CN108993413B - Preparation method of amino modified precipitated silica - Google Patents
Preparation method of amino modified precipitated silica Download PDFInfo
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- CN108993413B CN108993413B CN201810823990.7A CN201810823990A CN108993413B CN 108993413 B CN108993413 B CN 108993413B CN 201810823990 A CN201810823990 A CN 201810823990A CN 108993413 B CN108993413 B CN 108993413B
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28059—Surface area, e.g. B.E.T specific surface area being less than 100 m2/g
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention belongs to the field of preparation of new materials, and relates to a preparation method of amino modified precipitated silica. According to the method, the amino modified precipitated silica is prepared by coprecipitation of a silicon source and an amino modifier under an alkaline condition, so that the performance of the precipitated silica is improved, and the application of the precipitated silica is widened. The surface chemical structure of the precipitated silica is changed through amino functionalization, the bonding performance of the precipitated silica and rubber can be improved, the application field of the precipitated silica is expanded, and the precipitated silica can be used for adsorbing carbon dioxide, formaldehyde and heavy metal ions by virtue of the function of amino groups.
Description
Technical Field
The invention belongs to the field of preparation of new materials, and particularly relates to a preparation method of amino modified precipitated silica.
Background
The precipitated silica is a general name of anhydrous and hydrous silica in fine powder or ultrafine particle form or silicate substances, is a second largest rubber reinforcing filler next to carbon black, and can also be used in the fields of plastics, rubber products, papermaking, coatings, cosmetics, inks and the like, but the precipitated silica is used in the fields with lower added value. In addition, when the precipitated silica is used for reinforcing rubber, a silane coupling agent is required to be added to improve the bonding performance of the precipitated silica and the rubber.
Disclosure of Invention
In order to improve the defects of the precipitated silica in the aspects of structure and application, the invention provides a preparation method of amino modified precipitated silica, which realizes the preparation of the amino modified precipitated silica by coprecipitation of a silicon source and an amino modifier.
The technical scheme of the invention comprises the following steps: a preparation method of amino modified precipitated silica comprises the following specific steps:
(1) mixing a solvent, ammonia water, deionized water, a silicon source, an amino modifier and a precipitation promoter, and stirring to obtain a precipitate, wherein the raw materials comprise the following silicon sources: amino modifier: solvent: deionized water: ammonia water: the volume ratio of the precipitation promoter is 1: (0.1-10): (1-5): (1-3): (0.3-0.6): (0.1 to 0.3);
(2) and (2) filtering and washing the precipitate in the step (1), and drying to obtain the amino modified precipitated silica.
Preferably, the solvent in step (1) is one of methanol, ethanol or isopropanol. Preferably, the mass concentration of the ammonia water in the step (1) is 25-28%.
Preferably, the silicon source in step (1) is one of tetramethyl orthosilicate and tetraethyl orthosilicate.
Preferably, the amino modifier in step (1) is one of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, 3-ureidopropyltriethoxysilane, N-aminoethyl-gamma-aminopropyltriethoxysilane or m-aminophenyltrimethoxysilane.
Preferably, the precipitation promoter in step (1) is one of zirconium n-propoxide, zirconium isopropoxide, tetraethyl titanate, tetrabutyl titanate or titanium tetrachloride.
Preferably, the stirring temperature in the step (1) is 0-60 ℃, and the stirring time is 1-24 hours.
Preferably, the filtration in the step (2) is one of centrifugal filtration, suction filtration or pressure filtration.
Preferably, the washing in the step (2) is one of water washing or ethanol washing; the number of washing times is 3 to 5.
Preferably, the drying in step (2) is one of atmospheric drying, vacuum drying, supercritical drying, freeze drying or spray drying.
Has the advantages that:
the amino modified precipitated silica is an improvement on the traditional precipitated silica, the surface chemical structure of the precipitated silica is changed through amino functionalization, the bonding performance of the precipitated silica and rubber can be improved, the application field of the precipitated silica is expanded, and the precipitated silica can be used for adsorbing carbon dioxide, formaldehyde and heavy metal ions by virtue of the function of amino groups.
Drawings
FIG. 1 is an SEM photograph of the amino-modified precipitated silica prepared in example 1.
Detailed Description
Example 1
Mixing 500ml of methanol, 30mml of concentrated ammonia water (mass concentration is 25 percent), 100ml of deionized water, 100ml of tetramethyl orthosilicate, 10ml of 3-aminopropyltrimethoxysilane and 10ml of zirconium n-propoxide, stirring for 24 hours at 0 ℃ to obtain a precipitate, centrifugally filtering and washing the precipitate for 3 times, and drying the precipitate at normal pressure to obtain the amino modified precipitated silica, wherein the specific surface area of the sample is 50m2/g。
Referring to the drawings, FIG. 1 is a scanning electron micrograph of amino-modified precipitated silica prepared according to example 1. The scanning electron microscope test adopts a Zeiss 1530VP scanning electron microscope. It can be seen that the amino-modified precipitated silica particles prepared by the present invention have both submicron particles of several hundred nanometers and smaller nanoparticles.
Example 2
Mixing 100ml of ethanol, 60ml of concentrated ammonia water (mass concentration is 25 percent), 300ml of deionized water, 100ml of tetraethyl orthosilicate, 1000ml of 3-aminopropyltriethoxysilane and 30ml of zirconium isopropoxide, stirring for 1 hour at 60 ℃ to obtain a precipitate, carrying out suction filtration and ethanol washing for 5 times on the precipitate, and then carrying out vacuum drying to obtain amino modified precipitated silica, wherein the specific surface area of the sample is 28m2/g。
Example 3
200ml of isopropanol, 60ml of concentrated ammonia water (mass concentration of 28 percent), 300ml of deionized water, 100ml of tetraethyl orthosilicate, 500ml of 3-urea propyl triethoxysilane and 20ml of tetraethyl titanate are mixed and stirred for 4 hours at 20 ℃ to obtain precipitate, the precipitate is subjected to pressure filtration and ethanol washing for 5 times, and then subjected to supercritical drying to obtain amino modified precipitated silica, and a sample is obtainedSpecific surface area of 452m2/g。
Example 4
300ml of ethanol, 40ml of concentrated ammonia water (mass concentration of 28 percent), 200ml of deionized water, 100ml of tetramethyl orthosilicate, 100ml of N-aminoethyl-gamma-aminopropyltriethoxysilane and 20ml of tetrabutyl titanate are mixed and stirred for 12 hours at 40 ℃ to obtain precipitate, the precipitate is subjected to suction filtration and water washing for 4 times, and then spray drying is carried out to obtain amino modified precipitated silica, the specific surface area of the sample is 149m2/g。
Example 5
Mixing 400ml of isopropanol, 50ml of concentrated ammonia water (mass concentration is 25 percent), 200ml of deionized water, 100ml of tetraethyl orthosilicate, 300ml of m-aminophenyl trimethoxy silane and 10ml of titanium tetrachloride, stirring for 8 hours at 30 ℃ to obtain precipitate, carrying out suction filtration and water washing on the precipitate for 3 times, and then carrying out freeze drying to obtain amino modified precipitated silica, wherein the specific surface area of a sample is 84m2/g。
Claims (8)
1. A preparation method of amino modified precipitated silica comprises the following specific steps:
(1) mixing a solvent, ammonia water, deionized water, a silicon source, an amino modifier and a precipitation promoter, and stirring to obtain a precipitate, wherein the raw materials comprise the following silicon sources: amino modifier: solvent: deionized water: ammonia water: the volume ratio of the precipitation promoter is 1: (0.1-10): (1-5): (1-3): (0.3-0.6): (0.1 to 0.3); wherein the amino modifier is one of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, 3-urea propyl triethoxysilane, N-aminoethyl-gamma-aminopropyltriethoxysilane or m-aminophenyl trimethoxysilane; the precipitation accelerator is one of zirconium n-propoxide, zirconium isopropoxide, tetraethyl titanate, tetrabutyl titanate or titanium tetrachloride;
(2) and (2) filtering and washing the precipitate in the step (1), and drying to obtain the amino modified precipitated silica.
2. The method according to claim 1, wherein the solvent in the step (1) is one of methanol, ethanol and isopropanol.
3. The process according to claim 1, wherein the aqueous ammonia solution in the step (1) has a mass concentration of 25 to 28%.
4. The method according to claim 1, wherein the silicon source in step (1) is one of tetramethyl orthosilicate and tetraethyl orthosilicate.
5. The method according to claim 1, wherein the stirring temperature in the step (1) is 0 to 60 ℃ and the stirring time is 1 to 24 hours.
6. The method according to claim 1, wherein the filtration in the step (2) is one of centrifugal filtration, suction filtration and pressure filtration.
7. The method according to claim 1, wherein the washing in the step (2) is one of water washing or ethanol washing; the number of washing times is 3 to 5.
8. The method according to claim 1, wherein the drying in the step (2) is one of atmospheric drying, vacuum drying, supercritical drying, freeze drying and spray drying.
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| CN109762370A (en) * | 2019-03-01 | 2019-05-17 | 确成硅化学股份有限公司 | A kind of preparation method of amino modified silica |
| JP7290381B1 (en) * | 2022-11-10 | 2023-06-13 | 株式会社西部技研 | Carbon dioxide adsorbent, carbon dioxide adsorption device, manufacturing method thereof, and carbon dioxide adsorption method. |
Citations (6)
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| CN102220036A (en) * | 2011-06-02 | 2011-10-19 | 北京化工大学 | Method for preparing white carbon black modified by silane coupling agent |
| CN104437658A (en) * | 2014-11-28 | 2015-03-25 | 江苏大学 | Porous silicon oxide nano material as well as preparation method and application thereof |
| CN105038439A (en) * | 2015-08-18 | 2015-11-11 | 东北石油大学 | Superhydrophobic composite coating with self-repair function and preparation method thereof |
| CN106566290A (en) * | 2016-11-11 | 2017-04-19 | 青岛科技大学 | White carbon black with dyeing groups on surface and preparation method of white carbon black |
| CN107501951A (en) * | 2017-08-01 | 2017-12-22 | 成都博美实润科技有限公司 | A kind of single-component room temperature vulcanized dealcoholized silicone rubber and preparation method thereof |
| CN107841186A (en) * | 2017-11-10 | 2018-03-27 | 北京航天赛德科技发展有限公司 | The preparation facilities and preparation method and applications of improved silica |
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Patent Citations (6)
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| CN102220036A (en) * | 2011-06-02 | 2011-10-19 | 北京化工大学 | Method for preparing white carbon black modified by silane coupling agent |
| CN104437658A (en) * | 2014-11-28 | 2015-03-25 | 江苏大学 | Porous silicon oxide nano material as well as preparation method and application thereof |
| CN105038439A (en) * | 2015-08-18 | 2015-11-11 | 东北石油大学 | Superhydrophobic composite coating with self-repair function and preparation method thereof |
| CN106566290A (en) * | 2016-11-11 | 2017-04-19 | 青岛科技大学 | White carbon black with dyeing groups on surface and preparation method of white carbon black |
| CN107501951A (en) * | 2017-08-01 | 2017-12-22 | 成都博美实润科技有限公司 | A kind of single-component room temperature vulcanized dealcoholized silicone rubber and preparation method thereof |
| CN107841186A (en) * | 2017-11-10 | 2018-03-27 | 北京航天赛德科技发展有限公司 | The preparation facilities and preparation method and applications of improved silica |
Non-Patent Citations (2)
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