change energy-storing material has porous graphite as base material and is prepared through soaking organic phase change material. The porous graphite is prepared with natural flake graphite and through intercalation, swelling and compression. The organic phase change material is crystallized fatty acid, alkane, ester or their mixture. Compared with available composite phase change energy-storing material, the composite porous graphite base phase change energy-storing material has the advantages of high heat conducting efficiency, great energy storing amount, etc. The present invention can promote the application of phase change energy-storing material in various application fields.
Description
Technical field
The invention belongs to the energy-storage composite material field, be specifically related to a kind of porous graphite base phase-change energy-storage composite material and preparation method thereof that is.
Background technology
Energy storage is got up to be used for to satisfy At All Other Times or the energy requirement in place, significant values is all arranged for the utilization of eliminating inharmonic contradiction between power supply and demand, raising energy use efficiency and renewable energy source.Utilize material energy-absorbing and the characteristics of releasing energy in phase transition process, realize that the storage of energy and utilization are one of directions of enlivening in recent years in various fields such as the energy, material, aerospace, weaving, electric power, medical instrument, building.Phase-change accumulation energy has advantages such as energy storage density height, energy storage easy control of temperature and range of choice are wide, practicability and commercialization stage have been entered in some fields at present, as having adopted based on LiF-CaF in the solar thermal machine power generating system on the Freedom space station of US Airways Space Agency (NASA)
2The heat reservoir of excellent attitude salt phase-changing energy storage material is to satisfy the without interruption of no photophase electric power; At garment industry, commercialization phase-change energy-storage fibre-Outlast fiber has appearred, the heat that human body distributes can be collected and store to dress-goods by this fibrous woven manufacturing, improves the warming ability of clothes, has more application aspect sportwear and the extreme environment clothes.
The phase-changing energy storage material kind is a lot, can be divided into organic phase change material and inorganic phase-changing material by substance classes, can be divided into solid-liquid phase change material, solid-solid phase change material, solid and gas phase change material and liquid-gas phase transition material etc. by the phase transition process form.Attempt adopting phase-changing energy storage material to reduce building energy consumption at building field long history has been arranged.From the thirties in last century, just the someone explores and adopt phase change material in the heating buildings system on America and Europe and other places, comprises organic phase change material and inorganic phase-changing material.First relevant patent [US 2 342 211 (1944)]-phase-change accumulation energy refrigeration and warmer appearred.In 1948, doctor Telkes of masschusetts, u.s.a engineering college built first experiment room-Dover House that utilizes phase-changing energy storage material to store and utilize sun power.The energy dilemma of the seventies has further promoted the research and development of energy utilization technology.The research and development of phase-changing energy storage material are changed into by state organization by the loose behavior that has color among the people, even international organization's united and coordinating.Nineteen eighty-two, the Ministry of Energy of the U.S. at first started the R﹠D work of this respect.In recent years, (International EnergyAgency IEA) has also carried out research and application plan (Annex10 and 17) that phase-changing energy storage material uses to International Energy Agency aspect building energy saving field, some developed countries participate in by Europe, the United States, day etc.Obtained some achievements in succession, various organic phase changing matters have been encapsulated in the polymkeric substance such as high-density polyethylene, polyacetal and polyureas as adopting encapsulation technology, the preparation shape is the fixed phase change material relatively; Or adopt macromolecular materials such as crosslined polyacetal and cellulose graft copolymer to prepare phase change material.Make a general survey of the applicable cases of present phase-changing energy storage material in building energy conservation, mainly there are the following problems:
(1) heat conductivility is not good: because at present the thermal conductivity of the body material that adopts is generally less than normal, cause the heat conduction heat exchange property of phase-change energy-storage composite material in phase transition process very poor, influenced its energy storage-release can efficient.
(2) energy storage capacity is low: because the porous medium porosity is less, it is less that matrix material includes phase change material, causes the energy storage capacity of matrix material on the low side.
Summary of the invention
The objective of the invention is to propose a kind of good heat conductivity, energy-storage composite material that energy storage capacity is high and preparation method thereof.
The energy-storage composite material that the present invention proposes adopts porous graphite as body material, and the organic phase change material that infiltrates again constitutes.Wherein porous graphite is to be prepared from through intercalation, expanded, condensing routine by natural flake graphite; Organic phase change material comprises a kind of of organic materialss such as crystallinity straight chain fatty acid, alkane, ester class and composition thereof.
The present invention is a porous graphite base phase-change energy-storage composite material.Because porous graphite has very high thermal conductivity and porosity, can effectively overcome problems such as ubiquitous heat conductivility difference of present phase-change energy-storage composite material and energy storage capacity are low.
The preparation of above-mentioned porous graphite base phase-change energy-storage composite material comprises following two steps:
(1) preparation of porous graphite
(a) intercalation: with the natural flake graphite is starting material, adopts thermochemical method that it is carried out intercalation processing.Adopt the vitriol oil and potassium permanganate respectively as intercalator and oxygenant.The crystalline flake graphite of cleaning oven dry is mixed stirring heating certain hour under the water bath with thermostatic control condition with intercalator, oxygenant etc.Filtration and water washed mixture are to certain pH value then.Again this mixture being put into baking oven dries.The intercalation temperature is controlled between 25～60 ℃.The weight ratio of mixture is got following scope: graphite: intercalator: oxygenant=1: 3～10: 0.1～1.The stirring heating time gets in 20 minutes to 60 minutes scopes.Washing pH value gets 0～3.Bake out temperature is got 60～80 ℃, drying time 6～12 hours.
(b) expanded: as to adopt microwave method expanded graphite intercalation thing.At first take by weighing a certain amount of graphite intercalation compound, put into terrine, then terrine is put into common microwave stove and carried out expanded.Desirable 200～the 2000ml of terrine volume.Expanded power is taken in 100～800W scope, and the expanded time got 10～30 seconds.
(c) compression: expanded graphite is put into pipe or square tube, with expanded graphite in the piston extruded tube identical of section area in section area and shape and the pipe with shape to compression ratio necessarily.Generally getting compression ratio is 0.1～0.5 of graphite expansion ratio.
(2) organic phase change material can adopt a kind of of following two kinds of infiltration methods to the infiltration of porous graphite:
(a) common infiltration: this method is simple.Directly porous graphite is immersed in the organic phase change material.Soak time can be between 30 minutes to 24 hours.Soak the back and take out porous graphite, clean its surface.Adopt polymer matrix composite to add the sealing rete then on the porous graphite surface.Can select the body material as sealing rete matrix material such as resin, emulsion for use, adopt high metal of thermal conductivity or non-metal powder filler as the rete matrix material.
(b) vacuum infiltration: at first adopt the method vacuumize to extract air in the porous graphite, vacuum is pressed must be higher than 80kPa, and the pumpdown time was greater than 30 minutes (as 30-40 minute).Then, under vacuum environment,, remove vacuum, continue to soak more than 1 hour (for example 1-3 hour), take out porous graphite, clean its surface, and add the sealing rete on its surface with organic phase changing matter soaked with liquid porous graphite.Compare with common infiltration, vacuum infiltration method cost is higher, but required time shortens greatly, and the infiltration effect significantly improves.
Compare with existing phase-change energy-storage composite material, porous graphite base phase-change energy-storage composite material has advantages such as the big and electrically heated accumulation of heat of heat transfer efficiency height, energy storage capacity, can effectively promote the application of phase-change energy-storage composite material at numerous areas.
Embodiment
Embodiment 1
Get fineness and be 80 orders, carbon content and be 90% crystalline flake graphite 30 grams, concentration and be 98% sulfuric acid 300 grams and potassium permanganate 20 grams, put into Glass Containers and mix.Then this Glass Containers is put into water bath with thermostatic control, the temperature of water-bath is set at 45 ℃.Mixture is continued to stir, stir RPM and be decided to be 300.Carry out water wash procedures behind the intercalation.Mixture is filtered with 200 purpose stainless (steel) wires, will filter residuum then and put into beaker, add clear water and covered mixture, fully stir with glass stick, and then filter with 200 purpose stainless (steel) wires.Twice of repeated washing.The pH value of measuring last stirring liquid is 2.Last filtering residuum is put into the glass pallet, put into baking oven then and dry.Oven temperature is 60 ℃, and drying time is 10 hours.Get the good graphite intercalation compound of oven dry 5 grams, put into terrine, then terrine is put into microwave oven.With the power setting of microwave oven on 200W.Start microwave oven, the microwave time of origin is 30 seconds.Then expanded graphite is put into compressed pipe and push, press ratio is 0.2 of a rate of expansion.Adopt common infiltration method, the porous graphite material that compression is good is immersed in the alkane organic phase change material 12 hours.Take out, clean its surface, and adopt Resins, epoxy to make seal coating on the porous graphite surface.In Resins, epoxy, add aluminium powder.
Embodiment 2
Get fineness and be 50 orders, carbon content and be 94% crystalline flake graphite 30 grams, concentration and be 98% sulfuric acid 300 grams and potassium permanganate 20 grams, put into Glass Containers and mix.Then this Glass Containers is put into water bath with thermostatic control, the temperature of water-bath is set at 45 ℃.Mixture is continued to stir, stir RPM and be decided to be 300.Carry out water wash procedures behind the intercalation.Mixture is filtered with 200 purpose stainless (steel) wires, will filter residuum then and put into beaker, add clear water and covered mixture, fully stir with glass stick, and then filter with 200 purpose stainless (steel) wires.Repeated washing 3 times.The pH value of measuring last stirring liquid is 4.Last filtering residuum is put into the glass pallet, put into baking oven then and dry.Oven temperature is 60 ℃, and drying time is 10 hours.Get the good graphite intercalation compound of oven dry 5 grams, put into terrine, then terrine is put into microwave oven.With the power setting of microwave oven on 200W.Start microwave oven, the microwave time of origin is 30 seconds.Then expanded graphite is put into compressed pipe and push, press ratio is 0.2 of a rate of expansion.Adopt the vacuum infiltration method, immerse organic phase change material-crystallinity straight chain fatty acid mixture at the porous graphite material.Vacuum is pressed and is 82kPa, and the pumpdown time is 40 minutes, and soak time is 1.5 hours.Take out, clean its surface, and adopt Resins, epoxy to make seal coating on the porous graphite surface.In Resins, epoxy, add aluminium powder.
Embodiment 3
Get fineness and be 80 orders, carbon content and be 90% crystalline flake graphite 30 grams, concentration and be 98% sulfuric acid 300 grams and potassium permanganate 20 grams, put into Glass Containers and mix.Then this Glass Containers is put into water bath with thermostatic control, the temperature of water-bath is set at 60 ℃.Mixture is continued to stir, stir RPM and be decided to be 300.Carry out water wash procedures behind the intercalation.Mixture is filtered with 200 purpose stainless (steel) wires, will filter residuum then and put into beaker, add clear water and covered mixture, fully stir with glass stick, and then filter with 200 purpose stainless (steel) wires.Repeated washing 4 times.The pH value of measuring last stirring liquid is 6.Last filtering residuum is put into the glass pallet, put into baking oven then and dry.Oven temperature is 60 ℃, and drying time is 10 hours.Get the good graphite intercalation compound of oven dry 5 grams, put into terrine, then terrine is put into microwave oven.With the power setting of microwave oven on 200W.Start microwave oven, the microwave time of origin is 30 seconds.Then expanded graphite is put into compressed pipe and push, press ratio is 0.2 of a rate of expansion.Adopt the vacuum infiltration method, immerse organic phase change material-crystallinity straight chain fatty acid mixture at the porous graphite material.Vacuum is pressed and is 82kPa, and the pumpdown time is 30 minutes, and soak time is 2 hours.Take out, clean its surface, and adopt acrylic resin to make seal coating on the porous graphite surface.In acrylic resin, add aluminium powder.
Claims (2)
1, a kind of porous graphite base phase-change energy-storage composite material is characterized in that adopting porous graphite as body material, and the organic phase change material that infiltrates again constitutes; Wherein, porous graphite by natural flake graphite through intercalation, expanded, the compression be prepared from, organic phase change material is a kind of of crystallinity lipid acid, alkane, ester class and composition thereof.
2, a kind of preparation method of porous graphite base phase-change energy-storage composite material as claimed in claim 1 is characterized in that step is as follows:
(1) preparation of porous graphite
(a) intercalation: with the natural flake graphite is starting material, adopt thermochemical method that it is carried out intercalation processing: to adopt the vitriol oil and potassium permanganate respectively as intercalator and oxygenant, the crystalline flake graphite of cleaning oven dry is mixed with intercalator, oxygenant etc., and the weight proportion of mixture is: graphite: intercalator: oxygenant=1: 3～10: 0.1～1; Under 25-60 ℃ of water bath with thermostatic control condition stirring heating 20-60 minute; Filtration and water washed mixture to pH value are 0-3 then; Again this mixture being put into baking oven dries;
(b) expanded: as to adopt microwave method expanded graphite intercalation thing: at first take by weighing a certain amount of graphite intercalation compound, put into terrine, then terrine is put into microwave oven and carried out expanded.Expanded power is 100～800W, and the expanded time is 10～30 seconds;
(c) compression: expanded graphite is put into pipe or square tube, and with expanded graphite in the piston extruded tube, compression ratio is 0.1～0.5 of a graphite expansion ratio;
(2) organic phase change material adopts a kind of of following infiltration method to the infiltration of porous graphite:
(a) common infiltration: directly porous graphite is immersed in the organic phase change material, soak time is 30 minutes to 24 hours; Soak the back and take out porous graphite, clean its surface.Adopt polymer matrix composite to add the sealing rete then on the porous graphite surface;
(b) vacuum infiltration: at first adopt the method vacuumize to extract air in the porous graphite, vacuum is pressed be higher than 80kPa, then, under vacuum environment, use organic phase changing matter soaked with liquid porous graphite, remove vacuum, continue to soak more than 1 hour, take out porous graphite, clean its surface, and add the sealing rete on its surface.
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| CN101928551A (en) * | 2010-07-15 | 2010-12-29 | 盐城师范学院 | Higher alcohols co-blending composite phase change energy storage material and preparation method thereof |
| CN101693823B (en) * | 2009-10-28 | 2011-07-27 | 哈尔滨工业大学 | Method for preparing energy-storing materials through using phase-change materials to fill graphitized foam carbon |
| CN102505574A (en) * | 2011-10-21 | 2012-06-20 | 中国科学院合肥物质科学研究院 | Intelligent energy-saving graphene oxide composite paper and preparation method thereof |
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| CN103374338A (en) * | 2012-04-17 | 2013-10-30 | 夏华松 | Porous large-flake graphite based phase-changed energy storage composite and preparation method thereof |
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| FR2710553B1 (en) * | 1993-09-30 | 1995-11-10 | Elf Aquitaine | Method for producing an active composite. |
| CN1140146A (en) * | 1995-07-10 | 1997-01-15 | 苗常岚 | Process for producing expandable sulfur-free graphite |
| DE19630073B4 (en) * | 1996-07-25 | 2004-04-01 | Sgl Carbon Ag | Device for storing heat or cold in a storage system made of pressed graphite expandate and a solid-liquid phase change material and method for its production |
| DE10023572A1 (en) * | 2000-05-15 | 2001-11-22 | Merck Patent Gmbh | Process for producing a storage system for storing heat and cold |
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| CN101693823B (en) * | 2009-10-28 | 2011-07-27 | 哈尔滨工业大学 | Method for preparing energy-storing materials through using phase-change materials to fill graphitized foam carbon |
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