CN104710965A - Method for preparing multilevel porous carbon base composite phase change material - Google Patents
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Abstract
The invention provides a method for preparing a multilevel porous carbon base composite phase change material, and belongs to the field of composite phase change materials. The method comprises the following steps: at first, preparing an organic metal skeleton material by using such methods as a solution method, a solvothermal method or a stirring synthesis method; with the organic metal skeleton material as a template, high temperature carbonizing under the protection of an inert gas, and changing the carbonizing temperature and the post treatment manner to obtain a multilevel porous carbon material with a super-large specific surface area and a super-large pore volume; selecting proper solvents according to different kinds of phase change core materials, preparing the phase change core materials to a solution, dispersing the porous carbon material into the solution, removing the solvent by such manners as heating, and meanwhile the phase change core materials are adsorbed and limited in the porous carbon material. The composite phase change material prepared by the method provided by the invention has good thermal storage property, can effectively avoid the leakage problem of the phase change core material, and has the advantages of excellent heat transfer property, good cycling stability and wide application range, and the process is simple and is suitable for large-scale production.
Description
Technical field
The invention belongs to composite phase-change material field, be specifically related to a kind of preparation method of multi-stage porous carbon base composite phase-change material.
Background technology
Along with the development of global economy, energy shortage in recent years becomes distinct issues gradually, causes the attention of national governments.Traditional energy is due to non-renewable, and the quick consumption of these energy forces the mankind to be obliged to go to seek new forms of energy to meet the demand of social development for the energy.At present, human development has also come into operation some clean energies as sun power, wind energy, sea energy etc.But this type of energy often exists the defect such as discontinuity, fluctuation, add the limitation of use procedure, the requirement of the round-the-clock continuous use of the mankind cannot be met.There is by phase-changing energy storage material (Phase change materials, PCMs) object that phase in version realizes energy absorption and release and effective temperature control in phase change energy storage technology, is the effective way solving above-mentioned clean energy defect.Phase-changing energy storage material is now at indoor temperature control, and used heat recycles, and electric power peak load shifting, space space flight and military field etc. are widely used.
Solid-liquid phase change material, owing to having excellent energy storage performance and good recycling performance, obtains at present and applies the most widely.But liquid phase change material causes the inconvenience of actual use owing to there is leakage problem, limit the further application of this type of material, conventional terms of settlement is by preparing compound phase change material with porous material compound.The surface tension of porous material passing hole channel, Hyarogen-bonding and capillary force can be effectively immobilized in duct by solid-liquid phase change material.Common porous carrier materials generally has ordered mesoporous silica dioxide, metal foam, porous carbon materials (as expanded graphite, Graphene, carbon nanotube) and some porous mineral materials.Such as, patent CN102061403A discloses the preparation method of a kind of porous material substrate and composite phase change heat-accumulation material.Patent CN101560377A discloses a kind of preparation method of foamed-metal based high-temperature phase change heat storage composite material.Although these preparation methods to some extent solve the problem that liquid phase change material leaks.But porous material used to there is specific surface area little, the shortcomings such as porosity is low, and aperture is narrow, heat transfer property is poor in actual applications, heat storage capacity utilization ratio is low to cause it, and price (as Graphene) expensive in addition also limit the application of the marketization.Therefore, develop a kind of there is high-specific surface area, high porosity, aperture is adjustable, thermal conductivity good and low-cost porous material for effective utilization of phase-changing energy storage material and application significant.
Summary of the invention
The object of the invention is to, be that template prepares the porous carbon materials carrier with multistage pore canal by the mode that high temperature cabonization decomposes with metallic organic framework, and then develop a kind of novel composite phase-change material, such composite phase-change material has core variation (from low temperature to high temperature), good heat conduction effect, the advantages such as heat storage capacity excellence and good cycle.
Technical scheme of the present invention is: 1) first by solution method, and solvent-thermal method or stirring synthesis method prepare metal-organic framework materials; 2) using metal-organic framework materials as template, high temperature cabonization under the protection of rare gas element, obtains the multistage pore canal carbon material with extra specific surface area and pore volume; 3) according to different types of phase transformation core, select suitable solvent, porous carbon materials is scattered in the homogeneous phase solution containing phase transformation core, by modes such as heating except desolventizing, owing to being subject to the reactive force in carbon material duct, phase transformation core is limited among the duct of porous carbon materials by absorption.
Concrete preparation process is:
(1) preparation of metallic organic framework mould material:
Soluble metallic salt and organic carboxyl acid part are dissolved in certain solvent and are mixed with homogeneous phase solution, under 40 ~ 220 DEG C of conditions, adopted by this solution hydrothermal method to react 4 ~ 120 h, obtain crystalline product; Or in the homogeneous phase solution of preparation, add a certain amount of additive, stir 10 ~ 60 min at ambient temperature, obtain solid product.After reaction terminates, filter and repetitive scrubbing, at 80 ~ 150 DEG C, obtain metallic organic framework mould material after dry 24 ~ 72 h.Wherein, metal-salt: organic carboxyl acid class part: the mol ratio of additive is: 1 ~ 10:1 ~ 10:0 ~ 100.
(2) preparation of multistage pore canal carbon material:
Pour metal-organic framework materials into porcelain boat, transfer in tube furnace, under the protection of rare gas element, be warming up to 600 ~ 1200 DEG C with the speed of 1 ~ 5 DEG C/min, and be incubated 1 ~ 6 h at such a temperature.Naturally cool to room temperature, wash repeatedly with the hydrochloric acid soln of 1 ~ 5 mol/L, the metal oxide generated in removing porous material and metal simple-substance particle, then with deionized water wash to neutral, 100 ~ 150 DEG C of dryings 1 ~ 2 day, obtain multistage pore canal carbon material.
(3) preparation of composite phase-change material
Multistage pore canal carbon material prepared by step (2) is scattered in 10 ~ 50 ml containing in the solvent of phase transformation core, after being uniformly dispersed, at 40 ~ 500 DEG C, dry 24 ~ 72 h, obtain multistage pore canal carbon back composite phase-change material.The mass ratio of phase transformation core and metallic organic framework matrix is 1 ~ 100:1 ~ 100.
Soluble metallic salt described in step (1) comprises chromium nitrate, chromium chloride, chromium sulphate, chromium acetate, zirconium nitrate, zirconium chloride, zirconium sulfate, acetic acid zirconium, cupric nitrate, cupric chloride, copper sulfate, neutralized verdigris, zinc nitrate, zinc chloride, zinc sulfate, zinc acetate, nickelous nitrate, nickelous chloride, single nickel salt, nickel acetate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, cobalt chloride, rose vitriol, Cobaltous diacetate, iron nitrate, iron(ic) chloride, ferric sulfate, iron acetate, aluminum nitrate, aluminum chloride, Tai-Ace S 150, Burow Solution, manganous nitrate, Manganous chloride tetrahydrate, manganous sulfate, manganese acetate, Titanium Nitrate, titanium chloride, wherein one or more such as titanium sulfate.
Organic carboxyl acid part described in step (1) comprises wherein one or more such as terephthalic acid, 2-amino terephthalic acid, 2-hydroxyterephthalic acid, trimesic acid, 1,2,4,5-pyromellitic acid, 1,2,4-inclined tricarboxylic acid.
Additive described in step (1) comprises wherein one or more such as hydrogen peroxide, triethylamine, pyridine, acetic acid, hydrochloric acid, hydrofluoric acid, fluoroboric acid.
Step (1) and the solvent described in step (3) comprise wherein one or more such as dehydrated alcohol, anhydrous methanol, water, DMF, DMF, dimethyl sulfoxide (DMSO), trichloromethane, tetrahydrofuran (THF).
Described phase transformation core is one or more the solubility phase change materials in polyalcohols, fatty acid, paraffin class, crystalline hydrate salt, inorganic salts.Polyalcohols, specifically comprises polyoxyethylene glycol (molecular-weight average is 1000-20000), tetramethylolmethane, neopentyl glycol etc.; Fatty acid, specifically comprises stearic acid, tetradecanoic acid, palmitinic acid, capric acid, lauric acid, pentadecylic acid, sebacic acid etc.; Paraffin class, specifically comprises paraffin 58; Crystalline hydrate salt, specifically comprises Sodium carbonate decahydrate, sal glauberi, ten hydrogen phosphate dihydrate sodium, calcium chloride hexahydrate, Sodium acetate trihydrate, five water Sulfothiorine; Inorganic salts, specifically comprises sodium-chlor, SODIUMNITRATE, sodium carbonate, sodium sulfate, saltpetre, lithium nitrate, Repone K, lithium chloride, lithium chromate, Quilonum Retard etc.
If when the phase change material of filling in step (3) is inorganic salt, dried product need be placed in retort furnace, at 100 ~ 500 DEG C, calcine 1 ~ 10 h, furnace cooling, obtains multistage pore canal carbon back composite phase-change material.
The invention has the advantages that: prepared composite phase-change material, not only can improve the hot memory property of composite phase-change material, and the problem can effectively avoiding phase transformation core to reveal; Prepared composite phase-change material temperature range is wide, is applicable to the interval energy storage of differing temps and temperature control, applied range; Composite phase-change material excellent heat transfer properties, the good cycling stability prepared with the present invention, and technique is simple, is applicable to large-scale production.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of the porous carbon materials MOF5C-1000 that the embodiment of the present invention 1 obtains.
Fig. 2 is the stereoscan photograph of the multistage pore canal carbon back composite phase-change material PEG-4000@MOF5C-1000 that the embodiment of the present invention 1 obtains.
Fig. 3 is the infrared figure that the PEG of the embodiment of the present invention 1, MOF5C-1000 and PEG-4000@MOF5C-1000 composite phase-change material is corresponding.
Fig. 4 is the stereoscan photograph of the multistage pore canal carbon back composite phase-change material palmitic acid@3C-1000 that the embodiment of the present invention 2 obtains.
Fig. 5 is the stereoscan photograph of the multistage pore canal carbon back composite phase-change material paraffin 58@BTMC-1000 that the embodiment of the present invention 3 obtains.
Embodiment
Below in conjunction with concrete embodiment, technical scheme of the present invention is described further.
Embodiment 1
(1) preparation of metallic organic framework mould material:
Be dissolved in 360 ml DMF by the nine nitric hydrate zinc of the terephthalic acid of 3.06 g and 10.89 g and be mixed with homogeneous phase solution, magnetic agitation 30 mins, adds the triethylamine of 14.4 g in solution, stirs 30 min at ambient temperature, obtains solid product.After reaction terminates, filter and repetitive scrubbing, at 120 DEG C, obtain metallic organic framework mould material MOF-5 after dry 24 h.
(2) preparation of multistage pore canal carbon material:
Metal-organic framework materials MOF-5 powder is put into porcelain boat and transfers to tube furnace, first logical 30 mins nitrogen, under the protection of rare gas element, are then warmed up to 1000 with the speed of 5 DEG C/min
oc is also incubated 6 h, then naturally cools to room temperature, washs repeatedly with the hydrochloric acid soln of 1 mol/L, then with deionized water wash to neutral, 150 DEG C of dryings 1 day, obtaining multistage pore canal carbon material and ordering was MOF5C-1000, and its scintigram as shown in Figure 1.
(3) preparation of composite phase-change material
0.081g MOF5C-1000 is scattered in containing in 1 g PEG-4000 ethanolic soln of 30 ml, after being uniformly dispersed, dry 72 h in 80 DEG C of baking ovens, obtain many composite phase-change materials [email protected] shown in Figure 2, it is 60.03 that DSC test result shows its transformation temperature to its scintigram
oc, latent heat of phase change is 162 J/g.Its infared spectrum as shown in Figure 3, after absorption phase change material, 2871 and 950cm
-1the methylene peak of PEG obviously can be seen by place.
Embodiment 2
(1) preparation of metallic organic framework mould material:
The nine nitric hydrate zinc of amino for the 2-of 3.06 g terephthalic acid and 10.89 g are dissolved in 360 ml DMF and are mixed with homogeneous phase solution, magnetic agitation 30 mins, in solution, add 30 wt%H of 2.7 ml
2o
2with the triethylamine of 14.4 g, stir 30 min at ambient temperature, obtain solid product.After reaction terminates, filter and use DMF and methyl alcohol priority repetitive scrubbing repeatedly, at 120 DEG C, obtaining metallic organic framework mould material IRMOF-3 after dry 24 h.
(2) preparation of multistage pore canal carbon material:
Metal-organic framework materials IRMOF-3 powder is put into porcelain boat and transfers to tube furnace, first logical 30 mins nitrogen, under the protection of rare gas element, are then warmed up to 1000 with the speed of 5 DEG C/min
oc is also incubated 6 h, then naturally cools to room temperature, washs repeatedly with the hydrochloric acid soln of 1 mol/L, then with deionized water wash to neutral, 150 DEG C of dryings 1 day, obtaining multistage pore canal carbon material and ordering was 3C-1000.
(3) composite setting phase change material adopts physical mixed and pickling process.
0.081 g 3C-1000 is scattered in 30 ml containing in 0.5 g palmitic acid ethanolic soln, after being uniformly dispersed, dry 72 h in 80 DEG C of (on the fusing point of PEG) baking ovens, obtain many composite phase-change materials palmitic acid@3C-1000, its scintigram as shown in Figure 4.
Embodiment 3
(1) preparation of metallic organic framework mould material:
Be dissolved in 360 ml DMF by the nine nitric hydrate zinc of the TDBTM of 3.0 g and 10.89 g and be mixed with homogeneous phase solution, magnetic agitation 30 mins, adds the triethylamine of 14.4 g in solution, stirs 30 min at ambient temperature, obtains solid product.After reaction terminates, filter trichloromethane repetitive scrubbing repeatedly, at 80 DEG C, obtain metallic organic framework mould material Zn-TPBTM after dry 24 h.
(2) preparation of multistage pore canal carbon material:
Metal-organic framework materials Zn-TPBTM powder is put into porcelain boat and transfers to tube furnace, first logical 30 min nitrogen, under the protection of rare gas element, are then warmed up to 1000 with the speed of 5 DEG C/min
oc is also incubated 6 h, then naturally cools to room temperature, washs repeatedly with the hydrochloric acid soln of 1 mol/L, then with deionized water wash to neutral, 150 DEG C of dryings 1 day, obtaining multistage pore canal carbon material and ordering was BTMC-1000.
(3) composite setting phase change material adopts physical mixed and pickling process.
0.11 g BTMC-1000 is scattered in containing in the trichloromethane of 1 g paraffin-58 of 30 ml, after being uniformly dispersed, dry 72 h in 80 DEG C of baking ovens, obtain many composite phase-change materials paraffin-58@BTMC-1000, its scintigram as shown in Figure 5.
Embodiment 4
(1) preparation of metallic organic framework mould material:
The ANN aluminium nitrate nonahydrate of the terephthalic acid of 3.0 g and 10.89 g be dissolved in 360 ml DMF and be mixed with homogeneous phase solution, magnetic agitation 30 min, adds the triethylamine of 20 mL in solution, stirs 30 min at ambient temperature, obtains solid product.After reaction terminates, filter trichloromethane repetitive scrubbing repeatedly, at 80 DEG C, obtain metallic organic framework mould material Al-MOF after dry 24 h.
(2) preparation of multistage pore canal carbon material:
Metal-organic framework materials Al-MOF powder is put into porcelain boat and transfers to tube furnace, first logical 30 min nitrogen, under the protection of rare gas element, are then warmed up to 1000 with the speed of 5 DEG C/min
oc is also incubated 6 h, then naturally cools to room temperature, washs repeatedly with the hydrochloric acid soln of 1 mol/L, then with deionized water wash to neutral, 150 DEG C of dryings 1 day, obtaining multistage pore canal carbon material and ordering was AlC-1000.
(3) composite setting phase change material adopts physical mixed and pickling process.
0.1 g AlC-1000 is scattered in 30 ml containing 1 g anhydrous nitric acid sodium deionized water in, after being uniformly dispersed, 130
oin C baking oven, dry 72 h, calcine 2 h at 500 DEG C, obtain SODIUMNITRATE@AlC-1000 composite phase-change material.
Embodiment 5
(1) preparation of metallic organic framework mould material:
Be dissolved in 360 ml DMF by the nine nitric hydrate zinc of the TDPAT of 3.0 g and 10.0 g and be mixed with homogeneous phase solution, magnetic agitation 30 min, adds the triethylamine of 20 mL in solution, stirs 30 min at ambient temperature, obtains solid product.After reaction terminates, filter trichloromethane repetitive scrubbing repeatedly, at 80 DEG C, obtain metallic organic framework mould material Zn-TDPAT after dry 24 h.
(2) preparation of multistage pore canal carbon material:
Metal-organic framework materials Zn-TDPAT powder is put into porcelain boat and transfers to tube furnace, first logical 30 min nitrogen, under the protection of rare gas element, are then warmed up to 600 with the speed of 5 DEG C/min
oc is also incubated 6 h, then naturally cools to room temperature, washs repeatedly with the hydrochloric acid soln of 1 mol/L, then with deionized water wash to neutral, 150 DEG C of dryings 1 day, obtaining multistage pore canal carbon material and ordering was PATC-600.
(3) composite setting phase change material adopts physical mixed and pickling process.
0.1 g PATC-600 is scattered in 30 ml containing 1 g six calcium chloride hydrate dehydrated alcohol in, after being uniformly dispersed, 80
odry 72 h in C baking oven, obtain six calcium chloride hydrate@PATC-600 composite phase-change materials.
Embodiment 6
(1) preparation of metallic organic framework mould material:
The nine nitric hydrate zinc of the terephthalic acid of 1.0 g and 3 g are dissolved in 60 ml DEF and are mixed with homogeneous phase solution, in the baking oven of 100 DEG C, leave standstill 24 h obtain crystalline product.After reaction terminates, filter and soak three times with DMF and trichloromethane respectively, at 100 DEG C after dry 24 h, obtaining metallic organic framework mould material IRMOF-1.
(2) preparation of multistage pore canal carbon material:
Metal-organic framework materials IRMOF-1 crystal is put into porcelain boat and transfers to tube furnace, first logical 30 min nitrogen, under the protection of rare gas element, are then warmed up to 1000 with the speed of 5 DEG C/min
oc is also incubated 6 h, then naturally cools to room temperature, washs repeatedly with the hydrochloric acid soln of 1 mol/L, then with deionized water wash to neutral, 150 DEG C of dryings 1 day, obtaining multistage pore canal carbon material and ordering was 1C-1000.
(3) composite setting phase change material adopts physical mixed and pickling process.
0.1 g 1C-1000 is scattered in 30 ml containing 1 g anhydrous nitric acid sodium deionized water in, after being uniformly dispersed, 130
oin C baking oven, dry 72 h, calcine 2 h at 500 DEG C, obtain SODIUMNITRATE@lC-1000 composite phase-change material.
Claims (7)
1. a preparation method for multistage pore canal carbon back composite phase-change material, is characterized in that, preparation process is as follows:
1) preparation of metallic organic framework mould material
Soluble metallic salt and organic carboxyl acid part are dissolved in certain solvent and are mixed with homogeneous phase solution, under 40 ~ 220 DEG C of conditions, adopted by this solution hydrothermal method to react 4 ~ 120 h, obtain crystalline product; Or in the homogeneous phase solution of preparation, add a certain amount of additive, stir 10 ~ 60 min at ambient temperature, obtain solid product, after reaction terminates, filter and repetitive scrubbing, metallic organic framework mould material is obtained after dry 24 ~ 72 h at 80 ~ 150 DEG C, wherein, metal-salt: organic carboxyl acid class part: the mol ratio of additive is: 1 ~ 10:1 ~ 10:0 ~ 100;
2) preparation of multistage pore canal carbon material
Pour metal-organic framework materials into porcelain boat, transfer in tube furnace, under the protection of rare gas element, be warming up to 600 ~ 1200 DEG C with the speed of 1 ~ 5 DEG C/min, and be incubated 1 ~ 6 h at such a temperature, naturally cool to room temperature again, wash repeatedly with the hydrochloric acid soln of 1 ~ 5 mol/L, the metal oxide generated in removing porous material and metal simple-substance particle, then with deionized water wash to neutral, 100 ~ 150 DEG C of dryings 1 ~ 2 day, obtain multistage pore canal carbon material;
3) preparation of composite phase-change material
By step 2) the multistage pore canal carbon material prepared be scattered in 10 ~ 50 ml containing in the solvent of solubility phase transformation core, after being uniformly dispersed, dry 24 ~ 72 h at 40 ~ 500 DEG C, obtain multistage pore canal carbon back composite phase-change material, the mass ratio of phase transformation core and metallic organic framework matrix is 1 ~ 100:1 ~ 100.
2. the preparation method of multistage pore canal carbon back composite phase-change material as claimed in claim 1, it is characterized in that, step 1) described in soluble metallic salt comprise chromium nitrate, chromium chloride, chromium sulphate, chromium acetate, zirconium nitrate, zirconium chloride, zirconium sulfate, acetic acid zirconium, cupric nitrate, cupric chloride, copper sulfate, neutralized verdigris, zinc nitrate, zinc chloride, zinc sulfate, zinc acetate, nickelous nitrate, nickelous chloride, single nickel salt, nickel acetate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, cobalt chloride, rose vitriol, Cobaltous diacetate, iron nitrate, iron(ic) chloride, ferric sulfate, iron acetate, aluminum nitrate, aluminum chloride, Tai-Ace S 150, Burow Solution, manganous nitrate, Manganous chloride tetrahydrate, manganous sulfate, manganese acetate, Titanium Nitrate, titanium chloride, titanium sulfate wherein one or more.
3. the preparation method of multistage pore canal carbon back composite phase-change material as claimed in claim 1, it is characterized in that, step 1) described in organic carboxyl acid part comprise terephthalic acid, the amino terephthalic acid of 2-, 2-hydroxyterephthalic acid, trimesic acid, 1,2,4, one or more in 5-pyromellitic acid, 1,2,4-inclined tricarboxylic acid.
4. the preparation method of multistage pore canal carbon back composite phase-change material as claimed in claim 1, it is characterized in that, the additive described in step 1) comprises one or more in hydrogen peroxide, triethylamine, pyridine, acetic acid, hydrochloric acid, hydrofluoric acid, fluoroboric acid.
5. the preparation method of multistage pore canal carbon back composite phase-change material as claimed in claim 1, it is characterized in that, step 1) and the solvent described in step 3) comprise dehydrated alcohol, anhydrous methanol, water, N, one or more in dinethylformamide, DMF, dimethyl sulfoxide (DMSO), trichloromethane, tetrahydrofuran (THF).
6. the preparation method of multistage pore canal carbon back composite phase-change material as claimed in claim 1, it is characterized in that, described phase transformation core material is one or more the solubility phase change materials in polyalcohols, fatty acid, paraffin class, crystalline hydrate salt, inorganic salts, wherein polyalcohols, specifically comprises polyoxyethylene glycol, tetramethylolmethane, neopentyl glycol that molecular-weight average is 1000-20000; Fatty acid, specifically comprises stearic acid, tetradecanoic acid, palmitinic acid, capric acid, lauric acid, pentadecylic acid, sebacic acid; Paraffin class, specifically comprises paraffin 58; Crystalline hydrate salt, specifically comprises Sodium carbonate decahydrate, sal glauberi, ten hydrogen phosphate dihydrate sodium, calcium chloride hexahydrate, Sodium acetate trihydrate, five water Sulfothiorine; Inorganic salts, specifically comprises sodium-chlor, SODIUMNITRATE, sodium carbonate, sodium sulfate, saltpetre, lithium nitrate, Repone K, lithium chloride, lithium chromate, Quilonum Retard.
7. the preparation method of the multistage pore canal carbon back composite phase-change material as described in claim 1 or 6, it is characterized in that, when the phase transformation core material filled is inorganic salts, dried product need be placed in retort furnace, 1 ~ 10 h is calcined at 100 ~ 500 DEG C, furnace cooling, obtains multistage pore canal carbon back composite phase-change material.
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