CN107140646A - A kind of method that pH value swing method prepares big pore volume hydrated SiO 2 - Google Patents
A kind of method that pH value swing method prepares big pore volume hydrated SiO 2 Download PDFInfo
- Publication number
- CN107140646A CN107140646A CN201710452069.1A CN201710452069A CN107140646A CN 107140646 A CN107140646 A CN 107140646A CN 201710452069 A CN201710452069 A CN 201710452069A CN 107140646 A CN107140646 A CN 107140646A
- Authority
- CN
- China
- Prior art keywords
- hydrated sio
- value
- pore volume
- minutes
- sulfuric acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- C01B33/126—Preparation of silica of undetermined type
- C01B33/128—Preparation of silica of undetermined type by acidic treatment of aqueous silicate solutions
-
- 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
-
- 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
- C01P2006/14—Pore volume
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a kind of method that pH value swing method prepares big pore volume hydrated SiO 2, it is characterised in that comprises the steps：（1）Add mass fraction into reactor to stir for 7% 10% sodium silicate solution and dispersant, oil bath is to 80 90 DEG C；（2）It is 9 10 with ammoniacal liquor regulation pH value, stablizes 20 minutes；（3）It is 34 that sulfuric acid solution to pH value, which is added dropwise, is stablized 10 minutes；（4）Repeat the above steps（2）With（3）Totally three times；（5）By sediment undergoes washing, drying, hydrated SiO 2 is obtained.The method of the present invention for preparing hydrated SiO 2 is pH value swing method, and this method hydrated SiO 2 simple to operate and obtained has the excellent properties such as big pore volume, high dispersive.
Description
Technical field
The present invention relates to field of chemical preparation, and in particular to a kind of pH value swing method prepares big pore volume hydrated SiO 2
Method.
Background technology
Hydrated SiO 2 also known as white carbon, 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, no
Combustion, it is tasteless, odorless, with good electrical insulating property.
At present, the preparation method of hydrated SiO 2 has vapor phase method, the precipitation method.Vapor phase method is the chlorination of chloride four with silicon
Silicon or trichlorine monomethyl silane are raw material, are produced using flame hydrolysis, burnt the 1000 DEG C of high-temperature water vapors to be formed by hydrogen, oxygen
Hydrolysis is obtained.Importance of the precipitation method hydrated SiO 2 in synthetic silica ranks first, and it is by waterglass
（Na2SiO3）Acted on sulfuric acid or hydrochloric acid, generate silicic acid, then decompose and white carbon is made.
Vapor phase method and the precipitation method however as described above has deficiency, although such as vapor phase method hydrated SiO 2 property
Can be good, but preparation method is complicated, it is not easy to operate；Although precipitation method hydrated SiO 2 is prepared simply, performance is not ideal enough, example
Such as pore volume and dispersiveness not enough rationality.
The content of the invention
According to the above-mentioned state of the art, the present invention provides a kind of preparation method of new hydrated SiO 2.
Specifically, the present invention provides a kind of method that pH value swing method prepares big pore volume hydrated SiO 2, under it includes
State step：
（1）Add mass fraction into reactor to stir for 7%-10% sodium silicate solution and dispersant, oil bath to 80-90
℃；
（2）It is 9-10 with ammoniacal liquor regulation pH value, stablizes 20 minutes；
（3）It is 3-4 that sulfuric acid solution to pH value, which is added dropwise, is stablized 10 minutes；
（4）Repeat the above steps（2）With（3）Totally three times；
（5）By sediment undergoes washing, drying, hydrated SiO 2 is obtained.
Wherein, the dispersant is the 2-3% of sodium silicate solution weight.
In addition, the dispersant is one kind in sodium citrate, Sodium Toluene Sulphonate.
In addition, the mass fraction of the sulfuric acid solution is 5-10%.
In addition, the rate of addition of the sulfuric acid is 0.5-0.8L/ hours.
Hydrated SiO 2 preparation method of the present invention is simple, and obtained hydrated SiO 2 performance is good, especially disperses
Property it is good, and with big pore volume.
Embodiment
With reference to being described in detail to the present invention in conjunction with the embodiments, but the present invention is not limited to these embodiments, ability
The change of conventional technical means is within domain.
Embodiment 1
（1）Add 2L mass fractions into reactor to stir for 7% sodium silicate solution and 40g sodium citrates, oil bath to 80
℃；
（2）It is 9-10 with ammoniacal liquor regulation pH value, stablizes 20 minutes；
（3）Sulfuric acid solution that mass fraction is 5% was added dropwise to pH value as 3-4 using the speed of 0.5L/ hours, stablized 10 minutes；
（4）Repeat the above steps（2）With（3）Totally three times；
（5）By sediment undergoes washing, drying, hydrated SiO 2 is obtained.
Embodiment 2
（1）Add 2L mass fractions into reactor to stir for 10% sodium silicate solution and 60g Sodium Toluene Sulphonates, oil
Bath is to 90 DEG C；
（2）It is 9-10 with ammoniacal liquor regulation pH value, stablizes 20 minutes；
（3）Sulfuric acid solution that mass fraction is 10% was added dropwise to pH value as 3-4 using the speed of 0.8L/ hours, stablized 10 minutes；
（4）Repeat the above steps（2）With（3）Totally three times；
（5）By sediment undergoes washing, drying, hydrated SiO 2 is obtained.
Embodiment 3
（1）Add 2L mass fractions into reactor to stir for 8% sodium silicate solution and 50g Sodium Toluene Sulphonates, oil bath
To 80 DEG C；
（2）It is 9-10 with ammoniacal liquor regulation pH value, stablizes 20 minutes；
（3）Sulfuric acid solution that mass fraction is 8% was added dropwise to pH value as 3-4 using the speed of 0.6L/ hours, stablized 10 minutes；
（4）Repeat the above steps（2）With（3）Totally three times；
（5）By sediment undergoes washing, drying, hydrated SiO 2 is obtained.
Embodiment 4
（1）Add 2L mass fractions into reactor to stir for 7% sodium silicate solution and 50g sodium citrates, oil bath to 90
℃；
（2）It is 9-10 with ammoniacal liquor regulation pH value, stablizes 20 minutes；
（3）Sulfuric acid solution that mass fraction is 7% was added dropwise to pH value as 3-4 using the speed of 0.6L/ hours, stablized 10 minutes；
（4）Repeat the above steps（2）With（3）Totally three times；
（5）By sediment undergoes washing, drying, hydrated SiO 2 is obtained.
Comparative example
Using conventional white carbon as comparative example, hydrated SiO 2 is made with each performance measurement of the same terms progress with embodiment 1-4,
As a result it is as shown in table 1.
Obtained hydrated SiO 2 in embodiment 1-4 is subjected to performance test with following each methods
Specific surface area is tested：According to GB/T3073-1999《The measure N2 adsorption method of precipitated hydrated silica specific surface area》
The specific surface area of measure.Also, with carbon tetrachloride determination of adsorption method pore volume.
According to HG/T2404-2008《Identification of the precipitated hydrated silica in butadiene-styrene rubber》Carry out rubber processing.According to
GB/T531 determines shore hardness, determines tearing strength according to GB/T529.
The hydrated SiO 2 as made from preparation method of the present invention it can be seen from above-described embodiment and comparative example,
While possessing normal mechanical property such as shore hardness and tearing strength, specific surface area is big, pore volume is big, it may be said that be a kind of big
The white carbon of pore volume high dispersive.
Claims (5)
1. a kind of method that pH value swing method prepares big pore volume hydrated SiO 2, it is characterised in that comprise the steps：
（1）Add mass fraction into reactor to stir for 7%-10% sodium silicate solution and dispersant, oil bath to 80-90
℃；
（2）It is 9-10 with ammoniacal liquor regulation pH value, stablizes 20 minutes；
（3）It is 3-4 that sulfuric acid solution to pH value, which is added dropwise, is stablized 10 minutes；
（4）Repeat the above steps（2）With（3）Totally three times；
（5）By sediment undergoes washing, drying, hydrated SiO 2 is obtained.
2. according to the method described in claim 1, it is characterised in that the dispersant is the 2-3% of sodium silicate solution weight.
3. method according to claim 2, it is characterised in that the dispersant is in sodium citrate, Sodium Toluene Sulphonate
One kind.
4. according to the method described in claim 1, it is characterised in that the mass fraction of the sulfuric acid solution is 5-10%.
5. according to the method described in claim 1, it is characterised in that the rate of addition of the sulfuric acid is 0.5-0.8L/ hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710452069.1A CN107140646B (en) | 2017-06-15 | 2017-06-15 | A kind of method that pH value swing method prepares macropore appearance hydrated SiO 2 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710452069.1A CN107140646B (en) | 2017-06-15 | 2017-06-15 | A kind of method that pH value swing method prepares macropore appearance hydrated SiO 2 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107140646A true CN107140646A (en) | 2017-09-08 |
| CN107140646B CN107140646B (en) | 2019-08-23 |
Family
ID=59782869
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710452069.1A Active CN107140646B (en) | 2017-06-15 | 2017-06-15 | A kind of method that pH value swing method prepares macropore appearance hydrated SiO 2 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107140646B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108439414A (en) * | 2018-02-11 | 2018-08-24 | 确成硅化学股份有限公司 | A kind of method that pH value swing method prepares high dispersive macropore appearance precipitated silica |
| CN110054193A (en) * | 2019-06-05 | 2019-07-26 | 确成硅化学股份有限公司 | A kind of preparation method of high-dispersion high-thermal-conductivity white carbon black |
| CN111153411A (en) * | 2020-01-13 | 2020-05-15 | 福建省三明正元化工有限公司 | Preparation method of silicon dioxide with excellent physical application performance |
| CN113753905A (en) * | 2021-09-27 | 2021-12-07 | 无锡恒诚硅业有限公司 | Preparation method of high-dispersion white carbon black |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102451707A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Method for preparing hydrotreating catalyst composition |
| CN102451705A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Preparation method of hydrotreatment catalyst composition |
| CN103769147A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Preparation method of hydrogenation catalyst |
| CN103769232A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Preparation method of alumina dry glue containing silicon |
| CN103787342A (en) * | 2012-11-03 | 2014-05-14 | 中国石油化工股份有限公司 | Preparation method of high-silicon macroporous amorphous silicon aluminum dry glue by utilization of carbonation method |
-
2017
- 2017-06-15 CN CN201710452069.1A patent/CN107140646B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102451707A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Method for preparing hydrotreating catalyst composition |
| CN102451705A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Preparation method of hydrotreatment catalyst composition |
| CN103769147A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Preparation method of hydrogenation catalyst |
| CN103769232A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Preparation method of alumina dry glue containing silicon |
| CN103787342A (en) * | 2012-11-03 | 2014-05-14 | 中国石油化工股份有限公司 | Preparation method of high-silicon macroporous amorphous silicon aluminum dry glue by utilization of carbonation method |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108439414A (en) * | 2018-02-11 | 2018-08-24 | 确成硅化学股份有限公司 | A kind of method that pH value swing method prepares high dispersive macropore appearance precipitated silica |
| CN110054193A (en) * | 2019-06-05 | 2019-07-26 | 确成硅化学股份有限公司 | A kind of preparation method of high-dispersion high-thermal-conductivity white carbon black |
| CN111153411A (en) * | 2020-01-13 | 2020-05-15 | 福建省三明正元化工有限公司 | Preparation method of silicon dioxide with excellent physical application performance |
| CN111153411B (en) * | 2020-01-13 | 2023-10-24 | 福建省三明正元化工有限公司 | Preparation method of silicon dioxide |
| CN113753905A (en) * | 2021-09-27 | 2021-12-07 | 无锡恒诚硅业有限公司 | Preparation method of high-dispersion white carbon black |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107140646B (en) | 2019-08-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107140646A (en) | A kind of method that pH value swing method prepares big pore volume hydrated SiO 2 | |
| US10556800B2 (en) | Method of preparing metal oxide-silica composite aerogel and metal oxide-silica composite aerogel prepared thereby | |
| US20190309190A1 (en) | Modified colloidal silica and method for producing the same, and polishing agent using the same | |
| TWI549911B (en) | High purity silica sol and its production method | |
| US10792650B2 (en) | Method of preparing metal oxide-silica composite aerogel and metal oxide-silica composite aerogel prepared thereby | |
| KR100997410B1 (en) | method for preparing silica aerogel | |
| KR101703849B1 (en) | Eco-friendly Method for producing of silica using ionic liquids | |
| CN103466640B (en) | A kind of method reducing the standby white carbon black specific surface area BET of sulfuric acid precipitation legal system | |
| CN106315596B (en) | A kind of production technology of low CTAB specific surface areas low-heat-generation white carbon | |
| CN104650432B (en) | Modification method of nano white carbon black used as rubber additive | |
| CN100381526C (en) | Composition for forming porous film, porous film and method for forming the same, interlevel insulator film and semiconductor device | |
| CN101172610B (en) | Method of producing high-temperature silica powder | |
| CN106277750A (en) | The preparation method of quartz glass | |
| JPH04300206A (en) | Purification of silicon chloride | |
| KR20060097223A (en) | Manufacturing method for spherical silica | |
| CN104891504A (en) | A method of extracting white carbon black from coal cinder | |
| CN102795787B (en) | Super-hydrophobic silica coating is prepared with water glass | |
| TW201404718A (en) | Method of purifying inorganic salt and use thereof | |
| CN103435059B (en) | Method for bulking artificially synthesized fluorophlogopite sheet | |
| JP6047395B2 (en) | High purity silica sol and method for producing the same | |
| JP4065757B2 (en) | External toner additive | |
| CN103739010A (en) | Method for deep desilication in acid system by silica sol | |
| CN115849387B (en) | Method for preparing silica gel by utilizing steel slag powder | |
| TWI730259B (en) | Treatment liquid and treatment method | |
| JPS61209909A (en) | Production of colloidal silica for polishing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |