CN104556057A - Method for preparing nano-porous light silicon oxide microspheres - Google Patents
Method for preparing nano-porous light silicon oxide microspheres Download PDFInfo
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- CN104556057A CN104556057A CN201510018324.2A CN201510018324A CN104556057A CN 104556057 A CN104556057 A CN 104556057A CN 201510018324 A CN201510018324 A CN 201510018324A CN 104556057 A CN104556057 A CN 104556057A
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Abstract
The invention discloses a method for preparing nano-porous light silicon oxide microspheres. The nano-porous light silicon oxide microspheres are prepared by adding a surfactant to form an emulsion system and carrying out chemical reaction by mainly adopting water glass as a precursor, a solvent with a low surface tension as a replacement solvent and an organic silane compound as a hydrophobic modifier in the presence of inorganic acid as a catalyst. The method for preparing the nano-porous light silicon oxide microspheres is simple in process flow; in addition, the production raw materials are low in price, the solvent is easy to recover, and low production cost and high yield are achieved; in the preparation process adopted in the invention, no cation exchange resin is needed in the ion-exchange process, so that large-scale industrial production is facilitated; and the nano-porous light silicon oxide microspheres prepared by the method are of a typical nano-porous structure and can be applied to the fields, such as thermal insulation, chromatographic separation, catalysis and biological drug loading.
Description
Technical field
The present invention relates to field of material preparation, be specifically related to a kind of preparation method of nanoporous light silicon dioxide microballoon.
Background technology
Nanoporous light silicon dioxide also can be described as SiO
2aeroge, SiO
2aeroge is formed nanoporous network structure a kind of mutually gathering with nanometer scale particle, and in hole, be full of a kind of high dispersive solid-state material of gaseous state decentralized medium, because it has nano-porous structure, low-density, low-k, low thermal conductivity, high porosity, the features such as high-specific surface area, at mechanics, acoustics, calorifics, the aspects such as optics demonstrate peculiar property, in space flight, military, oil, chemical industry, mineral products, communication, medical, building materials, electronics, the various fields such as metallurgy have extensive and huge using value, be called as " the magical material changing the world ".
At present, SiO
2aeroge is widely applied in fields such as heat insulation, dielectric layer, biological medicine carrying and space technologies, have received the great attention of material researchers.At present, SiO
2the research of aeroge mainly concentrates on aerogel block body and irregular shape powder.And spherical SiO
2the well-regulated shape of aeroge microparticle tool, the powder aerogel material be made up of it has higher apparent density and good mobility, is conducive to it heat insulation, the application of the aspect such as chromatographic isolation and catalysis.In addition, spherical SiO
2aeroge microparticle have also been obtained important application in the controlled release of medicine.Therefore, spherical SiO is developed
2the novel preparation method of aeroge microparticle has important practical significance.
In spherical SiO
2preparation method's research aspect of aeroge microparticle, people have carried out a large amount of research work, it is desirable to develop that cost is low, technique is simple, the short and preparation method that can accomplish scale production consuming time.At present, spherical SiO
2the preparation method of aeroge microparticle mainly comprises supercritical drying and constant pressure and dry two kinds of modes.SiO2 aeroge performance prepared by supercritical methanol technology is comparatively excellent, but the power consumption of equipment complex and expensive, drying process is high, dangerous large.Constant pressure and dry prepares SiO2 aeroge without the need to large number quipments, workable, safety and environmental protection, for the large-scale industrial production of SiO2 aeroge provides possibility.But the normal pressure preparation technology of report is loaded down with trivial details at present, needs through long surface-hydrophobicized modification and solvent replacement process.Chinese patent CN101200293A and Chinese patent CN1011649881A discloses two kinds and prepares spherical SiO
2the method of aeroge microparticle, main employing stirs into ball and liquid spherical container shaping method obtains spherical wet gel, but will replace and the Process of Surface Modification time through the solvent of 5 ~ 6 days.Chinese patent 201310046976.8 discloses one and utilizes constant pressure and dry technology to prepare SiO fast
2the method of aerogel microball, it adopts silicate aqueous solution/non-polar solven inverse emulsion system to carry out being obtained by reacting SiO
2aerogel microball, but its presoma silicate solution needs, through cationic ion-exchange resin, water glass solution is carried out ion-exchange, this process is loaded down with trivial details consuming time and cost is high.Generally speaking, current spherical SiO
2still there is complex process, length consuming time, high in cost of production shortcoming in the technology of preparing of aeroge microparticle, a kind of cost of continuation research and development is low, technique simple and the technology that can accomplish scale production prepares spherical SiO
2aeroge microparticle is of great practical significance.
Summary of the invention
The present invention is directed in prior art the method complex process preparing nanoporous light silicon dioxide microballoon, the technical problem that cost is high, object is to provide that a kind of cost is low, technique simple and the constant pressure and dry technology that can accomplish scale production prepares the method for nanoporous light silicon dioxide microballoon.
Object of the present invention has been come in the following manner:
The preparation method of a kind of nanoporous light silicon dioxide microballoon provided by the invention: employing waterglass is presoma, low surface tension solvent is replacement solvent, chemical reaction is carried out by adding surfactant formation emulsion system, wherein using inorganic acid as catalyst, organic silane compound is hydrophobic modifier, and process is carried out in the steps below successively:
(1) waterglass is at room temperature mixed with deionized water, add organic silane compound and low surface tension solvent, stir and obtain mixed solution;
(2) in mixed solution, add surfactant, after making System forming emulsion by high-speed stirred, add inorganic acid catalyst wherein, heating stirring reaction, after reaction terminates, leave standstill, filter, obtain white depositions;
(3) white depositions is washed, constant pressure and dry, obtain nanoporous light silicon dioxide microballoon.
In described step (1), in mixed solution, the mass ratio of waterglass, deionized water, organic silane compound and low surface tension solvent is 1:(3 ~ 10): (0.1 ~ 2): (3 ~ 15);
In described step (2), the mass ratio of surfactant and waterglass is (0.01 ~ 0.5): 1;
In described step (2), the mass ratio of inorganic acid catalyst and waterglass is (0.1 ~ 1): 1;
In order to realize the present invention better, described inorganic acid is at least one in hydrochloric acid, sulfuric acid, nitric acid and perchloric acid;
In order to realize the present invention better, at least one in described low surface tension solvent normal heptane, n-hexane and normal octane;
In order to realize the present invention better, described organic silane compound is at least one in dimethyldiethoxysilane, dimethyldimethoxysil,ne, HMDO, HMDS, MTES, MTMS, dodecyltrimethoxysilane, dodecyl triethoxysilane, hexadecyl trimethoxy silane, hexadecyl, octamethylcy-clotetrasiloxane, hexamethyl cyclotrisiloxane;
In order to realize the present invention better, described surfactant is Tween-20, Tween-40, Tween-60, Tween-80, Tween-65, Tween-85, Si Ban-20, Si Ban-40, Si Ban-60, Si Ban-65, Span-80, at least one of Si Ban-85;
In order to realize the present invention better, in the high-speed stirred described in described step (2), refer at 400 ~ 1500rpm rotating speed stirring condition; At the heating stirring reaction described in described step (2), refer to that reaction temperature is 30 ~ 70 DEG C, the reaction time is 0.5h ~ 5h; Constant pressure and dry in described step (3) refers in atmospheric conditions, dry 1 ~ 6h at 80 ~ 180 DEG C.
Nanoporous light silicon dioxide microballoon prepared by the present invention is regular spherical particle, and particle diameter is 1 ~ 1000 μm, and specific area is 300 ~ 1200 m
2/ g, aperture is 10 ~ 100nm.
Relative to prior art, tool of the present invention has the following advantages and beneficial effect:
1, nanoporous light silicon dioxide microspheres flow process of the present invention is simple; In addition, raw materials for production are cheap, and solvent easily reclaims, and production cost is low, and productive rate is high.
2, nanoporous light silicon dioxide microballoon preparation process of the present invention is with cheap waterglass for raw material, need not carry out ion exchange process through cationic ion-exchange resin, is convenient to large-scale industrial and produces.
3, the nanoporous light silicon dioxide microballoon prepared by the present invention is regular spherical particle, and average grain diameter can regulate and control within the scope of 1 ~ 1000 μm, and has typical nano-porous structure, can be applicable to heat insulation, chromatographic isolation, the field such as catalysis and biological medicine carrying.
Accompanying drawing explanation
The SEM figure of the nanoporous light silicon dioxide microballoon of Fig. 1 prepared by the embodiment of the present invention 1.
The SEM figure of the nanoporous light silicon dioxide microsphere surface microstructure of Fig. 2 prepared by the embodiment of the present invention 1.
The EDS figure of the nanoporous light silicon dioxide microballoon of Fig. 3 prepared by the embodiment of the present invention 1.
Detailed description of the invention
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
embodiment 1
100g waterglass (modulus is 3.0) is at room temperature mixed with 300g deionized water, adds 50g hydrochloric acid (37 wt%) and 300g n-hexane, stir and obtain mixed solution; In mixed solution, add 10g Tween-20 surfactant, after rapid stirring makes System forming emulsion under 400rpm rotating speed, add 10g dimethyldiethoxysilane to it, stirring reaction 3h under 30 DEG C of heating conditions, after reaction terminates, leaves standstill, filter, obtain white depositions; By n-hexane white depositions 3 times, be then positioned in air dry oven, under 100 DEG C of conditions, dry process 6h, obtains the nanoporous light silicon dioxide microballoon of white.
The scanning electron microscope (SEM) photograph of prepared nanoporous light silicon dioxide microballoon as shown in Figures 1 and 2, particle is spherical shape, particle size distribution is between 10 ~ 20 μm, can be found out by accompanying drawing 2, obtained nanoporous light silicon dioxide microballoon is the porous material with contiguous network structure, pore size is 5 ~ 50nm, and nano aperture is evenly distributed.Accompanying drawing 3, for preparing the EDS figure of product, can find out do not have the appearance of Na element in prepared nanoporous light silicon dioxide microsphere sample, illustrate in after chemical reaction modifying process, can reach Na by accompanying drawing 3
+synchronously carrying out of the processes such as ion exchange, sol-gel process, surface-hydrophobicized modification, solvent displacement.
Test result:
Particle diameter: 10 ~ 20 μm;
Apparent density: 0.1g/cm3;
Specific area: 1200 m2/g;
Average pore size: 50nm.
embodiment 2
At room temperature mixed with 800g deionized water by 100g waterglass (modulus is 3.0), ((50 wt %) and 600g normal heptane, stir and obtain mixed solution to add 120g perchloric acid; In mixed solution, add 1g Tween-40 surfactant, after rapid stirring makes System forming emulsion under 1500rpm rotating speed, add 90g octamethylcy-clotetrasiloxane to it, stirring reaction 1.5h under 60 DEG C of heating conditions, after reaction terminates, leaves standstill, filter, obtain white depositions; Wash white depositions 3 times with normal heptane, be then positioned in air dry oven, under 80 DEG C of conditions, dry process 3h, obtains the nanoporous light silicon dioxide microballoon of white.
Test result:
Particle diameter: 50 ~ 120 μm;
Apparent density: 0.15g/cm3;
Specific area: 1000 m2/g;
Average pore size: 80nm.
embodiment 3
100g waterglass (modulus is 3.2) is at room temperature mixed with 600g deionized water, adds 100g hydrochloric acid (37 wt%) and 1200g normal octane, stir and obtain mixed solution; 20g Tween-60 surfactant is added in mixed solution, after under 800rpm rotating speed, rapid stirring makes System forming emulsion, 80g dodecyl triethoxysilane is added to it, stirring reaction 1.5h under 50 DEG C of heating conditions, after reaction terminates, leave standstill, filter, obtain white depositions; Wash white depositions 3 times with normal octane, be then positioned in air dry oven, under 180 DEG C of conditions, dry process 2h, obtains the nanoporous light silicon dioxide microballoon of white.
Test result:
Particle diameter: 1 ~ 20 μm;
Apparent density: 0.05g/cm3;
Specific area: 1200 m2/g;
Average pore size: 10nm.
embodiment 4
100g waterglass (modulus is 3.3) is at room temperature mixed with 450g deionized water, adds 80g sulfuric acid (50 wt %) and 800g n-hexane, stir and obtain mixed solution; 50g Tween-65 surfactant is added in mixed solution, after under 1000rpm rotating speed, rapid stirring makes System forming emulsion, 150g MTMS is added to it, stirring reaction 1.5h under 45 DEG C of heating conditions, after reaction terminates, leave standstill, filter, obtain white depositions; By n-hexane white depositions 3 times, be then positioned in air dry oven, under 90 DEG C of conditions, dry process 6h, obtains the nanoporous light silicon dioxide microballoon of white.
Test result:
Particle diameter: 100 ~ 500 μm;
Apparent density: 0.15g/cm3;
Specific area: 800 m2/g;
Average pore size: 100nm.
embodiment 5
100g waterglass (modulus is 3.4) is at room temperature mixed with 600g deionized water, adds 100g nitric acid (50 wt %), 20g HMDS and 600g normal heptane, stir and obtain mixed solution; 5g Si Ban-20 surfactant is added in mixed solution, after under 600rpm rotating speed, rapid stirring makes System forming emulsion, 30g hexadecyl trimethoxy silane is added to it, stirring reaction 0.5h under 60 DEG C of heating conditions, after reaction terminates, leave standstill, filter, obtain white depositions; Wash white depositions 3 times with normal heptane, be then positioned in air dry oven, under 130 DEG C of conditions, dry process 5h, obtains the nanoporous light silicon dioxide microballoon of white.
Test result:
Particle diameter: 100 ~ 1000 μm;
Apparent density: 0.09g/cm3;
Specific area: 1100 m2/g;
Average pore size: 70nm.
embodiment 6
100g waterglass (modulus is 3.0) is at room temperature mixed with 500g deionized water, adds 50g perchloric acid (50 wt %) and 1000g normal octane, stir and obtain mixed solution; In mixed solution, add 40g Si Ban-40 surfactant, after rapid stirring makes System forming emulsion under 900rpm rotating speed, add 100g HMDS to it, stirring reaction 1.5h under 40 DEG C of heating conditions, after reaction terminates, leaves standstill, filter, obtain white depositions; Wash white depositions 3 times with normal octane, be then positioned in air dry oven, under 120 DEG C of conditions, dry process 3h, obtains the nanoporous light silicon dioxide microballoon of white.
Test result:
Particle diameter: 50 ~ 200 μm;
Apparent density: 0.08g/cm3;
Specific area: 900 m2/g;
Average pore size: 40nm.
embodiment 7
100g waterglass (modulus is 2.2) is at room temperature mixed with 300g deionized water, adds 20g nitric acid (50 wt %) and 1500g n-hexane, stir and obtain mixed solution; In mixed solution, add 15g Si Ban-60 surfactant, after rapid stirring makes System forming emulsion under 700rpm rotating speed, add 200g HMDO to it, stirring reaction 1.5h under 50 DEG C of heating conditions, after reaction terminates, leaves standstill, filter, obtain white depositions; By n-hexane white depositions 3 times, be then positioned in air dry oven, under 180 DEG C of conditions, dry process 1h, obtains the nanoporous light silicon dioxide microballoon of white.
Test result:
Particle diameter: 50 ~ 100 μm;
Apparent density: 0.12g/cm3;
Specific area: 600 m2/g;
Average pore size: 40nm.
embodiment 8
100g waterglass (modulus is 3.7) is at room temperature mixed with 1000g deionized water, adds 200g sulfuric acid (50 wt%) and 400g normal heptane, stir and obtain mixed solution; 30g Span-80 surfactant is added in mixed solution, after under 1200rpm rotating speed, rapid stirring makes System forming emulsion, 50g dimethyldimethoxysil,ne is added to it, stirring reaction 0.5h under 70 DEG C of heating conditions, after reaction terminates, leave standstill, filter, obtain white depositions; Wash white depositions 3 times with normal heptane, be then positioned in air dry oven, under 80 DEG C of conditions, dry process 6h, obtains the nanoporous light silicon dioxide microballoon of white.
Test result:
Particle diameter: 60 ~ 120 μm;
Apparent density: 0.16g/cm3;
Specific area: 300 m2/g;
Average pore size: 100nm.
Claims (5)
1. the preparation method of a nanoporous light silicon dioxide microballoon, it is characterized in that: employing waterglass is presoma, low surface tension solvent is replacement solvent, chemical reaction is carried out by adding surfactant formation emulsion system, wherein using inorganic acid as catalyst, organic silane compound is hydrophobic modifier, and process is carried out in the steps below successively:
(1) waterglass is at room temperature mixed with deionized water, add organic acid catalyst and low surface tension solvent, stir and obtain mixed solution;
(2) in mixed solution, add surfactant, after making System forming emulsion by high-speed stirred, add organic silane compound wherein, heating stirring reaction, after reaction terminates, leave standstill, filter, obtain white depositions;
(3) white depositions is washed, constant pressure and dry, obtain nanoporous light silicon dioxide microballoon.
2. method according to claim 1, is characterized in that:
In described step (1), in mixed solution, the mass ratio of waterglass, deionized water, organic acid catalyst and low surface tension solvent is 1:(3 ~ 10): (0.1 ~ 1): (3 ~ 15);
In described step (2), the mass ratio of surfactant and waterglass is (0.01 ~ 0.5): 1;
In described step (2), the mass ratio of organic silane compound and waterglass is (0.1 ~ 2): 1.
3. method according to claim 1, is characterized in that: described inorganic acid is at least one in hydrochloric acid, sulfuric acid, nitric acid and perchloric acid;
At least one in described low surface tension solvent normal heptane, n-hexane and normal octane;
Described organic silane compound is at least one in dimethyldiethoxysilane, dimethyldimethoxysil,ne, HMDO, HMDS, MTES, MTMS, dodecyltrimethoxysilane, dodecyl triethoxysilane, hexadecyl trimethoxy silane, hexadecyl, octamethylcy-clotetrasiloxane, hexamethyl cyclotrisiloxane;
Described surfactant is Tween-20, Tween-40, Tween-60, Tween-80, Tween-65, Tween-85, Si Ban-20, Si Ban-40, Si Ban-60, Si Ban-65, Span-80, at least one of Si Ban-85.
4. method according to claim 1, is characterized in that:
In the high-speed stirred described in described step (2), refer at 400 ~ 1500rpm rotating speed stirring condition;
At the heating stirring reaction described in described step (2), refer to that reaction temperature is 30 ~ 70 DEG C, the reaction time is 0.5h ~ 5h;
Constant pressure and dry in described step (3) refers in atmospheric conditions, dry 1 ~ 6h at 80 ~ 180 DEG C.
5. method according to claim 1, is characterized in that: described nanoporous light silicon dioxide microballoon is regular spherical particle, and particle diameter is 1 ~ 1000 μm, and specific area is 300 ~ 1200 m
2/ g, aperture is 10 ~ 100nm.
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