CN101462728A - Method for preparing waterglass - Google Patents
Method for preparing waterglass Download PDFInfo
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- CN101462728A CN101462728A CNA2008102049869A CN200810204986A CN101462728A CN 101462728 A CN101462728 A CN 101462728A CN A2008102049869 A CNA2008102049869 A CN A2008102049869A CN 200810204986 A CN200810204986 A CN 200810204986A CN 101462728 A CN101462728 A CN 101462728A
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Abstract
The invention relates to a method for preparing water glass. The method comprises the steps of taking common silica sol as raw material and obtaining a finished product through purification, negative-positive resin exchange and alkali-adding dissolution. The method can control the appearance of the water glass as well as the species and content of impurity ions, and is used for producing the raw material of ultra-pure silica sol (the mass ratio of metallic elements to silicon dioxide is less than 1,000 ppm). The production of ultra-pure silica sol, which takes the water glass produced by the method as the raw material, has the characteristic of low cost.
Description
Technical field
The present invention relates to a kind of manufacture method of water glass, be intended for the production method of the water glass of producing the hyperpure silicasol raw material or rather, belong to inorganic fine chemicals production field.
Background technology
Hyperpure silicasol has the low characteristics of metal element content, is used for industries such as the chemically machinery polished of semiconducter device production process, high-grade refractory materials production, is a kind of at the current inorganic fine chemicals that market outlook are arranged very much.
The production method of hyperpure silicasol is that the expensive organosilicon of employing is that raw material makes through hydrolysis at present, and perhaps adopting the expensive white carbon black of gas phase is that raw material is dispersed into colloidal solution under the effect of mechanical force.
The silicon sol that traditional water glass ion exchange method is produced, owing to contain a large amount of impurity negatively charged ion in the water glass, the anionic existence of impurity has influenced the exchange degree of metal ion, water glass still has a large amount of metal ions to remain in the solution after resin cation exchange, with still containing more metallic element in this its silica particle inside of solution synthetic silicon sol, micelle surface and the solution, therefore adopt water glass to reach the purpose of producing hyperpure silicasol for the raw material difficulty or ease.
Summary of the invention
The technical problem to be solved in the present invention has been to provide a kind of method that can control impurity anion-content in the water glass, the anionic content of impurity is controlled effectively in the feasible water glass of producing, impurity negatively charged ion quantity is seldom in cationic exchange is crossed because in the solution for the water glass of producing with this method, metal ion has obtained sufficient exchange, also just obtain control corresponding with its metallic element of solution synthetic silicon sol after this exchange, thereby reached hyperpure purpose.
In order to solve the problems of the technologies described above, the solution that the present invention proposes is: a kind of preparation method of water glass is characterized in that this preparation method may further comprise the steps:
Step 1, the preparation silicon sol, dioxide-containing silica is 5-50% in this silicon sol;
Step 2 purifies, and adopts the mode of sedimentation or micro-filtration through the deep bed filter filtration, purification to above-mentioned silicon sol;
Step 3, yin and yang resin exchange, the resin cation (R.C.) of employing is to have-resin cation (R.C.) of H, the resin anion(R.A) that is adopted is to have-resin anion(R.A) of 0H;
Step 4 adds alkali dissolution, and the kind of the alkali that adopts is caustic soda or potassium hydroxide or sum of the two, and the inorganic salt content of the alkali that adopts must be less than 8%.
As one of preferred version of the present invention, the order of yin and yang resin exchange is to exchange through resin cation exchange and then through resin anion(R.A) earlier in the described step 3.
As one of preferred version of the present invention, the exchanged form of yin and yang resin exchange is dynamic exchange or static exchange in the described step 3.
As one of preferred version of the present invention, described dynamic exchange is under whipped state yin and yang resin to be added silicon sol successively or simultaneously.
As one of preferred version of the present invention, described static exchange is the silicon sol yin and yang resin layer of flowing through.
As one of preferred version of the present invention, the dynamic exchange of described yin and yang resin exchange is more than 10 minutes.
As one of preferred version of the present invention, the static exchange time of described yin and yang resin exchange is 1-10 minute.
As one of preferred version of the present invention, the alkali dissolution that adds in the described step 4 is that caustic soda or potassium hydroxide or sum of the two are made into 5% to saturated solution, is warming up to 40-100 ℃ under whipped state gradually.
As one of preferred version of the present invention, the alkali dissolution that adds in the described step 4 is that caustic soda or potassium hydroxide or sum of the two are made into 5% to saturated solution, is warming up to 80-95 ℃ under whipped state gradually.
The method that the present invention takes is to be raw material with ordinary silicon colloidal sol, removes suspended particle, removes foreign ion through the yin and yang resin exchange by purification, adds alkali dissolution and obtains required finished product.The water glass of producing with present method is that raw material is used for hyperpure silicasol production and has the low characteristics of cost.
Description of drawings
Fig. 1 is preparation method's process flow sheet of the present invention.
Embodiment
Detailed step of the present invention is as follows:
The first step is made into the concentration (normally 30%) of 5-50% as required with silicon sol, through deep bed filter filtration, purification (also can be sedimentation or micro-filtration) to remove suspended substance.
Second step, will flow through resin cation (R.C.) (H type) to remove the solution metal ion through the silicon sol after purifying, the resin anion(R.A) of flowing through again (OH type) is to remove the impurity negatively charged ion; The negative and positive hybrid resin of also can flowing through; Also can add resin cation exchange under whipped state, the elimination resin cation (R.C.) adds the resin anion(R.A) exchange more then; Also can under whipped state, add resin cation (R.C.) and resin anion(R.A) simultaneously.The time of exchange is generally more than colloidal sol contact pressure resin time 1-10 minute (static exchange), and dynamic exchange is more than 10 minutes, and normally more than 30 minutes, more excellent is 2 hours.The number of times of exchange is decided on the required index of removing foreign ion that reaches, and the general needs that only just can satisfy the making hyperpure silicasol through a zwitterion exchange reach purer index as need and can adopt repeatedly repeated exchanged.
The 3rd step, with caustic soda and (or) potassium hydroxide is made into 5% to saturated solution (usually the purity to alkali has strict requirement, generally is controlled at more than 98%), is warming up to 40-100 ℃ gradually under whipped state, normally 80-95 ℃.
The 4th step added the silicon sol of handling through second step in the solution gradually in the 3rd step, and the add-on of silicon sol is decided according to required modulus and concentration, treated the water glass that solution stops to heat requiredly after transparent.
Example 1
Get silicon sol (dioxide-containing silica is 30%) 2000ml, standby after 45 μ m microporous membrane suction filtrations purify.
Add the silicon sol of 1600 grams after above-mentioned purification in the there-necked flask of 2000ml, open and stir, add resin cation (R.C.) 400ml, stir elimination resin cation (R.C.) after 1 hour, add resin anion(R.A) 400ml again, it is standby to stir after 1 hour the elimination resin anion(R.A).
Being 98% sodium hydroxide with content is made into 40% solution 400 grams with deionized water, adds in the there-necked flask of 1000ml the back and opens and stir, and adds above-mentioned through 800 grams of the silicon sol after the yin and yang resin exchange gradually.Heat temperature raising treats that to 80-95 ℃ of maintenance 30 minutes solution becomes clear after cooling promptly gets required water glass.
With this water glass is that raw material makes orthosilicic acid after ion-exchange, then the orthosilicic acid polymerization is made hyperpure silicasol (silica concentration is 30%, and metal element content is 9ppm, and metallic element is 30ppm with the ratio of the quality of silicon-dioxide).
Example 2
Get silicon sol (dioxide-containing silica is 30%) 2000ml, standby after 45 μ m microporous membrane suction filtrations purify.
Being 98% sodium hydroxide with content is made into 40% solution 400 grams with deionized water, adds in the there-necked flask of 1000ml the back and opens and stir, and adds above-mentioned through the silicon sol after the yin and yang resin exchange gradually.Heat temperature raising treats that to 80-95 ℃ of maintenance 30 minutes solution becomes clear after cooling promptly gets required water glass.
With this water glass is that raw material makes orthosilicic acid after ion-exchange, then the orthosilicic acid polymerization is made hyperpure silicasol (concentration of silicon dioxide is 30%, metal element content 0.9ppm, metallic element is ppm with the ratio of the quality of silicon-dioxide).
Example 3
It is standby to get silicon sol (dioxide-containing silica is 30%) 2000ml with 5 μ m filter bag leachings.
In the there-necked flask of 2000ml, add through above-mentioned silicon sol 1600 grams after filtering, open and stir, add resin cation (R.C.) 400ml, stir elimination resin cation (R.C.) after 1 hour, add resin anion(R.A) 400ml again, it is standby to stir after 1 hour the elimination resin anion(R.A).
Being 98% potassium hydroxide with content is made into 25% solution 520 grams with deionized water, adds in the there-necked flask of 1000ml, opens and stirs, and adds above-mentioned through 800 grams of the silicon sol after the yin and yang resin exchange gradually.Heat temperature raising treats that to 80-95 ℃ of maintenance 30 minutes solution becomes clear after cooling promptly gets required water glass.
With this water glass is that raw material makes orthosilicic acid after ion-exchange, then the orthosilicic acid polymerization is made hyperpure silicasol (silica concentration is 30%, and metal element content is 6ppm, and metallic element is 20ppm with the ratio of the quality of silicon-dioxide).
Example 4
It is standby to get silicon sol (dioxide-containing silica is 30%) 2000ml with 5 μ m filter bag leachings.
Resin cation (R.C.) layer height 100cm is housed in the polypropylene plastics tubing of DN50, with the silicon sol of 1600 grams after the above-mentioned filtration resin layer of flowing through, the control flow velocity is at per second 0.5ml, and is then that the silicon sol of collecting is standby after the resin anion(R.A) exchange of same size same way as again.
Being 98% potassium hydroxide with content is made into 25% solution 370 grams with deionized water, adds in the there-necked flask of 1000ml, opens and stirs, and adds above-mentioned through 800 grams of the silicon sol after the yin and yang resin exchange gradually.Heat temperature raising treats that to 80-95 ℃ of maintenance 30 minutes solution becomes clear after cooling promptly gets required water glass.
With this water glass is that raw material makes orthosilicic acid after ion-exchange, then the orthosilicic acid polymerization is made hyperpure silicasol (silica concentration is 30%, and metal element content is 0.9pm, and metallic element is 3.0ppm with the ratio of the quality of silicon-dioxide).
Above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art should be within protection scope of the present invention for improvement and modification that the present invention makes according to announcement of the present invention.
Claims (9)
1. the preparation method of a water glass is characterized in that, this preparation method may further comprise the steps:
Step 1, the preparation silicon sol, dioxide-containing silica is 5-50% in this silicon sol;
Step 2 purifies, and adopts the mode of sedimentation or micro-filtration through the deep bed filter filtration, purification to above-mentioned silicon sol;
Step 3, yin and yang resin exchange, the resin cation (R.C.) of employing is to have-resin cation (R.C.) of H, the resin anion(R.A) that is adopted is to have-resin anion(R.A) of OH;
Step 4 adds alkali dissolution, and the kind of the alkali that adopts is caustic soda or potassium hydroxide or sum of the two, and the inorganic salt content of the alkali that adopts must be less than 8%.
2. the preparation method of a kind of water glass as claimed in claim 1 is characterized in that, the order of yin and yang resin exchange is to exchange through resin cation exchange and then through resin anion(R.A) earlier in the described step 3.
3. the preparation method of a kind of water glass as claimed in claim 1 is characterized in that, the exchanged form of yin and yang resin exchange is dynamic exchange or static exchange in the described step 3.
4. the preparation method of a kind of water glass as claimed in claim 3 is characterized in that, described dynamic exchange is under whipped state yin and yang resin to be added silicon sol successively or simultaneously.
5. the preparation method of a kind of water glass as claimed in claim 3 is characterized in that, described static exchange is the silicon sol yin and yang resin layer of flowing through.
6. the preparation method of a kind of water glass as claimed in claim 4 is characterized in that, the dynamic exchange of described yin and yang resin exchange is more than 10 minutes.
7. the preparation method of a kind of water glass as claimed in claim 5 is characterized in that, the static exchange time of described yin and yang resin exchange is 1-10 minute.
8. the preparation method of a kind of water glass as claimed in claim 1 is characterized in that, the alkali dissolution that adds in the described step 4 is that caustic soda or potassium hydroxide or sum of the two are made into 5% to saturated solution, is warming up to 40-100 ℃ under whipped state gradually.
9. the preparation method of a kind of water glass as claimed in claim 1 is characterized in that, the alkali dissolution that adds in the described step 4 is that caustic soda or potassium hydroxide or sum of the two are made into 5% to saturated solution, is warming up to 80-95 ℃ under whipped state gradually.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102049869A CN101462728A (en) | 2008-12-30 | 2008-12-30 | Method for preparing waterglass |
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|---|---|---|---|
| CNA2008102049869A CN101462728A (en) | 2008-12-30 | 2008-12-30 | Method for preparing waterglass |
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| CN101462728A true CN101462728A (en) | 2009-06-24 |
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| CNA2008102049869A Pending CN101462728A (en) | 2008-12-30 | 2008-12-30 | Method for preparing waterglass |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092735A (en) * | 2011-03-11 | 2011-06-15 | 福建省三明汇丰化工有限公司 | Purification method of sodium silicate |
| CN101658898B (en) * | 2009-09-16 | 2011-07-13 | 沈阳汇亚通铸造材料有限责任公司 | Preparation method of casting water glass |
| CN103030153A (en) * | 2013-01-18 | 2013-04-10 | 昆明道尔森科技有限公司 | Method for preparing potash water glass |
| CN103030152A (en) * | 2013-01-18 | 2013-04-10 | 昆明道尔森科技有限公司 | Method for preparing electronic potassium silicate solution |
| CN103043671A (en) * | 2012-12-27 | 2013-04-17 | 上海新安纳电子科技有限公司 | Production method for polysilicic acid |
| CN103764563A (en) * | 2011-09-05 | 2014-04-30 | 日产化学工业株式会社 | Method for producing purified silicic acid alkali aqueous solution and silica sol |
| CN108002393A (en) * | 2017-12-27 | 2018-05-08 | 上海新安纳电子科技有限公司 | A kind of method that Ludox polishing fluid using recycling prepares silicic acid |
| CN111592003A (en) * | 2020-06-10 | 2020-08-28 | 华章检测技术服务南通有限公司 | Method for preparing large-particle-size silica sol by cation, anion and cation three-time ion exchange |
-
2008
- 2008-12-30 CN CNA2008102049869A patent/CN101462728A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101658898B (en) * | 2009-09-16 | 2011-07-13 | 沈阳汇亚通铸造材料有限责任公司 | Preparation method of casting water glass |
| CN102092735A (en) * | 2011-03-11 | 2011-06-15 | 福建省三明汇丰化工有限公司 | Purification method of sodium silicate |
| CN102092735B (en) * | 2011-03-11 | 2013-01-16 | 福建海能新材料有限公司 | Purification method of sodium silicate |
| CN103764563A (en) * | 2011-09-05 | 2014-04-30 | 日产化学工业株式会社 | Method for producing purified silicic acid alkali aqueous solution and silica sol |
| CN103043671A (en) * | 2012-12-27 | 2013-04-17 | 上海新安纳电子科技有限公司 | Production method for polysilicic acid |
| CN103043671B (en) * | 2012-12-27 | 2014-12-03 | 上海新安纳电子科技有限公司 | Production method for polysilicic acid |
| CN103030153A (en) * | 2013-01-18 | 2013-04-10 | 昆明道尔森科技有限公司 | Method for preparing potash water glass |
| CN103030152A (en) * | 2013-01-18 | 2013-04-10 | 昆明道尔森科技有限公司 | Method for preparing electronic potassium silicate solution |
| CN103030153B (en) * | 2013-01-18 | 2014-09-24 | 昆明道尔森科技有限公司 | Method for preparing potash water glass |
| CN103030152B (en) * | 2013-01-18 | 2015-01-21 | 昆明道尔森科技有限公司 | Method for preparing electronic potassium silicate solution |
| CN108002393A (en) * | 2017-12-27 | 2018-05-08 | 上海新安纳电子科技有限公司 | A kind of method that Ludox polishing fluid using recycling prepares silicic acid |
| CN111592003A (en) * | 2020-06-10 | 2020-08-28 | 华章检测技术服务南通有限公司 | Method for preparing large-particle-size silica sol by cation, anion and cation three-time ion exchange |
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Application publication date: 20090624 |