CN103058171B - Preparation method of filled high-heat-conduction foamy carbon material for energy storage - Google Patents
Preparation method of filled high-heat-conduction foamy carbon material for energy storage Download PDFInfo
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- CN103058171B CN103058171B CN201310004952.6A CN201310004952A CN103058171B CN 103058171 B CN103058171 B CN 103058171B CN 201310004952 A CN201310004952 A CN 201310004952A CN 103058171 B CN103058171 B CN 103058171B
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Abstract
The invention relates to a preparation method of a filled high-heat-conduction foamy carbon material for energy storage, and belongs to the technical field of inorganic functional materials. The preparation method comprises the following steps: foaming mesophase pitch to obtain a foamy carbon raw material or a semi-carbonized raw material; preparing a precursor sol of a carbon aerogel, dipping the sol into the pores of the foamy carbon raw material or the semi-carbonized raw material, and ageing to obtain the gel; and carrying out high temperature treatment to form the carbon aerogel filled high-heat-conduction foamy carbon material. According to the invention, the heat conductivity and the compressive strength of the foamy carbon material prepared through the method are increased by 10-20% and 15-20% respectively; the filling uniformity of the phase transition material in the foamy carbon material is substantially improved; and the fluidity of the molten phase transition material in the foamy carbon is inhibited, so it is possible for the phase change energy storage under a speed-variable flight condition.
Description
Technical field
The preparation method who the present invention relates to energy storage filled-type high heat conducting foam carbon material, belongs to inorganic functional material technical field.
Background technology
Owing to having good heat conductivility and abundant open-celled structure, high heat conducting foam carbon material is considered to heat management system high heat conduction framework material the most with potential applications.Conventionally high heat conducting foam carbon material is obtained through technological processs such as foaming, carbonization, greyings by mesophase pitch, foamy carbon foamy carbon hole wall in high-temperature process shrinks, subsiding and hole wall crackle of local hole wall be can produce, the decline of foamy carbon heat conductivility and the decline of mechanical property caused.In order to improve heat conductivility and the mechanical property of foamy carbon material, (main method has chemical vapor carbon deposition layer in document, to have adopted foamy carbon hole wall to strengthen method, repeat filled bitumen carbon coating, metal coating etc.), precursor modification method (is added crystalline flake graphite, add carbonaceous mesophase spherules, add fluorochemical etc.) etc. foamy carbon is carried out to mechanics enhancing and/or heat conductivility improves, but these researchs all do not have to carry out necessary adjustment and change for phase-change accumulation energy high heat conducting foam carbon, cause and strengthen rear foamy carbon structural changes, be unfavorable for the filling of phase change material in hole, cause the decline of stored energy usefulness.The energy storage material of filling phase change material formation with high heat conducting foam carbon is in the speed change flight course of aircraft, can be because the effect of inertia causes the unexpected directed flow of phase change material in foamy carbon hole, cause the reduction of phase-change accumulation energy body running efficiency or lost efficacy in short-term.The foamy carbon Enhancement Method providing in document at present all can not address this problem.
Summary of the invention
The object of this invention is to provide the preparation method of a kind of energy storage filled-type high heat conducting foam carbon material, by adopting the method for filling high specific area carbon aerogel in hole, improve the filling homogeneity of phase change material in foamy carbon and heat conductivility and the mechanical property of reinforced foam carbon material, improve the task performance of phase-changing energy storage material in the time that aircraft speed change is on active service simultaneously.
The object of the invention is to be achieved through the following technical solutions.
Adopt mesophase pitch to foam, obtain foamy carbon raw material or partial carbonization raw material, then prepare the precursor glue of carbon aerogels, sol impregnation is entered in foamy carbon raw material or partial carbonization raw material hole, carry out aging formation gel, then carry out pyroprocessing, form carbon aerogels filled-type high heat conducting foam carbon material.Concrete steps are as follows:
1) foamy carbon raw material preparation: taking mesophase pitch as precursor, place it in foaming vessel, then foaming forms foamy carbon raw material in high temperature and high pressure kettle;
Described mesophase pitch can be the mixture of any or they in mesophase pitch, coal measures mesophase pitch and petroleum mesophase pitch for naphthalene;
Blowing temperature is SP+(150～300 DEG C), the softening temperature that wherein SP is mesophase pitch.In order to promote the opening of foamy carbon hole, can further be warming up to SP+(300～600 DEG C), form partial carbonization raw material;
2) preparation of the precursor of carbon aerogels: with Resorcinol and formaldehyde with 1: the mol ratio of (2 ± 0.2) is dissolved in solvent, obtain solution, then in solution, add catalyzer, be then sealed in water bath with thermostatic control heating 1-10h in closed container, form the precursor of carbon aerogels;
Described solvent is alcohols material or deionized water; Described alcohols material is methyl alcohol, ethanol or propyl alcohol; The ratio of the mixture of solvent and Resorcinol and formaldehyde is 100mL:(3～30g);
Described catalyzer is hexamethylenetetramine, salt of wormwood, sodium carbonate, hydrochloric acid or ammoniacal liquor; The volume of described catalyzer is 0.1% ~ 1% of liquor capacity;
3) preparation of organic aerogel filled and process carbon material: by step 2) formerly pressurize after vacuum dipping under combined action of the precursor of the carbon aerogels that obtains enters in the hole of foamy carbon raw material that step 1) obtains or partial carbonization raw material, aging until form organic aerogel under 75～90 DEG C of water bath condition; Foamy carbon raw material or the partial carbonization raw material unnecessary aerogel around of filling organic aerogel are removed, obtained foamy carbon raw material or partial carbonization raw material that organic aerogel is filled;
4) organic aerogel is dry: the foamy carbon raw material that the organic aerogel that step 3) is obtained is filled or the seasoning at normal temperatures and pressures of partial carbonization raw material are until constant weight obtains gel-filled foamy carbon raw material or the partial carbonization raw material of dry gas, or the foamy carbon raw material of the organic aerogel that step 3) is obtained filling or partial carbonization raw material dry gel-filled foamy carbon raw material or partial carbonization raw material of dry gas that obtain in supercritical co, ethanol, sherwood oil environment; Before dry, can carry out pre-permutation to the water in aerogel, alcohol with acetone, to improve dry effect;
5) pyroprocessing forms carbon aerogels filled-type high heat conducting foam carbon: the foamy carbon raw material that dry gas that step 4) is obtained is gel-filled or partial carbonization raw material are under protection of inert gas; temperature rise rate according to 0.5 DEG C/min～5 DEG C/min is warming up to T1(T1 within the scope of 900 DEG C～1500 DEG C); constant temperature 0.5h～5h forms carbonization filled-type foamy carbon material; then be warming up to T2(T2 within the scope of 2800 DEG C～3000 DEG C according to the temperature rise rate of 0.2 DEG C/min～10 DEG C/min); constant temperature 0.5h～5h, obtains the high heat conducting foam carbon material that carbon aerogels is filled.
In order to improve the filling ratio of carbon aerogels in foamy carbon hole, also can use colloidal sol to carry out 1～2 time according to (3), (4) and (5) process to the high heat conducting foam carbon material of carbonization filled-type foamy carbon material and the final carbon aerogels filling obtaining, finally form repeatedly the high heat conducting foam carbon material that carbon aerogels is filled.
Beneficial effect
1) thermal conductivity of the foamy carbon material that prepared by method of the present invention improves 10%～20%, and ultimate compression strength improves 15%～20%; 2) phase change material filling homogeneity is therein improved greatly; 3) mobility of molten state phase change material in foamy carbon is inhibited, for the phase-change accumulation energy under speed change flying condition provides possibility.
Embodiment
Embodiment 1
1) foamy carbon raw material preparation: taking softening temperature as the naphthalene of 280 DEG C be mesophase pitch powder as presoma, presoma is placed in to stainless steel foaming vessel, under 1MPa original pressure, in 480 DEG C of foaming 3h, form foamy carbon raw material;
2) preparation of the precursor of carbon aerogels: in 1:2(mol ratio) ratio obtain Resorcinol and formaldehyde mixture, 10g mixture is dissolved in the alcohol solvent of 100mL, obtain solution, then in solution, add the hexamethylenetetramine of 1mL, then be sealed in closed container the water bath with thermostatic control heating 5h of 55 DEG C, form the precursor of carbon aerogels;
3) preparation of organic aerogel filled and process carbon material: the foamy carbon raw material that step 1) is obtained are placed in container, then container is put into vacuum impregnation equipment, be evacuated to gauge pressure-0.1MPa, then suck step 2) precursor of the carbon aerogels that obtains, the precursor that ensures carbon aerogels floods partial carbonization raw material, keeps taking out after 1h, then said vesse is placed in to autoclave, be forced into 3MPa, keep taking out after 1h; Again container is placed in to 80 DEG C of aging 70h of water bath with thermostatic control, the precursor of carbon aerogels is formed to organic aerogel, take out after foamy carbon unnecessary gel around, form the foamy carbon raw material that organic aerogel is filled;
4) organic aerogel is dry: the foamy carbon raw material acetone that the organic aerogel that step 3) is obtained is filled soaks three times, soaks 2h at every turn, then takes out, and is placed in the dry 5h of Supercritical Ethanol, then takes out;
5) pyroprocessing forms carbon aerogels filled-type high heat conducting foam carbon: the gel-filled foamy carbon raw material of dry gas that step 4) is obtained are under argon gas protection; be warming up to 1000 DEG C by the temperature rise rate of 1 DEG C/min; constant temperature 1h; then be warming up to 2800 DEG C according to the temperature rise rate of 5 DEG C/min; after constant temperature 2h; naturally cooling, obtains the high heat conducting foam carbon material that carbon aerogels is filled.
The high heat conducting foam carbon material that the carbon aerogels obtaining is filled carries out thermal conductivity and intensity test, and obtaining its thermal conductivity is 57W/(m.K), compressive strength is 0.98MPa; The filling ratio of paraffin phase change material is 92%, and fills evenly.
Comparative example 1
1) foamy carbon raw material preparation: taking softening temperature as the naphthalene of 280 DEG C be mesophase pitch powder as presoma, presoma is placed in to stainless steel foaming vessel in 480 DEG C of foaming 3h, form foamy carbon raw material;
2) pyroprocessing forms high heat conducting foam carbon: the foamy carbon raw material that step 1) is obtained are under argon gas protection; be warming up to 1000 DEG C by the temperature rise rate of 1 DEG C/min; constant temperature 1h; then be warming up to 2800 DEG C according to the temperature rise rate of 5 DEG C/min; after constant temperature 2h; naturally cooling, obtains high heat conducting foam carbon material.
The high heat conducting foam carbon material obtaining is carried out to thermal conductivity and intensity test, and obtaining its thermal conductivity is 49W/(m.K), compressive strength is 0.82MPa; The mean cut-off rate of paraffin phase change material is 85%, but the filling ratio of foamy carbon middle part only has 70%.
Compared with the high heat conducting foam carbon material that the high heat conducting foam carbon that the carbon aerogels that embodiment 1 obtains is filled obtains with comparative example 1, thermal conductivity improves 16.4%, and ultimate compression strength improves 19.5%; Phase change material filling homogeneity has therein obtained obvious improvement.
Embodiment 2
1) partial carbonization foamy carbon raw material preparation: taking softening temperature as the petroleum mesophase pitch powder of 290 DEG C is as presoma, presoma is placed in to stainless steel foaming vessel, under 1.5MPa original pressure in 490 DEG C foaming 3h, and then process 1h in 850 DEG C of inert environments, obtain partial carbonization foamy carbon raw material;
2) preparation of the precursor of carbon aerogels: in 1:2(mol ratio) ratio obtain Resorcinol and formaldehyde mixture, 10g mixture is dissolved in the alcohol solvent of 100mL, obtain solution, then the concentrated hydrochloric acid of 0.5mL in solution, then be sealed in closed container the water bath with thermostatic control heating 2h of 60 DEG C, form the precursor of carbon aerogels;
3) organic aerogel is filled the preparation of partial carbonization foamy carbon material: the partial carbonization foamy carbon raw material that step 1) is obtained are placed in container, then container is put into vacuum impregnation equipment, be evacuated to gauge pressure-0.1MPa, then suck step 2) precursor of the carbon aerogels that obtains, the precursor that ensures carbon aerogels floods partial carbonization foamy carbon raw material, keeps taking out after 1h, then said vesse is placed in to autoclave, be forced into 3MPa, keep taking out after 1h; Again container is placed in to 80 DEG C of aging 60h of water bath with thermostatic control, the precursor of carbon aerogels is formed to organic aerogel, take out after foamy carbon unnecessary gel around, form the partial carbonization raw material that organic aerogel is filled;
4) organic aerogel is dry: the partial carbonization foamy carbon raw material acetone that the organic aerogel that step 3) is obtained is filled soaks three times, soaks 2h at every turn, then takes out, and is placed in the dry 3h of Supercritical Ethanol, then takes out;
5) pyroprocessing forms carbon aerogels filled-type high heat conducting foam carbon: the gel-filled partial carbonization foamy carbon raw material of dry gas that step 4) is obtained are under argon gas protection; be warming up to 1300 DEG C by the temperature rise rate of 3 DEG C/min; constant temperature 1h; then be warming up to 3000 DEG C according to the temperature rise rate of 8 DEG C/min; after constant temperature 2h; naturally cooling, obtains the high heat conducting foam carbon material that carbon aerogels is filled.
The high heat conducting foam carbon material that the carbon aerogels obtaining is filled carries out thermal conductivity and intensity test, and obtaining its thermal conductivity is 87W/(m.K), compressive strength is 1.24MPa; The filling ratio of paraffin phase change material is 90%, and fills evenly.
Comparative example 2
1) foamy carbon raw material preparation: taking softening temperature as the petroleum mesophase pitch powder of 290 DEG C is as presoma, presoma is placed in to stainless steel foaming vessel, under 1.5MPa original pressure, in 490 DEG C of foaming 3h, and then process 1h in 850 DEG C of inert environments, obtain partial carbonization raw material;
2) pyroprocessing forms high heat conducting foam carbon: the partial carbonization foamy carbon raw material that step 1) is obtained are under argon gas protection; be warming up to 1300 DEG C by the temperature rise rate of 3 DEG C/min; constant temperature 1h; then be warming up to 3000 DEG C according to the temperature rise rate of 8 DEG C/min; after constant temperature 2h; naturally cooling, obtains high heat conducting foam carbon material.
The high heat conducting foam carbon material obtaining is carried out to thermal conductivity and intensity test, and obtaining its thermal conductivity is 73W/(m.K), compressive strength is 1.05MPa; The mean cut-off rate of paraffin phase change material is 81%, and the filling ratio of foamy carbon middle part only has 72%.
Compared with the high heat conducting foam carbon material that the high heat conducting foam carbon that the carbon aerogels that embodiment 2 obtains is filled obtains with comparative example 2, thermal conductivity improves 19.2%, and ultimate compression strength improves 18.4%; Phase change material filling homogeneity has therein obtained obvious improvement.
Claims (4)
1. the preparation method of filled-type high heat conducting foam carbon material for energy storage, is characterized in that the step of the method comprises:
1) foamy carbon raw material preparation: taking mesophase pitch as precursor, place it in foaming vessel, then foaming forms foamy carbon raw material under blowing temperature in high temperature and high pressure kettle;
2) preparation of the precursor of carbon aerogels: with Resorcinol and formaldehyde with 1: the mol ratio of (2 ± 0.2) is dissolved in solvent, obtain solution, then in solution, add catalyzer, be then sealed in water bath with thermostatic control heating 1-10h in closed container, form the precursor of carbon aerogels;
3) preparation of organic aerogel filled and process carbon material: by step 2) precursor of the carbon aerogels that the obtains dipping under combined action that formerly pressurizes after vacuum enters step 1) in the foamy carbon raw material hole that obtains, aging until form organic aerogel under 75～90 DEG C of water bath condition; The foamy carbon raw material of filling organic aerogel unnecessary aerogel is around removed, obtained the foamy carbon raw material that organic aerogel is filled;
4) organic aerogel is dry: by step 3) the foamy carbon raw material seasoning at normal temperatures and pressures of filling of the organic aerogel that obtains is until constant weight obtains the gel-filled foamy carbon raw material of dry gas, or by step 3) organic aerogel that obtains foamy carbon raw material dry gel-filled foamy carbon raw material of dry gas that obtain in supercritical co, ethanol or sherwood oil environment of filling;
5) pyroprocessing forms carbon aerogels filled-type high heat conducting foam carbon: by step 4) the gel-filled foamy carbon raw material of the dry gas that obtains are under protection of inert gas, temperature rise rate according to 0.5 DEG C/min～5 DEG C/min is warming up to T1, constant temperature 0.5h～5h forms carbonization filled-type foamy carbon material, then be warming up to T2 according to the temperature rise rate of 0.2 DEG C/min～10 DEG C/min, constant temperature 0.5h～5h, obtains the high heat conducting foam carbon material that carbon aerogels is filled;
Step 1) in blowing temperature be SP+ (150～300 DEG C), the softening temperature that wherein SP is mesophase pitch; Or step 1) in blowing temperature be SP+ (300～600 DEG C), the softening temperature that wherein SP is mesophase pitch;
Step 2) described in catalyzer be hexamethylenetetramine, salt of wormwood, sodium carbonate, hydrochloric acid or ammoniacal liquor; The volume of described catalyzer is 0.1%～1% of liquor capacity;
Step 2) described in solvent be alcohols material or deionized water; The ratio of the mixture of solvent and Resorcinol and formaldehyde is 100ml:(3～30g); Described alcohols material is methyl alcohol, ethanol or propyl alcohol;
Step 5) described in T1 within the scope of 900 DEG C～1500 DEG C; Described T2 is within the scope of 2800 DEG C～3000 DEG C.
2. the preparation method of filled-type high heat conducting foam carbon material for energy storage according to claim 1, is characterized in that: step 1) described in mesophase pitch be that naphthalene is the mixture of any or they in mesophase pitch, coal measures mesophase pitch and petroleum mesophase pitch.
3. the preparation method of filled-type high heat conducting foam carbon material for energy storage according to claim 1, is characterized in that: step 4) in before dry, with acetone, the water in aerogel, alcohol are carried out to pre-permutation.
4. the preparation method of filled-type high heat conducting foam carbon material for energy storage according to claim 1, is characterized in that: repeating step 3), 4) and 5) process carries out 1～2 time.
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| CN104893674B (en) * | 2015-06-03 | 2018-05-18 | 中国科学院空间应用工程与技术中心 | A kind of foamy carbon/paraffin class phase change composite material and its method for packing |
| CN106045554A (en) * | 2016-05-30 | 2016-10-26 | 南京工业大学 | Phase-change material doped SiO 2 aerogel composite heat-insulating material and preparation method thereof |
| CN106085367B (en) * | 2016-06-17 | 2019-10-18 | 航天材料及工艺研究所 | A kind of flexibility fixed phase change heat-barrier material and preparation method thereof |
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| CN111117575A (en) * | 2019-12-31 | 2020-05-08 | 中国电子科技集团公司第三十八研究所 | Modification method of phase change energy storage material |
| CN114552051A (en) * | 2021-07-21 | 2022-05-27 | 万向一二三股份公司 | Battery module and heat-conducting plate for enhancing heat dissipation of battery module |
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