CN104176739B - A kind of sodium silicate prepares the method for high-purity silicon dioxide powder - Google Patents
A kind of sodium silicate prepares the method for high-purity silicon dioxide powder Download PDFInfo
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- CN104176739B CN104176739B CN201410405731.4A CN201410405731A CN104176739B CN 104176739 B CN104176739 B CN 104176739B CN 201410405731 A CN201410405731 A CN 201410405731A CN 104176739 B CN104176739 B CN 104176739B
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Abstract
The present invention relates to a kind of method that step-by-step precipitation method prepares high-purity silicon dioxide powder.First in sodium silicate solution, sulfuric acid solution is dripped to pH=11 ~ 13, filter out this part solid sediment rich in impurity, dropping sulfuric acid solution is continued again to precipitating completely in filtrate, filter, in precipitate, add a certain amount of acid and water is stirred, filtration washing precipitate, carry out drying, calcine after obtain high-purity silicon dioxide powder.Use said method, the high-purity silicon dioxide powder that major impurity content is about 20 ppm can be obtained.Preparation method of the present invention is with low cost, and technological process is simple, it is easy to industrialized production.
Description
Technical field
The present invention relates to the technology of preparing of a kind of silicon dioxide, particularly one sodium silicate and prepare high-purity silicon dioxide powder
Method.
Background technology
Along with electronics technology, the fast development of information technology, fine silica powder has become irreplaceable core material.
The physico-chemical property of its uniqueness makes it in high-end industries such as circuit package, optical fibers, aviation, war industry, special optical glass
In be used widely, be the important support material of electronics and information industry, simultaneously also have the highest in fields such as the cosmetics of super quality
Practical value.
China is the big producing country of low side silicon dioxide powder, and China Patent Publication No. CN1830774A discloses one sky
The method that so high-purity spherical nano amorphous silicon micropowder prepared by konilite, SiO2Percentage by weight is 99.89 ~ 99.95%, SiO2Contain
Measure relatively low, be not suitable for high-end product market；China Patent Publication No. CN103265036A discloses a kind of normal temperature condition and prepares
The method of nanometer silicon dioxide material, has obtained the silicon dioxide powder that particle diameter is 15 ~ 50nm, but purity is relatively low；Chinese patent is public
The number of opening CN101125657A discloses a kind of method that industrial waterglass prepares high-purity silicon dioxide equally, but technical process phase
To loaded down with trivial details, it is difficult to be used widely.For the application of silicon dioxide powder, the simplest technology of preparing of research has great
Theory and realistic meaning.
Summary of the invention
The technical problem to be solved in the present invention is for the deficiencies in the prior art, it is proposed that a kind of technical process is the most steady
The method preparing high-purity silicon dioxide powder with sodium silicate that fixed, with low cost, product purity is higher.
The technical problem to be solved in the present invention is achieved through the following technical solutions, and one sodium silicate is prepared high-purity
The method of silicon dioxide powder, is characterized in:
(1) taking the sodium silicate solution that mass concentration is 20 ~ 35%, be heated to 70 ~ 95 DEG C, mixing speed is 200 ~ 400r/
min；
(2) it is gradually added into sulfuric acid solution that mass concentration is 10 ~ 20% to pH=11 ~ 13, filters this partly precipitated；
(3) take the sulfuric acid solution that filtrate continuation dropping mass concentration in step (2) is 10 ~ 20% to react to pH less than 5, old
Change 2 ~ 3 hours, filter taking precipitate；
(4) precipitate in step (3) will be taken add in the pickle that mass concentration is 10 ~ 15%, and be heated to 50 ~ 80 DEG C and stir
Mix 0.5 ~ 1 hour；
(5) solution after stirring in step (4) is crossed leaching precipitation, be then washed with deionized to filtrate pH=7, heavy
Shallow lake thing carries out drying, calcining, and obtains high-purity silicon dioxide powder.
The technical problem to be solved in the present invention can also be come to realize further by the following technical programs, and described pickle is
Nitric acid or hydrochloric acid.
The technical problem to be solved in the present invention can also be come to realize further by the following technical programs, dries in step (5)
Dry temperature is 120 DEG C；It is placed in heating by electric cooker to calcine to 500 DEG C, is incubated 1 hour, finally obtains high-purity silicon dioxide powder.
Compared with prior art, it is an advantage of the current invention that: use above-mentioned technological process to can get high-purity silicon dioxide micro-
Powder, product major impurity content is about 20 ppm.The low in raw material price preparing high-purity silicon dioxide powder that the present invention uses,
Technique is relatively easy, relatively low to equipment requirements, beneficially industrialized production.High-purity silicon dioxide powder purity prepared by the present invention
Height, has a good application prospect.
Detailed description of the invention
A kind of sodium silicate prepares the method for high-purity silicon dioxide powder,
(1) taking the sodium silicate solution that mass concentration is 20 ~ 35%, be heated to 70 ~ 95 DEG C, mixing speed is 200 ~ 400r/
min；
(2) it is gradually added into sulfuric acid solution that mass concentration is 10 ~ 20% to pH=11 ~ 13, filters this part rich in impurity
Solid sediment,；
(3) take the sulfuric acid solution that filtrate continuation dropping mass concentration in step (2) is 10 ~ 20% to react to pH less than 5, old
Change 2 ~ 3 hours, filter taking precipitate；
(4) precipitate in step (3) will be taken add in the pickle that mass concentration is 10 ~ 15%, and be heated to 50 ~ 80 DEG C and stir
Mix 0.5 ~ 1 hour；
(5) solution after stirring in step (4) is crossed leaching precipitation, be then washed with deionized to filtrate pH=7, heavy
Shallow lake thing carries out drying, calcining, and obtains high-purity silicon dioxide powder.
Described pickle is nitric acid or hydrochloric acid.
Drying temperature in step (5) is 120 DEG C；It is placed in heating by electric cooker to calcine to 500 DEG C, is incubated 1 hour, finally
To high-purity silicon dioxide powder.
Following example further illustrate the present invention.
Comparative example 1:
Taking the sodium silicate solution that 100 ~ 150ml mass concentration is 20 ~ 35%, be heated to 70 ~ 95 DEG C, mixing speed is 200 ~
400r/min.It is gradually added into 10 ~ 20% sulfuric acid solutions to pH=12 ~ 13, crosses leaching precipitation.Take 100ml deionized water and 30 ~ 50ml
Concentration be 30% ~ 35% mixed in hydrochloric acid after add precipitate, at 50 ~ 80 DEG C stir 0.5 ~ 1 hour, then filter, use deionization
Water washing precipitation until filtrate pH=7, afterwards 120 DEG C of drying, is placed in heating by electric cooker to 500 DEG C, is incubated 1 hour, obtains titanium dioxide
Silica flour.
Testing through ICP with impurity content in silicon dioxide powder prepared by above step, its result is as follows:
| Element term | Al | Na | K | Ca | Mg | Ti | Fe | Cr | Add up to |
| Impurity content (ppm) | 86.39 | 1.27 | 0.67 | 2.25 | 1.31 | 3.4 | 6.85 | 2.25 | 104.39 |
Comparative example 2
Taking the sodium silicate solution that 100 ~ 150ml mass concentration is 20 ~ 35%, be heated to 70 ~ 95 DEG C, mixing speed is 200 ~
400r/min.It is gradually added into 10 ~ 20% sulfuric acid solutions to pH less than 5, is aged 2 ~ 3 hours, cross leaching precipitation；Taking mass concentration is
The nitric acid of 10 ~ 15% adds precipitate, stirs 0.5 ~ 1 hour, then filter at 50 ~ 80 DEG C；Be washed with deionized precipitation until
Filtrate pH=7, afterwards 120 DEG C of drying, be placed in heating by electric cooker to 500 DEG C, be incubated 1 hour, obtain silicon dioxide powder.
The impurity content of silicon dioxide powder prepared by above step is tested through ICP, and its result is as follows:
| Element term | Al | Na | K | Ca | Mg | Ti | Fe | Cr | Add up to |
| Impurity content (ppm) | 41.95 | 1.21 | 1.15 | 0.57 | 0.75 | 4.94 | 2.81 | 0.56 | 53.94 |
Embodiment 1:
Taking the sodium silicate solution that 100 ~ 150ml mass concentration is 20 ~ 35%, be heated to 70 ~ 95 DEG C, mixing speed is 200 ~
400r/min.It is gradually added into 10 ~ 20% sulfuric acid solutions to pH=12 ~ 13, filters this partly precipitated；Take filtrate and continue dropping sulphuric acid
Solution reaction, is aged 2 ~ 3 hours to pH less than 5, crosses leaching precipitation；Take the nitric acid that mass concentration is 10 ~ 15%, after addition once
Precipitate, at 50 ~ 80 DEG C stir 0.5 ~ 1 hour, then filter, be washed with deionized to filtrate pH=7, afterwards 120 DEG C of bakings
Dry, it is placed in heating by electric cooker to 500 DEG C, is incubated 1 hour, obtains silicon dioxide powder.
Impurity SiO in silicon dioxide powder prepared by above step2Content is tested through ICP, and major impurity content is as follows:
| Element term | Al | Na | K | Ca | Mg | Ti | Fe | Cr | Add up to |
| Impurity content (ppm) | 15.1 | 0.39 | 0.35 | 0.62 | 1.3 | 0.18 | 2.72 | 0.33 | 20.99 |
Embodiment 2:
Taking the sodium silicate solution that 100 ~ 150ml mass concentration is 20 ~ 35%, be heated to 70 ~ 95 DEG C, mixing speed is 200 ~
400r/min.It is gradually added into 10 ~ 20% sulfuric acid solutions to pH=11 ~ 12, filters this partly precipitated；Take filtrate and continue dropping sulphuric acid
Solution reaction, is aged 2 ~ 3 hours to pH less than 5, crosses leaching precipitation；Take 100ml deionized water and 30 ~ 50ml concentration be 30% ~
The mixed in hydrochloric acid of 35%, primary sedimentation thing after addition, 50 ~ 80 DEG C are stirred 0.5 ~ 1 hour, then filter, and it is heavy to be washed with deionized
Form sediment until filtrate pH=7, afterwards 120 DEG C of drying, be placed in heating by electric cooker to 500 DEG C, be incubated 1 hour, obtain silicon dioxide powder.
Silicon dioxide powder prepared by above step is tested through ICP, and major impurity content is as follows:
| Element term | Al | Na | K | Ca | Mg | Ti | Fe | Cr | Add up to |
| Impurity content (ppm) | 14.2 | 2.82 | 0.29 | 3.44 | 2.58 | 1.02 | 0.66 | 0.09 | 25.1 |
Claims (2)
1. the method preparing high-purity silicon dioxide powder with sodium silicate, it is characterised in that:
(1) taking the sodium silicate solution that mass concentration is 20～35%, be heated to 70～95 DEG C, mixing speed is 200～400r/
min；
(2) be gradually added into mass concentration be 10～20% sulfuric acid solution to pH=11～13, filter this partly precipitated；
(3) take filtrate in step (2) continue dropping mass concentration be 10～20% sulfuric acid solution reaction to pH less than 5, be aged 2
～3 hours, filter taking precipitate；
(4) by step (3) precipitate add mass concentration be 10～15% pickle in, be heated to 50～80 DEG C of stirrings
0.5～1 hour, described pickle was nitric acid or hydrochloric acid；
(5) solution after stirring in step (4) is crossed leaching precipitation, be then washed with deionized to filtrate pH=7, precipitate
Carry out drying, calcining, obtain high-purity silicon dioxide powder.
Sodium silicate the most according to claim 1 prepares the method for high-purity silicon dioxide powder, it is characterised in that: step (5)
Middle drying temperature is 120 DEG C；It is placed in heating by electric cooker to calcine to 500 DEG C, is incubated 1 hour, finally obtains high-purity silicon dioxide
Powder.
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| CN107140645B (en) * | 2017-06-15 | 2019-08-23 | 确成硅化学股份有限公司 | A kind of preparation method of the dedicated hydrated SiO 2 of engineering tyre |
| CN112938989B (en) * | 2021-03-17 | 2023-07-25 | 江苏微纳光膜科技有限公司 | High-purity silicon dioxide for optical coating and preparation process thereof |
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