CN102774843A - Preparation method of microspherical hydrophobic organic aerogel - Google Patents
Preparation method of microspherical hydrophobic organic aerogel Download PDFInfo
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- CN102774843A CN102774843A CN201110122266XA CN201110122266A CN102774843A CN 102774843 A CN102774843 A CN 102774843A CN 201110122266X A CN201110122266X A CN 201110122266XA CN 201110122266 A CN201110122266 A CN 201110122266A CN 102774843 A CN102774843 A CN 102774843A
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- resorcinol
- microballoon
- formaldehyde
- hexanaphthene
- organic aerogel
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Abstract
The invention provides a preparation method of a microspherical hydrophobic organic aerogel. A microspherical organic aerogel synthesized through treating resorcinol and formaldehyde as precursors is hydrophobically modified by a modifier which is a mixed solution of trimethylchlorosilane and cyclohexane. The shrinkage of the hydrophobically modified organic aerogel in the normal pressure drying process is substantially reduced, so the structure and performances of the organic aerogel can be maintained.
Description
Technical field
The present invention relates to a kind of organic aerogel field of materials, be specifically related to a kind of preparation method of hydrophobicity organic aerogel microballoon.
Background technology:
Gas gel is a kind of novel porous material, has advantages such as controlled and ultralow thermal conductivity of high porosity, high-specific surface area, pore size distribution and low density.Though aerogel material excellent performance; But traditional supercritical drying cycle is very long; Apparatus expensive, influenced its suitability for industrialized production [Li Jihui, Hu Jingsong. organic aerogel progress (I)-organic aerogel is found, preparation and analysis [J] Hebei Normal University journal (natural science edition); Vol 2, No.3].The organic aerogel that obtains through normal pressure method drying often shrinks and subsides seriously, and pattern is difficult to keep and performance is had a strong impact on.Causing the reason that these contractions are subsided is the inner contraction internal stress that produces of gas gel in the drying process, can eliminate this contraction internal stress through the gas gel skeleton being carried out the surface hydrophobicity modification, thereby keep the structure and the performance of gas gel.Use cheaply atmosphere pressure desiccation to prepare the critical process that aerogel material is the aerogel material suitability for industrialized production.
The research of at present aerogel material being carried out hydrophobically modified mainly is placed on SiO
2On the aerogel material.Wang Fei etc. are the silicon source with tetraethoxy (TEOS), and trimethylchlorosilane (TMCS) is a properties-correcting agent, and constant pressure and dry has prepared mullite fiber and strengthened SiO
2Aerogel heat-insulating material.The result shows to have typical gas gel constitutional features on the gained sample microcosmic, kept on the macroscopic view its functional materials integrity [Wang Fei, beard monarch, Chen Xiaohong, Song Huaihe. mullite fiber strengthens hydrophobic SiO
2The preparation of gas gel [J]. aerospace material technology, 2009 (1)].Zheng Wenzhis etc. are raw material with the tetraethoxy, prepare the silicon-dioxide alcogel through sol-gel process, utilize dimethyldichlorosilane(DMCS) that village's gel is carried out chemical surface again and modify, and obtain hydrophobic silicon dioxide aerogel at last.The result shows that there is hydrophobic grouping-CH in this sample surfaces
3, have higher thermostability [Zheng Wenzhi, old whetstone, Wang Honglin, old Yao. hydrophobic silicon dioxide aerogel synthetic and characterize [J]. silicate circular, 2008.12, Vol.27, No.6].
Above-mentioned work concentrates on SiO
2Gas gel carries out hydrophobically modified work, does not but have the report of this respect work as the another important branch-organic aerogel in gas gel field.With SiO
2Gas gel is similar, and it is cracked that organic aerogel also exists constant pressure and dry, and the moisture absorption causes cracked problem in the use.Therefore organic aerogel is carried out hydrophobically modified work has considerable meaning.
Summary of the invention
The present invention is directed to the problems referred to above of prior art, providing a kind of is the preparation method of the hydrophobicity organic aerogel microballoon of presoma based on Resorcinol and formaldehyde, makes by following step:
Step 1: according to mol ratio 1: 2: 20: 0.01 amount takes by weighing Resorcinol, formaldehyde, deionized water and yellow soda ash, stir under the room temperature, Resorcinol-formaldehyde colloidal sol;
Step 2: took by weighing tensio-active agent Span-80 and hexanaphthene in 1: 9～1: 49 according to volume ratio; Under 400r/min～2000r/min rotating speed, stir and form even mixed solution; Volume ratio according to this mixing solutions and Resorcinol-formaldehyde colloidal sol is 3: 1 adding Resorcinol-formaldehyde colloidal sol then; Continue to stir and in water-bath 25 ℃～50 ℃ reaction 72h, then product is cleaned up Span-80 with acetone and hexanaphthene respectively, promptly get organic wet gel microballoon;
Step 3: react obtain in the step 2 to 1～72h under the room temperature in organic wet gel microballoon be immersed in volume ratio trimethylchlorosilane and cyclohexane solution of 1: 9～1: 49, take out sample after, soak 24h with hexanaphthene, carry out repeatedly three times;
Step 4: the sample that obtains in the step 3 is at room temperature dried naturally, promptly get hydrophobicity organic aerogel microballoon.
Advantage of the present invention is simple to operate, and uses the resultant traditional aerogel material of supercritical drying to compare to have shrinking percentage little, and pattern remains intact, low cost and other advantages.Organic aerogel microballoon through behind the hydrophobically modified has hydrophobicity, in the constant pressure and dry process, can avoid shrinking the generation of internal stress, thereby has avoided cracked and generation deformation, has still kept good spherical morphology.
Description of drawings
Accompanying drawing 1 is the hydrophobic organic aerogel microballoon through constant pressure and dry preparation behind the hydrophobically modified.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated:
Embodiment 1
According to mol ratio 1: 2: 20: 0.01 took by weighing 8.808g Resorcinol, 11.2ml formaldehyde, 30ml deionized water and 0.0848g yellow soda ash, stir 15min under the room temperature and mix, glassy yellow or flavous Resorcinol-formaldehyde colloidal sol;
Take by weighing 2mL tensio-active agent Span-80 and 98mL hexanaphthene at 1: 49 according to volume ratio; Under the 400r/min rotating speed, stir and form even mixed solution; Volume ratio according to this mixing solutions and Resorcinol-formaldehyde colloidal sol is 3: 1 adding 33mL Resorcinol-formaldehyde colloidal sol then; Continue to stir and in water-bath 25 ℃ of reaction 72h, then product is cleaned up Span-80 with acetone and hexanaphthene respectively, promptly get organic wet gel microballoon;
The organic wet gel microballoon that obtains is immersed in the 100mL mixing solutions of 1: 49 trimethylchlorosilane of volume ratio and hexanaphthene; React 72h under the room temperature; After taking out sample, soak 24h, carry out repeatedly three times with hexanaphthene; The sample that obtains is at room temperature dried naturally, promptly get hydrophobicity organic aerogel microballoon.
Shown in accompanying drawing 1 ESEM (SEM) figure, product is made up of the microballoon of a large amount of size distribution about 50 μ m, and situation such as contraction, cracked, depression appear in smooth surface under the constant pressure and dry condition.
Embodiment 2
According to mol ratio 1: 2: 20: 0.01 took by weighing 8.808g Resorcinol, 11.2ml formaldehyde, 30ml deionized water and 0.0848g yellow soda ash, stir 15min under the room temperature and mix, glassy yellow or flavous Resorcinol-formaldehyde colloidal sol;
Take by weighing 10mL tensio-active agent Span-80 and 90mL hexanaphthene at 1: 9 according to volume ratio; Under the 2000r/min rotating speed, stir and form even mixed solution; Volume ratio according to this mixing solutions and Resorcinol-formaldehyde colloidal sol is 3: 1 adding 33mL Resorcinol-formaldehyde colloidal sol then; Continue to stir and in water-bath 50 ℃ of reaction 72h, then product is cleaned up Span-80 with acetone and hexanaphthene respectively, promptly get organic wet gel microballoon;
The organic wet gel microballoon that obtains is immersed in the 100mL mixing solutions of 1: 9 trimethylchlorosilane of volume ratio and hexanaphthene; React 72h under the room temperature; After taking out sample, soak 24h, carry out repeatedly three times with hexanaphthene; The sample that obtains is at room temperature dried naturally, promptly get hydrophobicity organic aerogel microballoon.
Embodiment 3
According to mol ratio 1: 2: 20: 0.01 took by weighing 8.808g Resorcinol, 11.2ml formaldehyde, 30ml deionized water and 0.0848g yellow soda ash, stir 15min under the room temperature and mix, glassy yellow or flavous Resorcinol-formaldehyde colloidal sol;
Take by weighing 6mL tensio-active agent Span-80 and 94mL hexanaphthene at 1: 16 according to volume ratio; Under the 1000r/min rotating speed, stir and form even mixed solution; Volume ratio according to this mixing solutions and Resorcinol-formaldehyde colloidal sol is 3: 1 adding 33mL Resorcinol-formaldehyde colloidal sol then; Continue to stir and in water-bath 35 ℃ of reaction 72h, then product is cleaned up Span-80 with acetone and hexanaphthene respectively, promptly get organic wet gel microballoon;
The organic wet gel microballoon that obtains is immersed in the 100mL mixing solutions of 1: 16 trimethylchlorosilane of volume ratio and hexanaphthene; React 72h under the room temperature; After taking out sample, soak 24h, carry out repeatedly three times with hexanaphthene; The sample that obtains is at room temperature dried naturally, promptly get hydrophobicity organic aerogel microballoon.
Below preferred embodiment of the present invention is specified; But the present invention is not limited to said embodiment; Those of ordinary skill in the art also can make all modification that is equal to or replacement under the prerequisite of spirit of the present invention, modification that these are equal to or replacement all are included in the application's claim institute restricted portion.
Claims (1)
1. the preparation method of a hydrophobic organic aerogel microballoon is characterized in that making by following step:
Step 1: according to mol ratio 1: 2: 20: 0.01 amount takes by weighing Resorcinol, formaldehyde, deionized water and yellow soda ash, stir under the room temperature, Resorcinol-formaldehyde colloidal sol;
Step 2: took by weighing tensio-active agent Span-80 and hexanaphthene in 1: 9～1: 49 according to volume ratio; Under 400r/min～2000r/min rotating speed, stir and form even mixed solution; Volume ratio according to this mixing solutions and Resorcinol-formaldehyde colloidal sol is 3: 1 adding Resorcinol-formaldehyde colloidal sol then; Continue to stir and in water-bath 25 ℃～50 ℃ reaction 72～120h, then product is cleaned up Span-80 with acetone and hexanaphthene respectively, promptly get organic wet gel microballoon;
Step 3: react obtain in the step 2 to 1～72h under the room temperature in organic wet gel microballoon be immersed in volume ratio trimethylchlorosilane and cyclohexane solution of 1: 9～1: 49, take out sample after, soak 24h with hexanaphthene, carry out repeatedly three times;
Step 4: the sample that obtains in the step 3 is at room temperature dried naturally, promptly get hydrophobicity organic aerogel microballoon.
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| CN201110122266XA CN102774843A (en) | 2011-05-12 | 2011-05-12 | Preparation method of microspherical hydrophobic organic aerogel |
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| CN201110122266XA CN102774843A (en) | 2011-05-12 | 2011-05-12 | Preparation method of microspherical hydrophobic organic aerogel |
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| CN201110122266XA Pending CN102774843A (en) | 2011-05-12 | 2011-05-12 | Preparation method of microspherical hydrophobic organic aerogel |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104707662A (en) * | 2015-02-13 | 2015-06-17 | 南京航空航天大学 | Phenolic organic aerogel-doped catalyst and preparation method thereof |
| CN110817871A (en) * | 2019-10-09 | 2020-02-21 | 贵州梅岭电源有限公司 | Preparation method and application of nitrogen-doped graphene-based carbon aerogel microspheres |
| CN116929005A (en) * | 2023-09-19 | 2023-10-24 | 新乡职业技术学院 | Normal-pressure drying method and system for silicon-based aerogel |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994025149A1 (en) * | 1993-04-28 | 1994-11-10 | University Of New Mexico | Preparation of high porosity xerogels by chemical surface modification |
| CN1891622A (en) * | 2005-07-06 | 2007-01-10 | 同济大学 | Method for preparing high specific area carbon aerogel |
-
2011
- 2011-05-12 CN CN201110122266XA patent/CN102774843A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994025149A1 (en) * | 1993-04-28 | 1994-11-10 | University Of New Mexico | Preparation of high porosity xerogels by chemical surface modification |
| CN1891622A (en) * | 2005-07-06 | 2007-01-10 | 同济大学 | Method for preparing high specific area carbon aerogel |
Non-Patent Citations (1)
| Title |
|---|
| CHANDRA S.SHARMA ET AL.: "Synthesis of carbon xerogel particles and fractal-like structures", 《CHEMICAL ENGINEERING SCIENCE》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104707662A (en) * | 2015-02-13 | 2015-06-17 | 南京航空航天大学 | Phenolic organic aerogel-doped catalyst and preparation method thereof |
| CN110817871A (en) * | 2019-10-09 | 2020-02-21 | 贵州梅岭电源有限公司 | Preparation method and application of nitrogen-doped graphene-based carbon aerogel microspheres |
| CN116929005A (en) * | 2023-09-19 | 2023-10-24 | 新乡职业技术学院 | Normal-pressure drying method and system for silicon-based aerogel |
| CN116929005B (en) * | 2023-09-19 | 2023-12-05 | 新乡职业技术学院 | Normal-pressure drying method and system for silicon-based aerogel |
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Application publication date: 20121114 |