CN102452654A - Cheap preparation method for mesoporous silicon dioxide - Google Patents
Cheap preparation method for mesoporous silicon dioxide Download PDFInfo
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- CN102452654A CN102452654A CN2010105226472A CN201010522647A CN102452654A CN 102452654 A CN102452654 A CN 102452654A CN 2010105226472 A CN2010105226472 A CN 2010105226472A CN 201010522647 A CN201010522647 A CN 201010522647A CN 102452654 A CN102452654 A CN 102452654A
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Abstract
The invention belongs to the technical field of preparation of nanometer porous materials, in particular to a cheap preparation method for mesoporous silicon dioxide. The preparation method is characterized in that: under the condition of no surfactant, cheap citric acid serving as a template and ethyl orthosilicate, sodium silicate and the like serving as silicon sources are hydrolyzed and concentrated in one step in an aqueous or alcohol solution to obtain a vermicular mesoporous silicon dioxide material. During material preparation, the citric acid plays roles in serving as the template and performing acid catalysis, and the citric acid and the like serving as templates can be recycled by washing with water and concentrating. The preparation method has the advantages of cheapness, economical efficiency, simple process and environmental friendliness, and can be used for industrially preparing mesoporous silicon dioxide.
Description
Technical field
The invention belongs to the nano-porous materials preparing technical field, specifically a kind of preparation method of cheap mesoporous silica material.
Background technology
Pore size between the mesopore silica material of 2-50nm because have big specific surface area, the high adjustable characteristics such as aperture of pore volume, homogeneous have broad application prospects at aspects such as catalysis, absorption, sensing, medicine transmission and nano-reactors.Therefore the preparation method who researches and develops a kind of mesopore silicon oxide of cheapness has great practical value.
Be the surfactant templates technology about what generally use synthesizing of mesopore silicon oxide at present; Promptly earlier tensio-active agent is dissolved in the solution of certain pH value; Add silicon precursor and make its hydrolysis self-assembly at a certain temperature, remove the title product that organic formwork agent obtains having central hole structure more under certain condition.Yet there is complicated process of preparation in this method, and cost is higher, and calcination method is removed tensio-active agent and not only wasted but also cause easily environmental pollution.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, the mesoporous silica preparation method that a kind of with low cost, environmental protection and preparation technology are simple, be produced on a large scale is provided.
The method for preparing cheap mesoporous silica that the present invention proposes; Be that Hydrocerol A with cheapness is a template; Tetraethoxy or water glass are the silicon source; Hydrocerol A had not only served as template but also as the acid catalyst of silicon source hydrolysis, can effectively control the mesopore aperture of resultant silicon oxide through the ratio in control Hydrocerol A and silicon source in the preparation process.Final template can be removed through simple washing, and the Hydrocerol A after the washing can be through reusing behind the condensing crystal.
Cheap mesoporous silica provided by the invention has high specific surface area (500-1200m
2g
-1), big pore volume (0.4-1.8cm
3g
-1), unified and adjustable mesopore aperture (2-20nm).
Concrete preparation process of the present invention is following:
(1) at first a certain amount of Hydrocerol A is dissolved in (ratio of second alcohol and water is 0-1000) in the aqueous ethanolic solution; Obtain clear solution with magnetic stirrer; Add the silicon source then; Wherein the mol ratio in Hydrocerol A and silicon source is 0.1-10, and continuously stirring 10-300 minute, obtain even mixed solution.
(2) mixing solutions of step 1 preparation is transferred in the petridish, made it under 15-80 ℃ of temperature, concentrate solvent flashing 5-20 hour, treat that solvent evaporates was placed on 50-100 ℃ of oven drying 3-10 hour fully, can obtain the solid particulate of white or edematus.
(3) white that step 2 is obtained or the solid particulate of edematus place the deionized water washing to remove the template Hydrocerol A, can obtain mesoporous silica material after the drying.Hydrocerol A after the washing can be through recycling behind the condensing crystal.
Description of drawings
Fig. 1 is the transmission electron microscope photo of mesoporous silica.
Embodiment
Embodiment 1
The Hydrocerol A that takes by weighing 10mmol is dissolved in the 50mL deionized water; Stirring is dissolved it fully and is obtained clear solution; Drip the tetraethoxy (mol ratio of Hydrocerol A and tetraethoxy is 1: 2) of 20mmol then, and continuously stirring 60 minutes, even mixed solution obtained; This mixing solutions dress is moved on in the petridish, make it under 50 ℃ of temperature, concentrate solvent flashing 10 hours, place 80 ℃ of oven dryings to obtain the solid particulate of white or edematus in 4 hours then; Place the deionized water washing to remove template solid particulate, can obtain mesoporous silica material after 100 ℃ of dryings.Wherein the Hydrocerol A after the washing can reclaim after concentrating the crystallization of anhydrating.
Embodiment 2
The Hydrocerol A that takes by weighing 20mmol is dissolved in the 50mL deionized water; Stirring is dissolved it fully and is obtained clear solution; Drip the tetraethoxy (mol ratio of Hydrocerol A and tetraethoxy is 1: 1) of 20mmol then, and continuously stirring 90 minutes, even mixed solution obtained; This mixing solutions dress is moved on in the petridish, make it under 50 ℃ of temperature, concentrate solvent flashing 10 hours, place 80 ℃ of oven dryings to obtain the solid particulate of white or edematus in 4 hours then; Place the deionized water washing to remove template solid particulate, can obtain mesoporous silica material after 100 ℃ of dryings.Wherein the Hydrocerol A after the washing can reclaim after concentrating the crystallization of anhydrating.Fig. 1 is the transmission electron microscope photo of this mesopore carbonic acid gas.
Embodiment 3
The Hydrocerol A that takes by weighing 40mmol is dissolved in the 50mL deionized water; Stirring is dissolved it fully and is obtained clear solution; Drip the tetraethoxy (mol ratio of Hydrocerol A and tetraethoxy is 2: 1) of 20mmol then, and continuously stirring 120 minutes, even mixed solution obtained; This mixing solutions dress is moved on in the petridish, make it under 50 ℃ of temperature, concentrate solvent flashing 10 hours, place 80 ℃ of oven dryings to obtain the solid particulate of white or edematus in 4 hours then; Place the deionized water washing to remove template solid particulate, can obtain mesoporous silica material after 100 ℃ of dryings.Wherein the Hydrocerol A after the washing can reclaim after concentrating the crystallization of anhydrating.
Embodiment 4
The Hydrocerol A that takes by weighing 20mmol is dissolved in the 50mL ethanol; Stirring is dissolved it fully and is obtained clear solution; Drip the tetraethoxy (mol ratio of Hydrocerol A and tetraethoxy is 1: 1) of 20mmol then, and continuously stirring 90 minutes, even mixed solution obtained; This mixing solutions dress is moved on in the petridish, make it under 30 ℃ of temperature, concentrate solvent flashing 15 hours, place 80 ℃ of oven dryings to obtain the solid particulate of white or edematus in 5 hours then; Place the deionized water washing to remove template solid particulate, can obtain mesoporous silica material after 100 ℃ of dryings.Wherein the Hydrocerol A after the washing can reclaim after concentrating the crystallization of anhydrating.
Embodiment 5
The Hydrocerol A that takes by weighing 20mmol is dissolved in the 50mL deionized water; Stirring is dissolved it fully and is obtained clear solution; Drip 30ml then and contain the sodium silicate solution (mol ratio of Hydrocerol A and water glass is 1: 1.5) of 30mmol, and continuously stirring 120 minutes, even mixed solution obtained; This mixing solutions dress is moved on in the petridish, make it under 60 ℃ of temperature, concentrate solvent flashing 10 hours, place 90 ℃ of oven dryings to obtain the solid particulate of white or edematus in 4 hours then; Place the deionized water washing to remove template solid particulate, can obtain mesoporous silica material after 100 ℃ of dryings.Wherein the lemon sodium after the washing can reclaim after concentrating the crystallization of anhydrating.
Embodiment 6
The Hydrocerol A that takes by weighing 40mmol is dissolved in the 50mL deionized water; Stirring is dissolved it fully and is obtained clear solution; Drip 30ml then and contain the sodium silicate solution (mol ratio of Hydrocerol A and water glass is 2: 1) of 20mmol, and continuously stirring 120 minutes, even mixed solution obtained; This mixing solutions dress is moved on in the petridish, make it under 60 ℃ of temperature, concentrate solvent flashing 10 hours, place 90 ℃ of oven dryings to obtain the solid particulate of white or edematus in 4 hours then; Place the deionized water washing to remove template solid particulate, can obtain mesoporous silica material after 100 ℃ of dryings.Wherein Hydrocerol A after the washing and Trisodium Citrate can reclaim after concentrating the crystallization of anhydrating.
Claims (5)
1. the preparation method of a cheap mesoporous silica is characterized in that comprising the steps:
(a) at first a certain amount of Hydrocerol A is dissolved in the aqueous ethanolic solution, obtains clear solution with magnetic stirrer, add the silicon source then, wherein the mol ratio in Hydrocerol A and silicon source is 0.1-10, and continuously stirring 10-300 minute, obtain even mixed solution.
(b) mixing solutions of step a preparation is transferred in the petridish, made it under 15-80 ℃ of temperature, concentrate solvent flashing 5-20 hour,, obtain the solid particulate of white or edematus then in 50-100 ℃ of oven drying 3-10 hour.
(c) white that step b is obtained or the solid particulate of edematus place the deionized water washing to remove template, can obtain mesoporous silica material after the drying.Hydrocerol A after the washing can be through recycling behind the condensing crystal.
2. according to the described preparation method of claim 1, it is characterized in that used template is a kind of nonsurfactant and cheap Hydrocerol A.
3. according to the described preparation method of claim 1, it is characterized in that described solvent is the mixing solutions of water or second alcohol and water, wherein the ratio of second alcohol and water is 0-1000.
4. according to the described preparation method of claim 1, it is characterized in that described silicon source is tetraethoxy and water glass.
5. according to the described preparation method of claim 1; The removal that it is characterized in that template need not through calcination processing; As long as can remove fully through simple washing; Avoided the toxic and harmful that produces because of burning, and the Hydrocerol A that comes out of washing etc. can be through the means recycling of condensing crystal, not only energy-conservation but also environmental protection.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105226472A CN102452654A (en) | 2010-10-27 | 2010-10-27 | Cheap preparation method for mesoporous silicon dioxide |
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|---|---|---|---|
| CN2010105226472A CN102452654A (en) | 2010-10-27 | 2010-10-27 | Cheap preparation method for mesoporous silicon dioxide |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103803573A (en) * | 2012-11-07 | 2014-05-21 | 中国石油化工股份有限公司 | Preparation method of mesoporous silica molecular sieve |
| CN109135670A (en) * | 2018-07-20 | 2019-01-04 | 济南大学 | A kind of organic acid catalysis prepares the method and obtained solid acid and nanoporous silica material of solid acid |
| CN110628074A (en) * | 2019-09-30 | 2019-12-31 | 天津大学 | Method for preparing internal structure based on porous PDMS |
| CN111620362A (en) * | 2020-04-24 | 2020-09-04 | 广西科学院 | Microwave preparation method of mesoporous holmium oxide powder |
| CN114870829A (en) * | 2022-05-31 | 2022-08-09 | 赣州瑞德化工有限公司 | Preparation method of tin oxide/silicon oxide photocatalyst porous nano composite material |
-
2010
- 2010-10-27 CN CN2010105226472A patent/CN102452654A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103803573A (en) * | 2012-11-07 | 2014-05-21 | 中国石油化工股份有限公司 | Preparation method of mesoporous silica molecular sieve |
| CN103803573B (en) * | 2012-11-07 | 2016-01-20 | 中国石油化工股份有限公司 | A kind of preparation method of mesoporous silica molecular sieve |
| CN109135670A (en) * | 2018-07-20 | 2019-01-04 | 济南大学 | A kind of organic acid catalysis prepares the method and obtained solid acid and nanoporous silica material of solid acid |
| CN110628074A (en) * | 2019-09-30 | 2019-12-31 | 天津大学 | Method for preparing internal structure based on porous PDMS |
| CN111620362A (en) * | 2020-04-24 | 2020-09-04 | 广西科学院 | Microwave preparation method of mesoporous holmium oxide powder |
| CN114870829A (en) * | 2022-05-31 | 2022-08-09 | 赣州瑞德化工有限公司 | Preparation method of tin oxide/silicon oxide photocatalyst porous nano composite material |
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Application publication date: 20120516 |