CN103933900A - Method for preparing resorcinol-formaldehyde aerogel - Google Patents
Method for preparing resorcinol-formaldehyde aerogel Download PDFInfo
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- CN103933900A CN103933900A CN201410160787.8A CN201410160787A CN103933900A CN 103933900 A CN103933900 A CN 103933900A CN 201410160787 A CN201410160787 A CN 201410160787A CN 103933900 A CN103933900 A CN 103933900A
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- resorcinol
- formaldehyde
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- aeroge
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Abstract
The invention provides a method for preparing resorcinol-formaldehyde aerogel. The preparation method comprises the following steps: adding a certain amount of water-soluble and neutral light initiator to a reaction of base catalysis of resorcinol-formaldehyde aerogel, and synthesizing organic aerogel under ultraviolet light irradiation. The method has the characteristics that by virtue of the selected water-soluble and neutral light initiator, the structure of the organic aerogel is not greatly changed due to introduction of the light initiator besides that the gelation time of a resorcinol-formaldehyde solution can be greatly shortened. The resorcinol-formaldehyde aerogel and a derivative, carbon aerogel, thereof prepared by the method disclosed by the invention can be applied to related fields of a laser inertial confinement fusion target material, a supercapacitor electrode material, a lithium battery electrode material, a hydrogen storage material, a thermal insulation material, other composite nano materials and the like.
Description
Technical field
The invention belongs to aeroge preparation field, be specifically related to a kind of preparation method of resorcinol-formaldehyde aeroge.
Background technology
Resorcinol-formaldehyde aeroge has nanometer porous network structure, specific area is high, pore structure is adjustable, density is adjustable in a big way, radioresistance, the feature such as transparent, thereby makes it have extensive use in association areas such as laser inertial confinement fusion target material, electrode material for super capacitor, electrode material of lithium battery, hydrogen storage material, heat-barrier materials.
The preparation method of resorcinol-formaldehyde aeroge is mainly sol-gel process at present.With the greatest problem that the method is prepared resorcinol-formaldehyde aeroge be need to be longer preparation time.Conventionally adopt the method to need 3～5 days ability gels, this has limited the application of resorcinol-formaldehyde aeroge.
The current domestic patent that resorcinol formaldehyde aerogels is relevant that do not have, can consult the only patent about ultraviolet light polymerization aspect.If the patent No. is CN 103333648 " a kind of preparation method who utilizes light polymerization method synthesizing ultraviolet solidified pressure-sensitive ", introduces and adopted ultraviolet lamp to irradiate the method for free radical photo-initiation solidified pressure-sensitive; The patent No. be CN's 103396722 " fluorine-alcohol modified epoxy coating of a kind of water-based UV-curable and preparation method thereof ", introduced fluorine-alcohol modified epoxy resin that first utilizes solution polymerization process to prepare water-based uV curable etc.
Summary of the invention
The technical barrier that the present invention will solve is to provide a kind of preparation method of resorcinol-formaldehyde aerogel block body.
The preparation method of resorcinol-formaldehyde aeroge of the present invention, comprises following step successively:
The preparation of a, resorcinol-formaldehyde solution
Resorcinol, formaldehyde, sodium carbonate and water are mixed in proportion, stir, until dissolve completely;
B, step a gained solution is placed, until solution will be from water white transparency yellowing solution, placed cool to room temperature;
C, step b gained solution is added to light trigger, fully stir, dissolve;
D, step c gained solution is irradiated with ultraviolet light, become gel until solution loses flowability;
E, steps d gained gel is carried out to exchange of solvent with acetone or aqueous isopropanol;
F, gained gel in step e is put into supercritical extract instrument, carry out CO 2 supercritical dry.
Resorcinol, formaldehyde amount of substance ratio in described step a are 2:1, and the amount of substance of resorcinol, sodium carbonate is than being 250:1-25:1.
In described step c, light trigger is: the acetophenone derivs, the nonionic long-chain oxethyl-diphenyl-ketone analog derivative that contain water soluble sidechains, contain the one in the follow-on benzoyl type of neutral side chain compound.
The amount of the light trigger in described step c is 2wt%-14wt%.
In described steps d, ultraviolet source used is high-pressure sodium lamp.
Beneficial effect of the present invention is: resorcinol-formaldehyde aeroge of the present invention is synthetic is to adopt ultraviolet light initiation legal system standby, and reaction rate is very fast, greatly Reaction time shorten; Course of reaction is controlled, by regulating sample to control reaction rate and the extent of reaction apart from the position of light source, has obtained having the resorcinol-formaldehyde aeroge of certain productive rate.The resorcinol-formaldehyde aeroge obtaining, light trigger does not participate in the formation of aeroge skeleton.The resorcinol-formaldehyde aeroge that the present invention prepares still has specific pore structure and porosity, can be used in the association areas such as laser inertial confinement fusion target material, electrode material for super capacitor, electrode material of lithium battery, hydrogen storage material, heat-barrier material and other nano material.
Brief description of the drawings
Fig. 1 is the scanning electron microscope image that causes the standby resorcinol-formaldehyde aeroge of legal system with ultraviolet light;
Fig. 2 is the suction-attached desorption curve of the resorcinol-formaldehyde aeroge prepared by ultraviolet light initiation method;
Fig. 3 is the infrared spectrum curve of the resorcinol-formaldehyde aeroge prepared by ultraviolet light initiation method.
Specific embodiments
Further illustrate below in conjunction with accompanying drawing specific embodiment.
Embodiment 1 utilizes ultraviolet light to cause legal system for resorcinol formaldehyde aerogels
First configure certain density resorcinol formaldehyde solution 30ml, solution composition is: the sodium carbonate liquor of the resorcinol of 0.9706g, the 0.05mol/L of 0.88ml, the formalin of 1.33ml stir it is fully mixed, in the waters of 60 DEG C, place 30min, cool to room temperature, the light trigger 659 that adds 10wt%, mixes, and moves 0.1ml and seals to little container, with wave-length coverage 250-720nm, apart from being 2cm, light intensity is 18.26w/cm
3high voltage mercury lamp radiation.The time that definition solution loses flowability is gel time.The resorcinol-formaldehyde aeroge of making after 35min.The specific area of resorcinol-formaldehyde aeroge is 433m
2/ g, total pore volume 4.77cm
3/ g, average pore size 2.996nm.
Embodiment 2 utilizes ultraviolet light to cause legal system for resorcinol formaldehyde aerogels
According to the preparation process of the resorcinol-formaldehyde aeroge described in embodiment 1, difference is, be 40min the water-bath standing time in parameter, the resorcinol-formaldehyde aeroge of 15min system.The specific area of prepared resorcinol formaldehyde aerogels is 294m
2/ g, total pore volume is 2.502cm
3/ g, average pore size is 2.384nm.Fig. 1 is the scanning electron microscope image of sample, as can be seen from the figure causes the standby RF of legal system with ultraviolet light and has certain network structure, and exist certain pore structure.Fig. 2 is the adsorption/desorption curve of sample, can calculate specific area, total pore volume and average pore size with adsorbing software.Fig. 3 is the infrared spectrum curve of sample, can find out that causing the standby RF aeroge of legal system with ultraviolet light does not have characteristic absorption peak 1114.3 cm of methylene ether link from infrared spectrum
-1existence, hence one can see that with ultraviolet light cause legal system be to be mainly cross-linked and not have the non-crystalline solids material with spacial framework being cross-linked to form by methylene ether link by methene key for RF aeroge.
Embodiment 3 utilizes ultraviolet light to cause legal system for resorcinol formaldehyde aerogels
With reference to the preparation process of the resorcinol-formaldehyde aeroge described in embodiment 1, difference is, be 50min the water-bath standing time in parameter.The resorcinol-formaldehyde aeroge of 25min system.The specific area of resorcinol-formaldehyde aeroge is 260m
2/ g, total pore volume 2.370m
3/ g, average pore size 3.996nm.
Embodiment 4 utilizes ultraviolet light to cause legal system for resorcinol formaldehyde aerogels
With reference to the preparation process of the resorcinol-formaldehyde aeroge described in embodiment 1, difference is, be 60min the water-bath standing time in parameter.The resorcinol-formaldehyde aeroge of 25min system.The specific area of resorcinol-formaldehyde aeroge is 239 m
2/ g, total pore volume 2.060cm
3/ g, average pore size 4.060nm.
Embodiment 5 utilizes ultraviolet light to cause legal system for resorcinol formaldehyde aerogels
With reference to the preparation process of the resorcinol-formaldehyde aeroge described in embodiment 1, difference is, be 40min the water-bath standing time in parameter, and the amount that adds light trigger is 2%.The resorcinol-formaldehyde aeroge of 35min system.The specific area of resorcinol-formaldehyde aeroge is 396m
2/ g, total pore volume 4.600 cm
3/ g, average pore size 1.986nm.
Embodiment 6 utilizes ultraviolet light to cause legal system for resorcinol formaldehyde aerogels
With reference to the preparation process of the resorcinol-formaldehyde aeroge described in embodiment 1, difference is, be 40min the water-bath standing time in parameter, and the amount that adds light trigger is 4%.The resorcinol-formaldehyde aeroge of 35min system.Prepare the scanning electron microscope (SEM) photograph of sample as shown in Figure 3, infared spectrum as shown in Figure 2.The specific area of resorcinol-formaldehyde aeroge is 339m
2/ g, total pore volume 3.899cm
3/ g, average pore size 2.010nm.
Embodiment 7 utilizes ultraviolet light to cause legal system for resorcinol formaldehyde aerogels
With reference to the preparation process of the resorcinol-formaldehyde aeroge described in embodiment 1, difference is, be 40min the water-bath standing time in parameter, and the amount that adds light trigger is 6%.The resorcinol-formaldehyde aeroge of 25min system.The specific area of resorcinol-formaldehyde aeroge is 326m
2/ g, total pore volume 3.760cm
3/ g, average pore size 2.109nm.
Embodiment 8 utilizes ultraviolet light to cause legal system for resorcinol formaldehyde aerogels
With reference to the preparation process of the resorcinol-formaldehyde aeroge described in embodiment 1, difference is, be 40min the water-bath standing time in parameter, and the amount that adds light trigger is 8%.The resorcinol-formaldehyde aeroge of 25min system.The specific area of resorcinol-formaldehyde aeroge is 301m
2/ g, total pore volume 2.971 cm
3/ g, average pore size 2.221nm.
Embodiment 9 utilizes ultraviolet light to cause legal system for resorcinol formaldehyde aerogels
With reference to the preparation process of the resorcinol-formaldehyde aeroge described in embodiment 1, difference is, be 50min the water-bath standing time in parameter, and the amount that adds light trigger is 2%.The resorcinol-formaldehyde aeroge of 35min system.The specific area of resorcinol-formaldehyde aeroge is 368m
2/ g, total pore volume 4.310m
3/ g, average pore size 2.976nm.
Embodiment 10 utilizes ultraviolet light to cause legal system for resorcinol formaldehyde aerogels
With reference to the preparation process of the resorcinol-formaldehyde aeroge described in embodiment 1, difference is, be 50min the water-bath standing time in parameter, and the amount that adds light trigger is 4%.The resorcinol-formaldehyde aeroge of 35min system.The specific area of resorcinol-formaldehyde aeroge is 326m
2/ g, total pore volume 3.670m
3/ g, average pore size 3.025 nm.
Embodiment 11 utilizes ultraviolet light to cause legal system for resorcinol formaldehyde aerogels
With reference to the preparation process of the resorcinol-formaldehyde aeroge described in embodiment 1, difference is, be 50min the water-bath standing time in parameter, and the amount that adds light trigger is 6%.The resorcinol-formaldehyde aeroge of 15min system.The specific area of resorcinol-formaldehyde aeroge is 319cm
2/ g, total pore volume is 3.640cm
2/ g, average pore size is 3.169nm.
Embodiment 12 utilizes ultraviolet light to cause legal system for resorcinol formaldehyde aerogels
With reference to the preparation process of the resorcinol-formaldehyde aeroge described in embodiment 1, difference is, be 50min the water-bath standing time in parameter, and the amount that adds light trigger is 8%.The resorcinol-formaldehyde aeroge of 35min system.The specific area of resorcinol-formaldehyde aeroge is 289m
2/ g, total pore volume 2.793 m
3/ g, average pore size 3.874nm.
Claims (5)
1. a preparation method for resorcinol-formaldehyde aeroge, is characterized in that, described preparation method comprises following steps:
The preparation of a, resorcinol-formaldehyde solution
Resorcinol, formaldehyde, sodium carbonate and water are mixed in proportion, stir, until dissolve completely;
B, step a gained solution is placed, until solution will be from water white transparency yellowing solution, placed cool to room temperature;
C, step b gained solution is added to light trigger, fully stir, dissolve;
D, step c gained solution is irradiated with ultraviolet light, become gel until solution loses flowability;
E, steps d gained gel is carried out to exchange of solvent with acetone or aqueous isopropanol;
F, gained gel in step e is put into supercritical extract instrument, carry out CO 2 supercritical dry.
2. according to the preparation method of a kind of resorcinol-formaldehyde aeroge described in claim 1, it is characterized in that, the resorcinol in described step a, the amount of substance of formaldehyde are than being 2:1, and the amount of substance of resorcinol, sodium carbonate is than being 250:1～25:1.
3. according to the preparation method of a kind of resorcinol-formaldehyde aeroge described in claim 1, it is characterized in that, in described step c, light trigger is: the acetophenone derivs, the nonionic long-chain oxethyl-diphenyl-ketone analog derivative that contain water soluble sidechains, contain the one in the follow-on benzoyl type of neutral side chain compound.
4. according to the preparation method of a kind of resorcinol-formaldehyde aeroge described in claim 1, it is characterized in that, the amount of the light trigger in described step c is 2wt%～14wt%.
5. according to the preparation method of a kind of resorcinol-formaldehyde aeroge described in claim 1, it is characterized in that, in described steps d, ultraviolet source used is high-pressure sodium lamp.
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Cited By (6)
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| CN105236385A (en) * | 2015-10-09 | 2016-01-13 | 四川睿光科技有限责任公司 | High-density activated carbon aerogel and preparation method thereof |
| CN106340726A (en) * | 2016-10-31 | 2017-01-18 | 中国工程物理研究院激光聚变研究中心 | Magnetic conductive nano-metal/carbon airgel absorbing material and the preparation method thereof |
| CN108316487A (en) * | 2018-01-20 | 2018-07-24 | 金粤幕墙装饰工程有限公司 | A kind of inertia aeroge and preparation method |
| US10450399B2 (en) | 2016-04-12 | 2019-10-22 | Southern Research Institute | Porous material and methods related thereto |
| WO2020186495A1 (en) | 2019-03-21 | 2020-09-24 | Hefei Guoxuan High-Tech Power Energy Co., Ltd. | Multilayer composite materials with anisotropic thermal conductivity for high safety pack design |
| CN113426385A (en) * | 2021-06-11 | 2021-09-24 | 武汉大学 | Carbon aerogel pellet, preparation method thereof and application of carbon aerogel pellet as heavy metal adsorption material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236385A (en) * | 2015-10-09 | 2016-01-13 | 四川睿光科技有限责任公司 | High-density activated carbon aerogel and preparation method thereof |
| CN105236385B (en) * | 2015-10-09 | 2017-12-01 | 四川睿光科技有限责任公司 | A kind of high density activation carbon aerogels and preparation method thereof |
| US10450399B2 (en) | 2016-04-12 | 2019-10-22 | Southern Research Institute | Porous material and methods related thereto |
| US11220569B2 (en) | 2016-04-12 | 2022-01-11 | Southern Research Institute | Porous material and methods related thereto |
| CN106340726A (en) * | 2016-10-31 | 2017-01-18 | 中国工程物理研究院激光聚变研究中心 | Magnetic conductive nano-metal/carbon airgel absorbing material and the preparation method thereof |
| CN106340726B (en) * | 2016-10-31 | 2019-01-25 | 中国工程物理研究院激光聚变研究中心 | Magnetic conductive nano metal/carbon aerogels absorbing material and preparation method thereof |
| CN108316487A (en) * | 2018-01-20 | 2018-07-24 | 金粤幕墙装饰工程有限公司 | A kind of inertia aeroge and preparation method |
| WO2020186495A1 (en) | 2019-03-21 | 2020-09-24 | Hefei Guoxuan High-Tech Power Energy Co., Ltd. | Multilayer composite materials with anisotropic thermal conductivity for high safety pack design |
| CN113426385A (en) * | 2021-06-11 | 2021-09-24 | 武汉大学 | Carbon aerogel pellet, preparation method thereof and application of carbon aerogel pellet as heavy metal adsorption material |
| CN113426385B (en) * | 2021-06-11 | 2022-06-03 | 武汉大学 | Carbon aerogel pellet, preparation method thereof and application of carbon aerogel pellet as heavy metal adsorption material |
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Application publication date: 20140723 |