CN86104144A - The manufacture method of big particle diameter, low viscosity silicon sol - Google Patents
The manufacture method of big particle diameter, low viscosity silicon sol Download PDFInfo
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- CN86104144A CN86104144A CN 86104144 CN86104144A CN86104144A CN 86104144 A CN86104144 A CN 86104144A CN 86104144 CN86104144 CN 86104144 CN 86104144 A CN86104144 A CN 86104144A CN 86104144 A CN86104144 A CN 86104144A
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Abstract
A kind of big particle diameter of manufacturing that belongs to non-metallic element and compound field thereof, the method for low viscosity silicon sol.Manufacture method feature provided by the invention is to be that metallic silicon power and silicate solutions react directly to prepare the silicon sol of high density low-viscosity stable.
Silicon sol manufacture method of the present invention needn't ion-exchange, needn't concentrate, and the expansion colloidal particle size that needn't pressurize, thus saved expensive facility investment, simplified production technique greatly, product cost is sharply descended, and the anxious strong increase of the stability of product.
Description
The invention belongs to non-metallic element and compound field thereof, is a kind of manufacture method about big particle diameter, low viscosity silicon sol.
At present, the method for industrial manufacturing silicon sol roughly can be divided into two big classes: a class is an ion exchange method, and another kind of is silica flour and diluted alkaline reaction method.But, obtain particle diameter and generally all need pressurize greater than the silicon sol of 20m μ, for example particle diameter is the silicon sol of 30u, pressure is 15～40 normal atmosphere, thereby equipment requirements is improved.In application number was 86100503 innovation and creation, the contriver made widely known the manufacture method of the silicon sol that has just proposed a kind of non-freezing type, good stability.It is characterized in that metallic silicon power directly reacts with the dilute alkaline soln that is heated to certain temperature with form of powder, economize deoxidation, two steps of activation, make the SiO of the silicon sol of the resulting non-freezing type in reaction back
2Content 29%(weight percentage) more than, about particle diameter 15～20mu.Though this method and Japanese Patent, clear 55-10534 compares, and province deactivates, two steps of oxidation, not only shortens the cycle, has reduced equipment, saves investment and owing to saved activation step, has avoided silicon loss in rinsing.But the particle diameter of silicon sol is 15～20mu, and the viscosity of colloidal sol is bigger.
The present invention is to be the further improvement of 86100503 innovation and creation to application number, makes the silicon sol particle diameter that makes bigger, and viscosity is low and stable better.It is characterized in that metallic silicon power directly reacts with water glass that is heated to certain temperature or potassium silicate with powder type after crushed, directly prepare high density, big particle diameter good stability, the silicon sol that viscosity is low.Needn't ion-exchange, needn't concentrate also and needn't pressurize.
As everyone knows, silica flour can generate silicon sol with water reaction, but must be with alkali as a catalyst:
In water glass or the diluted potassium silicate solution, contain silicon-dioxide ion and basic ion (Na
+Or K
+), when water glass or diluted potassium silicate solution and silica flour reaction, diluted alkaline and silica flour reaction generate fresh silica sol particle, constantly wrap in silicon dioxide colloid particulate outside in original water glass, along with reaction is carried out, the silicon-dioxide particle diameter is increasing, and silica flour adds manyly more, particle diameter is big more, and this is a mechanism of the present invention.
Silica flour used in the present invention is the commercially available following silica flour of 100～300 orders, and particle is too thick, is difficult for reaction, causes the reaction times long, the forfeiture industrial applicibility, and particle is too thin, and reaction is too fierce, is difficult to control.
Water glass used in the present invention can be that sodium type water glass also can be potassium type water glass, and technical grade gets final product.Commercially available neutral or alkaline sodium silicate gets final product.That is to say SiO
2/ Na
2All can use between the modulus ratio 2.4～3.3 of O.
When silica flour after making pulverizing and sodium type or the reaction of potassium type water glass, if for special purpose can be in water glass all mineral alkalis or organic bases dilute alkaline soln total concn 1%(weight percentage such as hydro-oxidation potassium, lithium hydroxide, ammonium hydroxide, sodium hydroxide, organic amine) below, so that make the pH value of finished product be unlikely to too high, make free alkali concentration can be reduced to Schwellenwert and stability can obtain to greatest extent satisfying.And above-mentioned dilute alkaline soln can be that use is wherein a kind of separately, can also be two kinds or multiple compound, for example adds a small amount of ammonium hydroxide in the sodium hydroxide, and two kinds of compound effects often surpass single the kind, thereby speed of response is increased substantially.
Temperature of reaction of the present invention is 65～100 ℃ (to be no more than 83 ℃ for well), and silica flour slowly adds without steps such as oxidation, activation, directly with commercially available sodium type or the reaction of potassium type water glass solution.For special purpose can add a spot of dilute alkaline soln, as sodium hydroxide, potassium hydroxide, ammonium hydroxide, organic amine etc., can add separately also and can any two kinds to add simultaneously, after finishing, reaction needs limit stirring, limit cooling, to be cooled to about 50 ℃ filtrations, remaining unreacted silica flour is recyclablely used again.
Advantage of the present invention is that investment and cost are well below the silicon sol with ion exchange method production, also needn't exchange, regenerate by spent ion exchange resin, output is not limited by ion exchange resin yet, needn't pressurize, and be that 86100503 innovation and creation are compared with application number, pH value of the present invention is low, the particle diameter of the silicon sol that equipment corrosion is little and the present invention makes is between 20～30mu, and is bigger than the former, and stability is again a little more than the former, be generally about 4 years the SiO of the silicon sol that makes in addition
2Concentration also is higher than the former, and the former generally is no more than the SiO of the silicon sol that 30% method provided by the invention makes
2Content concentrates between 32-36% slightly, can reach 50%.
Because the silicon sol particle diameter that method provided by the invention makes is big, viscosity lower concentration height, therefore has purposes widely.Be used for outer wall building coating, can with the organic emulsion thorough mixing, bring into play the advantage of organic and inorganic mixed type coating more; Be used for wool textile industry, easily be penetrated in the wool fabric with the crude oil adapted time, reduce the woolen end breakage rate; Be used for paper-making industry, be penetrated into and improve intensity in the paper pulp; Be used for foundry industry, the precision that can improve casting dimension is convenient to accurate the manufacturing.
As one of embodiments of the invention is with 1000 parts of distilled water, it is (commercially available to add 60 parts of neutral sodium silicates, technical grade) places the reactor that thermometer and reflux exchanger are housed, be warming up to 65 ℃, start agitator, take by weighing 160 parts of 180～240 commercially available order silica flours, join lentamente by stages and in groups in above-mentioned rare sodium silicate solution, silica flour adds that the back produces is thermopositive reaction and emits hydrogen-oxygen.Silica flour adds soon more, it is fierce more to react, and the control silica flour adds speed and is no more than 83 ℃ for well with temperature of reaction, overflows in order to avoid reaction is too causus, after a collection of silica flour adds, add second batch again slightly steadily, silica flour reacts climax, container outside used water cooling in case of necessity often when being added to total digit rate 3/4, in order to avoid it is excessive, after treating that silica flour all adds, continue under 75 ℃ of temperature, to stir 2-3 hour, make to react completely.Initial reaction stage, the pH value of solution is 12-14 often, along with reaction is carried out pH value and descended at leisure, when PH reduces to 9-10, but sampling analysis can continue reaction if content still falls short of the target, if touch the mark, but stopped reaction, stir on limit cooling, limit, filters in the time of 50 ℃.The unreacted silica flour that filters out is recyclable.
This example after silica flour adds, through reaction in 4 hours, can reach following index:
SiO
2Content 36%(weight percentage)
Na
2O content 0.33%(weight percentage)
PH content 9.7
Viscosity (25 ℃) 5.3CPS
Particle diameter 20～30mu
Yield 82-85%(decides on silica flour quality quality)
Stationary phase is more than 4 years
If concentration is the 36%(weight percentage) the further vacuum concentration of finished silicon colloidal sol, its concentration can reach the 50%(weight percentage) more than, granularity also increases thereupon.
As embodiments of the invention 2 be: in 1000 parts of distilled water, add 50 parts of alkaline sodium silicates (commercially available, technical grade), place the reactor that wet bulb thermometer and reflux exchanger are housed, be warmed up to 65 ℃, add 3 parts of strong aquas, start agitator, take by weighing 160 parts of 180～240 commercially available order silica flours, press the method operation of example 1, after silica flour adds, can reach following index through reaction in 4 hours again.
SiO
2Content 32%(weight percentage)
Na
2O content 0.28%(weight percentage)
PH value 9.35
Viscosity (25 ℃) 5CPS
Particle diameter 20-30mu
Stationary phase is more than 4 years
Yield 82～85%(decides on the silica flour quality)
Claims (3)
1, the big particle diameter of a kind of manufacturing, the manufacture method of low viscosity silicon sol comprises that metallic silicon power is without oxidation, steps such as activation, it is characterized in that metallic silicon power direct and water glass or potassium silicate solution reaction, 65 ℃～100 ℃ of range of reaction temperature are optimum temps with 72～83 ℃ wherein.
2, by the described manufacture method of claim 1, it is characterized in that described rare water glass, or can add ammonium hydroxide in the potassium silicate solution, lithium hydroxide, sodium hydroxide, all mineral alkalis such as potassium hydroxide, organic amine, or organic bases, in order to make the silicon sol of special purpose.These alkali can be independent addings, also can be several compound.
3, by claim 1 or 2 described manufacture method, the diluted alkaline total concn that it is characterized in that adding is in (weight percentage) below 1%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 86104144 CN86104144A (en) | 1986-12-29 | 1986-12-29 | The manufacture method of big particle diameter, low viscosity silicon sol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 86104144 CN86104144A (en) | 1986-12-29 | 1986-12-29 | The manufacture method of big particle diameter, low viscosity silicon sol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN86104144A true CN86104144A (en) | 1988-07-20 |
Family
ID=4802366
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 86104144 Pending CN86104144A (en) | 1986-12-29 | 1986-12-29 | The manufacture method of big particle diameter, low viscosity silicon sol |
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| CN (1) | CN86104144A (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100358653C (en) * | 2004-05-07 | 2008-01-02 | 章浩龙 | Method for preparing silica sol binding agent |
| CN100411982C (en) * | 2006-04-07 | 2008-08-20 | 北京国瑞升科技有限公司 | Preparation method of large grain size nanometer grade silicon dioxide colloid |
| CN101547860A (en) * | 2006-12-12 | 2009-09-30 | 扶桑化学工业股份有限公司 | Method for producing silica gel |
| CN101857236A (en) * | 2010-06-04 | 2010-10-13 | 西南科技大学 | Method for preparing high-concentration silica sol by using superfine silica powder |
| CN102040868A (en) * | 2010-11-24 | 2011-05-04 | 上海迪升防腐新材料科技有限公司 | Method for preparation and surface modification of alkaline silicon sol |
| CN102745697A (en) * | 2012-07-09 | 2012-10-24 | 山东百特新材料有限公司 | Method for preparing small-grain-diameter silica sol |
| CN103265107A (en) * | 2012-01-19 | 2013-08-28 | 株式会社韩美Entec | Treatment system for wastewater equipped with redox metal reactor |
| CN103265045A (en) * | 2013-06-03 | 2013-08-28 | 田辉明 | Method for producing potassium silicate solution for electronic industry |
| CN104445222A (en) * | 2014-11-27 | 2015-03-25 | 齐鲁工业大学 | Preparation method of acidic silica sol with large particle size and uniform distribution |
| CN104556058A (en) * | 2014-12-31 | 2015-04-29 | 上海新安纳电子科技有限公司 | Method for producing silica sol low in viscosity and small in particle size |
| CN104671248A (en) * | 2013-11-30 | 2015-06-03 | 天津晶美微纳科技有限公司 | Method for directly preparing high-purity silica sol with large particle size by using silicon powder method |
| CN106145123A (en) * | 2016-08-19 | 2016-11-23 | 安徽元琛环保科技股份有限公司 | A kind of Ludox preparation method of simple and fast |
| CN110197912A (en) * | 2018-02-24 | 2019-09-03 | 航天特种材料及工艺技术研究所 | A kind of graphite bipolar plate material and preparation method |
| CN115893436A (en) * | 2022-10-25 | 2023-04-04 | 英德市东鸿化工科技有限公司 | Treatment process for recycling industrial byproducts |
-
1986
- 1986-12-29 CN CN 86104144 patent/CN86104144A/en active Pending
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100358653C (en) * | 2004-05-07 | 2008-01-02 | 章浩龙 | Method for preparing silica sol binding agent |
| CN100411982C (en) * | 2006-04-07 | 2008-08-20 | 北京国瑞升科技有限公司 | Preparation method of large grain size nanometer grade silicon dioxide colloid |
| CN101547860A (en) * | 2006-12-12 | 2009-09-30 | 扶桑化学工业股份有限公司 | Method for producing silica gel |
| CN101547860B (en) * | 2006-12-12 | 2014-05-28 | 扶桑化学工业股份有限公司 | Method for producing silica gel |
| CN101857236B (en) * | 2010-06-04 | 2012-08-29 | 西南科技大学 | Method for preparing high-concentration silica sol by using superfine silica powder |
| CN101857236A (en) * | 2010-06-04 | 2010-10-13 | 西南科技大学 | Method for preparing high-concentration silica sol by using superfine silica powder |
| CN102040868A (en) * | 2010-11-24 | 2011-05-04 | 上海迪升防腐新材料科技有限公司 | Method for preparation and surface modification of alkaline silicon sol |
| CN102040868B (en) * | 2010-11-24 | 2013-08-07 | 上海迪升防腐新材料科技有限公司 | Method for preparation and surface modification of alkaline silicon sol |
| CN103265107B (en) * | 2012-01-19 | 2015-09-23 | 株式会社韩美Entec | Utilize the sewage and wastewater treatment system of redox metal reactor |
| CN103265107A (en) * | 2012-01-19 | 2013-08-28 | 株式会社韩美Entec | Treatment system for wastewater equipped with redox metal reactor |
| CN102745697A (en) * | 2012-07-09 | 2012-10-24 | 山东百特新材料有限公司 | Method for preparing small-grain-diameter silica sol |
| CN102745697B (en) * | 2012-07-09 | 2015-11-11 | 山东百特新材料有限公司 | Prepare the method for small-grain-diametersilica silica sol |
| CN103265045A (en) * | 2013-06-03 | 2013-08-28 | 田辉明 | Method for producing potassium silicate solution for electronic industry |
| CN104671248A (en) * | 2013-11-30 | 2015-06-03 | 天津晶美微纳科技有限公司 | Method for directly preparing high-purity silica sol with large particle size by using silicon powder method |
| CN104445222A (en) * | 2014-11-27 | 2015-03-25 | 齐鲁工业大学 | Preparation method of acidic silica sol with large particle size and uniform distribution |
| CN104445222B (en) * | 2014-11-27 | 2016-08-24 | 齐鲁工业大学 | A kind of big particle diameter and the preparation method of the acidic silicasol that is evenly distributed |
| CN104556058A (en) * | 2014-12-31 | 2015-04-29 | 上海新安纳电子科技有限公司 | Method for producing silica sol low in viscosity and small in particle size |
| CN106145123A (en) * | 2016-08-19 | 2016-11-23 | 安徽元琛环保科技股份有限公司 | A kind of Ludox preparation method of simple and fast |
| CN110197912A (en) * | 2018-02-24 | 2019-09-03 | 航天特种材料及工艺技术研究所 | A kind of graphite bipolar plate material and preparation method |
| CN115893436A (en) * | 2022-10-25 | 2023-04-04 | 英德市东鸿化工科技有限公司 | Treatment process for recycling industrial byproducts |
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