CN108996510A - The preparation method of dustless easy dispersed silicon dioxide - Google Patents
The preparation method of dustless easy dispersed silicon dioxide Download PDFInfo
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- CN108996510A CN108996510A CN201810660625.9A CN201810660625A CN108996510A CN 108996510 A CN108996510 A CN 108996510A CN 201810660625 A CN201810660625 A CN 201810660625A CN 108996510 A CN108996510 A CN 108996510A
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- Prior art keywords
- preparation
- silicon dioxide
- dispersed silicon
- dustless
- easy dispersed
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of preparation methods of dustless easy dispersed silicon dioxide, comprising the following steps: (1), by diatomite is immersed in 0.02ml/L~0.1ml/L ammonium fluoride aqueous solution, back flow reaction 7~10 hours at 80~90 DEG C；(2), acid solution is added dropwise into step (1) reaction solution, adjusting pH value is 4~6, is stirred evenly；(3), stand, filter to obtain precipitating, it is dry.Preparation method of the present invention is simple, and process stabilizing, condition is controllable, and production cost is low, low in the pollution of the environment, can industrialized production, can effectively improve silica in water with the dispersibility in nonpolar solvent.
Description
Technical field
The present invention relates to silica preparation technical field, especially a kind of preparation side of dustless easy dispersed silicon dioxide
Method.
Background technique
Silica is manufacture glass, quartz glass, waterglass, optical fiber, the important component of electronics industry, optics instrument
The raw material of device, craftwork and refractory material is the important materials of scientific research.In recent years, silica is used for battery separator
Material, partition pore-forming are made up of silica micropore itself and pore former the hole left after extraction or volatilization,
This porous and detour structure, it is desirable that the advantages that its specific surface area is low, electrolyte storage characteristics are good.Silica has greatly well
Tackifying effect is widely used in all trades and professions because it is with very high electrical insulating property and good dispersibility.To meet different use
The requirement of the silica on way, certain fields require the dispersibility of silica high, and dispersed quality is to measure silica etc.
One important indicator of grade.
There are mainly two types of the production methods of silica: vapor phase method and the precipitation method, and the silica of vapor phase method production is general
Physical and chemical performance is all fine, but vapor phase method raw material are expensive, equipment requirement is high, technology is complicated, low output.The precipitation method mostly use sulphur
Acid or hydrochloric acid and sodium metasilicate carry out neutralization reaction, and simple process, equipment and raw material are cheap, but product quality has with vapor phase method
Larger difference.There are many precipitated silica manufacturers in the country, but most of product is all located in conventional tyre and system
Collar domain, belongs to general silica.
Summary of the invention
It is at low cost in view of the deficiencies of the prior art, the present invention proposes a kind of preparation method of dustless easy dispersed silicon dioxide
Honest and clean, operating procedure is simple and production process non-pollutant discharge.
In order to achieve the above-mentioned object of the invention, the present invention is the following technical schemes are provided: a kind of dustless easy dispersed silicon dioxide
Preparation method, comprising the following steps:
(1), diatomite is immersed in 0.02ml/L~0.1ml/L ammonium fluoride aqueous solution, the back flow reaction at 80~90 DEG C
7~10 hours；
(2), acid solution is added dropwise into step (1) reaction solution, adjusting pH value is 4~6, is stirred evenly；
(3), stand, filter to obtain precipitating, it is dry.
Further, (3) sediment is handled step through depickling.
Further, the diatomite is that partial size is less than 5mm.
Further, the acid solution that (3) is step is added dropwise the sulfuric acid solution of 1~1.5mol/L.
Further, step (3) washed by sediment, until conductivity is not more than 20000 μ s.
Compared with prior art, the invention has the following advantages that preparation method is simple, process stabilizing, condition is controllable, production
It is at low cost, it is low in the pollution of the environment, can industrialized production, can effectively improve silica in water with the dispersion in nonpolar solvent
Property.Silica produced by the present invention is high with the dispersibility in nonpolar solvent (such as n-hexane) in water, partial size at 4-7 μm,
Oil factor is 150~200ml/100g, apparent density≤0.2g/mL, specific surface area 300-450 ㎡/g, pH value in 6.5-8.5,
Dioxide-containing silica >=99%；Product can be applied to daily use chemicals industry and do supporting surfactant or divide applied to pharmaceuticals industry
Powder.
Specific embodiment
Below with reference to embodiment, the present invention will be described in detail, the description of this part be only it is exemplary and explanatory, no
Reply protection scope of the present invention has any restriction effect.
Embodiment 1
A kind of preparation method of dustless easy dispersed silicon dioxide, comprising the following steps:
(1), the diatomite that partial size is 3mm is immersed in 0.02ml/L ammonium fluoride aqueous solution, the back flow reaction 7 at 90 DEG C
Hour；
(2), the sulfuric acid solution of 1mol/L is added dropwise into step (1) reaction solution, adjusting pH value is 6, is stirred evenly；
(3), stand, filter to obtain precipitating, it is dry.
Embodiment 2
A kind of preparation method of dustless easy dispersed silicon dioxide, comprising the following steps:
(1), the diatomite that partial size is 2mm is immersed in 0.1ml/L ammonium fluoride aqueous solution, the back flow reaction 10 at 80 DEG C
Hour；
(2), the sulfuric acid solution of 1.5mol/L is added dropwise into step (1) reaction solution, adjusting pH value is 4, is stirred evenly；
(3), stand, filter to precipitate, sediment is handled through depickling, dry.
Further, step (3) washed by sediment, until conductivity is not more than 20000 μ s.
Embodiment 3
A kind of preparation method of dustless easy dispersed silicon dioxide, comprising the following steps:
(1), the diatomite that partial size is 4mm is immersed in 0.06ml/L ammonium fluoride aqueous solution, the back flow reaction 8 at 85 DEG C
Hour；
(2), the sulfuric acid solution of 1.2mol/L is added dropwise into step (1) reaction solution, adjusting pH value is 5, is stirred evenly；
(3), standing, filter to precipitate, sediment is washed, until conductivity is not more than 20000 μ s, it is dry.
Above-described embodiment product obtained is tested and analyzed, the result is as follows:
As seen from the above table, the dispersibility of silica obtained by each embodiment is high, and purity is high is applicable in and is applied to excipient substance
In, it is also applied for industrial production.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (5)
1. a kind of preparation method of dustless easy dispersed silicon dioxide, it is characterised in that: the following steps are included:
(1), diatomite is immersed in 0.02ml/L~0.1ml/L ammonium fluoride aqueous solution, at 80~90 DEG C back flow reaction 7~
10 hours；
(2), acid solution is added dropwise into step (1) reaction solution, adjusting pH value is 4~6, is stirred evenly；
(3), stand, filter to obtain precipitating, it is dry.
2. the preparation method of dustless easy dispersed silicon dioxide as described in claim 1, it is characterised in that: (3) sediment warp is de- for step
Acid processing.
3. the preparation method of dustless easy dispersed silicon dioxide as claimed in claim 2, it is characterised in that: the diatomite is partial size
Less than 5mm.
4. the preparation method of dustless easy dispersed silicon dioxide as described in claim 1, it is characterised in that: (3) acid solution that step is added dropwise
For the sulfuric acid solution of 1~1.5mo l/L.
5. the preparation method of dustless easy dispersed silicon dioxide as described in claim 1, it is characterised in that: (3) sediment carries out step
Washing, until conductivity is not more than 20000 μ s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810660625.9A CN108996510A (en) | 2018-06-25 | 2018-06-25 | The preparation method of dustless easy dispersed silicon dioxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810660625.9A CN108996510A (en) | 2018-06-25 | 2018-06-25 | The preparation method of dustless easy dispersed silicon dioxide |
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| Publication Number | Publication Date |
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| CN108996510A true CN108996510A (en) | 2018-12-14 |
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| CN201810660625.9A Pending CN108996510A (en) | 2018-06-25 | 2018-06-25 | The preparation method of dustless easy dispersed silicon dioxide |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2785953A (en) * | 1954-08-04 | 1957-03-19 | Grace W R & Co | Process for preparing a dry mixture of ammonium fluosilicate and silica |
| CN87105499A (en) * | 1987-08-03 | 1988-09-21 | 金凌石油化工公司南京炼油厂 | Production method of binder-free spherical model-a molecular sieves |
| CN1036746A (en) * | 1989-03-13 | 1989-11-01 | 重庆市化工研究院 | Produce the novel process of white carbon black with silica sand |
| FR2883278B1 (en) * | 2005-03-21 | 2007-05-04 | Rhodia Chimie Sa | FLUORINATED PRECIPITATED SILICA WITH LOW WATER RESPONSE, PREPARATION METHOD AND USES, IN PARTICULAR AS LOAD IN SILICONE MATRICES |
| CN101028930A (en) * | 2006-03-01 | 2007-09-05 | 多氟多化工股份有限公司 | Method for linked producing ammonium fluoride and white carbon black |
| CN102874821A (en) * | 2012-10-31 | 2013-01-16 | 天津舜能润滑科技股份有限公司 | Preparation method of high-purity silicon dioxide |
| CN102951611A (en) * | 2012-12-24 | 2013-03-06 | 贵州省化工研究院 | Method for preparing anhydrous hydrogen fluoride by utilizing fluorine-containing waste liquid or fluorosilicic acid in phosphate fertilizer enterprises |
| CN102951649A (en) * | 2012-11-15 | 2013-03-06 | 北京橡胶工业研究设计院 | Preparation method of modified precipitated white carbon black |
| CN108101069A (en) * | 2017-12-28 | 2018-06-01 | 天津普恒康泰科技有限公司 | A kind of exhaust gas produces ammonium fluosilicate co-producing white carbon black raw material process after recycling |
-
2018
- 2018-06-25 CN CN201810660625.9A patent/CN108996510A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2785953A (en) * | 1954-08-04 | 1957-03-19 | Grace W R & Co | Process for preparing a dry mixture of ammonium fluosilicate and silica |
| CN87105499A (en) * | 1987-08-03 | 1988-09-21 | 金凌石油化工公司南京炼油厂 | Production method of binder-free spherical model-a molecular sieves |
| CN1036746A (en) * | 1989-03-13 | 1989-11-01 | 重庆市化工研究院 | Produce the novel process of white carbon black with silica sand |
| FR2883278B1 (en) * | 2005-03-21 | 2007-05-04 | Rhodia Chimie Sa | FLUORINATED PRECIPITATED SILICA WITH LOW WATER RESPONSE, PREPARATION METHOD AND USES, IN PARTICULAR AS LOAD IN SILICONE MATRICES |
| CN101028930A (en) * | 2006-03-01 | 2007-09-05 | 多氟多化工股份有限公司 | Method for linked producing ammonium fluoride and white carbon black |
| CN102874821A (en) * | 2012-10-31 | 2013-01-16 | 天津舜能润滑科技股份有限公司 | Preparation method of high-purity silicon dioxide |
| CN102951649A (en) * | 2012-11-15 | 2013-03-06 | 北京橡胶工业研究设计院 | Preparation method of modified precipitated white carbon black |
| CN102951611A (en) * | 2012-12-24 | 2013-03-06 | 贵州省化工研究院 | Method for preparing anhydrous hydrogen fluoride by utilizing fluorine-containing waste liquid or fluorosilicic acid in phosphate fertilizer enterprises |
| CN108101069A (en) * | 2017-12-28 | 2018-06-01 | 天津普恒康泰科技有限公司 | A kind of exhaust gas produces ammonium fluosilicate co-producing white carbon black raw material process after recycling |
Non-Patent Citations (1)
| Title |
|---|
| 中国航海学会危险货物运输专业委员会: "《危险货物运输安全技术手册》", 30 April 1994, 中国标准出版社 * |
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Application publication date: 20181214 |