CN107162009A - A kind of preparation method of high structure high abrasion hydrated SiO 2 - Google Patents
A kind of preparation method of high structure high abrasion hydrated SiO 2 Download PDFInfo
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- CN107162009A CN107162009A CN201710451487.9A CN201710451487A CN107162009A CN 107162009 A CN107162009 A CN 107162009A CN 201710451487 A CN201710451487 A CN 201710451487A CN 107162009 A CN107162009 A CN 107162009A
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- Prior art keywords
- sodium
- preparation
- hydrated sio
- silicate solution
- sulfuric acid
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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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
- C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
-
- 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
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
Abstract
The invention discloses a kind of preparation method of high structure high abrasion hydrated SiO 2, it is characterised in that comprises the steps：（1）By quartz sand and soda ash with 1:After 1.5 mol ratio is calcined 1 hour at 1,420 1450 DEG C, solid-state sodium metasilicate is obtained；（2）Solid-state sodium metasilicate is dissolved in sodium carbonate, sodium silicate solution is obtained, the removal of impurity is gone in filtering；（3）Dispersant is added into sodium silicate solution, under agitation, 4 6mol/L sulfuric acid solution is added dropwise into sodium silicate solution, there is Precipitation；4）By washing of precipitate, dry hydrated SiO 2.By the preparation method of the present invention, high structure, the hydrated SiO 2 of high abrasion can be prepared.
Description
Technical field
The present invention relates to organic matter preparation field, and in particular to a kind of preparation side of high structure high abrasion hydrated SiO 2
Method.
Background technology
Hydrated SiO 2, also known as light silicon dioxide, main component are silica, white amorphous powder, light weight
And it is loose, caustic alkali and hydrofluoric acid, water insoluble, solvent and acid can be dissolved in（Except hydrofluoric acid）.High temperature resistant, non-ignitable, tasteless, nothing
Smell, with good electrical insulating property.Its performance is similar to carbon black, but white.Molecular formula and structural formula can use SiO2·nH2O tables
Show, wherein nH2O is present in the form of surface hydroxyl.Its macrostructure is similar to carbon black, particle in spherical, list particle it
Between be in contact with face, in chain connecting structure（Secondary structure）.Chain branch structure forms round and round poly- again with hydrogen bond force phase separation
Collective.There is hydroxyl in hydrated SiO 2 microparticle surfaces, mainly there is isolation hydroxyl, adjacent hydroxyl groups, three kinds of siloxy.It is wherein adjacent
Absorption of the hydroxyl to polar substances is extremely important, and the presence of these groups makes its surface have a very strong hydrophily, surface area and point
Scattered ability is all larger, and mechanical strength and anti-tear index are very high.High temperature is not decomposed, and insulating properties is high, specific surface area small with particle
Greatly, structural high the features such as.However, in current production, hydrated SiO 2 is difficult to high structural.
The content of the invention
To solve defect present in above-mentioned prior art, the present invention provides a kind of high structure high abrasion hydrated SiO 2
Preparation method.
That is, the present invention provides a kind of preparation method of high structure high abrasion hydrated SiO 2, and it comprises the steps：
（1）By quartz sand and soda ash with 1:After 1.2-1.4 mol ratio is calcined 1 hour at 1420-1450 DEG C, solid-state silicic acid is obtained
Sodium；
（2）Solid-state sodium metasilicate is dissolved in concentration is 3-5mol/L sodium carbonate, sodium silicate solution is obtained, removal of impurities is gone in filtering
Matter；
（3）Dispersant is added into sodium silicate solution, under agitation, 4-6mol/L sulfuric acid is added dropwise into sodium silicate solution
Solution, there is Precipitation；
（4）By washing of precipitate, dry hydrated SiO 2.
Wherein, the dispersant is sodium lignin sulfonate.
In addition, the mol ratio of the sodium metasilicate, sodium carbonate, dispersant, sulfuric acid is 1: 1.2-1.5:0.2-0.5:1.2-
1.5。
In addition, the rate of addition of sulfuric acid solution is calculated as 5mol/h with sulfuric acid.
Sodium lignin sulfonate is a kind of natural polymerses, anionic surfactant, and it has very strong point
The ability of dissipating, suitable for solid is dispersed in aqueous medium.Disperseed due to the difference of molecular weight and functional group with different degrees of
Property, it can adsorb on the surface of various solid particles, metal ion exchanged effect can be carried out, also because existing in its institutional framework
Various active groups, thus condensation can be produced or occur hydrogen bond action with other compounds.Industrially, sodium lignin sulfonate
It is widely used as dispersant and wetting agent.
The present invention can prepare high structure by using sodium lignin sulfonate as dispersant, and by controlling sulfuric acid drop speed
Hydrated SiO 2, and find that the hydrated SiO 2 has high-wear resistance.
Embodiment
The present invention is described in detail with reference to embodiment, but the present invention and be not limited by the example, conventional technical means
Replacement belong to scope.
Embodiment 1
（1）After 5mol quartz sands and 6mol soda ash are calcined 1 hour at 1420 DEG C, solid-state sodium metasilicate is obtained；
（2）4.5mol solid-states sodium metasilicate is dissolved in 1.8L concentration is 3mol/L sodium carbonate, sodium silicate solution is obtained, filtered
Go the removal of impurity；
（3）0.9mol dispersants are added into sodium silicate solution, under agitation, are added dropwise 6mol/L's into sodium silicate solution
The common 1.125L of sulfuric acid solution, rate of addition is 5mol/L, there is Precipitation；
（4）By washing of precipitate, dry hydrated SiO 2.
Embodiment 2
（1）After 5mol quartz sands and 7mol soda ash are calcined 1 hour at 1450 DEG C, solid-state sodium metasilicate is obtained；
（2）4.5mol solid-states sodium metasilicate is dissolved in 1.35L concentration is 5mol/L sodium carbonate, sodium silicate solution, mistake is obtained
Filter off the removal of impurity；
（3）2.25mol dispersants are added into sodium silicate solution, under agitation, 4mol/L are added dropwise into sodium silicate solution
The common 1.35L of sulfuric acid solution, rate of addition is 5mol/h, there is Precipitation；
（4）By washing of precipitate, dry hydrated SiO 2.
Embodiment 3
（1）After 5mol quartz sands and 6.5mol soda ash are calcined 1 hour at 1450 DEG C, solid-state sodium metasilicate is obtained；
（2）4.5mol solid-states sodium metasilicate is dissolved in 1.575L concentration is 4mol/L sodium carbonate, sodium silicate solution, mistake is obtained
Filter off the removal of impurity；
（3）1.35mol dispersants are added into sodium silicate solution, under agitation, 5mol/L are added dropwise into sodium silicate solution
The common 1.26L of sulfuric acid solution, rate of addition is 5mol/h, there is Precipitation；
（4）By washing of precipitate, dry hydrated SiO 2.
70- is accounted for the ratio that hydrated SiO 2 resulting in embodiment 1-3 carries out the adjacent hydroxyl on structural analysis, silicon
90%, it is a kind of hydrated SiO 2 of high structure.
According to HG/T2404-2008《Identification of the hydrated SiO 2 in butadiene-styrene rubber》Carry out rubber processing.According to GB/
T531 determines shore hardness, determines tearing strength according to GB/T529.Commercially available hydrated SiO 2 is comparative example.With embodiment 1-3
And the hydrated SiO 2 in comparative example is filler, with butadiene-styrene rubber and accelerator, coupling agent etc. by kneading into tire tread glue,
Then high temperature vulcanized shaping.Treadwear indexes are determined, it is as a result as shown in the table.
Table 1
As shown in Table 1, hydrated SiO 2 produced by the present invention has high-wearing feature while high structure.
Claims (4)
1. a kind of preparation method of high structure high abrasion hydrated SiO 2, it is characterised in that comprise the steps：
（1）By quartz sand and soda ash with 1:After 1.2-1.4 mol ratio is calcined 1 hour at 1420-1450 DEG C, solid-state silicic acid is obtained
Sodium；
（2）Solid-state sodium metasilicate is dissolved in concentration is 3-5mol/L sodium carbonate, sodium silicate solution is obtained, removal of impurities is gone in filtering
Matter；
（3）Dispersant is added into sodium silicate solution, under agitation, 4-6mol/L sulfuric acid is added dropwise into sodium silicate solution
Solution, there is Precipitation；
（4）By washing of precipitate, dry hydrated SiO 2.
2. preparation method according to claim 1, it is characterised in that the dispersant is sodium lignin sulfonate.
3. preparation method according to claim 1, it is characterised in that the sodium metasilicate, sodium carbonate, dispersant, sulfuric acid
Mol ratio is 1: 1.2-1.5:0.2-0.5:1.2-1.5.
4. preparation method according to claim 1, it is characterised in that the rate of addition of sulfuric acid solution is calculated as with sulfuric acid
5mol/h。
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| CN201710451487.9A CN107162009B (en) | 2017-06-15 | 2017-06-15 | Preparation method of high-structure high-wear-resistance hydrated silicon dioxide |
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| CN201710451487.9A CN107162009B (en) | 2017-06-15 | 2017-06-15 | Preparation method of high-structure high-wear-resistance hydrated silicon dioxide |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109205632A (en) * | 2018-09-19 | 2019-01-15 | 安徽龙泉硅材料有限公司 | The ultrapure sodium metasilicate of delustering agent |
| CN114516637A (en) * | 2022-03-24 | 2022-05-20 | 福建省三明同晟化工有限公司 | High additive feed additive silicon dioxide and preparation method thereof |
| CN114560471A (en) * | 2022-03-25 | 2022-05-31 | 福建省三明同晟化工有限公司 | Silica for wear-resistant tire rubber and preparation method thereof |
| CN114804121A (en) * | 2022-03-24 | 2022-07-29 | 福建省三明同晟化工有限公司 | Preparation method of silica for glass cement for shoes |
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| US3219590A (en) * | 1961-08-01 | 1965-11-23 | Union Carbide Corp | Bonded molecular sieves |
| CN101172608A (en) * | 2006-10-31 | 2008-05-07 | 中南大学 | Method of producing high-specific area nano-silicon dioxide |
| CN103466637A (en) * | 2013-08-29 | 2013-12-25 | 中国科学院过程工程研究所 | Method for producing precipitate silicon dioxide by using sodium bicarbonate to control supersaturation degree |
| CN103754885A (en) * | 2014-01-26 | 2014-04-30 | 乌鲁木齐金石徽龙矿业有限公司 | Method for preparing porous silicon dioxide in acid leaching way |
| CN106276929A (en) * | 2016-07-29 | 2017-01-04 | 广州市飞雪材料科技有限公司 | A kind of preparation method of the type silicon dioxide that rubs |
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2017
- 2017-06-15 CN CN201710451487.9A patent/CN107162009B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3219590A (en) * | 1961-08-01 | 1965-11-23 | Union Carbide Corp | Bonded molecular sieves |
| CN101172608A (en) * | 2006-10-31 | 2008-05-07 | 中南大学 | Method of producing high-specific area nano-silicon dioxide |
| CN103466637A (en) * | 2013-08-29 | 2013-12-25 | 中国科学院过程工程研究所 | Method for producing precipitate silicon dioxide by using sodium bicarbonate to control supersaturation degree |
| CN103754885A (en) * | 2014-01-26 | 2014-04-30 | 乌鲁木齐金石徽龙矿业有限公司 | Method for preparing porous silicon dioxide in acid leaching way |
| CN106276929A (en) * | 2016-07-29 | 2017-01-04 | 广州市飞雪材料科技有限公司 | A kind of preparation method of the type silicon dioxide that rubs |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109205632A (en) * | 2018-09-19 | 2019-01-15 | 安徽龙泉硅材料有限公司 | The ultrapure sodium metasilicate of delustering agent |
| CN114516637A (en) * | 2022-03-24 | 2022-05-20 | 福建省三明同晟化工有限公司 | High additive feed additive silicon dioxide and preparation method thereof |
| CN114804121A (en) * | 2022-03-24 | 2022-07-29 | 福建省三明同晟化工有限公司 | Preparation method of silica for glass cement for shoes |
| CN114560471A (en) * | 2022-03-25 | 2022-05-31 | 福建省三明同晟化工有限公司 | Silica for wear-resistant tire rubber and preparation method thereof |
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| CN107162009B (en) | 2020-03-17 |
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