CN106422998A - Method for preparing millimeter-scale hydrophobic SiO2 aerogel bead through dripping method - Google Patents
Method for preparing millimeter-scale hydrophobic SiO2 aerogel bead through dripping method Download PDFInfo
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- CN106422998A CN106422998A CN201611068050.9A CN201611068050A CN106422998A CN 106422998 A CN106422998 A CN 106422998A CN 201611068050 A CN201611068050 A CN 201611068050A CN 106422998 A CN106422998 A CN 106422998A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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Abstract
The invention relates to a method for preparing a millimeter-scale hydrophobic SiO2 aerogel bead, in particular to a method for preparing the millimeter-scale hydrophobic SiO2 aerogel bead through a dripping method. The method for preparing the millimeter-scale hydrophobic SiO2 aerogel bead through the dripping method comprises the following steps: firstly, tiling SiO2 aerogel powder on a flat plate to be used as a platform carrier; preparing uniform sol by carrying out ion exchange of strongly acidic styrene type cation exchange resin on sodium silicate, and standing and hydrolyzing for 24 hours for standby use; dropping out the sol on the aerogel platform carrier to form spherical sol by using an injector, then slightly injecting 1 mol/L of ammonium hydroxide solution in the spherical sol drop by using another injector, accelerating gelatinization by regulating the pH (Potential of Hydrogen) value of the sol bead, and forming spherical gel; carrying out aging treatment on the spherical gel, carrying out surface modification for 24 hours, washing by using n-hexane, and finally putting the spherical gel in a 35-DEG C drying oven for 3 to 4 days, thus preparing the millimeter-scale hydrophobic SiO2 aerogel bead. A dropping preparation technology is simple and fast, and the appearance controllability of the SiO2 aerogel is also increased to a large extent.
Description
Technical field
The present invention relates to one kind prepares grade hydrophobicity SiO2The method of airsetting glueballs is and in particular to a kind of drip legal system
Standby grade hydrophobicity SiO2The method of airsetting glueballs.
Background technology
SiO2Aeroge, because of the continuous pore space structure of its distinctive nano-scale, has that density is low, porosity is high, specific surface
Long-pending high, pore size distribution is uniform, the low feature of thermal conductivity, therefore possesses the properties having many uniquenesses, in extremely-low density high temperature resistant heat insulation
Material, efficient high energy electrode, acoustic impedance coupling material, gas absorption and membrance separation, effective catalyst and its carrier and adsorbent
Have broad application prospects Deng numerous areas.
At present, both at home and abroad with regard to preparing SiO2The report of aeroge is a lot, generally with esters of silicon acis or waterglass as raw material, system
Standby large-sized SiO2Airsetting blob of viscose still has certain difficulty in technique；SiO is prepared using supercritical drying2Aerogel block body
High to equipment requirements, security requirement is higher, cost is high etc. it is difficult in broader daily field application；Prepared by constant pressure and dry
The size of special shape block of material is less easy to control, and blocks of large haves the shortcomings that matter is crisp frangible, no matter using super
The aeroge of critical drying process or the preparation of extremal stability technique is block not of uniform size or powder, in practical application
In filling uneven or reclaim difficult the problems such as then occurs. in order to expand SiO2The range of application of aeroge and efficiency it is desirable to
By SiO2Aeroge is prepared into the ball of profile rule and size tunable, makes up SiO2Deficiency in aerogel microball technology of preparing, carries
Its rollability high, is beneficial to expand its application in fields such as heat-barrier material, industrial catalyst and chromatograph column materials.
Content of the invention
It is contemplated that proposing a kind of drop method to prepare grade hydrophobicity SiO2The method of airsetting glueballs.
Technical program of the present invention lies in：
Drop method prepares grade hydrophobicity SiO2The method of airsetting glueballs, comprises the steps：
（1）First by SiO2Aerogel powder is laid on flat board as microscope carrier；By waterglass through strong-acid type polystyrene sun from
Sub-exchange resin ion exchange prepares uniform colloidal sol, stands hydrolysis 16 ~ 18h；
（2）First pass through syringe and colloidal sol oozed on aeroge microscope carrier spherical colloidal sol, then with another syringe by ammonia molten
In the liquid spherical colloidal sol of injection drips, by adjusting the pH value of colloidal sol ball to 8 ~ 9, accelerate gelation, form spherical gel；
（3）Spherical gel is carried out being aged, burin-in process to strengthen gel internal networking structure, using trim,ethylchlorosilane with just
The mixed solution of hexane carries out surface modification 22 ~ 24h to spherical gel, cleaning, is finally placed in constant pressure and dry in drying baker, preparation
Go out grade hydrophobic type SiO2Airsetting glueballs.
The volume ratio of described trim,ethylchlorosilane and normal hexane is 1：10~1：8.
Described waterglass is 1.8 ~ 2.3 for modulus.
The concentration of described ammonia spirit is 1 ~ 1.2 mol/L.
The baking temperature of described drying baker is 35 ~ 40 DEG C, and drying time is 3 ~ 5 days.
Described cleaning is to be cleaned by normal hexane.
That is invented has technical effect that：
Herein with waterglass as silicon source, on constant pressure and dry Process ba- sis, by prefabricated special microscope carrier, close and distant by colloid solution
The polymerization feature of aqueouss, prepares a diameter of grade other hydrophobic type SiO with drop method etc.2Airsetting glueballs, prepared by drop method
Process is simple, quick, SiO2The pattern Modulatory character of aeroge is also greatly improved.
Specific embodiment
Drop method prepares grade hydrophobicity SiO2The method of airsetting glueballs, comprises the steps：
Embodiment 1
（1）First by SiO2Aerogel powder is laid on flat board as microscope carrier；By waterglass through strong-acid type polystyrene sun from
Sub-exchange resin ion exchange prepares uniform colloidal sol, stands hydrolysis 16 ~ 18h；
（2）First pass through syringe and colloidal sol oozed on aeroge microscope carrier spherical colloidal sol, then with another syringe by ammonia molten
In the liquid spherical colloidal sol of injection drips, by adjusting the pH value of colloidal sol ball to 8 ~ 9, accelerate gelation, form spherical gel；
（3）Spherical gel is carried out being aged, burin-in process to strengthen gel internal networking structure, using trim,ethylchlorosilane with just
The mixed solution of hexane carries out surface modification 22 ~ 24h to spherical gel, cleaning, is finally placed in constant pressure and dry in drying baker, preparation
Go out grade hydrophobic type SiO2Airsetting glueballs.
Embodiment 2
（1）First by SiO2Aerogel powder is laid on flat board as microscope carrier；By waterglass through strong-acid type polystyrene sun from
Sub-exchange resin ion exchange prepares uniform colloidal sol, standing hydrolysis 16h；
（2）First pass through syringe and colloidal sol oozed on aeroge microscope carrier spherical colloidal sol, then with another syringe by ammonia molten
In the liquid spherical colloidal sol of injection drips, by adjusting the pH value of colloidal sol ball to 8, accelerate gelation, form spherical gel；
（3）Spherical gel is carried out being aged, burin-in process to strengthen gel internal networking structure, using trim,ethylchlorosilane with just
The mixed solution of hexane carries out surface modification 22h to spherical gel, cleaning, is finally placed in constant pressure and dry in drying baker, prepares
Grade hydrophobic type SiO2Airsetting glueballs.
Wherein, the volume ratio of described trim,ethylchlorosilane and normal hexane is 1：10.Described waterglass for modulus is
1.8.The concentration of described ammonia spirit is 1 mol/L.The baking temperature of described drying baker is 35 DEG C, and drying time is 3 days.
Described cleaning is to be cleaned by normal hexane.
Embodiment 3
（1）First by SiO2Aerogel powder is laid on flat board as microscope carrier；By waterglass through strong-acid type polystyrene sun from
Sub-exchange resin ion exchange prepares uniform colloidal sol, standing hydrolysis 18h；
（2）First pass through syringe and colloidal sol oozed on aeroge microscope carrier spherical colloidal sol, then with another syringe by ammonia molten
In the liquid spherical colloidal sol of injection drips, by adjusting the pH value of colloidal sol ball to 9, accelerate gelation, form spherical gel；
（3）Spherical gel is carried out being aged, burin-in process to strengthen gel internal networking structure, using trim,ethylchlorosilane with just
The mixed solution of hexane carries out surface modification 24h to spherical gel, cleaning, is finally placed in constant pressure and dry in drying baker, prepares
Grade hydrophobic type SiO2Airsetting glueballs.
Wherein, the volume ratio of described trim,ethylchlorosilane and normal hexane is 1：8.Described waterglass is 2.3 for modulus.
The concentration of described ammonia spirit is 1.2 mol/L.The baking temperature of described drying baker is 40 DEG C, and drying time is 5 days.Institute
The cleaning stated is to be cleaned by normal hexane.
Claims (6)
1. drop method prepares grade hydrophobicity SiO2The method of airsetting glueballs it is characterised in that：Comprise the steps：
（1）First by SiO2Aerogel powder is laid on flat board as microscope carrier；By waterglass through strong-acid type polystyrene cation
Exchanger resin ion exchange prepares uniform colloidal sol, stands hydrolysis 16 ~ 18h；
（2）First pass through syringe and colloidal sol oozed on aeroge microscope carrier spherical colloidal sol, then with another syringe by ammonia molten
In the liquid spherical colloidal sol of injection drips, by adjusting the pH value of colloidal sol ball to 8 ~ 9, accelerate gelation, form spherical gel；
（3）Spherical gel is carried out being aged, burin-in process to strengthen gel internal networking structure, using trim,ethylchlorosilane with just
The mixed solution of hexane carries out surface modification 22 ~ 24h to spherical gel, cleaning, is finally placed in constant pressure and dry in drying baker, preparation
Go out grade hydrophobic type SiO2Airsetting glueballs.
2. drop method according to claim 1 prepares grade hydrophobicity SiO2The method of airsetting glueballs it is characterised in that：
The volume ratio of described trim,ethylchlorosilane and normal hexane is 1：10~1：8.
3. drop method according to claim 1 prepares grade hydrophobicity SiO2The method of airsetting glueballs it is characterised in that：
Described waterglass is 1.8 ~ 2.3 for modulus.
4. drop method according to claim 1 prepares grade hydrophobicity SiO2The method of airsetting glueballs it is characterised in that：
The concentration of described ammonia spirit is 1 ~ 1.2 mol/L.
5. drop method according to claim 1 prepares grade hydrophobicity SiO2The method of airsetting glueballs it is characterised in that：
The baking temperature of described drying baker is 35 ~ 40 DEG C, and drying time is 3 ~ 5 days.
6. drop method according to claim 1 prepares grade hydrophobicity SiO2The method of airsetting glueballs it is characterised in that：
Described cleaning is to be cleaned by normal hexane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611068050.9A CN106422998A (en) | 2016-11-29 | 2016-11-29 | Method for preparing millimeter-scale hydrophobic SiO2 aerogel bead through dripping method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611068050.9A CN106422998A (en) | 2016-11-29 | 2016-11-29 | Method for preparing millimeter-scale hydrophobic SiO2 aerogel bead through dripping method |
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| CN106422998A true CN106422998A (en) | 2017-02-22 |
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| CN201611068050.9A Pending CN106422998A (en) | 2016-11-29 | 2016-11-29 | Method for preparing millimeter-scale hydrophobic SiO2 aerogel bead through dripping method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107421938A (en) * | 2017-09-09 | 2017-12-01 | 合肥学院 | A kind of SiO for detecting malachite green2The preparation method of@ROX nanoparticle fluorescence probe arrays |
| CN112028080A (en) * | 2020-08-31 | 2020-12-04 | 山西大学 | High-strength hierarchical-pore silicon oxide millimeter ball and preparation method and application thereof |
-
2016
- 2016-11-29 CN CN201611068050.9A patent/CN106422998A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107421938A (en) * | 2017-09-09 | 2017-12-01 | 合肥学院 | A kind of SiO for detecting malachite green2The preparation method of@ROX nanoparticle fluorescence probe arrays |
| CN112028080A (en) * | 2020-08-31 | 2020-12-04 | 山西大学 | High-strength hierarchical-pore silicon oxide millimeter ball and preparation method and application thereof |
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Application publication date: 20170222 |