CN105236428A - Wormlike hollow silicon dioxide and preparation method thereof - Google Patents
Wormlike hollow silicon dioxide and preparation method thereof Download PDFInfo
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- CN105236428A CN105236428A CN201510559042.3A CN201510559042A CN105236428A CN 105236428 A CN105236428 A CN 105236428A CN 201510559042 A CN201510559042 A CN 201510559042A CN 105236428 A CN105236428 A CN 105236428A
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Abstract
The invention discloses a wormlike hollow silicon dioxide being composed of, by mass, 0.1-0.5 parts of an organic silane coupling agent, 50-100 parts of deionized water and 0.5-1.0 part of tetraethylortho silicate. The invention also provides a preparation method of the wormlike hollow silicon dioxide, which includes the steps of pre-hydrolyzing the organic silane coupling agent through sol-gel method, and then adding the tetraethylortho silicate and concentrated ammonia water to perform a reaction under an alkaline condition to obtain the wormlike hollow silicon dioxide. The wormlike hollow silicon dioxide is simple in preparation method, is strong in operability, is mild in reaction conditions, achieves one-step functionalization and has excellent application prospect.
Description
Technical field
The invention belongs to chemical field, relate to a kind of silicon-dioxide, specifically a kind of vermiform hollow silicon dioxide and preparation method thereof.
Background technology
Silicon-dioxide has good mechanical property, thermostability and unreactiveness, is all one of focus of science and technology field research all the time.It is always a kind of important Inorganic Chemicals, and silicate glass plays extremely important role in science and industrial technology always; On the other hand, as filling enhancing modified agent, be widely used in rubber, plastics, fiber industry.1956, Kolbe was by silicon alkoxide hydrolysis, polymerization, and in short chain alcohol solvent, after having synthesized atresia, monodisperse silica particle first, up till now, earth silicon material becomes study hotspot.
And the material of hollow ball structure is due to its potential micro-surface-area, void content, thermal conductivity, the performances such as optical index have attracted the extensive concern of people.Wherein, silicon-dioxide because the characteristic of its uniqueness, as: the features such as density is low and physical strength is high, stable chemical nature, and thermostability is very strong, can be applicable to the release of medicine and biomolecules, photochemical catalysis, energy storage, sensing control release etc.Silicon dioxide hollow material structure common mostly at present is spherical, surface is hydroxyl, and the later stage must adopt organo silane coupling agent again to carry out functionalization (Yu Shuhong, Wan Yong to silicon dioxide hollow material surface, a preparation method for hollow silica ball, CN1931718A; Zheng Nanfeng, Fang Xiaoliang, Chen Cheng, Li Yue, a kind of preparation method of ordered mesoporous silica dioxide, CN102153094A).
Summary of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of vermiform hollow silicon dioxide and preparation method thereof, the technical problem that described this vermiform hollow silicon dioxide and preparation method thereof solves silicon dioxide hollow material surface band hydroxyl in prior art, is of limited application.
The invention provides a kind of vermiform hollow silicon dioxide, calculate according to the mass fraction, its raw material composition and content as follows:
Organo silane coupling agent 0.1-0.5 part,
Deionized water 50-100 part,
Tetraethoxy 0.5-1.0 part.
Further, described organo silane coupling agent is vinyltrimethoxy silane, phenyltrimethoxysila,e or (3-mercaptopropyi) Trimethoxy silane.
Present invention also offers the preparation method of above-mentioned a kind of vermiform hollow silicon dioxide, comprise the steps:
1) organo silane coupling agent, deionized water and tetraethoxy is taken according to mass fraction;
2) join in deionized water by organo silane coupling agent, stirring at normal temperature 30-40min under 300-400r/min, is warming up to 50-60 DEG C, hydrolysis 0.5 ~ 3h;
3) tetraethoxy is added step 2) the aqueous solution in, and add simultaneously ammoniacal liquor regulate pH be 9-12, continue control mixing speed be 300-400r/min, stirring reaction 3-7h, obtains vermiform hollow silicon dioxide.
Concrete, the mass percent concentration of described ammoniacal liquor is 25%.
The present invention adopts sol-gel method, has prepared constitutionally stable vermiform silicon dioxide hollow material, effectively improve the specific surface area of hollow silica ball by the hydrolysis-condensation reaction of organo silane coupling agent and tetraethoxy; And can to vermiform silicon dioxide hollow material functionalization, this hollow material contains the functionalization group that can be used effectively, and as vinyl, phenyl, sulfydryl, expands the Application Areas of this hollow material to a great extent, has potential using value.
The present invention compares with prior art, and its technical progress is significant.The present invention makes the first prehydrolysis of organo silane coupling agent by sol-gel method, adds tetraethoxy subsequently and strong aqua reacts in the basic conditions, obtains vermiform hollow silicon dioxide.The preparation technology of this vermiform hollow silicon dioxide is simple, workable, and reaction conditions is gentle, and can realize, to the functionalization of this hollow silicon dioxide one step, having a good application prospect.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of the vermiform hollow silicon dioxide obtained by method of the present invention.
Embodiment
Below by embodiment, the present invention is described in further detail, but do not limit the present invention.
embodiment 1
A kind of vermiform hollow silicon dioxide, calculates according to the mass fraction, its raw material composition and content as follows:
(3-mercaptopropyi) Trimethoxy silane 0.1 part,
Deionized water 50 parts,
Tetraethoxy 0.5 part.
The preparation method of above-mentioned a kind of vermiform hollow silicon dioxide is as follows:
Join in 50 parts of deionized waters by 0.1 part of (3-mercaptopropyi) Trimethoxy silane, stirring at normal temperature 30min under 300r/min, is warming up to 50 DEG C, hydrolysis 1h; Added wherein by 0.5 part of tetraethoxy subsequently, and the ammoniacal liquor simultaneously adding 10ul massfraction 25% regulates pH to be 9, continuing to control mixing speed is 300r/min, and stirring reaction 3h, obtains vermiform hollow silicon dioxide.
Obtained sample is tested by the H-800 type transmission electron microscope of Li company, and this hollow material 80% is in vermiform hollow structure.
embodiment 2
A kind of vermiform hollow silicon dioxide, calculates according to the mass fraction, its raw material composition and content as follows:
Vinyl trimethylsilane 0.2 part
Deionized water 50 parts
Tetraethoxy 1 part
The preparation method of above-mentioned a kind of vermiform hollow silicon dioxide is as follows:
0.2 part of vinyl trimethylsilane joined in 50 parts of deionized waters, stirring at normal temperature 30min under 400r/min, is warming up to 60 DEG C, hydrolysis 30min; Added wherein by 1 part of tetraethoxy subsequently, and the ammoniacal liquor simultaneously adding 20ul massfraction 25% regulates pH to be 10, continuing to control mixing speed is 400r/min, and stirring reaction 7h, obtains vermiform hollow silicon dioxide.
Obtained sample is tested by the H-800 type transmission electron microscope of Li company, and this hollow material all becomes hollow vermiform, as shown in Figure 1.
embodiment 3
A kind of vermiform hollow silicon dioxide, calculates according to the mass fraction, its raw material composition and content as follows:
Vinyl trimethylsilane 0.3 part
Deionized water 80 parts
Tetraethoxy 0.8 part
The preparation method of above-mentioned a kind of vermiform hollow silicon dioxide is as follows:
0.3 part of vinyl trimethylsilane joined in 80 parts of deionized waters, stirring at normal temperature 1h under 400r/min, is warming up to 50 DEG C, hydrolysis 2h; Added wherein by 0.8 part of tetraethoxy subsequently, and the ammoniacal liquor simultaneously adding 30ul massfraction 25% regulates pH to be 11, continuing to control mixing speed is 400r/min, and stirring reaction 5h, obtains vermiform hollow silicon dioxide.
Obtained sample is tested by the H-800 type transmission electron microscope of Li company, and this hollow material 70% is vermiform hollow structure.
embodiment 4
A kind of vermiform hollow silicon dioxide, calculates according to the mass fraction, its raw material composition and content as follows:
Phenyltrimethoxysila,e 0.4 part
Deionized water 100 parts
Tetraethoxy 1.0 parts
The preparation method of above-mentioned a kind of vermiform hollow silicon dioxide is as follows:
0.4 part of phenyltrimethoxysila,e joined in 100 parts of deionized waters, stirring at normal temperature 1h under 400r/min, is warming up to 60 DEG C, hydrolysis 3h; Added wherein by 1 part of tetraethoxy subsequently, and the ammoniacal liquor simultaneously adding 40ul massfraction 25% regulates pH to be 12, continuing to control mixing speed is 400r/min, and stirring reaction 6h, obtains vermiform hollow silicon dioxide.
Obtained sample is tested by the H-800 type transmission electron microscope of Li company, and this hollow material is vermiform hollow structure.
embodiment 5
Getting 50ml concentration is that the cyclamen aldehyde ethanolic soln of 5g/L is placed in Erlenmeyer flask, add the vermiform hollow silicon dioxide 0.1g in embodiment 2, at room temperature with constant temperature oscillator shake 24h, with the centrifugal 10min of 10000r/min, get supernatant liquor and adopt UV2100 ultraviolet spectrophotometer test absorbancy.
Separately get 50ml ethanolic soln, add the vermiform hollow silicon dioxide 0.1g in embodiment 2, at room temperature with constant temperature oscillator shake 24h, with the centrifugal 10min of 10000r/min, get supernatant liquor as blank reference.
Above-mentioned load issue display, this vermiform hollow silicon dioxide is 39.98% to the load factor of cyclamen aldehyde.
Claims (4)
1. a vermiform hollow silicon dioxide, is characterized in that calculating according to the mass fraction, its raw material composition and content as follows:
Organo silane coupling agent 0.1-0.5 part,
Deionized water 50-100 part,
Tetraethoxy 0.5-1.0 part.
2. as claim 1 vermiform hollow silicon dioxide, it is characterized in that: described organo silane coupling agent is vinyltrimethoxy silane, phenyltrimethoxysila,e or (3-mercaptopropyi) Trimethoxy silane.
3. the preparation method of a kind of vermiform hollow silicon dioxide according to claim 1, is characterized in that comprising the steps:
1) organo silane coupling agent, deionized water and tetraethoxy is taken according to mass fraction;
2) join in deionized water by organo silane coupling agent, stirring at normal temperature 30-40min under 300-400r/min, is warming up to 50-60 DEG C, hydrolysis 0.5 ~ 3h;
3) tetraethoxy is added step 2) the aqueous solution in, and add simultaneously ammoniacal liquor regulate pH be 9-12, continue control mixing speed be 300-400r/min, stirring reaction 3-7h, obtains vermiform hollow silicon dioxide.
4. the preparation method of a kind of vermiform hollow silicon dioxide according to claim 3, is characterized in that: the mass percent concentration of described ammoniacal liquor is 25%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109607552A (en) * | 2019-01-15 | 2019-04-12 | 河北工业大学 | A method of preparing three-dimensional ball chain structure silica |
| CN115215348A (en) * | 2022-08-29 | 2022-10-21 | 吉林大学 | Preparation method of vermicular mesoporous silica |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101289190A (en) * | 2008-05-22 | 2008-10-22 | 同济大学 | Functional hollow earth silicon microballoons and method for preparing same |
| CN103508461A (en) * | 2012-06-29 | 2014-01-15 | 中国科学院大连化学物理研究所 | Method for preparing hollow silicon dioxide nanometer particles |
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2015
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101289190A (en) * | 2008-05-22 | 2008-10-22 | 同济大学 | Functional hollow earth silicon microballoons and method for preparing same |
| CN103508461A (en) * | 2012-06-29 | 2014-01-15 | 中国科学院大连化学物理研究所 | Method for preparing hollow silicon dioxide nanometer particles |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109607552A (en) * | 2019-01-15 | 2019-04-12 | 河北工业大学 | A method of preparing three-dimensional ball chain structure silica |
| CN109607552B (en) * | 2019-01-15 | 2021-10-22 | 河北工业大学 | Method for preparing silicon dioxide with three-dimensional ball chain structure |
| CN115215348A (en) * | 2022-08-29 | 2022-10-21 | 吉林大学 | Preparation method of vermicular mesoporous silica |
| CN115215348B (en) * | 2022-08-29 | 2023-11-17 | 吉林大学 | Preparation method of vermicular mesoporous silica |
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