CN104860319A - Controllable silica micro-powder preparation method - Google Patents
Controllable silica micro-powder preparation method Download PDFInfo
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- CN104860319A CN104860319A CN201510191512.5A CN201510191512A CN104860319A CN 104860319 A CN104860319 A CN 104860319A CN 201510191512 A CN201510191512 A CN 201510191512A CN 104860319 A CN104860319 A CN 104860319A
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Abstract
The invention relates to a controllable silica micro-powder preparation method. The method is characterized in that the controllable silica micro-powder is obtained through the steps of carbon dioxide acidification, precipitation and standing, filtration; calcination, and the like. The method has the following technical effects: 1, radial stirring is carried out with a flat-paddle stirrer, such that silicic acid particles can be delivered to a standing chamber as fast as possible; nano-grade particles are formed, and silicic acid agglomeration is prevented, such that controllable silica micro-powder can be prepared; 2, carbon dioxide gas is delivered in, such that excessively high reaction liquid acidity is prevented, and a problem of low reaction liquid concentration of a precipitation method for preparing silica micro-powder is alleviated; and 3, less equipment is needed; reaction conditions are mild; cost is low; production is safe and reliable; product purity is high; and yield is high.
Description
Technical field
The present invention relates to a kind of preparation method of controllability silicon powder.
Background technology
Modern scientific research shows, silicon powder is class purposes ceramic very widely, have dielectric properties excellence, thermal expansivity is low, thermal conductivity is high, silicon powder series product are processed by the Ultrafine Grinding technical process of pure silica powder through advanced person.It has, and whiteness is high, particle thin, rational size distribution, specific surface area are large, suspension property is excellent, purity advantages of higher, are widely used in coating, paint, tackiness agent, silicon rubber, precision casting, high-grade ceramic, epoxide resin encapsulation material and ordinary appliances, the insulation pouring of high pressure components and parts, the plastic cement of unicircuit and potting compound, powder coating, welding electrode protective layer and other resin extender etc.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of controllability silicon powder, the method required equipment is few, and reaction conditions is gentle, and cost is low, and production safety is reliable, and product purity is high, and productive rate is high.
The present invention is achieved like this, it is characterized in that processing method step is: first prepare the deionized water of 250ml in 500ml beaker, the water glass taking 10-25 gram is dissolved in the deionized water of 250ml and is mixed with sodium silicate solution, then with the total mass of 250ml deionized water for benchmark, the dispersion agent dehydrated alcohol that surfactant polyethylene and mass percent are 5-15% is taken by the mass percent of 5-15%, be added to 100 ml deionized waters, and stir with the rotating speed constant speed of 600 rpm, after stirring, rapidly the sodium silicate solution prepared is poured in 500ml beaker, continue constant speed and stir (straight leaf paddle stirrer) until add a 100ml plastic beaker (wall side-lower has side in intensive pore midfeather side atresia to have pore) when obtaining transparent mixing solutions to be fixed on 500ml beaker middle (alternate 2 cm of Liang Bidi), baffle plate is added in two beaker gaps, agitator stirs in small beaker, then slowly pass into bottom carbon dioxide to small beaker, with the change of acidometer record system pH, continue reaction after 1-5 hour, stable Off-white solid is obtained in two beaker gaps, stopped reaction, by the Off-white solid suction filtration obtained, washing repeatedly (deionized water, dehydrated alcohol respectively washes three times, filtrate Distillation recovery), the filter cake obtained vacuum-drying 5 hours at ambient temperature, then in retort furnace, 600 ° of C calcining at constant temperature obtain white powder in 2 hours.
The described centrifugal silicic acid particulate of effect of the radial shear force of straight leaf paddle stirrer that utilizes to rest chamber, thus stops growing up further of solid silicic acid.
Described evaporating solvent uses rotary evaporation, and under the low pressure even state of vacuum, remove most of solvent at a lower temperature, obtain concentrated solution, be convenient to subsequent disposal, solvent also can be reused.
Describedly pass into carbon dioxide, be beneficial to and prevent reaction solution acidity too high, alleviate the precipitator method simultaneously and prepare the low problem of silicon powder reaction solution concentration.
Technique effect of the present invention is: 1, utilize water glass to generate the feature of silicic acid precipitation in acid condition, carbonic acid gas plays an important role doing on silicon powder as sour reagent, simultaneously can relatively other precipitator method to do silicon powder sodium silicate silicate higher; 2, the feature of the radial shear force of straight leaf paddle stirrer is utilized, by the small-particle silicic acid of harsh one-tenth by centrifugal force band people rest chamber, thus effective control silicate particle size; 3, pass into speed, sodium silicate concentration, baffle angle by changing carbonic acid gas, the conditions such as pore size manufacture desirable silicon powder; 4, working method is easy, and use the preparation of rotary evaporation and vacuum-drying solid product, required equipment is few, and reaction conditions is gentle, and cost is low, and production safety is reliable, and product purity is high, and productive rate is high.
Embodiment
Embodiment one:
First the deionized water of 250ml is prepared in 500ml beaker, the water glass taking 10 grams is dissolved in the deionized water of 250ml and is mixed with sodium silicate solution, then with the total mass of 250ml deionized water for benchmark, mass percent by 5% takes the dispersion agent dehydrated alcohol that surfactant polyethylene and mass percent are 5%, be added to 100 ml deionized waters, and stir with the rotating speed constant speed of 600 rpm, after stirring, rapidly the sodium silicate solution prepared is poured in 500ml beaker, continue constant speed and stir (straight leaf paddle stirrer) until add a 100ml plastic beaker (wall side-lower has side in intensive pore midfeather side atresia to have pore) when obtaining transparent mixing solutions to be fixed on 500ml beaker middle (alternate 2 cm of Liang Bidi), baffle plate is added in two beaker gaps, agitator stirs in small beaker, then slowly pass into bottom carbon dioxide to small beaker, with the change of acidometer record system pH, continue reaction after 1 hour, stable Off-white solid is obtained in two beaker gaps, stopped reaction, by the Off-white solid suction filtration obtained, washing repeatedly (deionized water, dehydrated alcohol respectively washes three times, filtrate Distillation recovery), the filter cake obtained vacuum-drying 5 hours at ambient temperature, then in retort furnace, 600 ° of C calcining at constant temperature obtain white powder in 2 hours.
Embodiment two
First the deionized water of 250ml is prepared in 500ml beaker, the water glass taking 25 grams is dissolved in the deionized water of 250ml and is mixed with sodium silicate solution, then with the total mass of 250ml deionized water for benchmark, mass percent by 15% takes the dispersion agent dehydrated alcohol that surfactant polyethylene and mass percent are 15%, be added to 100 ml deionized waters, and stir with the rotating speed constant speed of 600 rpm, after stirring, rapidly the sodium silicate solution prepared is poured in 500ml beaker, continue constant speed and stir (straight leaf paddle stirrer) until add a 100ml plastic beaker (wall side-lower has side in intensive pore midfeather side atresia to have pore) when obtaining transparent mixing solutions to be fixed on 500ml beaker middle (alternate 2 cm of Liang Bidi), baffle plate is added in two beaker gaps, agitator stirs in small beaker, then slowly pass into bottom carbon dioxide to small beaker, with the change of acidometer record system pH, continue reaction after 5 hours, stable Off-white solid is obtained in two beaker gaps, stopped reaction, by the Off-white solid suction filtration obtained, washing repeatedly (deionized water, dehydrated alcohol respectively washes three times, filtrate Distillation recovery), the filter cake obtained vacuum-drying 5 hours at ambient temperature, then in retort furnace, 600 ° of C calcining at constant temperature obtain white powder in 2 hours.
Embodiment three
First the deionized water of 250ml is prepared in 500ml beaker, the water glass taking 20 grams is dissolved in the deionized water of 250ml and is mixed with sodium silicate solution, then with the total mass of 250ml deionized water for benchmark, mass percent by 8% takes the dispersion agent dehydrated alcohol that surfactant polyethylene and mass percent are 8%, be added to 100 ml deionized waters, and stir with the rotating speed constant speed of 600 rpm, after stirring, rapidly the sodium silicate solution prepared is poured in 500ml beaker, continue constant speed and stir (straight leaf paddle stirrer) until add a 100ml plastic beaker (wall side-lower has side in intensive pore midfeather side atresia to have pore) when obtaining transparent mixing solutions to be fixed on 500ml beaker middle (alternate 2 cm of Liang Bidi), baffle plate is added in two beaker gaps, agitator stirs in small beaker, then slowly pass into bottom carbon dioxide to small beaker, with the change of acidometer record system pH, continue reaction after 1-5 hour, stable Off-white solid is obtained in two beaker gaps, stopped reaction, by the Off-white solid suction filtration obtained, washing repeatedly (deionized water, dehydrated alcohol respectively washes three times, filtrate Distillation recovery), the filter cake obtained vacuum-drying 5 hours at ambient temperature, then in retort furnace, 600 ° of C calcining at constant temperature obtain white powder in 2 hours.
Claims (4)
1. the preparation method of a controllability silicon powder, it is characterized in that processing method step is: first prepare the deionized water of 250ml in 500ml beaker, the water glass taking 10-25 gram is dissolved in the deionized water of 250ml and is mixed with sodium silicate solution, then with the total mass of 250ml deionized water for benchmark, the dispersion agent dehydrated alcohol that surfactant polyethylene and mass percent are 5-15% is taken by the mass percent of 5-15%, be added to 100 ml deionized waters, and stir with the rotating speed constant speed of 600 rpm, after stirring, rapidly the sodium silicate solution prepared is poured in 500ml beaker, continue constant speed and stir (straight leaf paddle stirrer) until add a 100ml plastic beaker (wall side-lower has side in intensive pore midfeather side atresia to have pore) when obtaining transparent mixing solutions to be fixed on 500ml beaker middle (alternate 2 cm of Liang Bidi), baffle plate is added in two beaker gaps, agitator stirs in small beaker, then slowly pass into bottom carbon dioxide to small beaker, with the change of acidometer record system pH, continue reaction after 1-5 hour, stable Off-white solid is obtained in two beaker gaps, stopped reaction, by the Off-white solid suction filtration obtained, washing repeatedly (deionized water, dehydrated alcohol respectively washes three times, filtrate Distillation recovery), the filter cake obtained vacuum-drying 5 hours at ambient temperature, then in retort furnace, 600 ° of C calcining at constant temperature obtain white powder in 2 hours.
2. the preparation method of a kind of controllability silicon powder according to claim 1, the centrifugal silicic acid particulate of effect of the radial shear force of its characteristic use is straight leaf paddle stirrer is to rest chamber, thus the growing up further of prevention solid silicic acid.
3. the preparation method of a kind of controllability silicon powder according to claim 1, it is characterized in that evaporating solvent uses rotary evaporation, under the low pressure even state of vacuum, remove most of solvent at a lower temperature, obtain concentrated solution, be convenient to subsequent disposal, solvent also can be reused.
4. the preparation method of a kind of controllability silicon powder according to claim 1, its feature passes into carbon dioxide, is beneficial to and prevents reaction solution acidity too high, alleviates the precipitator method simultaneously and prepares the low problem of silicon powder reaction solution concentration.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510191512.5A CN104860319B (en) | 2015-04-22 | 2015-04-22 | A kind of preparation method of controllability silicon powder |
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| CN201510191512.5A CN104860319B (en) | 2015-04-22 | 2015-04-22 | A kind of preparation method of controllability silicon powder |
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| CN104860319A true CN104860319A (en) | 2015-08-26 |
| CN104860319B CN104860319B (en) | 2017-08-25 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB202306193D0 (en) | 2023-04-27 | 2023-06-14 | Univ Limerick | Process for synthesizing porous silica particles using low-pressure gaseous carbon dioxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999048813A1 (en) * | 1998-03-26 | 1999-09-30 | Rotem Amfert Negev Ltd. | Precipitated silica particulates with improved dispersability |
| CN101823720A (en) * | 2010-04-27 | 2010-09-08 | 重庆工商大学 | Preparation method of nano silica powder |
| CN102491345A (en) * | 2011-12-01 | 2012-06-13 | 安徽安纳达钛业股份有限公司 | Carbonization method for preparing precipitated white carbon black |
| CN103288091A (en) * | 2013-05-07 | 2013-09-11 | 贵州盘县紫森源（集团）实业发展投资有限公司 | Method for preparing white carbon black by utilizing water glass with low modulus through carbonizing method of precipitation |
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2015
- 2015-04-22 CN CN201510191512.5A patent/CN104860319B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999048813A1 (en) * | 1998-03-26 | 1999-09-30 | Rotem Amfert Negev Ltd. | Precipitated silica particulates with improved dispersability |
| CN101823720A (en) * | 2010-04-27 | 2010-09-08 | 重庆工商大学 | Preparation method of nano silica powder |
| CN102491345A (en) * | 2011-12-01 | 2012-06-13 | 安徽安纳达钛业股份有限公司 | Carbonization method for preparing precipitated white carbon black |
| CN103288091A (en) * | 2013-05-07 | 2013-09-11 | 贵州盘县紫森源（集团）实业发展投资有限公司 | Method for preparing white carbon black by utilizing water glass with low modulus through carbonizing method of precipitation |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB202306193D0 (en) | 2023-04-27 | 2023-06-14 | Univ Limerick | Process for synthesizing porous silica particles using low-pressure gaseous carbon dioxide |
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