CN105236422A - Method of preparing regular-shaped SiO2 aerogel granules through high-energy cutting - Google Patents
Method of preparing regular-shaped SiO2 aerogel granules through high-energy cutting Download PDFInfo
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- CN105236422A CN105236422A CN201510560234.6A CN201510560234A CN105236422A CN 105236422 A CN105236422 A CN 105236422A CN 201510560234 A CN201510560234 A CN 201510560234A CN 105236422 A CN105236422 A CN 105236422A
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Abstract
The invention relates to nano inorganic non-metal materials and particularly relates to a method of preparing regular-shaped SiO2 aerogel granules through high-energy cutting, which comprises the following steps: 1) dissolving organic silane, diluted hydrochloric acid and deionized water in an organic solvent at 0-40 DEG C, mixing the solution uniformly, and carrying out a reaction for 0.1-8 h to obtain silica sol; 2) at 0-40 DEG C, adding alkali with stirring, and carrying out a reaction for 0.01-1 h, and allowing the substances to stand; (3) after gelation, cutting gel to obtain the regular-shaped SiO2 aerogel granules through the high-energy cutting; and (4) drying the aerogel granules. In the invention, through the high-energy cutting, the regular-shaped SiO2 aerogel granules are prepared. The regular-shaped SiO2 aerogel granule is uniform in texture, is high in visible light transmittance, is good in filling property, is convenient to process subsequently and promotes industrialization of SiO2 aerogel greatly.
Description
Technical field
The present invention relates to Nanosized Inorganic Non-Metal Materials field, be specifically related to the method that irregular figure silica aerogel particles is prepared in high energy cutting.
Background technology
Aerogel, English aerogel.When most of solvent sloughed by gel, to make in gel content liquid than solids content much less, or the medium be full of in the space net structure of gel is gas, appearance is solid state, be aerogel, aerogel is usually mutually assembled with nanometer scale ultrafine particle and is formed nanoporous network structure, and in network hole, be full of the lightweight nano solid material of gaseous state dispersion medium.Aerogel, because of its translucent color and ultra-light-weight, is also sometimes referred to as " solid-state cigarette " or " cigarette frozen ".
Aerogel that is the most common and that the most extensively apply is aerosil.Aerosil is the very outstanding light nanoporous amorphous solid material of a kind of heat preservation and insulation, and its porosity can up to 99.8%, and the typical sizes of hole is 1 ~ 40nm, and specific surface area is 400 ~ 1200m
2/ g, and density can be low to moderate 3kg/m
3, room temperature thermal conductivity can be low to moderate 0.010W/ (mk) below.Silica aerogel material is made to have very wide application potential in calorifics, acoustics, optics, microelectronics, particle detection just because of these features.
The making processes of current aerosil is, first liquid organosilicon mixes with the liquid solvent of energy rapid evaporation, reacts with water, form gel, then gel is placed in drying plant dry, and through heating and step-down, forms nanoporous three-dimensional network-like structure.Its typical silicon precursor (tetraethoxy) reaction principle is as follows:
Publication number is that the Chinese patent application of CN104108720A discloses name and is called " a kind of preparation method of silica aerogel particles of high daylight rate ", this technology adopts collosol and gel soda acid two-step catalysis method, concrete steps mainly contain: tetraethyl orthosilicate, dilute hydrochloric acid, deionized water are dissolved in organic solvent and stir by (1), wherein, the adding proportion of tetraethyl orthosilicate, organic solvent, deionized water, dilute hydrochloric acid is 80 ~ 120ml:65 ~ 85ml:10 ~ 16ml:0.01 ~ 0.05ml; (2) mixing solutions of step (1) gained is refluxed 15 ~ 30 hours at the temperature of 60 ~ 80 degrees Celsius; (3) mixed with organic solvent by the solution of step (2) gained and stir, wherein the adding proportion of solution and organic solvent is 1 ~ 5ml:10 ~ 40ml; (4) solution of step (3) gained is mixed with proper ammonia, after leaving standstill, obtain wet gel; (5) wet gel of step (4) gained be dry, pulverize after normal temperature is aging, namely obtain required silica nanometer porous aerogel particle.But the method exists following problem: the silica aerogel particles that 1, the method obtains is all irregular particle, and fillibility is bad, quality is even not simultaneously; 2, the target size particle recovery rate of the method is lower, and recovery rate lower than 50%, thus causes the significant wastage of raw material, has raised product cost; 3, the method can not control visible light transmittance rate, cannot adapt to diverse requirements, be unfavorable for post-production; 4, the method return time is longer, and production efficiency is low, and therefore industrialization is a difficult problem; 5, the method that the method is broken again after adopting traditional drying, broken distribution of sizes is too wide, not of uniform size, have impact on lumber recovery, and produces a large amount of powder in shattering process, so powder contamination is large.
Summary of the invention
The present invention is in order to overcome the problems referred to above of prior art, and provide novel high energy cutting to prepare the method for irregular figure silica aerogel particles, the method prepares irregular figure silica aerogel particles first, and lumber recovery is high.
The method of irregular figure silica aerogel particles is prepared in high energy cutting of the present invention, comprises the following steps:
The method of irregular figure silica aerogel particles is prepared in high energy cutting, comprises the following steps:
Be dissolved in organic solvent by organosilane, dilute hydrochloric acid, deionized water at (1) 0 ~ 40 DEG C, mix, reaction 0.1 ~ 8h, obtains silicon sol;
Add alkali at (2) 0 ~ 40 DEG C to stir, after reaction 0.01 ~ 1h, leave standstill;
(3) after gel, high energy cutting is adopted to obtain the gelinite particle of profile rule;
(4) be drying to obtain.
For a long time, people can only prepare the silica aerogel particles of irregular profile, and contriver, through large quantity research, finally finds, by carrying out the mode of high energy cutting to gelinite, can obtain the silica gel particle of irregular figure.Therefore, the present invention improves prior art, high energy cutting method is incorporated in silica aerogel particles preparation, like this, prepare the silica aerogel particles with irregular figure first, homogeneous, transmission of visible light is high, fillibility is good, is extremely convenient to following process, greatly facilitates the industrialization of aerosil.The silica aerogel particles with irregular figure of gained of the present invention, mainly contains regular polygon, multiedge cylinder, polygonal pyramid body, many prismoids, right cylinder, cone, Rotary-table or spheroid etc.The present invention is cut by high energy, and by further for gelinite excision forming, gelinite can be cut into desired shape by this mode, and reduces the generation of scrap stock, substantially increases utilization ratio.
Preferred version of the present invention is, step (1) reaction times is 0.5 ~ 6h, and the large I of silicon sol colloidal solid that under this reaction times, the present invention obtains strictly controls, homogeneity and good stability, and the aerogel visible light transmissivity of follow-up acquisition is high.
Preferred version of the present invention is, described organosilane selects the mixture of one or more in methyl silicate, tetraethoxy, methyltrimethoxy silane, Union carbide A-162, dimethyldimethoxysil,ne, dimethyldiethoxysilane, ethyl trimethoxy silane, ethyl triethoxysilane.
Another preferred version of the present invention is, described organic solvent selects the mixture of one or more in methyl alcohol, ethanol, Virahol, acetone.
Another preferred version of the present invention is, described alkali is the one in ammoniacal liquor, sodium hydroxide, potassium hydroxide.
Another preferred version of the present invention is, the gelinite particle of described irregular figure is polyhedron, rotator or spheroid.
Another preferred version of the present invention is, described polyhedron is regular polygon, prism or pyramid.
Another preferred version of the present invention is, described polyhedron is prismoid.
Another preferred version of the present invention is, described regular polygon is positive tetrahedron, regular hexahedron, regular octahedron, regular dodecahedron or icosahedron.
Another preferred version of the present invention is, described prism is tri-prismoid, four prisms cylinder, pentagonal prism body, hexagonal prism, seven prisms, eight prisms, nine prisms or ten prisms.
Another preferred version of the present invention is, described pyramid is Rhizoma Sparganii cone, rectangular pyramid, pentaprismo body, hecaprismo body, seven pyramids, eight pyramids, nine pyramids or ten pyramids.
Another preferred version of the present invention is, chamfering also can be carried out in described at least one summit polyhedral.
Another preferred version of the present invention is, described rotator is right cylinder, cone, Rotary-table.
Another preferred version of the present invention is, step (3) gelinite particle size is 0.5 ~ 20mm.
Another preferred version of the present invention is, step (4) described drying is constant pressure and dry, lyophilize, vacuum-drying, subcritical drying or supercritical drying.
Another preferred version of the present invention is, also comprises aging and solvent exchange technique after described step (3) and before step (4).
Another preferred version of the present invention is, described aging and solvent exchange temperature is 0 ~ 65 DEG C.
Another preferred version of the present invention is, step (3) high energy is cut into high-pressure water cutting.High-pressure water cutting is by disposable shape gelinite being processed as various complexity of numerical control, easy to operate, lumber recovery is high.
Another preferred version of the present invention is, step (3) high energy is cut into ultrasonic wave cutting.The friction resistance of ultrasonic wave cutting is very little, can not cause breakage to the cut edge of gelinite.
Another preferred version of the present invention is, step (3) high energy is cut into high pressure gas cutting.Gelinite is processed as the shape of various complexity by numerical control continuity by high pressure gas cutting, easy to operate, lumber recovery is high.
The inventive method is carried out at 0 ~ 40 DEG C, namely can at room temperature react, and the reaction times is short, is conducive to industrialization; In addition, use present method to prepare the silica aerogel particles of irregular figure, lumber recovery is more than 95%, and compared with the existing methods, raw material obtains to be applied more fully, reduces product cost; Present method eliminates reflux technique, than existing method shorten 10 little time more than, production efficiency is high, be applicable to industrialization; The aerogel visible light transmissivity obtained is high; Present method does not almost have powder contamination in addition.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, and to help understanding the present invention better, but protection scope of the present invention is not limited in these embodiments.
Embodiment 1: at 40 DEG C, by methyl silicate, methyl alcohol, deionized water and dilute hydrochloric acid are according to volume ratio 1:0.5:0.1:0.0025, mixing, stir 0.1h, obtain colloidal sol, the ratio being 1:0.025 in the volume ratio of methyl silicate and ammoniacal liquor again adds ammoniacal liquor, after being uniformly mixed 1h, leave standstill, after gel, high energy cutting (selecting means from high-pressure water cutting or high pressure gas cutting or ultrasonic wave cutting) is adopted to obtain the silica gel particle of irregular figure, with ethanol age gelation body particle at 40 DEG C, an ethanol is replaced every 6h, replace 4 times, then 4 times are replaced with normal hexane, each 6h, use constant pressure and dry can obtain the silica aerogel particles of irregular figure.
The mode identical with embodiment 1 is adopted to carry out embodiment 2 ~ 20.Wherein, in embodiment 4,11,13,19,20, after obtaining the silica gel particle of irregular figure by preceding step cutting, directly use supercritical drying can obtain the silica aerogel particles of irregular figure, do not use Aging Step.
Table 1 is embodiment organosilane used, organic solvent kind and volume ratio thereof.
Table 2 is processing condition and the drying means of embodiment.
Table 3 is the performance perameter of the silica aerogel particles obtained by embodiment.
| Embodiment is numbered | Density (g/cm 3) | Visible light transmissivity (%) | Thermal conductivity (W/mK) |
| 1 | 0.161 | 80 | 0.015 |
| 2 | 0.134 | 81 | 0.013 |
| 3 | 0.104 | 87 | 0.014 |
| 4 | 0.063 | 89 | 0.013 |
| 5 | 0.080 | 81 | 0.013 |
| 6 | 0.104 | 85 | 0.014 |
| 7 | 0.093 | 82 | 0.014 |
| 8 | 0.105 | 86 | 0.015 |
| 9 | 0.087 | 89 | 0.013 |
| 10 | 0.078 | 85 | 0.014 |
| 11 | 0.151 | 80 | 0.015 |
| 12 | 0.061 | 88 | 0.014 |
| 13 | 0.065 | 89 | 0.013 |
| 14 | 0.123 | 80 | 0.014 |
| 15 | 0.130 | 83 | 0.014 |
| 16 | 0.125 | 81 | 0.014 |
| 17 | 0.156 | 80 | 0.015 |
| 18 | 0.110 | 86 | 0.014 |
| 19 | 0.081 | 88 | 0.013 |
| 20 | 0.079 | 87 | 0.014 |
Irregular figure silica aerogel particles prepared by the inventive method, high energy cutting technique can be adopted to be processed into various single particle size and desired shape, and follow-up workability is good, prepared irregular figure aerosil good heat insulating.Irregular figure silica aerogel particles the present invention prepared is filled in the double glazing of single chamber, and the heat transfer coefficient of single chamber glass can be made to be low to moderate 0.5W/m
2below K, transmission of visible light up to more than 70%, can have extraordinary heat preservation and insulation and lighting performance, is very suitable for green building and super low energy consumption building, nearly zero energy consumption building etc. to the demand with energy-efficient glass.
Comparative example
By publication number for the technology disclosed in the Chinese patent application of CN104108720A " a kind of preparation method of silica aerogel particles of high daylight rate " is tested, it is long that this technology obtains finished product required time; Non-defective unit recovery rate is 37% ~ 45%, and wastage of material is serious, and can only obtain the silica aerogel particles of irregular profile; Finished product transmission of visible light is 46% ~ 52%; Thermal conductivity is between 0.037 ~ 0.049W/mK; Produce a large amount of powder in shattering process simultaneously.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. a method for irregular figure silica aerogel particles is prepared in high energy cutting, it is characterized in that, comprises the following steps:
Be dissolved in organic solvent by organosilane, dilute hydrochloric acid, deionized water at (1) 0 ~ 40 DEG C, mix, reaction 0.1 ~ 8h, obtains silicon sol;
Add alkali at (2) 0 ~ 40 DEG C to stir, after reaction 0.01 ~ 1h, leave standstill;
(3) after gel, high energy cutting is adopted to obtain the gelinite particle of irregular figure;
(4) be drying to obtain.
2. the method for irregular figure silica aerogel particles is prepared in high energy cutting according to claim 1, it is characterized in that, described organosilane is the mixture of one or more in methyl silicate, tetraethoxy, methyltrimethoxy silane, Union carbide A-162, dimethyldimethoxysil,ne, dimethyldiethoxysilane, ethyl trimethoxy silane, ethyl triethoxysilane.
3. the method for irregular figure silica aerogel particles is prepared in high energy cutting according to claim 1, and it is characterized in that, described organic solvent is the mixture of one or more in methyl alcohol, ethanol, Virahol, acetone.
4. the method for irregular figure silica aerogel particles is prepared in high energy cutting according to claim 1, and it is characterized in that, described alkali is the one in ammoniacal liquor, sodium hydroxide, potassium hydroxide.
5. the method for irregular figure silica aerogel particles is prepared in high energy cutting according to claim 1, and it is characterized in that, the gelinite particle of described irregular figure is polyhedron, rotator or spheroid.
6. the method for irregular figure silica aerogel particles is prepared in high energy cutting according to claim 5, and it is characterized in that, described polyhedron is regular polygon, prism or pyramid.
7. the method for irregular figure silica aerogel particles is prepared in high energy cutting according to claim 5, and it is characterized in that, described polyhedron is prismoid.
8. the method for irregular figure silica aerogel particles is prepared in high energy cutting according to claim 6, and it is characterized in that, described regular polygon is positive tetrahedron, regular hexahedron, regular octahedron, regular dodecahedron or icosahedron.
9. the method for irregular figure silica aerogel particles is prepared in high energy cutting according to claim 6, it is characterized in that, described prism is tri-prismoid, four prisms cylinder, pentagonal prism body, hexagonal prism, seven prisms, eight prisms, nine prisms or ten prisms.
10. according to claim 1 to 9 any one claim, the method for irregular figure silica aerogel particles is prepared in high energy cutting, it is characterized in that, described pyramid is Rhizoma Sparganii cone, rectangular pyramid, pentaprismo body, hecaprismo body, seven pyramids, eight pyramids, nine pyramids or ten pyramids; Or chamfering also can be carried out in described at least one summit polyhedral; Or described rotator is right cylinder, cone, Rotary-table; Or step (3) gelinite particle size is 0.5 ~ 20mm; Or step (4) described drying is constant pressure and dry, lyophilize, vacuum-drying, subcritical drying or supercritical drying; Or also comprise aging and solvent exchange technique after described step (3) and before step (4); Or described aging and solvent exchange temperature is 0 ~ 65 DEG C; Or step (3) high energy is cut into high-pressure water cutting; Or step (3) high energy is cut into ultrasonic wave cutting; Or step (3) high energy is cut into high pressure gas cutting.
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Cited By (1)
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| CN108384517A (en) * | 2018-02-22 | 2018-08-10 | 四川艾施派尔新材料科技有限公司 | A kind of nanometer of ice bag and preparation method thereof |
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| CN104108720A (en) * | 2014-07-08 | 2014-10-22 | 同济大学 | Preparation method of silica aerogel particles with high daylighting rate |
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- 2015-09-06 CN CN201510560234.6A patent/CN105236422A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4564547A (en) * | 1983-08-04 | 1986-01-14 | Micropore International Limited | Handleable shapes of thermal insulation material |
| CN101823867A (en) * | 2009-03-02 | 2010-09-08 | 中国科学院过程工程研究所 | Preparation method of SiO2 aerogel composite material doped with aramid fibre |
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| CN103435055A (en) * | 2013-06-29 | 2013-12-11 | 浙江工业大学 | Method for preparing low density silica aerogel under normal pressure |
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Application publication date: 20160113 |