CN109553109A - A kind of method preparing silica solution and silica solution - Google Patents
A kind of method preparing silica solution and silica solution Download PDFInfo
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- CN109553109A CN109553109A CN201710888891.2A CN201710888891A CN109553109A CN 109553109 A CN109553109 A CN 109553109A CN 201710888891 A CN201710888891 A CN 201710888891A CN 109553109 A CN109553109 A CN 109553109A
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- silica solution
- silicon
- silicon source
- solution
- water
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/141—Preparation of hydrosols or aqueous dispersions
- C01B33/1412—Preparation of hydrosols or aqueous dispersions by oxidation of silicon in basic medium
Abstract
The invention discloses a kind of methods for preparing silica solution, method includes the following steps: in the mixture of the silicon source containing elemental silicon and water, basic catalyst or alkaline catalyst solution is added in (1)；(2) it is passed through direct current in reaction process, generates silica solution.This method is by providing hydroxide ion in addition basic catalyst, promote water power from generation hydroxide ion, to cause the reaction speed of initial elemental silicon and hydroxide ion, it is passed through direct current in the reaction process of silicon and water to accelerate the hydrolysis speed of silicon, generates silica solution.Above-mentioned preparation method accelerates the hydrolysis speed of silicon due to being passed through direct current, so basic catalyst used in step (1) is seldom for the quality of silicon source, so that the content of the cation in final silica solution obtained is few, the Cation adsorption of basic catalyst is reduced in the amount on the hydroxyl of silica solution shell.
Description
Technical field
The invention belongs to silica solution preparation technical fields, and in particular to a kind of method for preparing silica solution and silica solution.
Background technique
Polysilicon in process of production, can generate some fine particle silicon slags, and these silicon slags are not able to satisfy dimensionally
Customer demand, therefore fail normal sale and effective use.These tiny silicon slags can not only pollute working environment simultaneously,
Qualified product can also be polluted.In actual production process, polysilicon quality and working environment are polluted in order to prevent, only by these
Silicon slag carries out simple collection, is not efficiently used, causes certain wasting of resources.
Silica solution is amorphous silica particle evenly dispersed colloidal solution in water.Silica in silica solution
Great amount of hydroxy group is contained on grain surface, has biggish reactivity, can mix with organic polymer by surface modification, answer extensively
For industries such as coating, hot investment casting, papermaking, weaving, electronics.The silica solution of high-purity is applied to improve polishing fluid and special painting
Certain performances of material.Due to containing the alkali metal ions impurity such as sodium potassium in common silica solution, can generate during use
Negative effect, is unfavorable for the use of polishing fluid and coating, it is therefore desirable to control the concentration of alkali metal ion, general control exists
10ppm or less.
Existing high-purity silicasol the preparation method comprises the following steps: (1) using waterglass as Material synthesis: by certain density strong basicity
Waterglass carries out ion exchange by resin cation, is converted into acid silica solution, then by the aqueous solution of silica solution and highly basic
Or the silicate reaction of alkalinity, it is changed into the silica solution of alkalinity by nucleation, particle size growth etc.；(2) with water-disintegrable organic
Silane is raw material: using ethyl orthosilicate/methyl esters under the conditions of strong alkali catalyst, direct hydrolysis is poly- in the solution of water and alcohol
It closes, is prepared into silica solution.It is that product contains a certain amount of metal impurities using waterglass as the shortcomings that Material synthesis high-purity silicasol,
It can not completely remove；It is that product is needed in strong basicity environment using water-disintegrable organosilan as the shortcomings that Material synthesis high-purity silicasol
Lower use, at high cost, product design is low.
Summary of the invention
The technical problem to be solved by the present invention is to, provide a kind of to prepare silicon aiming at the above shortcomings existing in the prior art
The method and silica solution of colloidal sol solve and use strong alkali catalyst excessive during preparing silica solution in the prior art and introduce
The excessive technical problem of metal impurities.
It solves technical solution used by present invention problem and is to provide a kind of method for preparing silica solution, including is following
Step:
(1) in the mixture of the silicon source containing elemental silicon and water, basic catalyst or base catalysis agent solution is added；
(2) it is passed through direct current in reaction process, generates silica solution.
Preferably, the silicon source containing elemental silicon in the step (1) is high purity elemental silicon.
Preferably, the basic catalyst or base catalysis agent solution of catalytic amount are added in the step (1).
Water is weak electrolyte, and internal there are certain ionization equilibriums, under the action of direct current, the ionization equilibrium quilt of water
Break, generate more hydrogen ions and hydroxide ion, wherein hydrogen ion obtains electronics as hydrogen at cathode, hydroxyl from
Son loses electronics as oxygen at anode.Elemental silicon hydrolysis is exactly that silicon reacts with the water after ionization, and it is molten to generate silicon
Glue.
Preferably, the silicon source is the silicon slag generated in polysilicon production process；The main component of silicon slag is elemental silicon.
It, can be by the silicon in polysilicon production process using the silicon slag generated in polysilicon production process as the silicon source for preparing silica solution
Slag effective use, improves the economic benefit of enterprise, turns waste into wealth, not only save the post-processing expense of silicon slag, and save
Prepare the cost of material of silica solution.
Solute in the basic catalyst or base catalysis agent solution is sodium hydroxide and/or potassium hydroxide.
Preferably, the partial size of the silicon source is 10~200 mesh.
Preferably, the pH value of the solution of the basic catalyst is 10~14.
It preferably, further include that step (i) cleans the silicon source before the step (1), so that the silicon source
In impurity content≤1ppm, the purity of silicon is 99.9999mas% or more；
Water in the mixture is ultrapure water.
Preferably, the step (i) specifically:
Silicon source is added in ultrapure water, ultrasonic cleaning is carried out；
The silicon source immersion that ultrasonic cleaning finishes is cleaned in an acidic solution, removes the spot on silicon source surface；
Silicon source after pickling is added in ultrapure water, ultrasonic cleaning is first carried out, is added in ultrapure water and carries out again
Rinsing, rinsing are neutrality until ultrapure water.
Preferably, further include in the step (1) mixture of the silicon source containing elemental silicon and water is heated to 70~
95℃.Preferably, the mass ratio of silicon source and water is 1:(20~200 in the step (1)).
Preferably, the list in the solute and silicon source in step (1) the neutral and alkali catalyst or base catalysis agent solution
The mass ratio of matter silicon is 1:(500~2000).In preparation method of the invention, used basic catalyst is relative to silicon source
For quality seldom, so that the content of the cation of the basic catalyst in final silica solution obtained is few.The prior art
The middle mass ratio for generating the elemental silicon in the basic catalyst and silicon source that silica solution uses is 1:(50~200).
Preferably, the voltage of direct current described in the step (2) is 1.5~12V.
Preferably, the reaction time in the step (2) is 8~12 hours.
It preferably, further include that step (3) is concentrated at 90~95 DEG C after the step (2), it is high-purity after being concentrated
Spend silica solution.Metal ion content in high-purity silicasol is less than 10ppm.
The present invention also provides a kind of silica solution, for the silica solution being prepared by above-mentioned method.Preparation of the invention
The cations for the alkali metal in silica solution that method obtains are less than 10ppm.
The method for preparing silica solution of the invention is by providing hydroxide ion in addition basic catalyst, to cause
It is passed through direct current in the reaction process of the reaction speed of initial elemental silicon and hydroxide ion, silicon and water, to promote water
Ionization generates hydroxide ion, accelerates the hydrolysis speed of silicon, generates silica solution.Above-mentioned preparation method is straight due to being passed through
Galvanic electricity increases the ionization of water, to accelerate the hydrolysis speed of silicon, can reduce the usage amount of basic catalyst, and can mention
High pasc reaction generates the conversion ratio of silica solution, reaction speed is improved, so matter of the used basic catalyst relative to silicon source
For amount seldom, so that the content of the cation in final obtained silica solution is few, reduce the sun of basic catalyst from
Son is adsorbed in the amount on the hydroxyl of silica solution shell.The silica solution purity is high of this method preparation, operating process is simple and convenient, purity
It is easy to control.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, With reference to embodiment to this
Invention is described in further detail.
Embodiment 1
The present embodiment provides a kind of methods for preparing silica solution, comprising the following steps:
(1) silicon slag generated in the polysilicon production process being collected into is added in ultrapure water, carries out ultrasonic cleaning
0.5 hour, get rid of the impurity adhered in silicon slag, wherein the partial size of silicon slag is 10 mesh；Using being generated in polysilicon production process
Silicon slag as the silicon source for preparing silica solution, the silicon slag in polysilicon production process can be efficiently used, improve the warp of enterprise
Ji benefit, turns waste into wealth, not only saves the post-processing expense of silicon slag, and save the cost of material for preparing silica solution.
(2) silicon slag for finishing ultrasonic cleaning impregnates in an acidic solution, cleans 0.5 hour, removes silicon slag surface
Pollutant, wherein acid solution is the aqueous solution of nitric acid and hydrofluoric acid, pH value 5；
(3) silicon slag after pickling is added in ultrapure water, first carries out ultrasonic cleaning 0.5 hour, is added to again super
Rinsing 30 minutes is carried out in pure water, removes desilication slag acid remained on surface, impurity content≤1ppm in the silicon slag after cleaning, silicon
Purity is 99.9999mas% or more；
(4) silicon slag cleaned up is added to be mixed in ultrapure water and obtains mixture, mixture is placed on electricity
Carrying out heating stirring on magnetic stirring apparatus, the mass ratio of silicon slag and ultrapure water is 1:20,
(5) basic catalyst is added in ultrapure water, is configured to the base catalysis agent solution needed, wherein base catalysis
Agent is sodium hydroxide, pH value 10；
(6) after the mixture temperature of silicon slag and ultrapure water is raised to 95 DEG C, base catalysis agent solution, silicon and water are slowly added to
It is reacted, the mass ratio of basic catalyst and silicon slag in base catalysis agent solution is 1:500；The preparation method of the present embodiment
In, used catalyst is seldom for the quality of silicon source, so that the alkalinity in final silica solution obtained is urged
The content of the cation of agent is few.
(7) when base catalysis agent solution additional amount is more than more than half, direct current, the electricity of direct current are passed through into ultrapure water
Pressure is 9V, after base catalysis agent solution is added dropwise, reacts 12 hours, if there is unreacted filter residue to be filtered, is filtered
Liquid.
(8) filtrate is placed in water-bath and is stirred, be heated to 85 DEG C be evaporated concentration 2 hours, be prepared sodium from
The silica solution that sub- content is 8ppm, dioxide-containing silica is 20mas%.
The present embodiment also provides a kind of silica solution, for the silica solution being prepared by above-mentioned method.
The method for preparing silica solution of the present embodiment is by providing hydroxide ion in addition basic catalyst, to draw
It has sent out the reaction speed of initial elemental silicon and hydroxide ion, direct current is passed through in the reaction process of silicon and water to promote water
Ionization generates hydroxide ion, accelerates the hydrolysis speed of silicon, generates silica solution.Above-mentioned preparation method is straight due to being passed through
Galvanic electricity increases the ionization of water, to accelerate the hydrolysis speed of silicon, can reduce the usage amount of basic catalyst, and can mention
High pasc reaction generates the conversion ratio of silica solution, reaction speed is improved, so matter of the used basic catalyst relative to silicon source
For amount seldom, so that the content of the cation in final silica solution obtained is few, a large amount of basic catalysts are reduced
Cation adsorption is in the amount on the hydroxyl of silica solution shell.The silica solution purity is high of this method preparation, operating process is simple and convenient,
Purity is easy to control.
Embodiment 2
The present embodiment provides a kind of methods for preparing silica solution, comprising the following steps:
(1) silicon slag generated in the polysilicon production process being collected into is added in ultrapure water, carries out ultrasonic cleaning
1.5 hours, get rid of the impurity adhered in silicon slag, wherein the partial size of silicon slag is 100 mesh；
(2) silicon slag for finishing ultrasonic cleaning impregnates in an acidic solution, cleans 1 hour, removes the dirt on silicon slag surface
Contaminate object, wherein acid solution is the aqueous solution of nitric acid and hydrofluoric acid, pH value 3；
(3) silicon slag after pickling is added in ultrapure water, first carries out ultrasonic cleaning 1 hour, is added to again ultrapure
Carry out rinsing 30 minutes in water, remove desilication slag acid remained on surface, impurity content≤1ppm in the silicon slag after cleaning, silicon it is pure
Degree is 99.9999mas% or more；
(4) silicon slag cleaned up is added to be mixed in ultrapure water and obtains mixture, mixture is placed on electricity
Carry out heating stirring on magnetic stirring apparatus, the mass ratio of silicon slag and ultrapure water is 1:100；
(5) basic catalyst is added in ultrapure water, is configured to the base catalysis agent solution needed, wherein base catalysis
Agent is potassium hydroxide, pH value 12；
(6) after the mixture temperature of silicon slag and ultrapure water is raised to 85 DEG C, base catalysis agent solution, silicon and water are slowly added to
It is reacted, the mass ratio of basic catalyst and silicon slag in base catalysis agent solution is 1:1000；
(7) when base catalysis agent solution additional amount is more than more than half, direct current, the electricity of direct current are passed through into ultrapure water
Pressure is 6V, after base catalysis agent solution low price, reacts 9 hours, if there is unreacted filter residue to be filtered, is filtered
Liquid；
(8) filtrate is placed in water-bath and is stirred, be heated to 90 DEG C be evaporated concentration 3 hours, be prepared potassium from
The silica solution that sub- content is 8ppm, dioxide-containing silica is 10mas%.
The present embodiment also provides a kind of silica solution, for the silica solution being prepared by above-mentioned method.
Embodiment 3
The present embodiment provides a kind of methods for preparing silica solution, comprising the following steps:
(1) silicon slag generated in the silicon source polysilicon production process being collected into is added in ultrapure water, carries out ultrasonic wave
Cleaning 3 hours, gets rid of the impurity adhered in silicon slag, wherein the partial size of silicon slag is 200 mesh；
(2) silicon slag for finishing ultrasonic cleaning impregnates in an acidic solution, cleans 2 hours, removes the dirt on silicon slag surface
Contaminate object, wherein acid solution is the aqueous solution of nitric acid and hydrofluoric acid, pH value 1；
(3) silicon slag after pickling is added in ultrapure water, first carries out ultrasonic cleaning 1 hour, is added to again ultrapure
Carry out rinsing 30 minutes in water, remove desilication slag acid remained on surface, impurity content≤1ppm in the silicon slag after cleaning, silicon it is pure
Degree is 99.9999mas% or more；
(4) silicon slag cleaned up is added to be mixed in ultrapure water and obtains mixture, mixture is placed on electricity
Carry out heating stirring on magnetic stirring apparatus, the mass ratio of silicon slag and ultrapure water is 1:200；
(5) after the mixture temperature of silicon slag and ultrapure water is raised to 75 DEG C, it is slowly added to basic catalyst, pH value 14,
Wherein, basic catalyst is the mixture (the two mass ratio is 1:1) of sodium hydroxide and potassium hydroxide, and silicon is reacted with water,
The mass ratio of basic catalyst and silicon slag is 1:2000；
(6) when base catalysis agent solution additional amount is more than more than half, direct current, the electricity of direct current are passed through into ultrapure water
Pressure is 3V, after base catalysis agent solution low price, reacts 8 hours, if there is unreacted filter residue to be filtered, is filtered
Liquid；
(7) filtrate is placed in water-bath and is stirred, be heated to 95 DEG C be evaporated concentration 4 hours, be prepared sodium from
Son and potassium ion total content be 3ppm, the silica solution that dioxide-containing silica is 8mas%.
Certainly, the silicon source in the step in the present embodiment (1) is also possible to high purity elemental silicon, and silicon source is high purity elemental silicon
It is that can not have to wash silicon source, the purity of high purity elemental silicon is 99.9999mas% or more.
The present embodiment also provides a kind of silica solution, for the silica solution being prepared by above-mentioned method.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses
Mode, however the present invention is not limited thereto.For those skilled in the art, essence of the invention is not being departed from
In the case where mind and essence, various changes and modifications can be made therein, these variations and modifications are also considered as protection scope of the present invention.
Claims (12)
1. a kind of method for preparing silica solution, which comprises the following steps:
(1) in the mixture of the silicon source containing elemental silicon and water, basic catalyst or base catalysis agent solution is added；
(2) it is passed through direct current in reaction process, generates silica solution.
2. the method according to claim 1 for preparing silica solution, which is characterized in that the silicon source is polysilicon production process
The silicon slag of middle generation；
Solute in the basic catalyst or base catalysis agent solution is sodium hydroxide and/or potassium hydroxide.
3. according to right want 1 or 2 described in prepare the method for silica solution, which is characterized in that the partial size of the silicon source is 10~200
Mesh.
4. the method according to claim 1 for preparing silica solution, which is characterized in that further include step before the step (1)
Suddenly (i) cleans the silicon source, so that impurity content≤1ppm of the silicon source.
5. the method according to claim 4 for preparing silica solution, which is characterized in that the step (i) specifically:
Silicon source is added in ultrapure water, ultrasonic cleaning is carried out；
The silicon source immersion that ultrasonic cleaning finishes is cleaned in an acidic solution, removes the spot on silicon source surface；
Silicon source after pickling is added in ultrapure water, ultrasonic cleaning is first carried out, is added in ultrapure water is rinsed again.
6. the method according to claim 1 for preparing silica solution, which is characterized in that further include that will contain in the step (1)
The mixture of the silicon source and water that have elemental silicon is heated to 70~95 DEG C.
7. the method according to claim 1 for preparing silica solution, which is characterized in that silicon source and water in the step (1)
Mass ratio is 1:(20~200).
8. the method according to claim 1 for preparing silica solution, which is characterized in that step (1) the neutral and alkali catalyst
Or the mass ratio of the elemental silicon in the solute and silicon source in base catalysis agent solution is 1:(500~2000).
9. the method according to claim 1 for preparing silica solution, which is characterized in that direct current described in the step (2)
Voltage be 1.5~12V.
10. the method according to claim 9 for preparing silica solution, which is characterized in that the reaction time in the step (2)
It is 8~12 hours.
11. the method according to claim 1 for preparing silica solution, which is characterized in that further include step after the step (2)
Suddenly (3) are concentrated at 90~95 DEG C, the high-purity silicasol after being concentrated.
12. a kind of silica solution, which is characterized in that it was prepared for the method as described in claim 1~11 any one
Silica solution.
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| CN201710888891.2A CN109553109B (en) | 2017-09-27 | 2017-09-27 | Method for preparing silica sol and silica sol |
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| CN201710888891.2A CN109553109B (en) | 2017-09-27 | 2017-09-27 | Method for preparing silica sol and silica sol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112299423A (en) * | 2019-08-01 | 2021-02-02 | 新特能源股份有限公司 | Silicon dioxide preparation method and prepared silicon dioxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61242910A (en) * | 1985-04-18 | 1986-10-29 | Isao Sakai | Production of active silicic acid sol |
| CN102849748A (en) * | 2012-08-25 | 2013-01-02 | 安阳市凤凰光伏科技有限公司 | One-step method for preparing silica sol from silicon |
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2017
- 2017-09-27 CN CN201710888891.2A patent/CN109553109B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61242910A (en) * | 1985-04-18 | 1986-10-29 | Isao Sakai | Production of active silicic acid sol |
| CN102849748A (en) * | 2012-08-25 | 2013-01-02 | 安阳市凤凰光伏科技有限公司 | One-step method for preparing silica sol from silicon |
Non-Patent Citations (2)
| Title |
|---|
| 王娟等: "硅切割废砂浆制备硅溶胶及回收碳化硅的工艺研究", 《应用化工》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112299423A (en) * | 2019-08-01 | 2021-02-02 | 新特能源股份有限公司 | Silicon dioxide preparation method and prepared silicon dioxide |
| CN112299423B (en) * | 2019-08-01 | 2022-06-28 | 新特能源股份有限公司 | Silicon dioxide preparation method and prepared silicon dioxide |
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