CN102145897B - Large-pore-volume silicon dioxide with nanoparticle structure and preparation method thereof - Google Patents
Large-pore-volume silicon dioxide with nanoparticle structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses large-pore-volume silicon dioxide with a nanoparticle structure and a preparation method thereof. The large-pore-volume silicon dioxide is a product obtained by performing reaction, thermal activation, washing and supersonic air current cutting on alkaline silicate, a sulfuric acid solution and a dispersant serving as raw materials. The silicon dioxide content (dry base) is over 99.0, the BET specific surface area is between 280 m<2>/g and 450 m<2>/g, the void volume is between 2.0 and 3.6, the secondary particle average particle size is between 5 mum and 6 mum, and the primary particle size is between 10 nanometers and 15 nanometers. The average particle size, pore volume and specific surface area of a product produced with the preparation method are controllable; and large-pore-volume silicon dioxide products with different performances can be prepared according to different uses.
Description
Technical field
The present invention relates to a kind of preparation method with large aperture capacity silicon oxide of nanoparticle structure.
Background technology
Utilize large aperture capacity silicon oxide for a long time; As Coating Matting agent, thickening material, ink-jet printing media sorbing material, the agent of plastics opening, heat-insulating material etc. is common knowledge; Utilize wet method to prepare large aperture capacity silicon oxide at present the precipitator method and sol-gel method are arranged; Utilize its pore property of large aperture capacity silicon oxide of precipitator method preparation unstable, cause unstable product quality.US5231066, US5895770, US5372983 etc.The U5625023 disclosed method all is that potassium or sodium silicate and mineral acid mix the formation hydrogel through a special nozzle, and washing, drying obtain specific surface 10-1000m then
2/ g; Pore volume: 0.5-2.5ml/g, the silica product of aperture 40-200 discloses a kind of preparation method of large aperture capacity silicon oxide in patent US3959174; It adds hydrophobizing agent and (comprises inorganic ammonia salt, inorganic sodium and sylvite in water glass; Small-molecule substances such as organic alcohol, ketone) reaction is at room temperature regulated pH value at 10-11, continues to add acid to PH3-10 through ageing; Be warming up to 90 ℃ of ageings; Making pore volume through washing, drying, pulverizing again is that 1.2-3.0 gets large aperture capacity silicon oxide, and this patent limits the size of pore volume, but to the size of formation silicon-dioxide primary particle and the not control of mean particle size of offspring; And as the size and the offspring mean particle size of the silicon-dioxide primary particle of purposes such as Coating Matting agent, thickening material, ink-jet printing media sorbing material, heat-insulating material, the agent of plastics opening, to using the performance decisive role.
Summary of the invention
The object of the present invention is to provide a kind of preparation method with large aperture capacity silicon oxide of nanoparticle structure; To produce the large aperture capacity silicon oxide of its mean particle size, pore volume and controllable specific surface area, can prepare the large aperture capacity silicon oxide product of different performance according to different purposes.
The large aperture capacity silicon oxide of nanoparticle structure of the present invention is to be raw material with alkaline silicate and sulphuric acid soln and dispersion agent; The product of after reaction, thermal activation, washing, supersonic airstream cutting, processing; Its dioxide-containing silica is more than 99.0, and the BET specific surface area is 280～450m
2/ g, volume of voids are 2.0～3.6, and the offspring mean particle size is 5～6 μ m, and primary particle size is 10～15nm.
The preparation method of the large aperture capacity silicon oxide of nanoparticle structure may further comprise the steps:
(1) be that 5～15% alkaline silicate (A), weight percent concentration are that 6-20% sulphuric acid soln (B), dispersion agent (C) are raw material with weight percent concentration; Reacted 1～5 hour the weight ratio of its A:B:C=2～6:1:0.01～0.05, and the adjustment pH value is 3～4; Said dispersion agent is one or more of Fatty Alcohol(C12-C14 and C12-C18) and ethylene oxide condensate, polyoxyethylene glycol, oleic acid glyceride;
(2) above-mentioned reaction mass is carried out the thermal activation reaction 80～105 ℃ of temperature, be incubated 1～4 hour;
(3) washing: water or alcohol or its mixture wash to sodium ions content be below 0.2%,
(4) drying: spraying drying is carried out in the filter cake making beating under 400～600 ℃;
(5) with supersonic airstream with drying after product cut, control product offspring mean particle size is 5～6 microns; The total fugitive constituent of control below 950 ℃ is finished product below 10%.
The concentration of alkaline silicate is 6～12% described in the step (1).
Vitriolic concentration is 10～15% described in the step (1).
The A:B:C weight ratio is=3～5:1:0.02～0.04 described in the step (1).
Reaction times described in the step (1) is 2～5 hours.
The reaction of thermal activation described in the step (2) is 80～100 ℃.
Advantage of the present invention: the product that the present invention produces, its mean particle size, pore volume and specific surface area are all controlled; Can prepare the large aperture capacity silicon oxide product of different performance according to different purposes; This performance of products can reach, and dioxide-containing silica (butt) is greater than 99.0%, and the BET specific surface area is 280～450m
2/ g, volume of voids are 2.0～3.6, and mean particle size is 5～6 μ m, the index request of the primary particle 8～15nm of silicon-dioxide; Whole technological process need not to use the strict process raw material.
Embodiment
Below in conjunction with embodiment the present invention is described further.
Embodiment 1: do seven parallel sample experiments:
Each all prepares weight percent concentration is that 6% sodium silicate solution 1000g and weight percent concentration are 15% sulphuric acid soln 300g; Add dispersion agent Fatty Alcohol(C12-C14 and C12-C18) and ethylene oxide condensate 10g,, to react, the reaction times was controlled at 3 hours, and adding sulfuric acid adjustment pH value is 3-4; Material is warming up to 80 ℃ carries out thermal activation treatment.Control primary particle 8-10nm is again through washing, spraying drying and use supersonic airstream to cut into average 5-6 micron to the exsiccant particle.Its product performance are as shown in table 1:
Table 1
Embodiment 2: do seven parallel sample experiments:
Each preparation dioxide-containing silica is 12% sodium silicate solution 1000g; With formulation content be that the solution 200g of sulfuric acid 10% reacts and adds polyoxyethylene glycol 40g simultaneously; Reaction times was controlled at 5 hours, added the sulfuric acid pH value then and was 3-4 and material is warming up to 100 ℃ carries out thermal activation.Control primary particle 10-15nm, again through washing, spraying drying and use supersonic airstream to cut into average 5-6 micron to the exsiccant particle, its its product performance are as shown in table 2:
Table 2
Embodiment 3: do seven parallel sample experiments:
Each all prepares dioxide-containing silica is 12% sodium silicate solution 1000g; With formulation content be that 15% sulphuric acid soln 250g reacts and adds oleic acid glyceride 30g simultaneously; Reaction times was controlled at 2 hours, added sulfuric acid adjustment pH value and was 3-5 and be warming up to 90 ℃ and carry out thermal activation.Control primary particle 10-15nm is again through washing, spraying drying and use supersonic airstream to cut into average 5-6 micron to the exsiccant particle, and its its product performance are as shown in table 3:
Table 3
Embodiment 4: do seven parallel sample experiments:
Each all prepares dioxide-containing silica is 8% sodium silicate solution 1000g; The solution 330g of preparation sulfuric acid content 15%; Add oleic acid glyceride and each 10g of polyoxyethylene glycol, the reaction times was controlled at 5 hours, and adding sulfuric acid, to adjust pH value be 3.5 material is warming up to 80 ℃ carries out thermal activation.Control primary particle 8-15nm, again through washing, spraying drying and use supersonic airstream to cut into average 5-6 micron to the exsiccant particle, its its product performance are as shown in table 4:
Table 4
Claims (6)
1. the large aperture capacity silicon oxide of a nanoparticle structure; It is characterized in that; Be to be raw material with alkaline silicate and sulphuric acid soln and dispersion agent; The product of after reaction, thermal activation, washing, supersonic airstream cutting, processing, its dioxide-containing silica is more than 99.0%, the BET specific surface area is 280～450m
2/ g, volume of voids are 2.0～3.6, and the offspring mean particle size is 5～6 μ m, and primary particle size is 10～15nm;
The preparation method of the large aperture capacity silicon oxide of said nanoparticle structure may further comprise the steps:
(1) be that 5～15% alkaline silicate (A), weight percent concentration are that 6-20% sulphuric acid soln (B), dispersion agent (C) are raw material with weight percent concentration; Reacted 1～5 hour the weight ratio of its A:B:C=2～6:1:0.01～0.05, and the adjustment pH value is 3～4; Said dispersion agent is one or more of Fatty Alcohol(C12-C14 and C12-C18) and ethylene oxide condensate, polyoxyethylene glycol, oleic acid glyceride;
(2) above-mentioned reaction mass is carried out the thermal activation reaction 80～105 ℃ of temperature, be incubated 1～4 hour;
(3) washing: water or alcohol or its mixture wash to sodium ions content be below 0.2%,
(4) drying: spraying drying is carried out in the filter cake making beating under 400～600 ℃;
(5) with supersonic airstream with drying after product cut, control product offspring mean particle size is 5～6 microns; The total fugitive constituent of control below 950 ℃ is finished product below 10%.
2. the large aperture capacity silicon oxide of nanoparticle structure according to claim 1 is characterized in that, in said preparing method's step (1), the concentration of said alkaline silicate is 6～12%.
3. the large aperture capacity silicon oxide of nanoparticle structure according to claim 1 and 2 is characterized in that, in said preparing method's step (1), said vitriolic concentration is 10～15%.
4. the large aperture capacity silicon oxide of nanoparticle structure according to claim 1 and 2 is characterized in that, in said preparing method's step (1), said A:B:C weight ratio is=3～5:1:0.02～0.04.
5. the large aperture capacity silicon oxide of nanoparticle structure according to claim 1 and 2 is characterized in that, in said preparing method's step (1), the said reaction times is 2～5 hours.
6. the large aperture capacity silicon oxide of nanoparticle structure according to claim 1 and 2 is characterized in that, in said preparing method's step (2), said thermal activation reaction is 80～100 ℃.
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102989210A (en) * | 2011-09-14 | 2013-03-27 | 重庆工商大学 | Silica nanomaterial filter assembly for waste insulating oil |
| CN102530970B (en) * | 2012-03-01 | 2014-02-19 | 冷水江三A化工有限责任公司 | Preparation method of toothpaste abrasive silicon dioxide |
| CN105460940B (en) * | 2016-02-22 | 2017-05-31 | 冷水江三A新材料科技有限公司 | A kind of mesoporous pharmaceutical carrier silica and preparation method thereof |
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| US3959174A (en) * | 1971-08-24 | 1976-05-25 | W. R. Grace & Co. | Method of selectively producing high pore volume silica gel |
| CN1418811A (en) * | 2002-12-18 | 2003-05-21 | 天津化工研究设计院 | Macroporous precipitation silicon dioxide used for achromatic colours, and its prepn. method |
| CN1730392A (en) * | 2005-06-16 | 2006-02-08 | 复旦大学 | Large aperture capacity silicon oxide vesicle, foamed material and process for preparing the same |
| CN101112991A (en) * | 2006-07-24 | 2008-01-30 | 北京化工大学 | Method for preparing silicon dioxide with large pore volume and large aperture |
| CN101837982A (en) * | 2010-03-19 | 2010-09-22 | 福建师范大学 | Method for preparing silicon dioxide aerogel powder |
| CN102002120A (en) * | 2010-09-20 | 2011-04-06 | 中国海洋石油总公司 | Method for preparing special silica gel carrier with large pore volume and large specific surface area |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3959174A (en) * | 1971-08-24 | 1976-05-25 | W. R. Grace & Co. | Method of selectively producing high pore volume silica gel |
| CN1418811A (en) * | 2002-12-18 | 2003-05-21 | 天津化工研究设计院 | Macroporous precipitation silicon dioxide used for achromatic colours, and its prepn. method |
| CN1730392A (en) * | 2005-06-16 | 2006-02-08 | 复旦大学 | Large aperture capacity silicon oxide vesicle, foamed material and process for preparing the same |
| CN101112991A (en) * | 2006-07-24 | 2008-01-30 | 北京化工大学 | Method for preparing silicon dioxide with large pore volume and large aperture |
| CN101837982A (en) * | 2010-03-19 | 2010-09-22 | 福建师范大学 | Method for preparing silicon dioxide aerogel powder |
| CN102002120A (en) * | 2010-09-20 | 2011-04-06 | 中国海洋石油总公司 | Method for preparing special silica gel carrier with large pore volume and large specific surface area |
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