CN107473199A - A kind of high intensity large scale bulk charcoal-aero gel and its preparation method and application - Google Patents
A kind of high intensity large scale bulk charcoal-aero gel and its preparation method and application Download PDFInfo
- Publication number
- CN107473199A CN107473199A CN201610402653.1A CN201610402653A CN107473199A CN 107473199 A CN107473199 A CN 107473199A CN 201610402653 A CN201610402653 A CN 201610402653A CN 107473199 A CN107473199 A CN 107473199A
- Authority
- CN
- China
- Prior art keywords
- charcoal
- aero gel
- gel
- large scale
- high intensity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000004964 aerogel Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 13
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003610 charcoal Substances 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000003763 carbonization Methods 0.000 claims abstract description 3
- 230000008859 change Effects 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 238000002791 soaking Methods 0.000 claims description 18
- 239000000499 gel Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000011240 wet gel Substances 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 5
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 239000007772 electrode material Substances 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- 229910052799 carbon Inorganic materials 0.000 description 14
- 230000002708 enhancing effect Effects 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 5
- -1 37wt.% formalins Chemical compound 0.000 description 4
- 239000004966 Carbon aerogel Substances 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000008236 heating water Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000001994 activation Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000000352 supercritical drying Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000010327 methods by industry Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000005658 nuclear physics Effects 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/21—Attrition-index or crushing strength of granulates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of high intensity large scale bulk charcoal-aero gel and its preparation method and application, belong to charcoal-aero gel preparing technical field.Using resorcinol and formaldehyde as raw material, natrium carbonicum calcinatum is catalyst, and deionized water is solvent, and the high intensity large scale bulk charcoal-aero gel is prepared after solgel reaction, then through constant pressure and dry and high temperature carbonization.Size >=100mm × 100mm × 30mm of gained bulk charcoal-aero gel, with the change of charcoal-aero gel density, its charcoal particle size is adjustable between 30 800nm, and three-dimensional network skeleton structure is interconnected to form between charcoal particle.The 0.6g/cm of charcoal-aero gel density 0.3 prepared by the present invention3, compressive strength is up to 10 65MPa, and thermal conductivity is 0.06 0.09W/ (mK), may be directly applied to heat-barrier material.
Description
Technical field
The present invention relates to charcoal-aero gel preparing technical field, and in particular to a kind of high intensity large scale bulk charcoal-aero gel and
Its preparation method and application.
Background technology
Aeroge is made up of the network of nanoparticles loose structure of uniqueness, as a kind of " ultra heat insulating material " always by
To extensive concern, SiO common are2、Al2O3、ZrO2, charcoal-aero gel etc..Although the thermal conductivity of aerogel material is very low, its
Solid skeleton particle easily sinters at high temperature, is restricted its resistance to elevated temperatures.SiO2The maximum operation (service) temperature of aeroge
800 DEG C are usually no more than, Al2O3The maximum operation (service) temperature of aeroge is usually no more than 1100 DEG C, and ZrO2The highest of aeroge makes
It it is only~600 DEG C with temperature.Charcoal-aero gel has very high heat endurance, remains to keep mesoporous under 2800 DEG C of inert atmosphere
Structure, more than 2200 DEG C are can reach as heat-barrier material temperature in use, be that temperature resistant capability is best under current vacuum or inert atmosphere
Ultra heat insulating material.
However, the problems such as poor mechanical property of charcoal-aero gel, block difficult forming, still governs its application.Charcoal-aero gel
Preparation method mainly have：Supercritical drying and atmosphere pressure desiccation.Supercritical drying has that gel shrinks rate is small, compares surface
The features such as product is big, good moldability, higher intensity.But the method equipment is complicated, cost of manufacture is expensive, has potential safety hazard, so as to limit
Its application is made.Atmosphere pressure desiccation is low for equipment requirements, low manufacture cost, size adjusting is flexible, security is good, and its shortcoming is
Organic aerogel easily produces serious volume contraction or even ftractureed under the strong surface tension effects of solvent, causes large scale charcoal
Aeroge difficult forming, and low strength (Porous Mater, 2008,15:29-34；Process engineering journal, 2004,4 (5):
429-433；Adv Mater,2011,18(16):2073-2094).Mutually come often through addition enhancing in actual use
Improve the mechanical property of charcoal-aero gel, the enhancing that uses at present mutually based on carbon fiber, in addition with carbosphere, graphene and
Carbon foams etc. are as enhancing phase.Addition enhancing can mutually improve the mechanical property of material to a certain extent really, but also band simultaneously
Carry out the decline of other performances of material.For example, once someone uses atmosphere pressure desiccation to be prepared for density as 0.52g/cm3, bending strength
It is respectively 7.1MPa and 0.328W/ (mK) fibre reinforced carbon aerogel composite material with 300 DEG C of thermal conductivities, its intensity carries
It is high by 57.8%, and thermal conductivity also improve 18.8% (ACS Appl Mater Interfaces, 2011,3:4796-
4803).However, the research for the purpose of improving charcoal-aero gel intrinsic strength both at home and abroad and few, Main way is organogel
Surface be modified, such as by adding surfactant in gel process, the hydrophily of gel surface is reduced, so as to reduce gel
Shrinkage stress in the drying process, and maintenance frame strength (Carbon, 2004,42:2033-2039).This method reduces
The solvent surface tension being subject to during constant pressure and dry, but due to no improvement original network structure of organogel, strength enhancing effect
Fruit is limited.
The content of the invention
It is an object of the invention to provide a kind of high intensity large scale bulk charcoal-aero gel and its preparation method and application, leads to
Cross refinement organic nano cluster and improve the organic product degree of cross linking, and then realize prepared by the bulk of high-strength charcoal-aero gel.
To achieve the above object, the technical solution adopted in the present invention is as follows：
A kind of preparation method of high intensity large scale bulk charcoal-aero gel, this method are using resorcinol and formaldehyde as original
Material, natrium carbonicum calcinatum is catalyst, and deionized water is solvent, after sol gel reaction, then is replaced through solvent, constant pressure and dry
The high intensity large scale bulk charcoal-aero gel is prepared with high temperature carbonization.
The inventive method specifically comprises the following steps：
(1) solution is prepared：By resorcinol, 37wt.% formalins, deionized water and natrium carbonicum calcinatum according to (380
~2700)：(450~3060)：(860~5800)：1 part by weight is well mixed, and obtains mixed liquor；
(2) collosol and gel：Mixed liquor obtained by step (1) is placed in 15-95 DEG C of water-bath, obtained after being incubated 60-200 hours
The organic wet gel of kermesinus；In the step, when bath temperature is adjusted into 15~45 DEG C, soaking time 30-80 hours；By water-bath temperature
When degree is adjusted to 45~65 DEG C, soaking time 20-70 hours；When bath temperature is adjusted into 65~95 DEG C, soaking time 10-50 is small
When；
(3) solvent is replaced：Organic wet gel obtained by step (2) is soaked in alcohol solvent, the volume of alcohol solvent is
5~10 times of organic wet gel volume, soaking temperature are controlled between 40~60 DEG C, and immersion poured out ethanol after 12 hours, and
Repeat the process three times more than；
(4) constant pressure and dry：Gel after solvent is replaced is put into constant pressure and dry case, and temperature is set to 30~60 DEG C, dries 2
~10 days, obtain xerogel (according to product size adjustment drying time of different sizes)；
(5) charing process：Xerogel obtained by step (4) is put into vacuum carbonized stove and carbonized under inert atmosphere conditions,
2~10 DEG C/min of programming rate, charing final temperature is 900 DEG C, and is incubated two hours.The high intensity large scale is obtained after charing
Block charcoal-aero gel.
Size >=100mm × 100mm × 30mm of prepared charcoal-aero gel, with the change of charcoal-aero gel density, its
Charcoal particle size is adjustable between 30-800nm, and three-dimensional network skeleton structure is interconnected to form between charcoal particle.
The density of the charcoal-aero gel is 0.3-0.6g/cm3, compressive strength 10-65MPa, thermal conductivity 0.06-
0.09W/(m·K)。
Material of the present invention may be directly applied to heat-barrier material, can also pass through CO2The methods of activation, heat treatment, carries high-ratio surface
Product and electrical conductivity, applied to directions such as catalysis, absorption, capacitors.
Design principle of the present invention and have the beneficial effect that：
The present invention starts with from the intrinsic mechanical property of charcoal-aero gel is improved, using atmosphere pressure desiccation, by refining organic nano
Cluster simultaneously improves the organic product degree of cross linking, and then realizes prepared by the bulk of high-strength charcoal-aero gel.The present invention passes through collosol and gel mistake
The control of journey, hence it is evident that refined organic nano cluster size, and effectively increased the degree of cross linking of organogel.Carbon particle size
Refinement and the optimization of network skeleton structure so that charcoal-aero gel has evenly load-carrying construction, effectively suppresses due to stress concentration
Caused crack growth, so as to improve the intensity of the forming ability of large scale aeroge and aeroge.
Gained charcoal-aero gel of the invention has greatly compared to the high-strength carbon aeroge reported in existing literature, compressive strength
Width improves.Density is respectively 0.31,0.45,0.57g/cm3Charcoal-aero gel, intensity is up to 10 respectively, 28,64MPa, and document
Middle reported density be 0.26,0.35,0.48,0.59g/cm3Charcoal-aero gel, intensity is respectively 2,9,7,20MPa
(Langmuir,2007,23:10095-10101；Phys Chem Chem Phys,2010,12:10365-10372)；Meanwhile
The aeroge also has a very low thermal conductivity, respectively 0.065,0.070,0.085W/ (mK).
Gained charcoal-aero gel of the invention is to improve the intrinsic strong of charcoal-aero gel by changing charcoal-aero gel self structure
Degree, other elements or addition enhancing phase are not adulterated.It can be doped or add on the basis of the present invention according to being actually needed
Add enhancing phase, to obtain other species high-strength carbon aeroges.
High-strength carbon aeroge of the present invention not only has huge application value in anti-heat-insulated field, because its had into
Type ability and structural strength, by means such as technique adjustment, heat treatment, activation process, ultracapacitor, catalyst carrier,
The fields such as hydrogen storage, nuclear physics equally have good application prospect.
Brief description of the drawings
Fig. 1 is carbon aerogel particle size and schematic network structure；Wherein：(a) before modified technique, (b) modified technique
Afterwards.
Fig. 2 is 100mm × 100mm × 30mm large scale charcoal-aero gel macro morphologies.
Fig. 3 is bulk density 0.31g/cm3, compressive strength 10MPa charcoal-aero gel SEM microstructure morphologies.
Fig. 4 is bulk density 0.45g/cm3, compressive strength 28MPa charcoal-aero gel SEM microstructure morphologies.
Fig. 5 is bulk density 0.57g/cm3, compressive strength 64MPa charcoal-aero gel SEM microstructure morphologies.
Embodiment
For a further understanding of the present invention, present invention is described with reference to embodiments, but embodiment is only to this
The characteristics of invention and advantage are further elaborated, rather than limiting to the claimed invention.
The present invention is using resorcinol, formaldehyde, deionized water and sodium carbonate as raw material, with certain heating rate in water-bath
Collosol and gel polycondensation is carried out with the time, is replaced using alcohol solvent, constant pressure and dry obtains organic aerogel, and organic aerogel is existed
Charing obtains high-strength carbon aerogel block body under inert atmosphere.In following embodiment, according to different raw material proportioning and technique
Parameter, obtain the high-strength carbon aeroge of different structure, density and performance.
Embodiment 1：
By resorcinol, 37wt.% formalins, deionized water, natrium carbonicum calcinatum using mass ratio as 2637：2637：
5776：1 ratio uniform mixing and heating water bath, when bath temperature is adjusted into 15 DEG C, soaking time 30 hours；By bath temperature
When being adjusted to 45 DEG C, soaking time 20 hours；When bath temperature is adjusted into 65 DEG C, soaking time 20 hours；Bath temperature is adjusted to
At 95 DEG C, soaking time 10 hours, wet gel is obtained.By obtained wet gel at 50 DEG C, 10 times of gel volumes it is anhydrous
Soaked 24 hours in ethanol, and repeat the step 4 time.Afterwards, by wet gel in constant pressure and dry stove 50 DEG C of dryings 7 days.Will be dry
Gel after dry is placed in retort under argon gas protection in room temperature to 900 DEG C, and heating rate is 5 DEG C/min, and insulation two is small
When after furnace cooling, obtain high-strength carbon aeroge.
Fig. 1 compared for the microstructure before the present embodiment and process modification.It is apparent that improve work through the present embodiment
After skill, carbon particle size is reduced to 300nm or so from 550nm or so；The connected mode of carbon particle cluster is not only even closer, and
And the form interconnected from single point-to-point Innovation of Connection to multiple spot, three-dimensional network skeleton knot is interconnected to form between carbon particle
Structure.The refinement of carbon particle size and the optimization of network skeleton structure so that charcoal-aero gel has evenly load-carrying construction, effectively suppression
System is due to crack growth caused by stress concentration, so as to improve the intensity of the forming ability of large scale aeroge and aeroge.
The present invention is started with by improving charcoal-aero gel intrinsic strength, greatly reduces non-homogeneous stress when large scale aeroge is dried,
So as to alleviate the problems of crack caused by internal stress after drying.The charcoal-aero gel size that the present embodiment obtains is up to 100 × 100
× 30mm (length × width × height), and without cracked (Fig. 2).
The charcoal-aero gel bulk density that the present embodiment obtains is 0.31g/cm3, compressive strength 10MPa, thermal conductivity is
0.065W/ (mK), microstructure morphology is as shown in Figure 3 under ESEM.
Embodiment 2：
By resorcinol, 37wt.% formalins, deionized water, natrium carbonicum calcinatum using mass ratio as 1030：1530：
2880：1 ratio uniform mixing, obtains mixed liquor and heating water bath, when bath temperature is adjusted into 30 DEG C, soaking time 50 is small
When；When bath temperature is adjusted into 50 DEG C, soaking time 50 hours；When bath temperature is adjusted into 75 DEG C, soaking time 30 hours；Will
When bath temperature is adjusted to 95 DEG C, soaking time 10 hours, wet gel is obtained.By obtained wet gel at 50 DEG C, 10 times solidifying
Soaked 24 hours in the absolute ethyl alcohol of colloid product, and repeat the step 4 time.Afterwards, by obtained wet gel in constant pressure and dry stove
Interior 50 DEG C of dryings 7 days.Dried gel is placed in retort under argon gas protection in room temperature to 900 DEG C, heating rate
For 5 DEG C/min, furnace cooling after being incubated two hours, high-strength carbon aeroge is obtained.
The charcoal-aero gel bulk density that the present embodiment obtains is 0.45g/cm3, compressive strength 28MPa, thermal conductivity is
0.070W/ (mK), microstructure morphology is as shown in Figure 4 under ESEM.
Embodiment 3：
By resorcinol, 37wt.% formalins, deionized water, natrium carbonicum calcinatum using mass ratio as 520：760：1440：
1 ratio uniform mixing and heating water bath：By bath temperature be adjusted to for 45 DEG C when, soaking time 80 hours；Bath temperature is adjusted
During to 65 DEG C, soaking time 70 hours；When bath temperature is adjusted into 95 DEG C, soaking time 50 hours, wet gel is obtained.It will obtain
Wet gel soaked 24 hours in the absolute ethyl alcohol of 10 times of gel volumes under the conditions of 50 DEG C, and repeat the step 4 time.It
Afterwards, by obtained wet gel in constant pressure and dry stove 50 DEG C of dryings 7 days.Dried gel is placed in into argon gas in retort to protect
Under in room temperature to 900 DEG C, heating rate is 5 DEG C/min, insulation two hours after furnace cooling, obtain high-strength carbon airsetting
Glue.
The charcoal-aero gel bulk density that the present embodiment obtains is 0.57g/cm3, compressive strength 64MPa, thermal conductivity is
0.085W/ (mK), microstructure morphology is as shown in Figure 5 under ESEM.
Claims (7)
- A kind of 1. preparation method of high intensity large scale bulk charcoal-aero gel, it is characterised in that：This method be with resorcinol and Formaldehyde is raw material, and natrium carbonicum calcinatum is catalyst, and deionized water is solvent, after sol gel reaction, then replace through solvent, Constant pressure and dry and high temperature carbonization prepare the high intensity large scale bulk charcoal-aero gel.
- 2. the preparation method of high intensity large scale bulk charcoal-aero gel according to claim 1, it is characterised in that：This method Specifically comprise the following steps：(1) solution is prepared：By resorcinol, formalin, deionized water and natrium carbonicum calcinatum according to (380~2700)： (450~3060)：(860~5800)：1 part by weight is well mixed, and obtains mixed liquor；(2) collosol and gel：Mixed liquor obtained by step (1) is placed in 15-95 DEG C of water-bath, obtained after being incubated 60-200 hours organic Wet gel；(3) solvent is replaced：Organic wet gel obtained by step (2) is soaked in alcohol solvent, soaking temperature is controlled 40~60 Between DEG C, immersion 12 hours after ethanol is poured out, and repeat the step three times more than；(4) constant pressure and dry：Gel after solvent is replaced is put into constant pressure and dry case, and temperature is set to 30~60 DEG C, according to product It is of different sizes, dry 2~10 days, obtain xerogel；(5) charing process：Xerogel obtained by step (4) is put into vacuum carbonized stove and carbonized under inert atmosphere conditions, is heated up 2~10 DEG C/min of speed, charing final temperature is 900 DEG C, and is incubated two hours.It is block that the high intensity large scale is obtained after charing Charcoal-aero gel.
- 3. the preparation method of high intensity large scale bulk charcoal-aero gel according to claim 2, it is characterised in that：Step (2) in, when bath temperature is adjusted into 15~45 DEG C, soaking time 30-80 hours；When bath temperature is adjusted into 45~65 DEG C, protect Warm time 20-70 hours；When bath temperature is adjusted into 65~95 DEG C, soaking time 10-50 hours.
- 4. the high intensity large scale bulk charcoal-aero gel that according to claim 1 prepared by method, it is characterised in that：The bulk Size >=100mm × 100mm × 30mm of charcoal-aero gel, three-dimensional network skeleton structure is interconnected to form between charcoal particle, with The change of charcoal-aero gel density, its charcoal particle size is adjustable between 30-800nm.
- 5. high intensity large scale bulk charcoal-aero gel according to claim 4, it is characterised in that：The charcoal-aero gel it is close Spend for 0.3-0.6g/cm3, compressive strength 10-65MPa.
- 6. high intensity large scale bulk charcoal-aero gel according to claim 5, it is characterised in that：The heat of the charcoal-aero gel Conductance is 0.06-0.09W/ (mK).
- 7. the application of high intensity large scale bulk charcoal-aero gel according to claim 4, it is characterised in that：The charcoal-aero gel It can be applied to heat-barrier material, catalysis material, sorbing material or electrode material.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610402653.1A CN107473199A (en) | 2016-06-08 | 2016-06-08 | A kind of high intensity large scale bulk charcoal-aero gel and its preparation method and application |
| PCT/CN2017/086920 WO2017211227A1 (en) | 2016-06-08 | 2017-06-02 | High-strength large dimension block-form aerographite, and manufacturing method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610402653.1A CN107473199A (en) | 2016-06-08 | 2016-06-08 | A kind of high intensity large scale bulk charcoal-aero gel and its preparation method and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107473199A true CN107473199A (en) | 2017-12-15 |
Family
ID=60594442
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610402653.1A Pending CN107473199A (en) | 2016-06-08 | 2016-06-08 | A kind of high intensity large scale bulk charcoal-aero gel and its preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107473199A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108285135A (en) * | 2018-04-03 | 2018-07-17 | 上海电力学院 | A kind of preparation method of desulfurizing agent for high-temp gas carrier charcoal-aero gel |
| CN108609606A (en) * | 2018-06-25 | 2018-10-02 | 中国人民解放军国防科技大学 | Preparation method of carbon aerogel heat insulation material |
| CN108726501A (en) * | 2018-05-23 | 2018-11-02 | 东莞理工学院 | A method of preparing charcoal-aero gel with infiltration evaporation membrane separation device |
| CN108975300A (en) * | 2017-06-02 | 2018-12-11 | 中国科学院金属研究所 | High-intensitive large scale bulk charcoal-aero gel and its preparation method and application |
| CN110746833A (en) * | 2019-11-18 | 2020-02-04 | 湖南道尔顿新材料科技有限公司 | Waterproof heat-insulating coating and preparation method thereof |
| CN110951103A (en) * | 2019-12-10 | 2020-04-03 | 中国科学院金属研究所 | Carbon fiber reinforced phenolic aerogel composite material, preparation method thereof and carbon fiber reinforced carbon aerogel composite material |
| CN111019321A (en) * | 2019-11-27 | 2020-04-17 | 内蒙古民族大学 | High-molecular heat-insulating material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1462723A (en) * | 2003-06-07 | 2003-12-24 | 大连理工大学 | Method for preparing nano material of gel of charcoal gas |
| CN1830769A (en) * | 2006-03-15 | 2006-09-13 | 大连理工大学 | Preparation method of high superficial area porous carbon material |
| CN102515143A (en) * | 2011-12-23 | 2012-06-27 | 天津鑫日新能源科技有限公司 | Nano-grade porous aerogel and preparation method thereof |
-
2016
- 2016-06-08 CN CN201610402653.1A patent/CN107473199A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1462723A (en) * | 2003-06-07 | 2003-12-24 | 大连理工大学 | Method for preparing nano material of gel of charcoal gas |
| CN1830769A (en) * | 2006-03-15 | 2006-09-13 | 大连理工大学 | Preparation method of high superficial area porous carbon material |
| CN102515143A (en) * | 2011-12-23 | 2012-06-27 | 天津鑫日新能源科技有限公司 | Nano-grade porous aerogel and preparation method thereof |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108975300A (en) * | 2017-06-02 | 2018-12-11 | 中国科学院金属研究所 | High-intensitive large scale bulk charcoal-aero gel and its preparation method and application |
| CN108285135A (en) * | 2018-04-03 | 2018-07-17 | 上海电力学院 | A kind of preparation method of desulfurizing agent for high-temp gas carrier charcoal-aero gel |
| CN108726501A (en) * | 2018-05-23 | 2018-11-02 | 东莞理工学院 | A method of preparing charcoal-aero gel with infiltration evaporation membrane separation device |
| CN108726501B (en) * | 2018-05-23 | 2019-04-05 | 东莞理工学院 | A method of charcoal-aero gel is prepared with infiltration evaporation membrane separation device |
| CN108609606A (en) * | 2018-06-25 | 2018-10-02 | 中国人民解放军国防科技大学 | Preparation method of carbon aerogel heat insulation material |
| CN108609606B (en) * | 2018-06-25 | 2020-03-06 | 中国人民解放军国防科技大学 | Preparation method of carbon aerogel heat insulation material |
| CN110746833A (en) * | 2019-11-18 | 2020-02-04 | 湖南道尔顿新材料科技有限公司 | Waterproof heat-insulating coating and preparation method thereof |
| CN111019321A (en) * | 2019-11-27 | 2020-04-17 | 内蒙古民族大学 | High-molecular heat-insulating material and preparation method thereof |
| CN110951103A (en) * | 2019-12-10 | 2020-04-03 | 中国科学院金属研究所 | Carbon fiber reinforced phenolic aerogel composite material, preparation method thereof and carbon fiber reinforced carbon aerogel composite material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107473199A (en) | A kind of high intensity large scale bulk charcoal-aero gel and its preparation method and application | |
| CN110951210B (en) | High-strength nanopore ceramic ablation heat-proof composite material and preparation method thereof | |
| CN105541389B (en) | A kind of barium titanate foamed ceramics/thermoset ting resin composite and preparation method thereof | |
| CN108975300A (en) | High-intensitive large scale bulk charcoal-aero gel and its preparation method and application | |
| CN114524674B (en) | Heat-proof, heat-insulation and load-bearing integrated light carbon-ceramic composite material and preparation method thereof | |
| CN103044057B (en) | Carbon foam in-situ reinforced carbon aerogel high-temperature thermal insulation material and preparation method thereof | |
| US9869422B2 (en) | Method for preparing bulk C—AlN composite aerogel with high strength and high temperature resistance | |
| CN109251005B (en) | Preparation method of reinforced silica aerogel material | |
| CN108329046A (en) | Preparation method of carbon aerogel heat insulation composite material | |
| CN104261798A (en) | High-temperature-resistant SiCOB aerogel heat-insulation composite material and preparation method thereof | |
| CN104446656A (en) | Method for preparing oxidation resistant coating of porous carbon material | |
| CN108862234A (en) | A kind of preparation method of fibre reinforced carbon aerogel composite material | |
| CN103965505A (en) | Polyimide aerogel having infrared radiation resisting property and preparation method thereof | |
| CN106633652A (en) | Preparation method of bicontinuous-phase alumina/epoxy resin composite material | |
| CN113663611B (en) | High-temperature-resistant composite nanofiber aerogel material and preparation method thereof | |
| CN113831581B (en) | High-elasticity anti-radiation nanofiber aerogel material and preparation method thereof | |
| CN113248775A (en) | Bacterial cellulose-silicon dioxide P-COF aerogel and preparation method and application thereof | |
| CN111647293A (en) | Infrared radiation insulating coating, coating thereof and preparation method thereof | |
| CN107473761B (en) | Heat-proof and load-bearing integrated carbon aerogel/ceramic layered composite material and preparation method and application thereof | |
| CN103588495A (en) | Preparation method of low-heat-conduction processable ceramic matrix composite material | |
| CN108484097B (en) | Preparation method of lignin-enhanced silicon dioxide aerogel felt | |
| CN108609603B (en) | Carbon foam containing graphene coating and preparation method thereof | |
| CN104276835A (en) | Preparation method of carbon/carbon composite thermal insulation material containing anti-oxidization coating | |
| WO2017211227A1 (en) | High-strength large dimension block-form aerographite, and manufacturing method and application thereof | |
| CN112679793A (en) | Preparation and application of light, heat-insulating and flame-retardant PIPD nanofiber aerogel |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171215 |
|
| RJ01 | Rejection of invention patent application after publication |