CN104860319B - A kind of preparation method of controllability silicon powder - Google Patents
A kind of preparation method of controllability silicon powder Download PDFInfo
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- CN104860319B CN104860319B CN201510191512.5A CN201510191512A CN104860319B CN 104860319 B CN104860319 B CN 104860319B CN 201510191512 A CN201510191512 A CN 201510191512A CN 104860319 B CN104860319 B CN 104860319B
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Abstract
A kind of preparation method of controllability silicon powder, it is characterized in that being acidified by carbon dioxide, precipitating the steps such as standing filtering, calcining, obtains controllability silicon powder, the solution have the advantages that：1. radially being stirred using straight leaf dasher, silicate particle is set to arrive standing as early as possible, forming the particle of Nano grade prevents silicic acid reunionization, to prepare the silicon powder of controllability；2nd, carbon dioxide is passed through, beneficial to preventing that reaction liquid acidity is too high, while alleviating the precipitation method prepares the problem of silicon powder reaction solution concentration is low；3rd, required equipment is few, and reaction condition is gentle, and cost is low, and production safety is reliable, and 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 that silicon powder is the extremely wide inorganic non-metallic material of a class purposes, with dielectricity
The excellent, thermal coefficient of expansion of energy is low, thermal conductivity factor is high, and silicon powder series of products are through advanced ultra-fine grinding process by pure silica flour
Flow is processed.It has thin whiteness height, particle, rational size distribution, specific surface area is big, suspendability is excellent, purity is high etc.
Advantage, is widely used in coating, paint, adhesive, silicon rubber, hot investment casting, high-grade ceramic, epoxide resin encapsulation material and common electricity
Device, the insulation pouring of high pressure component, the plastic packaging material of integrated circuit and potting compound, powdery paints, welding rod protective layer and other
Resin extender etc..
The content of the invention
It is an object of the invention to provide a kind of preparation method of controllability silicon powder, equipment needed for this method is few, reaction
Mild condition, cost is low, and production safety is reliable, and product purity is high, and yield is high.
The present invention is achieved like this, it is characterized in that process step is：First prepare 250ml deionized water in
In 500ml beakers, weigh 10-25 grams of sodium metasilicate and be dissolved in 250ml deionized water and be configured to sodium silicate solution, then with
On the basis of the gross mass of 250ml deionized waters, surfactant polyethylene and quality hundred are weighed by 5-15% mass percent
Divide than the dispersant absolute ethyl alcohol for 5-15%, be added to 100 ml deionized waters, and stirred with 600 rpm rotating speed constant speed,
After stirring, the sodium silicate solution prepared is poured into 500ml beakers rapidly, continues constant speed stirring（Straight leaf paddle stirring
Device）A 100ml plastic beaker is added when obtaining transparent mixed solution（Wall side-lower has intensive pore midfeather side
There is pore non-porous upper side）It is fixed in the middle of 500ml beakers（Alternate 2 cm in two wall bottoms）, baffle plate is added in two beaker gaps, is stirred
Mix device to stir in small beaker, be then slowly introducing carbon dioxide to small beaker bottom, system pH is recorded with acidometer
Change, continue react 1-5 hour after, the Off-white solid stablize in two beaker gaps, stopping react, by obtained breast
Repeatedly (deionized water, absolute ethyl alcohol are respectively washed three times, and filtrate is distilled to recover), obtained filter cake is in room for white solid suction filtration, washing
It is dried in vacuo 5 hours under the conditions of temperature, then 600 °C of calcining at constant temperature obtain white powder in 2 hours in Muffle furnace.
The effect using straight leaf dasher radial direction shear force centrifuges silicic acid particulate to rest chamber, so as to prevent solid
Body silicic acid is further grown up.
The evaporation solvent uses rotary evaporation, in the state of low pressure even vacuum, goes at a lower temperature
Except most of solvent, concentrate is obtained, is easy to subsequent treatment, solvent can also be reused.
Described to be passed through carbon dioxide, beneficial to preventing that reaction liquid acidity is too high, while alleviating the precipitation method, to prepare silicon micro-
The problem of powder reaction solution concentration is low.
The solution have the advantages that：1st, the characteristics of silicic acid is precipitated, titanium dioxide are generated in acid condition using sodium metasilicate
Carbon plays an important role doing as acid reagent on silicon powder, while silicon powder sodium silicate silicate can be done with respect to other precipitation method more
It is high；2nd, using straight leaf dasher radial direction shear force it is the characteristics of, the little particle silicic acid just generated is quiet by centrifugal force band people
Room is put, so as to effectively control silicate particle size；3rd, speed, sodium silicate concentration, baffle plate angle are passed through by changing carbon dioxide
Spend, the condition such as pore size manufactures preferable silicon powder；4th, operating method is easy, is produced using rotary evaporation and vacuum drying solid
The preparation of thing, required equipment is few, and reaction condition is gentle, and cost is low, and production safety is reliable, and product purity is high, and yield is high.
Embodiment
Embodiment one：
Prepare 250ml deionized water first in 500ml beakers, weigh 10 grams of sodium metasilicate be dissolved in 250ml go from
Sodium silicate solution is configured in sub- water, then on the basis of the gross mass of 250ml deionized waters, is weighed by 5% mass percent
Surfactant polyethylene and mass percent are 5% dispersant absolute ethyl alcohol, are added to 100 ml deionized waters, and with
600 rpm rotating speed constant speed stirring, after stirring, rapidly pours into the sodium silicate solution prepared in 500ml beakers, continues permanent
Speed stirring（Straight leaf dasher）A 100ml plastic beaker is added when obtaining transparent mixed solution（Under wall side
Side has the intensive non-porous upper side in pore midfeather side to have pore）It is fixed in the middle of 500ml beakers（Alternate 2 cm in two wall bottoms）,
Two beaker gaps add baffle plate, and agitator is stirred in small beaker, is then slowly introducing carbon dioxide to small beaker bottom,
The change of system pH is recorded with acidometer, is continued after reacting 1 hour, the Off-white solid stablized in two beaker gaps,
Stop reaction, repeatedly (deionized water, absolute ethyl alcohol are respectively washed three times, and filtrate is distilled back by obtained Off-white solid suction filtration, washing
Receive), obtained filter cake is dried in vacuo 5 hours at ambient temperature, and then 600 °C of calcining at constant temperature are obtained for 2 hours in Muffle furnace
White powder.
Embodiment two
Prepare 250ml deionized water first in 500ml beakers, weigh 25 grams of sodium metasilicate be dissolved in 250ml go from
Sodium silicate solution is configured in sub- water, then on the basis of the gross mass of 250ml deionized waters, is claimed by 15% mass percent
It is 15% dispersant absolute ethyl alcohol to take surfactant polyethylene and mass percent, is added to 100 ml deionized waters,
And stirred with 600 rpm rotating speed constant speed, after stirring, the sodium silicate solution prepared is poured into 500ml beakers rapidly, after
Continuous constant speed stirring（Straight leaf dasher）A 100ml plastic beaker is added when obtaining transparent mixed solution（Wall
Side-lower has the intensive non-porous upper side in pore midfeather side to have pore）It is fixed in the middle of 500ml beakers（Two wall bottoms alternate 2
cm）, baffle plate is added in two beaker gaps, agitator is stirred in small beaker, is then slowly introducing carbon dioxide and is burnt to small
Cup bottom, the change of system pH is recorded with acidometer, is continued after reacting 5 hours, that is stablized in two beaker gaps is milky white
Color solid, stops reaction, and by obtained Off-white solid suction filtration, washing, repeatedly (deionized water, absolute ethyl alcohol are respectively washed three times, filter
Liquid is distilled to recover), obtained filter cake is dried in vacuo 5 hours at ambient temperature, then 600 °C of calcining at constant temperature 2 in Muffle furnace
Hour obtains white powder.
Embodiment three
Prepare 250ml deionized water first in 500ml beakers, weigh 20 grams of sodium metasilicate be dissolved in 250ml go from
Sodium silicate solution is configured in sub- water, then on the basis of the gross mass of 250ml deionized waters, is weighed by 8% mass percent
Surfactant polyethylene and mass percent are 8% dispersant absolute ethyl alcohol, are added to 100 ml deionized waters, and with
600 rpm rotating speed constant speed stirring, after stirring, rapidly pours into the sodium silicate solution prepared in 500ml beakers, continues permanent
Speed stirring（Straight leaf dasher）A 100ml plastic beaker is added when obtaining transparent mixed solution（Under wall side
Side has the intensive non-porous upper side in pore midfeather side to have pore）It is fixed in the middle of 500ml beakers（Alternate 2 cm in two wall bottoms）,
Two beaker gaps add baffle plate, and agitator is stirred in small beaker, is then slowly introducing carbon dioxide to small beaker bottom,
The change of system pH is recorded with acidometer, is continued after reacting 1-5 hours, the milky stablized in two beaker gaps is consolidated
Body, stops reaction, and by obtained Off-white solid suction filtration, washing, repeatedly (deionized water, absolute ethyl alcohol are respectively washed three times, and filtrate is steamed
Evaporate recovery), obtained filter cake is dried in vacuo 5 hours at ambient temperature, then 600 °C of calcining at constant temperature 2 hours in Muffle furnace
Obtain white powder.
Claims (1)
1. a kind of preparation method of controllability silicon powder, it is characterized in that process step is：Prepare 250ml deionization first
Water weighs 10-25 grams of sodium metasilicate and is dissolved in 250ml deionized water and be configured to sodium silicate solution in 500ml beakers, then
On the basis of the gross mass of 250ml deionized waters, surfactant polyethylene and quality are weighed by 5-15% mass percent
Percentage is 5-15% dispersant absolute ethyl alcohol, is added to 100 ml deionized waters, and stir with 600 rpm rotating speed constant speed
Mix, after stirring, rapidly pour into the sodium silicate solution prepared in 500ml beakers, continue through straight leaf dasher
Constant speed is stirred, and a 100ml plastic beaker is added when obtaining transparent mixed solution and is fixed in the middle of 500ml beakers,
Two beaker gaps add baffle plate, and agitator is stirred in small beaker, is then slowly introducing carbon dioxide to small beaker bottom,
The change of system pH is recorded with acidometer, is continued after reacting 1-5 hours, the milky stablized in two beaker gaps is consolidated
Body, stops reaction, and obtained Off-white solid suction filtration, washing is multiple, and it is small that obtained filter cake is dried in vacuo 5 at ambient temperature
When, then 600 DEG C of calcining at constant temperature obtain white powder for 2 hours in Muffle furnace, and the wall side-lower of the plastic beaker has intensive
The non-porous upper side in pore midfeather side have a pore, plastic beaker with alternate 2 cm in two wall bottoms of 500ml beakers.
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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 CN104860319A (en) | 2015-08-26 |
| CN104860319B true CN104860319B (en) | 2017-08-25 |
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| 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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| IL123841A0 (en) * | 1998-03-26 | 1998-10-30 | 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 |
| CN103288091B (en) * | 2013-05-07 | 2014-12-31 | 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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