CN105060308A - Method for preparing regular-appearance silicon dioxide aerogel particles - Google Patents
Method for preparing regular-appearance silicon dioxide aerogel particles Download PDFInfo
- Publication number
- CN105060308A CN105060308A CN201510559825.1A CN201510559825A CN105060308A CN 105060308 A CN105060308 A CN 105060308A CN 201510559825 A CN201510559825 A CN 201510559825A CN 105060308 A CN105060308 A CN 105060308A
- Authority
- CN
- China
- Prior art keywords
- irregular
- aerogel particles
- silica aerogel
- prepare
- particles according
- 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
Abstract
The invention relates to a nano inorganic non-metal material, particularly a method for preparing regular-appearance silicon dioxide aerogel particles. The method comprises the following steps: (1) dissolving organosilane, dilute hydrochloric acid and deionized water in an organic solvent at 0-40 DEG C, uniformly mixing, and reacting at 45-55 DEG C for 5-70 hours to obtain a silica sol, wherein the volume ratio of the organosilane, dilute hydrochloric acid, deionized water and organic solvent is 1:(0.0025-0.5):(0.05-5):(0.5-8); (2) adding an organic solvent at 0-40 DEG C, mixing, adding alkali, stirring, and reacting for 0.01-1 hour; (3) casting the sol obtained in the step (2) into a mold to perform direct gelling formation, thereby obtaining the regular-appearance gel particles; and (4) drying. The silicon dioxide aerogel particles obtained by the method have the advantages of uniform texture, high visible light transmittivity and favorable filling property, are convenient for subsequent processing, and greatly promote the industrialization of the silicon dioxide aerogel.
Description
Technical field
The present invention relates to Nanosized Inorganic Non-Metal Materials field, be specifically related to the method preparing irregular figure silica aerogel particles.
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 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 the novel method preparing irregular figure silica aerogel particles, the method prepares irregular figure silica aerogel particles first, and lumber recovery is high.
The method preparing irregular figure silica aerogel particles of the present invention, comprises the following steps:
At (1) 0 ~ 40 DEG C, organosilane, dilute hydrochloric acid, deionized water are dissolved in organic solvent, wherein, silicon precursor, the volume ratio of dilute hydrochloric acid, deionized water, organic solvent is 1:0.0025 ~ 0.5:0.05 ~ 5:0.5 ~ 8, mix, then at 45 ~ 55 DEG C, react 5 ~ 70h, obtain silicon sol;
Add organic solvent, mix and blend at (2) 0 ~ 40 DEG C, and then add alkali stirring, reaction 0.01 ~ 1h;
(3) colloidal sol that step (2) obtains is watered to cast from DIRECT GEL in forming mould shaping, obtain the gelinite particle of irregular figure;
(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 casting mode, utilize forming mould DIRECT GEL shaping, can obtain the silica gel particle of irregular figure.Therefore, the present invention improves prior art, casting and mould DIRECT GEL forming method are 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.
Preferred version of the present invention is, step (1) reaction times is 10 ~ 20h, the large I of silicon sol colloidal solid that under this reaction times, the present invention obtains strictly controls, homogeneity and stability better, 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 die cavity of described forming mould 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.
The inventive method reaction times is shorter, is conducive to industrialization, and energy consumption is low, meets the requirement of energy-saving; In addition, use present method to prepare the silica aerogel particles of irregular figure, lumber recovery is more than 99%, and compared with the existing methods, raw material obtains to be applied more fully, reduces product cost; Present method optimizes colloidal sol preparation technology, than existing method shorten 5 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, then stirring reaction 30h at 45 DEG C, obtain colloidal sol, the ratio being 1:2 in the volume ratio of methyl silicate and methyl alcohol adds methyl alcohol in colloidal sol, mix and blend, 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, be poured in the forming mould with regular die cavity, leave standstill, the silica gel particle of irregular figure is obtained after gel, the demoulding, 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, obtained the silica gel particle of irregular figure by preceding step, after the demoulding, 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 | 0.160 | 80 | 0.015 |
| 2 | 0.125 | 81 | 0.013 |
| 3 | 0.097 | 87 | 0.014 |
| 4 | 0.060 | 89 | 0.013 |
| 5 | 0.074 | 81 | 0.013 |
| 6 | 0.098 | 85 | 0.014 |
| 7 | 0.086 | 82 | 0.014 |
| 8 | 0.097 | 86 | 0.015 |
| 9 | 0.081 | 89 | 0.013 |
| 10 | 0.073 | 85 | 0.014 |
| 11 | 0.134 | 80 | 0.015 |
| 12 | 0.057 | 88 | 0.014 |
| 13 | 0.060 | 89 | 0.013 |
| 14 | 0.114 | 80 | 0.014 |
| 15 | 0.109 | 83 | 0.014 |
| 16 | 0.116 | 81 | 0.014 |
| 17 | 0.145 | 80 | 0.015 |
| 18 | 0.102 | 86 | 0.014 |
| 19 | 0.075 | 88 | 0.013 |
| 20 | 0.073 | 87 | 0.014 |
Irregular figure silica aerogel particles prepared by the inventive method, forming mould DIRECT GEL forming technique can be adopted to be shaped to 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. prepare the method for irregular figure silica aerogel particles, it is characterized in that, comprise the following steps:
At (1) 0 ~ 40 DEG C, organosilane, dilute hydrochloric acid, deionized water are dissolved in organic solvent, wherein, silicon precursor, the volume ratio of dilute hydrochloric acid, deionized water, organic solvent is 1:0.0025 ~ 0.5:0.05 ~ 5:0.5 ~ 8, mix, then at 45 ~ 55 DEG C, react 5 ~ 70h, obtain silicon sol;
(2) solubilizing agent, then adds alkali and stirs at 0 ~ 40 DEG C, reaction 0.01 ~ 1h;
(3) colloidal sol that step (2) obtains is watered to cast from DIRECT GEL in forming mould shaping, obtain the gelinite particle of irregular figure;
(4) be drying to obtain.
2. prepare the method for irregular figure silica aerogel particles 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. prepare the method for irregular figure silica aerogel particles according to claim 1, it is characterized in that, described organic solvent is the mixture of one or more in methyl alcohol, ethanol, Virahol, acetone.
4. prepare the method for irregular figure silica aerogel particles according to claim 1, it is characterized in that, described alkali is the one in ammoniacal liquor, sodium hydroxide, potassium hydroxide.
5. prepare the method for irregular figure silica aerogel particles according to claim 1, it is characterized in that, the die cavity of described forming mould is polyhedron, rotator or spheroid.
6. prepare the method for irregular figure silica aerogel particles according to claim 5, it is characterized in that, described polyhedron is regular polygon, prism or pyramid.
7. prepare the method for irregular figure silica aerogel particles according to claim 5, it is characterized in that, described polyhedron is prismoid.
8. prepare the method for irregular figure silica aerogel particles according to claim 6, it is characterized in that, described regular polygon is positive tetrahedron, regular hexahedron, regular octahedron, regular dodecahedron or icosahedron.
9. prepare the method for irregular figure silica aerogel particles 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, prepare the method for irregular figure silica aerogel particles, 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510559825.1A CN105060308A (en) | 2015-09-06 | 2015-09-06 | Method for preparing regular-appearance silicon dioxide aerogel particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510559825.1A CN105060308A (en) | 2015-09-06 | 2015-09-06 | Method for preparing regular-appearance silicon dioxide aerogel particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105060308A true CN105060308A (en) | 2015-11-18 |
Family
ID=54489901
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510559825.1A Pending CN105060308A (en) | 2015-09-06 | 2015-09-06 | Method for preparing regular-appearance silicon dioxide aerogel particles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105060308A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098354A (en) * | 2016-02-20 | 2017-08-29 | 金承黎 | A kind of preparation method from hydrophobic silicon hydrochlorate aerogel material |
| CN107381581A (en) * | 2017-08-28 | 2017-11-24 | 优澎（嘉兴）新材料科技有限公司 | Hydrophobic silicon dioxide aerogel material and preparation method thereof |
| CN109138196A (en) * | 2017-06-15 | 2019-01-04 | 湖南尚成新材料科技有限责任公司 | A kind of aeroge compound sound-absorption structural |
| CN110713789A (en) * | 2019-09-24 | 2020-01-21 | 佛山市南海区里水镇经济促进局 | Adsorptive porous coating material and preparation method and application thereof |
| CN111453738A (en) * | 2020-06-02 | 2020-07-28 | 雪华铃家用电器(深圳)有限公司 | Coating material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557577A (en) * | 2011-11-01 | 2012-07-11 | 厦门纳美特新材料科技有限公司 | Preparation and method of silicon dioxide aerogel composite material |
| CN102659120A (en) * | 2012-04-18 | 2012-09-12 | 同济大学 | Preparation method for hydrophobic large-size bulk nanometer porous SiO2 aerogel |
| CN103435055A (en) * | 2013-06-29 | 2013-12-11 | 浙江工业大学 | Method for preparing low density silica aerogel under normal pressure |
| CN103754887A (en) * | 2013-12-25 | 2014-04-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Heat-resisting silica aerogel material and preparation method thereof |
-
2015
- 2015-09-06 CN CN201510559825.1A patent/CN105060308A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557577A (en) * | 2011-11-01 | 2012-07-11 | 厦门纳美特新材料科技有限公司 | Preparation and method of silicon dioxide aerogel composite material |
| CN102659120A (en) * | 2012-04-18 | 2012-09-12 | 同济大学 | Preparation method for hydrophobic large-size bulk nanometer porous SiO2 aerogel |
| CN103435055A (en) * | 2013-06-29 | 2013-12-11 | 浙江工业大学 | Method for preparing low density silica aerogel under normal pressure |
| CN103754887A (en) * | 2013-12-25 | 2014-04-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Heat-resisting silica aerogel material and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098354A (en) * | 2016-02-20 | 2017-08-29 | 金承黎 | A kind of preparation method from hydrophobic silicon hydrochlorate aerogel material |
| CN109138196A (en) * | 2017-06-15 | 2019-01-04 | 湖南尚成新材料科技有限责任公司 | A kind of aeroge compound sound-absorption structural |
| CN109138196B (en) * | 2017-06-15 | 2020-10-13 | 湖南尚成新材料科技有限责任公司 | Aerogel composite sound absorption structure |
| CN107381581A (en) * | 2017-08-28 | 2017-11-24 | 优澎（嘉兴）新材料科技有限公司 | Hydrophobic silicon dioxide aerogel material and preparation method thereof |
| CN110713789A (en) * | 2019-09-24 | 2020-01-21 | 佛山市南海区里水镇经济促进局 | Adsorptive porous coating material and preparation method and application thereof |
| CN111453738A (en) * | 2020-06-02 | 2020-07-28 | 雪华铃家用电器(深圳)有限公司 | Coating material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105060308A (en) | Method for preparing regular-appearance silicon dioxide aerogel particles | |
| CN103664073B (en) | A kind of autoclave aerated concrete building block utilizing Yellow River Sand to prepare and preparation method thereof | |
| CN106630930B (en) | A method of continuously preparing aeroge insulation felt | |
| CN106316135B (en) | Silica aerogel filled open-cell foam glass particle and manufacturing method thereof | |
| CN103738971B (en) | Mechanical-enhanced SiO2 aerogel material and preparation method thereof | |
| CN106745002B (en) | A kind of method that co-precursor method constant pressure and dry prepares block aerosil | |
| CN103304252B (en) | Preparation method of SiO2 aerogel/porous Si3N4 composite material | |
| CN102964055B (en) | Ultra-fast preparation method for highly transparent aerogel glass | |
| CN104497688A (en) | Aerogel thermal insulation coating and preparation method thereof | |
| CN107089810B (en) | A kind of aeroge modified expanded perlite insulation board and preparation method thereof | |
| CN106892674A (en) | A kind of method for preparing gradient orienting stephanoporate cement based on two-phase pore creating material system freezing molding techniques | |
| CN102992333A (en) | Low-cost method for preparing aerosil | |
| CN105197943A (en) | Method for preparing regularly-shaped silicon dioxide aerogel particles in high-energy cutting manner | |
| CN109019613A (en) | A kind of preparation process of rare earth toughening solid-state silica aerogel | |
| CN101891209B (en) | Method for preparing nano powder of spherical silicon dioxide | |
| CN105197944A (en) | Method of preparing silica aerogel particles with regular shapes | |
| CN112279612A (en) | Bionic 3D printing aerogel thermal insulation board and preparation method thereof | |
| CN113651334A (en) | Preparation method of rare earth doped silicon dioxide aerogel | |
| CN101891210B (en) | Preparation method of nano silicon dioxide powder | |
| CN103738970A (en) | High transmittance nano-porous aerogel material and preparation method thereof | |
| CN106629751A (en) | Method for preparing hydrophobic SiO2 aerogel under normal pressure in dry manner | |
| CN106187295A (en) | The powder ash air-entrained concrete building block of a kind of low heat conduction and production method | |
| CN103396076B (en) | A kind of thermal insulation mortar that contains oxidized starch that utilizes complex mineral particle manufacture | |
| CN105060309A (en) | Method for preparing regular-appearance silicon dioxide aerogel particles by mechanical cutting | |
| CN105174273A (en) | Method for preparing silica aerogel particles with regular shapes by mechanical cutting |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20151118 |
|
| RJ01 | Rejection of invention patent application after publication |