CN101348708A - Preparation of organic inorganic composite phase-change material - Google Patents
Preparation of organic inorganic composite phase-change material Download PDFInfo
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Abstract
The invention relates to a method for preparing an organic and inorganic composite phase-transition material. The method comprises the following steps: firstly, inorganic porous minerals are added into a reaction kettle; and secondly, the reaction kettle is vacuumized and injected with an organic material and then pumped into the state of negative pressure, and the temperature and the stirring speed are required to be adequately controlled during the reaction process. The method takes the inorganic porous mineral materials as a carrier for vacsorb of organic phase-transition materials which accord with the phase-transition requirements; the composite phase-transition material product prepared has the characteristics of no leakage, inflaming retarding, high phase-transition potential, easily controllable phase-transition temperature and so on; and the preparation method has a simple technology and low cost, has no secondary pollution, and is suitable for flow production and industrial production.
Description
Technical field
The present invention relates to the energy-saving building materials field, relate in particular to organic inorganic composite phase-change material that is used for building field and preparation method thereof with phase-changing and temperature-regulating function.
Background technology
In recent years, problems such as fossil energy exhaustion and environmental pollution are more and more outstanding, and improving energy use efficiency and developing renewable energy source becomes the important topic that the mankind face.(Phase Change Materials PCM) can absorb or discharge a large amount of latent heat to phase change material in phase transition process, can be widely used in heat and store and domain of control temperature, is developed rapidly in American-European countries over nearly 20 years.Phase-change energy-storage composite material is a kind of hot merit energy matrix material, the form of energy with latent heat of phase change can be stored in its carrier, realizes the conversion of energy between different space-time positions.Utilizing the latent heat of phase change of phase change material to realize the storage and the utilization of energy, help to improve efficiency and exploitation renewable energy source, is very active forward position research direction in energy science and the material science in recent years.
In phase transition process, phase-changing energy storage material and environment carry out energy exchange, reach the purpose of control environment temperature and energy utilization.Compare with the sensible heat energy storage, phase-change accumulation energy has that energy storage density height, volume are small and exquisite, temperature control is constant, energy-saving effect significantly, the transformation temperature range of choice is wide, be easy to advantage such as control, has important use value and wide prospect in various fields such as aerospace, sun power utilization, heating and air-conditioning, power supply system optimization, engineering in medicine, military engineering, accumulation of heat building and extreme environment clothes.Organic phase change material is some alcohol, acid, higher alkane etc. normally.Problems such as these materials have suitable transformation temperature and higher latent heat and nontoxic, non-corrosiveness, it is cold not have, no layering, stability is strong, and the phase transition process good reversibility is adapted at using in the building field.The organism that is used as solid-liquid phase change is owing to functional group's difference, so they are differing greatly in nature.Shortcoming is poor thermal conductivity, price height, and some material can burn when high temperature or strong oxidizer exist, decomposition etc., therefore will be selected, to guarantee safety.
At present, phase change material generally adopts the solid-liquid phase change material, so the encapsulation of phase change material is most important.There is great number of issues in the phase change material storing technology, comprises the leakage problem of phase change material, the endurance issues of encapsulation and the heat exchange efficiency problem of phase transition process etc.If phase change material leaks out from metal or plastic containers, can cause problems such as energy-storage function deterioration and environmental pollution, and phase change material is if use with bigger bulk form, its heat exchange effect is inevitable not good, cause phase transition process incomplete, or need just can finish phase transformation for a long time, cause the on the low side or energy wastage of phase change material utilization ratio, reduced the utility value of latent heat of phase change energy storage.
From the process of the encapsulation technology of phase change material development, the main employing carried out phase change material and other body materials compound, makes phase-change energy-storage composite material.Three kinds of methods are arranged substantially: direct infusion method, microcapsule method and porous inorganic carrier composite algorithm.
By phase-change energy-storage composite material with phase change material and the compound preparation dimensionally stable of other materials, can not need container to load, thereby reduce unit thermal energy storage expense, had Many researchers directly to absorb phase change material and prepared phase-change energy-storage composite material with traditional building material.Initial research is mainly direct infusion method.Advantage is that technology is simple, is easy to existing material of construction is improved.But the compatibility problem of phase change material and body material is difficult to effective solution all the time.The weather resistance of phase-change energy-storage composite material is its widely used factor of restriction all the time, comprise that repeatedly decline, the phase change material of phase transformation circulation back thermophysical property leak phase change material, the phase change material carrier destroys, the phase change material thermophysical property begins to degenerate after solidifying circulation repeatedly fusing one.
In recent years, a kind of method that adopts porous medium as the phase change material encapsulation medium has also appearred.Adopting porous medium is a kind of new organic phase changing matter method for packing that occurs in the phase change energy storage technology field in recent years as the storage medium of organic phase changing matter, many porous mediums have very high porosity on the one hand, can store a large amount of organic phase changing matters reliably, the opposing party and, porous medium is stored at the organic phase changing matter differentiation in the tiny hole, can improve its phase-change heat-exchange efficient.The transformation behavior of organic phase changing matter in porous medium will inevitably be subjected to constraint of restrictive orifice spatial and adjusting in the porous medium, presents the transformation behavior that is different under the free state.
Porous medium is of a great variety, has to change abundant space, hole, is phase change material ideal storage medium.Alternative porous medium comprises gypsum, swelling clay, pearlstone, expansion leaf rock, cellular concrete etc.Adopt porous medium can make matrix material have the advantage of structure-function integration as the packaged material of phase change material, can conserve space on using, have excellent economy.The hole of porous medium inside is very tiny, can improve the storage reliability of phase change material in porous medium by capillary effect.Porous medium also is separated into phase change material tiny individuality, effectively improves the heat exchange efficiency of its phase transition process.
CN101121876 " a kind of method of utilizing pearlstone to prepare composite phase-change material ", CN101096298 " organic phase-change composite expanding perlite and preparation method thereof " has introduced the porous medium pearlstone and has been used to pack the method that organic phase change material forms inorganic-organic composite phase-change material, mainly be earlier porous support to be heated place to go moisture content in advance, join in the reactor together with organic phase change material then, be evacuated to reaction pressure, sample is taken out in reaction at last while stirring.It makes technology become complicated owing to needing earlier porous medium to be preheated, in addition, because the pressure in the reactor is directly to be reduced to peak suction, it is cracked to cause porous medium to be easy in the whipping process under peak suction, granularity diminishes, porous medium is reduced the adsorptive capacity of organic materials, thereby cause the phase transformation potential of inorganic-organic composite phase-change material of obtaining to be affected.
Summary of the invention
The purpose of this invention is to provide and a kind ofly have that stability is high, phase transformation potential is big, transformation temperature is easily controlled, technology is simple, cost is low, the preparation method of the organic inorganic composite phase-change material of easy enforcement.
Above-mentioned purpose of the present invention is achieved by the following technical programs:
The preparation method of organic inorganic composite phase-change material of the present invention may further comprise the steps:
Step 1: the inorganic porous mineral material is joined in the vacuum reaction still of heating, then the vacuum reaction still is evacuated down to negative pressure 0.05～0.07MPa, close extraction valve, add the liquid organic phase change material while stirring, continue several minutes;
Step 2: open extraction valve, the negative pressure of vacuum reaction still is extracted into 0.095～0.1MPa, continue to stir organic phase change material is fully adsorbed by inorganic materials;
Step 3: stop to stir, discharging promptly obtains organic inorganic composite phase-change material to the normal pressure.Wherein:
Adding the liquid organic phase change material time length in the described step 1 is 3～5 minutes, and organic phase change material is a shape and adds.
The Heating temperature of vacuum reaction still is about 80～100 ℃ in the described step 1.
After described step 3 stopped to stir, closing extraction valve and opening intake valve to reactor was normal pressure, opens discharge valve then.
Described organic phase change material is the mixture of solid paraffin, octadecane or whiteruss and octadecane.
Described inorganic porous mineral material is pearlstone, sepiolite, zeolite or attapulgite.
The organic inorganic composite phase-change material that is prepared by above method also belongs to the present invention.
Described organic inorganic composite phase-change material, wherein the inorganic porous mineral material is a matrix, adsorb organic phase change material in the hole of inorganic mineral material, the organic phase change material adsorptive capacity is 50～70% of a gross weight, and composite phase-change material and inorganic porous mineral material granule degree velocity of variation are less than 40%.
Concrete, described organic inorganic composite phase-change material, described organic phase change material are solid paraffin or octadecane, described inorganic porous mineral material is a pearlstone.
Or described organic phase change material is the mixture of paraffin and octadecane; Described inorganic porous mineral material is pearlstone, sepiolite, zeolite or attapulgite.
Compared with the prior art, the present invention has following beneficial effect:
1, organic phase change material is penetrated in the hole of inorganic porous mineral material, thereby organic phase change material and common building materials bonded gordian technique have been solved, the whole phase transition process of organic phase change material just carries out in the inside of inorganic materials, be subjected to the capillary restriction in duct, solved the problem that phase change material exosmoses.
2, made full use of the duct characteristics of inorganic porous mineral, can adsorb organic phase change material (adsorptive capacity is up to 70%) in a large number, guaranteed that this composite phase-change material has higher phase transformation potential.
3, experimentation uses the method for control pressure stage by stage, can keep the particulate integrity, makes the inorganic porous mineral material have maximal absorptive capacity to organic phase change material, and makes the organic phase change material homogenizing of adsorbing between the particle.
4, preparation technology is simple, and inorganic porous mineral need not to preheat, and only needs together to heat with organic materials in reactor, and operating process is easy to control, can realize streamline operration and suitability for industrialized production.
Description of drawings
Fig. 1 is the embodiment of the invention 2 organic inorganic composite phase-change material pearlstone-paraffin/octadecane (1: 8) differential scanning calorimeter detected results, shows tangible endotherm(ic)peak.
Fig. 2 is the embodiment of the invention 6 organic inorganic composite phase-change materials pearlstone-octadecane differential scanning calorimeter detected result, shows tangible endotherm(ic)peak.
Embodiment
The organic inorganic composite phase-change material characteristics are to be matrix with the inorganic porous mineral material, and vacuum suck organic phase change material, organic phase change material are present in the hole and structure pore of inorganic porous mineral material.
The important indicator of weighing a kind of organic inorganic composite phase-change material is that its enthalpy of phase change height, transformation temperature are easily controlled.The present invention knows through research that, reach these more excellent states, the microscopic pattern of composite phase-change material, granularity and inorganic materials are crucial to the adsorptive capacity of organic phase change material, and can realize control to these emphasis parameters by rational preparation technology.
Preparation method of the present invention is that the inorganic porous mineral material is directly joined in the vacuum reaction still, then the vacuum reaction still is evacuated down to negative pressure 0.05～0.07MPa, adds the liquid organic phase change material while stirring and continues several minutes; Then with the vacuum reaction still be extracted into negative pressure 0.095～0.1MPa, continue to stir organic phase change material fully adsorbed by inorganic materials; Stopped reaction is closed extraction valve and is opened intake valve, opens discharge valve, promptly obtains organic inorganic composite phase-change material.
Among the present invention, the inorganic porous mineral carrier is to be selected from a kind of in the porous materials such as pearlstone, sepiolite, zeolite, attapulgite, volcanic ash, have natural duct and hole in their structure, the size of these ducts and pore diameter is from several nanometers to tens micron, and is interconnected at inner these holes of mineral and duct;
Among the present invention, the organic phase change material that uses is the mixture of solid paraffin or octadecane or whiteruss and octadecane, when whiteruss mixes use with octadecane, can adjust the enthalpy of phase change of organic phase change material, suitably widen the transformation temperature amplitude, so blending ratio can be allocated arbitrarily according to need.
The present invention is described in detail in detail by the following examples, and these embodiment are only for clear open the present invention, not as limitation of the present invention.
Embodiment 1:
The inorganic porous mineral carrier is a pearlstone in the present embodiment, and granularity is at 3～5mm; Organic phase change material is paraffin (solid), and its enthalpy of phase change is at 180～220J/g, and transformation temperature is at 25～30 ℃.
Preparation process is:
At first the pearlstone with 20 grams, 3～5mm joins in the vacuum reaction still, the bath temperature of vacuum reaction still is controlled at about 80 ℃, then the vacuum reaction still is evacuated down to negative pressure 0.05MPa, close extraction valve, and open the liquid feeding valve simultaneously and add 20 gram paraffin (it is aqueous that heating earlier becomes it) and stir; After spending 3 minutes, open extraction valve the vacuum reaction still is extracted into negative pressure 0.095MPa, continue to stir and to make paraffin be inflated perlite to adsorb fully; After 10 minutes, stopped reaction is closed extraction valve and is opened intake valve, opens discharge valve for behind the normal pressure in the reactor by the time, and the composite phase-change material 40 that promptly obtains pearlstone and paraffin restrains.
The Performance Detection of composite phase-change material
1, microtexture is observed: by opticmicroscope the microtexture of composite phase-change material is observed and analyzed, the result:
1) matrix material form: 2～3 millimeters of solid granulars, granularity: compare variation with pearlstone little, compares the granularity velocity of variation with pearlstone 15～30%; Obviously reduce in the duct of composite phase-change material, and the duct is filled and sealed by organic phase change material, and paraffin has entered into the hole of expanded perlite granule fully.
2, organic phase change material adsorptive capacity: by the mode of weighing, the organic phase change material mass percent in the calculating composite phase-change material is as adsorptive capacity.As a result, paraffin adsorptive capacity in pearlstone is 50% in this example.
3, the variable quantity of adsorptive capacity: detect with thermogravimetry, to estimate absorption stability.The result: below 100 ℃, this routine matrix material weight free of losses illustrates this matrix material good stability, and organic phase change material is stable in matrix material.
4, enthalpy of phase change: with the differential scanning calorimeter test, the enthalpy of phase change of composite phase-change material is 90～120J/g as a result.
5, transformation temperature: with the differential scanning calorimeter test, the transformation temperature of composite phase-change material is 25～35 ℃ as a result.
Can recognize by above detection, the pearlstone that the example method prepares and the composite phase-change material of paraffin, its particle integrity degree is better, the paraffin adsorptive capacity reached 50% and adsorptive capacity stable, have higher enthalpy of phase change, transformation temperature is easy to control at 25～30 ℃.
Embodiment 2:
The inorganic porous mineral carrier is a pearlstone in the present embodiment, and granularity is at 3～5mm; Organic phase change material is the combined phase-change material (whiteruss and octadecane weight ratio are 1: 8) of whiteruss and octadecane, and its enthalpy of phase change is at 178～204J/g, and transformation temperature is at 27～35 ℃.
Preparation process is:
At first 20 gram pearlstones are joined in the vacuum reaction still, the bath temperature of vacuum reaction still is controlled at about 80 ℃, then the vacuum reaction still is evacuated down to negative pressure 0.05MPa, closes extraction valve and open the liquid feeding valve simultaneously and add the mixture of 35 gram whiterusss and octadecane and stir; After spending 3 minutes, open extraction valve the vacuum reaction still is extracted into negative pressure 0.095MPa, continue to stir and to make whiteruss and octadecane be inflated perlite fully to adsorb; After 10 minutes, stopped reaction is closed extraction valve and is opened intake valve, opens discharge valve for behind the normal pressure in the reactor by the time, and the composite phase-change material 55 that promptly obtains pearlstone and whiteruss octadecane restrains.
With with embodiment 1 in identical method this routine product is detected.
Result: observation analysis under the opticmicroscope, organic materials (mixture of whiteruss and octadecane) has entered into the hole of expanded perlite granule fully, the composite material granular integrity degree is better, granularity is at 2～3mm, the granularity velocity of variation is 10～30%, the organic materials adsorptive capacity be 64% and adsorptive capacity stable, enthalpy of phase change 116～132J/g, transformation temperature is at 25～35 ℃.The differential scanning calorimeter test result is referring to shown in Figure 1.The product that present embodiment obtains adheres to specification.
Embodiment 3:
The inorganic porous mineral carrier is a sepiolite in the present embodiment, and granularity is at 0.5～1mm; Organic phase change material is the combined phase-change material (whiteruss and octadecane weight ratio are 1: 5) of whiteruss and octadecane, and its enthalpy of phase change is at 167～192J/g, and transformation temperature is at 25～35 ℃.
The Composite Preparation process is with embodiment 2.
With with embodiment 1 in identical method this routine product is detected, result: observation analysis under the opticmicroscope, organic materials (mixture of whiteruss and octadecane) has entered into the hole of sepiolite particle fully, the composite material granular integrity degree is better, granularity is at 0.2～0.5mm, and the granularity velocity of variation is 20～40%, the organic materials adsorptive capacity reached 50% and adsorptive capacity stable, enthalpy of phase change 80～100J/g, transformation temperature is at 25～35 ℃.The product that present embodiment obtains adheres to specification.
Embodiment 4:
The inorganic porous mineral carrier is attapulgite 20 grams in the present embodiment, and granularity is at 0.5～1mm; Organic phase change material is octadecane 35 grams, and its enthalpy of phase change is at 200～230J/g, and transformation temperature is at 30～35 ℃.
The Composite Preparation process is with embodiment 1.
With with embodiment 1 in identical method this routine product is detected, result: observation analysis under the opticmicroscope, organic materials (octadecane) has entered into attapulgite particulate hole fully, the composite material granular integrity degree is better, granularity is at 0.2～0.5mm, and the granularity velocity of variation is 20～40%, the organic materials adsorptive capacity reached 63% and adsorptive capacity stable, enthalpy of phase change 120～145J/g, transformation temperature is at 30～35 ℃.The product that present embodiment obtains adheres to specification.
Embodiment 5:
The inorganic porous mineral carrier is pearlstone 20 grams in the present embodiment, and granularity is at 3～5mm; Organic phase change material is octadecane 47 grams, and its enthalpy of phase change is at 200～230J/g, and transformation temperature is at 30～35 ℃.
The Composite Preparation process is with embodiment 1.
With with embodiment 1 in identical method this routine product is detected, result: observation analysis under the opticmicroscope, organic materials (octadecane) has entered into inorganic mineral particulate hole fully, the composite material granular integrity degree is better, granularity is at 2～3mm, and the granularity velocity of variation is 15～30%, the organic materials adsorptive capacity reached 70% and adsorptive capacity stable, enthalpy of phase change 140～160J/g, transformation temperature is at 30～35 ℃.The product that present embodiment obtains adheres to specification.
Embodiment 6:
The inorganic porous mineral carrier is zeolite 20 grams in the present embodiment, and granularity is at 0.5～1mm; Organic phase change material is octadecane 40 grams, and its enthalpy of phase change is at 200～230J/g, and transformation temperature is at 30～35 ℃.
The Composite Preparation process is with embodiment 1.
With with embodiment 1 in identical method this routine product is detected, result: observation analysis under the opticmicroscope, organic materials (octadecane) has entered into inorganic mineral particulate hole fully, the composite material granular integrity degree is better, granularity is at 0.3～0.6mm, and the granularity velocity of variation is 20～35%, the organic materials adsorptive capacity reached 66% and adsorptive capacity stable, enthalpy of phase change 130～150J/g, transformation temperature is at 30～35 ℃.The product that present embodiment obtains adheres to specification.
Embodiment 7:
The inorganic porous mineral carrier is pearlstone 20 grams in the present embodiment, and granularity is at 3～5mm; Organic phase change material is octadecane 20 grams, and its enthalpy of phase change is at 200～230J/g, and transformation temperature is at 30～35 ℃.
The Composite Preparation process is with embodiment 1.
With with embodiment 1 in identical method this routine product is detected, result: observation analysis under the opticmicroscope, organic materials (octadecane) has entered into inorganic mineral particulate hole fully, the composite material granular integrity degree is better, granularity is at 2～3mm, and the granularity velocity of variation is 15～30%, the organic materials adsorptive capacity be 50% and adsorptive capacity stable, enthalpy of phase change 100～115J/g, transformation temperature is at 30～35 ℃.The differential scanning calorimeter test result is referring to shown in Figure 2.The product that present embodiment obtains adheres to specification.
Comparative example:
Raw material and consumption with CN101121876 method and embodiment 5 experimentize, and obtain composite phase-change material 55 grams of comparative example pearlstone and octadecane.The comparative example product is carried out the detection identical with embodiment 1, the result: calculating the organic materials maximal absorptive capacity is 63%, enthalpy of phase change 125～145J/g, and transformation temperature is at 30～35 ℃.Observation analysis under the opticmicroscope, the comparative example composite material granular is cracked, granularity is at 200～500um, the granularity velocity of variation is more than 80%, particle surface is stained with more organic phase change material, the organic phase change material that explanation can enter into the expanded perlite granule hole reduces in a large number, and active adsorption amount (hole absorption) reduces.The adsorptive capacity less stable, be put into asbestos plate and be heated to 100 ℃, perlite surface phase change material can fuse and be seeped in the asbestos plate, rate of weight loss reaches 15%, illustrate in use, organic phase change material in this type of composite phase-change material is easy to overflow and loses, and temperature adjustment function is reduced greatly, and pollute external environment easily.
Claims (10)
1, the preparation method of organic inorganic composite phase-change material is characterized in that, may further comprise the steps:
Step 1: the inorganic porous mineral material is joined in the vacuum reaction still of heating, then the vacuum reaction still is evacuated down to negative pressure 0.05～0.07MPa, close extraction valve, add the liquid organic phase change material while stirring, continue several minutes;
Step 2: open extraction valve, the negative pressure of vacuum reaction still is extracted into 0.095～0.1MPa, continue to stir organic phase change material is fully adsorbed by inorganic materials;
Step 3: stop to stir, discharging promptly obtains organic inorganic composite phase-change material to the normal pressure.
2, the preparation method of organic inorganic composite phase-change material according to claim 1 is characterized in that, adding the liquid organic phase change material time length in the described step 1 is 3～5 minutes, and organic phase change material is a shape and adds.
3, the preparation method of organic inorganic composite phase-change material according to claim 1 is characterized in that, the Heating temperature of vacuum reaction still is about 80～100 ℃ in the described step 1.
4, the preparation method of organic inorganic composite phase-change material according to claim 1 is characterized in that, after described step 3 stopped to stir, closing extraction valve and opening intake valve to reactor was normal pressure, opens discharge valve then.
5, the preparation method of organic inorganic composite phase-change material according to claim 1 is characterized in that, described organic phase change material is the mixture of solid paraffin, octadecane or whiteruss and octadecane.
6, the preparation method of organic inorganic composite phase-change material according to claim 1 is characterized in that, described inorganic porous mineral material is pearlstone, sepiolite, zeolite or attapulgite.
7, the organic inorganic composite phase-change material for preparing by the method for above arbitrary claim.
8, organic inorganic composite phase-change material according to claim 7, it is characterized in that, the inorganic porous mineral material is a matrix, adsorb organic phase change material in the hole of inorganic mineral material, the organic phase change material adsorptive capacity is 50～70% of a gross weight, and composite phase-change material and inorganic porous mineral material granule degree velocity of variation are less than 40%.
9, organic inorganic composite phase-change material according to claim 8 is characterized in that, described organic phase change material is solid paraffin or octadecane, and described inorganic porous mineral material is a pearlstone.
10, organic inorganic composite phase-change material according to claim 8 is characterized in that, described organic phase change material is the mixture of paraffin and octadecane; Described inorganic porous mineral material is pearlstone, sepiolite, zeolite or attapulgite.
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