CN103626189A - Method for preparing high-dispersion nano silica from organic acid and sodium silicate - Google Patents
Method for preparing high-dispersion nano silica from organic acid and sodium silicate Download PDFInfo
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- CN103626189A CN103626189A CN201310641227.XA CN201310641227A CN103626189A CN 103626189 A CN103626189 A CN 103626189A CN 201310641227 A CN201310641227 A CN 201310641227A CN 103626189 A CN103626189 A CN 103626189A
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Abstract
A method for preparing high-dispersion nano silica from organic acid and sodium silicate relates to a silica preparation method. The method comprises the following step: diluting a sodium silicate solution to a proper concentration, adding a certain amount of dispersant and electrolyte, dripping organic acid for acidic precipitation until the pH value is 7 so as to obtain a precipitate of nano silica; finally, filtering, washing, drying and smashing the precipitate to obtain nano silica. According to the method provided by the invention, the fact that in the traditional technology of preparing silica through a precipitation method, sulfuric acid, hydrochloric acid and other mineral acid are used for preparing silica is changed; organic acid is used for acidizing a sodium silicate solution, and then the high-grade high-dispersion nano silica can be prepared; the method has the advantages that the raw materials are cheap and easy to get, the technology is simple, the produced nano silica is uniform in particle diameter and high in dispersity, and the overall performance of the produced nano silica is better than that of silica prepared through the traditional precipitation method.
Description
Technical field
The present invention relates to a kind of method of preparing white carbon black, particularly relate to a kind of method of preparing high-dispersion nano white carbon black with organic acid and water glass.
Background technology
White carbon black in fields such as rubber, plastics, synthetic resins, coating, medicine, makeup, chemical fibres, be widely used and demand large.White carbon black main goods in rubber industry are doughnut, and as strengthening agent and properties-correcting agent, its reinforcing effect is better than other reinforcing filler beyond carbon black.China's tire white carbon black consumption ratio reaches developed country's level, and the white carbon black of being often only these field needs just will be over 1,100,000 tons.In recent years, outlet tire accounted for the share of domestic tire ultimate production 40%, if all outlet ports tire all adopts or part adopts white carbon black alternative carbon black, the annual white carbon black consumption increasing just will be over 200,000 tons.According to statistics, used in recent years the green tire of polymolecularity white carbon black keeping 10% ~ 20% annual growth, and in increasing first wife's tire index, start to specify to add white carbon black.Green tire is very fast in world market development, and much west has stipulated that new car first wife tire must adopt green tire, so the following usage quantity of high dispersive precipitated silica will be larger.
High-dispersion white carbon black is compared with common white carbon black, has primary particle thin, and the adsorbed hydroxyl content is low, and lipophilicity strengthens, and with the high molecular bonding force of rubber, feature that wetting property is high, is a kind of desirable reinforcement and filler material that is exclusively used in high-performance tire.High dispersive precipitated silica dispersing property in rubber is good, make the wear resistance of tire product high, rolling resistance is low, flex cracking resistance is good, data proves, the more performance tire that adds high-dispersion white carbon black can reduce rolling resistance more than 30%, thereby reduces oil consumption, reduce the discharge of tail gas, there is the feature of energy-conserving and environment-protective.
In coating industry, because white carbon black refractive index is 1.45-1.50, in varnish, there is good optical property.In recent years, along with developing rapidly of housing construction, the coating particularly market requirement of building coating has development faster.White carbon black is as the matting agent of coating, and its demand also will have corresponding development.
White carbon black is one of principal item of current toothpaste use friction agent.It has that specific surface area is large, high adsorption capacity, particle diameter evenly, stable in properties, the feature such as nontoxic, can be used as good raw material of toothpaste.White carbon black Applicative time in toothpaste is not long, but has demonstrated several functions, except doing friction agent, also can make inhibiter, thickening material, thixotropic agent.Although the Applicative time of white carbon black in toothpaste is not long, but because it has that specific surface area is large, the equal even characteristic such as nontoxic of high adsorption capacity, pellet, become at present toothpaste one of principal item of friction agent, expectation, along with the raising of living standards of the people, is used the consumption ratio of the high-grade toothpaste that white carbon black is abrasive material progressively to improve.Within 2006, toothpaste industry white carbon black usage quantity is approximately 1.0 ten thousand tons, and keeps year by year rate of growth faster.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing high-dispersion nano white carbon black with organic acid and water glass, the method is carried out acidification with organic acid to water glass solution, Nano carbon white particle size uniformity and dispersiveness thereof have been improved, and technique is simple, equipment requirements is low, easily realizes suitability for industrialized production.
The object of the invention is to be achieved through the following technical solutions:
The method of preparing high-dispersion nano white carbon black with organic acid and water glass, described in it, method is carried out purification and impurity removal by water glass solution, dilutes and adds dispersion agent, through organic acid acidifying, obtains flocks, after filtration, washing, obtain Nano carbon white after dry;
Concrete technology method comprises the following steps:
(1) by water glass solution removal of impurities redilution to suitable concn, add ionogen and dispersion agent, then evenly slowly drip organic acid and carry out acidification, obtain flocks, until PH stops dripping at 7 o'clock;
Its chemical equation is as follows:
Na
2SiO
3+2H
+→H
2SiO
3+2Na
+
H
2SiO
3→SiO
2·nH
2O(s)↓+(m-n)H
2O；
(2) by throw out after filtration, washing, dry, pulverize and can obtain product.
The described method of preparing high-dispersion nano white carbon black with organic acid and water glass, described dispersion agent is polyoxyethylene glycol, glycerol, propyl carbinol.Formic acid, acetic acid, propionic acid, butyric acid, sad, capric acid, oxalic acid, propanedioic acid, succinic acid, isopropylformic acid, toxilic acid, phenylformic acid, toluylic acid, Phenylsulfonic acid, phthalic acid, vinylformic acid.
The described method of preparing high-dispersion nano white carbon black with organic acid and water glass, described regulator solution potential of hydrogen PH is 7.
The described method of preparing high-dispersion nano white carbon black with organic acid and water glass, described organic acid mass percent is 10%-20%.
The described method of preparing high-dispersion nano white carbon black with organic acid and water glass, the described organic acid that utilizes carries out acidification to water glass solution, and temperature of reaction is controlled at 75 ℃-85 ℃, and in reaction process, continues to stir.
Advantage of the present invention and effect are:
The method is carried out acidification with organic acid to water glass solution, has improved Nano carbon white particle size uniformity and dispersiveness thereof, raw materials technology wide material sources, cheap, make white carbon black particle size uniformity and polymolecularity, and technique is simple, equipment requirements is low, easily realizes suitability for industrialized production.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
The method comprises purification and impurity removal processing and the concentration adjustment of water glass solution, adds a small amount of ionogen and dispersion agent, utilizes the acidification of organic acid to water glass solution.Conventional service water glass, derives from quartz sand, zeolite, wollastonite, coal gangue, opal, hard kaoline, kaolin, halloysite, diatomite, wilkinite, serpentine, flyash, yellow phosphorus ore deposit, sepiolite etc., and massfraction is greater than 24.6%.Remove the larger meta-aluminic acid radical ion of dialogue carbon black mass impact.Ionogen Na, Ca, Mg ionic concn 0.07mol/L-0.10 mol/L.Dispersion agent is polyoxyethylene glycol, glycerol, propyl carbinol.Formic acid, acetic acid, propionic acid, butyric acid, sad, capric acid, oxalic acid, propanedioic acid, succinic acid, isopropylformic acid, toxilic acid, phenylformic acid, toluylic acid, Phenylsulfonic acid, phthalic acid, vinylformic acid.Organic acid mass percent is 10%-20%.Regulator solution potential of hydrogen PH is 7.Utilize organic acid to carry out acidification to water glass solution, temperature of reaction is controlled at 75 ℃-85 ℃, and in reaction process, continues to stir.
Embodiment 1:
The dehydrated alcohol that adds 50ml at 500ml sodium silicate solution, utilize water glass solution and deionized water preparation water glass solution and add 1% ionogen, under 80 ℃ of constant temperatures, stir, add dispersion agent, the organic acid that preparation massfraction is 10%-20%, when constant temperature stirs, with constant rate of titration, slowly drip organic acid until there is flocks, to pH value, be within 7 o'clock, to stop dripping, the aging 20min of constant temperature, then carry out suction filtration, washing, and be dried 24h under the part of 80 ℃, obtain product Nano carbon white.After testing, sample has the characteristic peak of white carbon black, and make white carbon black and there is polymolecularity, particle diameter 90-200nm, PH5.0-6.0. oil-absorption(number) (DBP value) is 3.2, the good dispersity in sizing material.
Claims (5)
1. with organic acid and water glass, prepare the method for high-dispersion nano white carbon black, it is characterized in that, described method is carried out purification and impurity removal by water glass solution, dilutes and adds dispersion agent, through organic acid acidifying, obtain flocks, after filtration, washing, obtain Nano carbon white after dry;
Concrete technology method comprises the following steps:
(1) by water glass solution removal of impurities redilution to suitable concn, add ionogen and dispersion agent, then evenly slowly drip organic acid and carry out acidification, obtain flocks, until PH stops dripping at 7 o'clock;
Its chemical equation is as follows:
Na
2SiO
3+2H
+→H
2SiO
3+2Na
+
H
2SiO
3→SiO
2·nH
2O(s)↓+(m-n)H
2O；
(2) by throw out after filtration, washing, dry, pulverize and can obtain product.
2. the method for preparing high-dispersion nano white carbon black with organic acid and water glass according to claim 1, it is characterized in that, described dispersion agent is polyoxyethylene glycol, glycerol, propyl carbinol, formic acid, acetic acid, propionic acid, butyric acid, sad, capric acid, oxalic acid, propanedioic acid, succinic acid, isopropylformic acid, toxilic acid, phenylformic acid, toluylic acid, Phenylsulfonic acid, phthalic acid, vinylformic acid.
3. the method for preparing high-dispersion nano white carbon black with organic acid and water glass according to claim 1, is characterized in that, described regulator solution potential of hydrogen PH is 7.
4. the method for preparing high-dispersion nano white carbon black with organic acid and water glass according to claim 1, is characterized in that, described organic acid mass percent is 10%-20%.
5. the method for preparing high-dispersion nano white carbon black with organic acid and water glass according to claim 1, it is characterized in that, the described organic acid that utilizes carries out acidification to water glass solution, and temperature of reaction is controlled at 75 ℃-85 ℃, and in reaction process, continues to stir.
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|---|---|---|---|
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|---|---|---|---|
| CN201310641227.XA CN103626189A (en) | 2013-12-04 | 2013-12-04 | Method for preparing high-dispersion nano silica from organic acid and sodium silicate |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105860589A (en) * | 2016-04-01 | 2016-08-17 | 沈阳化工大学 | Method for preparing in-situ functionalized modified white carbon black |
| CN108002397A (en) * | 2017-12-29 | 2018-05-08 | 云南磷化集团有限公司 | A kind of method that industrial waterglass prepares white carbon |
| CN108069430A (en) * | 2017-12-28 | 2018-05-25 | 无锡恒诚硅业有限公司 | A kind of preparation method of high dispersive precipitated silica and precipitated silica therefrom |
| CN109415215A (en) * | 2016-04-14 | 2019-03-01 | 弗朗索瓦·帕尔芒捷 | A kind of method of organic acid synthetic mineral oxide not soluble in water |
| CN113604072A (en) * | 2021-09-06 | 2021-11-05 | 合肥工业大学 | Process for using composite dispersant for synergistically dispersing white carbon black powder by precipitation method |
| CN114286798A (en) * | 2021-12-01 | 2022-04-05 | 无锡恒诚硅业有限公司 | Preparation method and application of hydrophilic white carbon black |
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| CN102491351A (en) * | 2011-12-13 | 2012-06-13 | 沈阳化工大学 | Method for preparing white carbon black through natural clinoptilolite |
| CN103435053A (en) * | 2013-09-04 | 2013-12-11 | 沈阳化工大学 | Method for preparing high-dispersion nano white black carbon from sodium silicate |
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Patent Citations (6)
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| WO1999063958A1 (en) * | 1998-06-05 | 1999-12-16 | Crosfield Limited | Particulate materials for use in dentifrice compositions |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105860589A (en) * | 2016-04-01 | 2016-08-17 | 沈阳化工大学 | Method for preparing in-situ functionalized modified white carbon black |
| CN105860589B (en) * | 2016-04-01 | 2018-05-15 | 沈阳化工大学 | A kind of preparation method of original position functional modification white carbon |
| CN109415215A (en) * | 2016-04-14 | 2019-03-01 | 弗朗索瓦·帕尔芒捷 | A kind of method of organic acid synthetic mineral oxide not soluble in water |
| CN108069430A (en) * | 2017-12-28 | 2018-05-25 | 无锡恒诚硅业有限公司 | A kind of preparation method of high dispersive precipitated silica and precipitated silica therefrom |
| CN108002397A (en) * | 2017-12-29 | 2018-05-08 | 云南磷化集团有限公司 | A kind of method that industrial waterglass prepares white carbon |
| CN113604072A (en) * | 2021-09-06 | 2021-11-05 | 合肥工业大学 | Process for using composite dispersant for synergistically dispersing white carbon black powder by precipitation method |
| CN114286798A (en) * | 2021-12-01 | 2022-04-05 | 无锡恒诚硅业有限公司 | Preparation method and application of hydrophilic white carbon black |
| WO2023097541A1 (en) * | 2021-12-01 | 2023-06-08 | 无锡恒诚硅业有限公司 | Preparation method for hydrophilic white carbon black and application |
| CN114286798B (en) * | 2021-12-01 | 2023-09-01 | 无锡恒诚硅业有限公司 | Preparation method and application of hydrophilic white carbon black |
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Application publication date: 20140312 |