CN102838124A - Preparation method of high-purity silicon colloidal sol not containing metallic ion - Google Patents
Preparation method of high-purity silicon colloidal sol not containing metallic ion Download PDFInfo
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- CN102838124A CN102838124A CN2012103541081A CN201210354108A CN102838124A CN 102838124 A CN102838124 A CN 102838124A CN 2012103541081 A CN2012103541081 A CN 2012103541081A CN 201210354108 A CN201210354108 A CN 201210354108A CN 102838124 A CN102838124 A CN 102838124A
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Abstract
The invention discloses a preparation method of high-purity silicon colloidal sol not containing metallic ions, and belongs to the technical field of chemical material preparation. The method comprises the following steps of: putting calcium oxide and silicon dioxide powder into a graphite crucible, warming to 1550-1600 DEG C, and keeping temperature for 40 min to obtain a reaction product of the calcium oxide and silicon oxide; carrying water quenching treatment on the obtained reaction product to obtain water quenching calcium silicate, and then drying, smashing. screening and taking the product after screening to obtain water quenching calcium silicate powder; and slowly adding a sulphuric acid solution with a certain concentration into the water quenching calcium silicate powder while stirring, pumping and filtering after the reaction is finished, and carrying out separation to obtain an achromic transparent filtrate, namely the high-purity silicon colloidal sol not containing metallic ions. The high-purity silicon colloidal sol prepared through the method provided by the invention has the advantages that the products does not contain metallic ions, the impurity content is less, and the silica sol not containing metallic ions has the defect of low reaction rate compared with preparation with a simple substance silicon dissolution method, the reaction rate of the method is rapid, and the technological process is simple.
Description
Technical field
The invention belongs to technical field of chemical material preparation, be specifically related to a kind of high-temperature water quenching after acidolysis prepare the not method of the high-purity silicasol of metal ion.
Background technology
Silicon sol is that a kind of silicon dioxide microparticle is scattered in the colloidal solution in the water or in the solvent; Owing to have advantages such as bigger serface, high absorbability, high-adhesion, good light transmittance, high fireinsulation property and high-temperature resistant oxidation-resistance, be widely used in industries such as precision casting, papermaking, weaving, rubber, coating, catalyzer, refractory thermal insulating material.At present, the preparation method of silicon sol mainly contains: ion exchange method, elemental silicon dissolution method, dialysis, electrolytic electro-dialysis method, sol-gel method etc.Wherein, more sophisticated preparation method is ion exchange method and elemental silicon dissolution method in the industry.
Ion exchange method is a raw material with the water glass water glass usually, adopts ion exchange resin to remove the sodium Metal 99.5 ion in the water glass, however sodium ion can not be removed fully, still contain a small amount of sodium ion in the silicon sol of preparing; It is raw material that the elemental silicon dissolution method adopts metallic silicon power, though metal ion not in the silicon sol of preparing, preparation feedback speed is slow, and the silica flour transformation efficiency is low; Other method is a raw material with water glass mostly also, all contains metals ion in the silicon sol of preparing.Yet metals ion is all influential to water tolerance, physical strength and the film-forming properties etc. of silicon sol.
Summary of the invention
In order to overcome existing silicon sol preparing method's shortcoming, the present invention provides the preparation method of a kind of not metal ion, foreign matter content high-purity silicasol seldom.
The present invention is raw materials used following with preparation method silicon sol:
1, mainly prepares raw material
Main preparation raw material involved in the present invention is quicklime and silicon-dioxide.
2, preparing method's concrete steps of the present invention are following:
(1) takes by weighing quicklime and silicon-dioxide powdery is put into plumbago crucible; The mass ratio of said quicklime and silicon-dioxide is 1: (1.0 ~ 1.2); Temperature rise rate with 3 ~ 5 ℃/min is warmed up to 1550 ~ 1600 ℃, is incubated the reaction product that 40 min obtain quicklime and silicon-dioxide then;
(2) reaction product that said step (1) is obtained is carried out Water Quenching, obtains the shrend Calucium Silicate powder;
(3) the shrend Calucium Silicate powder that said step (2) is obtained carries out drying, the back extracting screen underflow of pulverizing, sieve obtains the shrend calcium silicate powder;
(4) prepare certain density sulphuric acid soln; Under stirring condition, slowly add the shrend calcium silicate powder that said step (3) obtains; Said shrend Calucium Silicate powder and vitriolic mass ratio are 1: (1.1 ~ 1.3); Suction filtration after reaction is accomplished separates the water white transparency filtrating that obtains, and is the not high-purity silicasol of metal ion.
3, preparing method's principle
Generally speaking, Calucium Silicate powder is difficult to react with sulfuric acid.Present method is utilized quicklime and silicon-dioxide to react down at 1550 ~ 1600 ℃ and is generated Calucium Silicate powder, and chilling shrend under high temperature then obtains the shrend Calucium Silicate powder.Because the shrend Calucium Silicate powder is that at high temperature chilling generates, the significant amount of energy of accumulated inside does not in time discharge, and makes its structure be in high-energy state, has higher activity.Therefore, when the shrend Calucium Silicate powder runs into sulfuric acid, can generate calcium sulfate with sulfuric acid reaction.Calcium sulfate is insoluble in water, can remove after the filtration, and the filtrating that obtains is the not high-purity silicasol of metal ion.
4, the advantage of the inventive method:
Present method prepares silicon sol with shrend Calucium Silicate powder and the sulfuric acid reaction that high-temperature water quenching obtains, metal ion not in the product not only, and foreign matter content is seldom; And, to compare the elemental silicon dissolution method and prepare the not slow shortcoming of metal ion silicon sol speed of response, present method speed of response is fast, and technological process is simple.
Embodiment
Embodiment 1: take by weighing 27 g CaO and 33 g SiO
2Powder is put into mortar and is fully ground, and it is mixed; The admixtion that mixes is put into plumbago crucible, in silicon molybdenum stove, be warmed up to 1550 ℃ and be incubated 40 min with the speed of 3 ~ 5 ℃/min; Under the high temperature, after the plumbago crucible taking-up, reaction product is carried out Water Quenching, obtain the shrend Calucium Silicate powder.The shrend Calucium Silicate powder that obtains is put into loft drier, dry 3 h under 100 ℃.30 mesh sieves are pulverized, crossed to shrend Calucium Silicate powder after the oven dry, and extracting screen underflow is subsequent use.Getting mass percentage concentration and be 98% the vitriol oil 14 mL slowly pours in the 66 mL water and dilutes; Under stirring condition, slowly add 20 g shrend calcium silicate powders; Behind reaction 10 min under 30 ℃; With the reaction product suction filtration, separate the water white transparency filtrating that obtains, be the not high-purity silicasol of metal ion.
Embodiment 2: take by weighing 28 g CaO and 32 g SiO
2Powder is put into mortar and is fully ground, and it is mixed; The admixtion that mixes is put into plumbago crucible, in silicon molybdenum stove, be warmed up to 1580 ℃ and be incubated 40 min with the speed of 3 ~ 5 ℃/min; Under the high temperature, after the plumbago crucible taking-up, reaction product is carried out Water Quenching, obtain the shrend Calucium Silicate powder.The shrend Calucium Silicate powder that obtains is put into loft drier, dry 3 h under 100 ℃.30 mesh sieves are pulverized, crossed to shrend Calucium Silicate powder after the oven dry, and extracting screen underflow is subsequent use.Getting mass percentage concentration and be 98% the vitriol oil 13 mL slowly pours in the 67 mL water and dilutes; Under stirring condition, slowly add 20 g shrend calcium silicate powders; Behind reaction 10 min under 40 ℃; With the reaction product suction filtration, separate the water white transparency filtrating that obtains, be the not high-purity silicasol of metal ion.
Embodiment 3: take by weighing 30 g CaO and 30 g SiO
2Powder is put into mortar and is fully ground, and it is mixed; The admixtion that mixes is put into plumbago crucible, in silicon molybdenum stove, be warmed up to 1600 ℃ and be incubated 40 min with the speed of 3 ~ 5 ℃/min; Under the high temperature, after the plumbago crucible taking-up, reaction product is carried out Water Quenching, obtain the shrend Calucium Silicate powder.The shrend Calucium Silicate powder that obtains is put into loft drier, dry 3 h under 100 ℃.30 mesh sieves are pulverized, crossed to shrend Calucium Silicate powder after the oven dry, and extracting screen underflow is subsequent use.Getting mass percentage concentration and be 98% the vitriol oil 12 mL slowly pours in the 68 mL water and dilutes; Under stirring condition, slowly add 20 g shrend calcium silicate powders; Behind reaction 10 min under 50 ℃; With the reaction product suction filtration, separate the water white transparency filtrating that obtains, be the not high-purity silicasol of metal ion.
Claims (1)
1. preparation method of the high-purity silicasol of metal ion not is characterized in that said preparing method's concrete steps are following:
(1), takes by weighing quicklime and silicon-dioxide powdery is put into plumbago crucible; The mass ratio of said quicklime and silicon-dioxide is 1: (1.0 ~ 1.2); Temperature rise rate with 3 ~ 5 ℃/min is warmed up to 1550 ~ 1600 ℃, is incubated the reaction product that 40 min obtain quicklime and silicon-dioxide then;
(2), reaction product that said step (1) is obtained carries out Water Quenching, obtains the shrend Calucium Silicate powder;
(3), the shrend Calucium Silicate powder that said step (2) is obtained carries out drying, the back extracting screen underflow of pulverizing, sieve obtains the shrend calcium silicate powder;
(4), prepare certain density sulphuric acid soln; Under stirring condition, slowly add the shrend calcium silicate powder that said step (3) obtains; Said shrend Calucium Silicate powder and vitriolic mass ratio are 1: (1.1 ~ 1.3); Suction filtration after reaction is accomplished separates the water white transparency filtrating that obtains, and is the not high-purity silicasol of metal ion.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107188187A (en) * | 2017-05-22 | 2017-09-22 | 如皋市下原科技创业服务有限公司 | A kind of preparation method of high-purity silicasol |
| CN109796020A (en) * | 2019-04-02 | 2019-05-24 | 青岛硕远硅胶科技有限公司 | A kind of preparation method of the dedicated fine silica powder of catalyst |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1036547A (en) * | 1988-03-16 | 1989-10-25 | 日产化学工业株式会社 | Stable silica sol and manufacture method thereof |
| CN1648042A (en) * | 2005-01-07 | 2005-08-03 | 安徽工业大学 | Method for preparing hydrated silicon dioxide |
| CN101549870A (en) * | 2009-05-13 | 2009-10-07 | 安徽工业大学 | Preparation method of silica sol by using blast furnace slag |
| CN102390837A (en) * | 2011-08-03 | 2012-03-28 | 南通海迅天恒纳米科技有限公司 | Preparation method of nonspherical nanometer-scale silica sol |
-
2012
- 2012-09-21 CN CN2012103541081A patent/CN102838124A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1036547A (en) * | 1988-03-16 | 1989-10-25 | 日产化学工业株式会社 | Stable silica sol and manufacture method thereof |
| CN1648042A (en) * | 2005-01-07 | 2005-08-03 | 安徽工业大学 | Method for preparing hydrated silicon dioxide |
| CN101549870A (en) * | 2009-05-13 | 2009-10-07 | 安徽工业大学 | Preparation method of silica sol by using blast furnace slag |
| CN102390837A (en) * | 2011-08-03 | 2012-03-28 | 南通海迅天恒纳米科技有限公司 | Preparation method of nonspherical nanometer-scale silica sol |
Non-Patent Citations (1)
| Title |
|---|
| 车传仁等: "《高炉炼铁》", 31 March 1981, article "高炉炼铁", pages: 23 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107188187A (en) * | 2017-05-22 | 2017-09-22 | 如皋市下原科技创业服务有限公司 | A kind of preparation method of high-purity silicasol |
| CN109796020A (en) * | 2019-04-02 | 2019-05-24 | 青岛硕远硅胶科技有限公司 | A kind of preparation method of the dedicated fine silica powder of catalyst |
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Application publication date: 20121226 |