CN101962188A - Method for preparing ultrafine high-purity SiO2 from volcanic ash - Google Patents
Method for preparing ultrafine high-purity SiO2 from volcanic ash Download PDFInfo
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- CN101962188A CN101962188A CN 201010544403 CN201010544403A CN101962188A CN 101962188 A CN101962188 A CN 101962188A CN 201010544403 CN201010544403 CN 201010544403 CN 201010544403 A CN201010544403 A CN 201010544403A CN 101962188 A CN101962188 A CN 101962188A
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Abstract
The invention discloses a method for preparing ultrafine high-purity SiO2 from volcanic ash. The method comprises the following steps of: A, taking 100 weight parts of the volcanic ash of which the SiO2 content by weight is more than or equal to 50 percent, crushing the volcanic ash to ensure that the particle size is less than or equal to 1 mm; B, adding and dispersing the volcanic ash into acid solution of which the temperature is between 40 and 95 DEG C, stirring for 10 to 180 minutes, and filtering and washing; and C, transferring the volcanic ash processed in the step B into 300 weight parts of water of which the temperature is between 35 and 100 DEG C, adding NaOH or KOH of which the equivalent weight of the SiO2 is equal to that of the SiO2 in the volcanic ash with stirring to form a uniform sol system, then adding 0.5 to 5 weight parts of hydrophobic substances into the uniform sol system, introducing 500 to 1,500 weight parts of organic solvent which is immiscible with water, stirring at a high speed to form a micro-emulsion system, dropping an acidic substance to generate a deposit, filtering to obtain the deposit, and washing and drying the deposit to obtain the ultrafine high-purity SiO2. The method has the advantages of low raw material cost, simple preparation process and easy industrialization; and the prepared ultrafine high-purity SiO2 has uniform particle size distribution and high purity, and can be used as a functional filling material directly.
Description
Technical field:
The present invention relates to a kind of ultra-fine high-purity Si O
2The preparation method.
Background technology:
Ultra-fine high-purity Si O
2As a kind of new function material, owing to have high-performances such as high dielectric, high heat-resisting, high moisture-proof, high filler loading capacity, low bulk, low-stress, low impurity, low-friction coefficient, having broad application prospects at numerous areas such as electronics, electrical equipment, chemical industry, is the high-quality functional stuffing of a kind of ideal electronics, electrical equipment, Chemicals.Since the ultra-fine high-purity Si O of Stober invention hydrolysis of alkoxide prepared
2Since, ultra-fine high-purity Si O appears in methods such as spraying drying, template self-assembly in succession
2The preparation method be in always constantly improve with upgrade among.At present, ultra-fine high-purity Si O
2Main three classes of preparation method: one, with the halosilanes be the vapor phase process of raw material, the primary narrow diameter distribution of product, good dispersion degree, be the preparation ultra-fine high-purity Si O
2Main method, shortcoming such as but the cost height of its raw material halosilanes, and be to react under pyritous gasification environment has complex process, to the equipment requirements harshness, and product easily runs off, and productive rate is low.Two, with water glass be the precipitator method of basic raw material, though this method raw material is extensive, relative low price, it is directly by water glass and alkali precipitation prepared in reaction silicon-dioxide, and water glass purity can not get guaranteeing, causes the SiO for preparing
2Purity is not high, owing to be to precipitate in common solution, the precipitation process time is different in size, causes that particle diameter is inhomogeneous, shape is difficult to control.Three, with the metal alkoxide be the sol-gel method of main raw material, metal alkoxide is as presoma, through hydrolytie polycondensation gelation gradually, then through getting SiO behind ageing, the supercritical drying
2Its shortcoming is, the raw materials cost height of tetraethoxysilance metal alkoxides such as (TEOS), and the supercritical drying arts demand uses autoclave, and productive rate is low, is difficult for industrialization.And, more than the ultra-fine high-purity Si O that makes of three class methods
2Before as functional stuffing, all need to carry out surface hydrophobicity and handle.
Summary of the invention:
Purpose of the present invention just provides a kind of ultra-fine high-purity Si O
2The preparation method, this method raw materials cost is low, preparation technology is simple, is easy to industrialization, the ultra-fine high-purity Si O that makes
2Size distribution is even, and the purity height can directly be used as functional stuffing.
The present invention realizes that the technical scheme that its goal of the invention adopts is, a kind ofly prepares ultra-fine high-purity Si O with volcanic ash
2Method, form by following steps:
A, take by weighing SiO
2The volcanic ash of 100 parts of weights of weight content 〉=50% is crushed to particle diameter≤1mm with it;
B, volcanic ash is added, is distributed to temperature is in 40～95 ℃ the acid solution, stirs 10～180 minutes, filters, washes, and obtains the purifying volcanic ash;
C, the purifying volcanic ash is changed in the water of 300 parts of weights, is heated to 35～100 ℃, stir add with volcanic ash in SiO
2The NaOH of equivalent or KOH form even sol system; Other takes by weighing the lyophobic dust of 0.5～5 part of weight, is scattered in the sol system; And then in this system, introduce the non-aqueous solvent of 500～1500 parts of weights, and stir with the rotating speed of 1000-3000r/min, form microemulsion system, drip acidic substance again and produce precipitation, end to no longer producing precipitation; Filter to such an extent that precipitate, washing, drying, promptly.
The above-mentioned B acid solution in the step is at least a in hydrochloric acid, nitric acid or the sulfuric acid;
The lyophobic dust of above-mentioned C in the step is oil soluble surfactant or silane coupling agent;
The above-mentioned microemulsion precipitator method prepare ultra-fine high-purity Si O
2Non-aqueous solvent be the arbitrary organic solvent immiscible with water.
Preparation principle of the present invention is:
Contain 50% above SiO in the volcanic ash
2, all the other components are theobromine dissolved Al
2O
3, metal oxides such as Mg and CaO, the metal oxide dissolving under the effect of acid in the volcanic ash, remainder is highly purified SiO
2SiO
2Can form the uniform sol system under the thermokalite effect, sol system is a Unstable Systems, produces cohesion and precipitation then under the charged situation in micelle surface changing.The present invention passes through the volcanic ash dissolving formation even colloidal sol of the effect of thermokalite with purifying, in system, introduce with water immiscible second mutually, high-speed stirring is dispersed in the second middle mutually microemulsion that forms with even colloidal sol again, thereby in microemulsion system, introduce the state-of-charge generation precipitation that acidic substance have promptly changed the micelle surface at last, and sedimentary generation is in the microemulsion environment, thereby the big I that therefore precipitates particle diameter is controlled realization SiO by microemulsion
2The control of particle diameter; In addition, the present invention introduces lyophobic dust in the microemulsion precipitation process, and it is adsorbed on sedimentary surface when precipitation forms, so the ultra-fine high-purity Si O of the present invention's preparation
2Do not need to show hydrophobicity, can be used as functional stuffing and be directly used in electronics, electrical equipment and chemical field by follow-up surface treatment.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention has following beneficial effect than prior art:
1, the present invention prepares ultra-fine high-purity Si O with the volcanic ash for the silicon source
2, overcome existing SiO
2Select SiCl in the preparation
4, water glass, limitation that the tetraethoxy cost is high, the volcanic ash reserves are abundant, and are cheap, thereby reduce ultra-fine high-purity Si O greatly
2Preparation cost.
2, volcanic ash with alkali precipitation reaction before carry out purification process with acid-respons earlier and removed alkaline impurities wherein, make the ultra-fine high-purity Si O for preparing
2Purity is guaranteed, and its purity is more than 99%.
3, preparation method of the present invention is the microemulsion precipitator method, and precipitation is to produce in the little aqua region that is cut by oil content in microemulsion, makes the ultra-fine high-purity Si O of its preparation
2Particle diameter is tiny, be evenly distributed.By adjusting kind, consumption and the stirring velocity of lyophobic dust, the ultra-fine high-purity Si O of may command
2Size and distribution have overcome traditional Si O
2The unmanageable difficult problem of particle diameter among the preparation method.
4, the present invention has introduced lyophobic dust in microemulsion precipitator method preparation process, ultra-fine high-purity SiO of preparation
2Itself just has hydrophobicity, can be directly used in fields such as electronics, electrical equipment and chemical industry as functional filler, has overcome the SiO of traditional method preparation
2Before using, it also needs to do the surface-treated limitation.
The present invention is described in further detail below in conjunction with the drawings and specific embodiments.
Description of drawings
Fig. 1 is the ultra-fine high-purity Si O of the inventive method preparation
2Sem photograph.
Embodiment
Embodiment 1
A kind ofly prepare ultra-fine high-purity Si O with volcanic ash
2Method, form by following steps:
A, take by weighing SiO
2The volcanic ash of 100 parts of weights of weight content 〉=50% is crushed to particle diameter≤1mm with it.
B, volcanic ash added, is distributed in 60 ℃ the hydrochloric acid, stirred 90 minutes, filter, wash, obtain the purifying volcanic ash;
C, the purifying volcanic ash is changed in the water of 300 parts of weights, is heated to 70 ℃, stir add with volcanic ash in SiO
2The NaOH of equivalent forms even sol system; Other takes by weighing the lyophobic dust of 3 parts of weights, is scattered in the sol system; And then in this system, introduce the non-aqueous solvent of 500 parts of weights, and stir with the rotating speed of 1500r/min, form microemulsion system, drip acidic substance again and produce precipitation, end to no longer producing precipitation; Filter to such an extent that precipitate, washing, drying, promptly.
After tested, the ultra-fine high-purity Si O that makes of this example
2Particle diameter be 90 ± 15nm.
Embodiment 2-24
The method of the ultra-fine high-purity sio2 of preparation of the embodiment 2-24 all method with embodiment 1 is identical, and different only is: the raw material type that each embodiment selects for use, proportioning and concrete processing parameter are replaced by corresponding raw material type listed in the following table, proportioning and concrete processing parameter.Non-aqueous material in the table is meant the organic solvent immiscible with water.
The raw material type that embodiment 1-24 selects for use, proportioning, processing parameter and make thing SiO
2The particle diameter table
As can be seen from the above table, the prepared SiO of the present invention
2Particle diameter is little, is evenly distributed.
Lyophobic dust can be any existing oil soluble surfactant or silane coupling agent among the present invention.The immiscible organic solvent of water that the present invention uses also is any existing and immiscible organic solvent of water, as: propyl carbinol, primary isoamyl alcohol, or chloroform-methanol.
Fig. 1 is the ultra-fine high-purity Si O of the inventive method preparation
2Sem photograph.From figure, also can find out the SiO that the present invention makes
2The purity height, particle diameter is little, is evenly distributed.
Claims (3)
1. one kind prepares ultra-fine high-purity Si O with volcanic ash
2Method, form by following steps:
A, get the raw materials ready: take by weighing SiO
2The volcanic ash of 100 parts of weights of weight content 〉=50% is crushed to particle diameter≤1mm with it;
B, volcanic ash is added, is distributed to temperature is in 40～95 ℃ the acid solution, stirs 10～180 minutes, filters, washes, and obtains the purifying volcanic ash;
C, the purifying volcanic ash is changed in the water of 300 parts of weights, is heated to 35～100 ℃, stir add with volcanic ash in SiO
2The NaOH of equivalent or KOH form even sol system; Other takes by weighing the lyophobic dust of 0.5～5 part of weight, is scattered in the sol system; And then in this system, introduce 500～1500 parts of weights with the immiscible organic solvent of water, stir with the rotating speed of 1000-3000r/min, form microemulsion system, drip acidic substance again and produce precipitation, end to no longer producing precipitation; Filter to such an extent that precipitate, washing, drying, promptly.
2. as claimed in claim 1ly a kind ofly prepare ultra-fine high-purity Si O with volcanic ash
2Method, it is characterized in that: the described B acid solution in the step is at least a in hydrochloric acid, nitric acid or the sulfuric acid;
3. as claimed in claim 1ly a kind ofly prepare ultra-fine high-purity Si O with volcanic ash
2Method, it is characterized in that: the described C lyophobic dust in the step is oil soluble surfactant or silane coupling agent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010544403 CN101962188A (en) | 2010-11-15 | 2010-11-15 | Method for preparing ultrafine high-purity SiO2 from volcanic ash |
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| CN 201010544403 CN101962188A (en) | 2010-11-15 | 2010-11-15 | Method for preparing ultrafine high-purity SiO2 from volcanic ash |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20150020595A (en) * | 2012-06-21 | 2015-02-26 | 에프티유 게엠베하 포르스청 운트 테크니스크 엔트빅클룽 아이엠 움벨트스쿠쯔 | Means for purifying fluids, method of its preparation and its use |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1097718A (en) * | 1994-04-13 | 1995-01-25 | 中国科学院感光化学研究所 | The preparation method of super fine monodisperse hydrophobic silicon dioxide granules |
| CN1508068A (en) * | 2002-12-18 | 2004-06-30 | 中国矿业大学（北京校区） | Method for preparing nano silicon dioxide using diatomaceous earth |
| CN101045538A (en) * | 2007-05-08 | 2007-10-03 | 浙江大学 | Method for preparing modified silicon oxide using coal series kaolin rock or flyash |
| CN101214963A (en) * | 2008-01-02 | 2008-07-09 | 吉林大学 | Method for preparing high pure nano silicon dioxide from oil shale slag |
-
2010
- 2010-11-15 CN CN 201010544403 patent/CN101962188A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1097718A (en) * | 1994-04-13 | 1995-01-25 | 中国科学院感光化学研究所 | The preparation method of super fine monodisperse hydrophobic silicon dioxide granules |
| CN1508068A (en) * | 2002-12-18 | 2004-06-30 | 中国矿业大学（北京校区） | Method for preparing nano silicon dioxide using diatomaceous earth |
| CN101045538A (en) * | 2007-05-08 | 2007-10-03 | 浙江大学 | Method for preparing modified silicon oxide using coal series kaolin rock or flyash |
| CN101214963A (en) * | 2008-01-02 | 2008-07-09 | 吉林大学 | Method for preparing high pure nano silicon dioxide from oil shale slag |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20150020595A (en) * | 2012-06-21 | 2015-02-26 | 에프티유 게엠베하 포르스청 운트 테크니스크 엔트빅클룽 아이엠 움벨트스쿠쯔 | Means for purifying fluids, method of its preparation and its use |
| CN104394960A (en) * | 2012-06-21 | 2015-03-04 | 技术研究和环境保护发展工联会有限公司 | Means for purifying fluids, method of preparation thereof and uses thereof |
| KR102136093B1 (en) * | 2012-06-21 | 2020-07-22 | 아이-스톤 게엠베하 | Means for purifying fluids, method of its preparation |
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Application publication date: 20110202 |