CN1546225A - TiO2/SiO2 aerogel globule and method for making same - Google Patents
TiO2/SiO2 aerogel globule and method for making same Download PDFInfo
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- CN1546225A CN1546225A CNA2003101094987A CN200310109498A CN1546225A CN 1546225 A CN1546225 A CN 1546225A CN A2003101094987 A CNA2003101094987 A CN A2003101094987A CN 200310109498 A CN200310109498 A CN 200310109498A CN 1546225 A CN1546225 A CN 1546225A
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- sio
- tio
- small ball
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Abstract
The invention discloses a kind of TiO2/SiO2 gas-condensate pellet and the manufacturing method, the pellet is made up of SiO2 and TiO2 whose weight percentage are 5-95% and 10-95 respectively, the parameter of the pellet is 1-5 mm. the manufacturing method includes following three steps: a. the producing of TiO2/SiO2; b. the producing of TiO2/SiO2 jell pellet; c. the producing of gas-condensate pellet. The pellet has good sorption performance, the photocatalysis efficiency is high, and it is convenient, easy to be reclaimed.
Description
Technical field
The present invention relates to a kind of mesoporous nano material, relate in particular to a kind of TiO
2/ SiO
2Gas gel small ball and preparation method thereof.
Background technology
TiO
2/ SiO
2Aeroge is a kind of novel mesoporous nano material, and it is good to have an absorption property, the photocatalysis efficiency advantages of higher, and the ability of its degradation of contaminant is much better than general T iO
2Powder, spherical TiO
2/ SiO
2Aeroge is extremely easy to use, is difficult for loss, and can overcomes general T iO
2The shortcoming of powder catalyst recovery difficulty, when being used for the improvement of industrial organic waste water, TiO
2/ SiO
2Gas gel small ball can be used as photochemical catalyst and directly drops in the waste water, and is easy to use, effective.When being used for unclean air and administering, can make TiO
2/ SiO
2Aeroge photochemical catalyst packed column, unpurified gas after cycling through packed column by photocatalytic degradation, TiO
2/ SiO
2Gas gel small ball can also be used for the deep purifying of running water as the packed column bead, therefore has wide development and application prospect.
Summary of the invention
The object of the present invention is to provide a kind of easy to use, effective TiO
2/ SiO
2Gas gel small ball.
Another object of the present invention is to provide this TiO
2/ SiO
2The preparation method of gas gel small ball.
The present invention is achieved through the following technical solutions: a kind of TiO
2/ SiO
2Gas gel small ball is the SiO of 5-90% by percentage by weight
2With percentage by weight be the TiO of 10-95%
2Form TiO
2/ SiO
2The gas gel small ball diameter is the 1-5 millimeter.
Wherein preferably: TiO
2/ SiO
2Gas gel small ball is the SiO of 50%-80% by percentage by weight
2With weight percentage be the TiO of 20%-50%
2Form TiO
2/ SiO
2The gas gel small ball diameter is the 2-3 millimeter.
This TiO
2/ SiO
2The preparation method of gas gel small ball comprises following three steps successively:
A, TiO
2/ SiO
2The preparation of colloidal sol;
B, TiO
2/ SiO
2The preparation of gelled pill;
C, TiO
2/ SiO
2The preparation of gas gel small ball;
Wherein prepare TiO
2/ SiO
2The method of colloidal sol can be divided into three kinds:
1, prepares TiO respectively
2Colloidal sol and SiO
2Colloidal sol is then with the two mixing.Prepare TiO in this way
2/ SiO
2During complex sol, SiO
2The silicon source of colloidal sol is generally ethyl orthosilicate, methyl silicate, waterglass etc., and they are made SiO after the hydrolysis in water or ethanol
2Colloidal sol, or directly use industrial Ludox (usually as industrial binding agent, the mass ratio of producing as the permanent letter in Shanghai chemical industrial company is the Ludox of 25-30%) to be raw material.Preparation TiO
2The titanium source of colloidal sol is organic metal alkoxide and TiCl such as butyl titanate, tetraethyl titanate
4, TiSO
4, TiOSO
4Etc. inorganic titanium salt.Form TiO behind organic metal such as butyl titanate, the tetraethyl titanate hydrolysis of alkoxide
2Colloidal sol.TiCl
4, TiSO
4, TiOSO
4Etc. making TiO behind the inorganic titanium salt hydrolysis
2Precipitation, TiO
2Form TiO after precipitating further peptization
2Colloidal sol.With the SiO that makes
2Colloidal sol and TiO
2Colloidal sol makes TiO after mixing
2/ SiO
2Colloidal sol.
Wherein preferably: SiO
2Colloidal sol directly uses industrial Ludox, TiO
2Colloidal sol uses industrial TiOSO
4Be the titanium source.
2, (inorganic salts or organic salt compound are as TiCl with the salt compounds of titanium
4, butyl titanate etc.) add SiO
2In the colloidal sol, after the titanium salt hydrolysis, make TiO in addition
2/ SiO
2Complex sol.Perhaps just the salt compounds of silicon (inorganic salts or organic salt compound are as ethyl orthosilicate, waterglass etc.) adds TiO
2In the colloidal sol, behind the silicon salt hydrolysis, make TiO in addition
2/ SiO
2Complex sol.
3, the common hydrolysis in water and pure equal solvent with titanium salt and silicon salt makes TiO
2/ SiO
2Complex sol.
TiO
2/ SiO
2It is that the device that " 2346499 " name is called the Chinese patent of " a kind of spheric catalyst shaped device " carries out that the preparation method of gelled pill adopts publication number, the ammoniacal liquor of adding 25% in also can be in the drum type reaction kit of the high about 40cm of 500ml, highly be 8cm, add 2ml cetyl ammonium bromide saturated solution then, highly be the kerosene of 24cm last the adding in measuring tank.With above-mentioned TiO
2/ SiO
2Colloidal sol drips in flexible reactor, can obtain TiO
2/ SiO
2Gelled pill.
With the TiO that makes
2/ SiO
2Gelled pill adopts supercritical drying drying method or non-supercritical drying means to make TiO
2/ SiO
2Gas gel small ball.
The device that supercritical drying adopted is the CO 2 supercritical drying system, is broadly divided into high-pressure liquid CO
2Generation, autoclave, control system and 4 parts of gas blow-off system, the autoclave volume is 500mL, and design pressure is 30Mpa, and the supercritical drying process is undertaken by following 4 steps: (1) exchange of solvent: will be immersed in the TiO in the absolute ethyl alcohol
2/ SiO
2The gelled pill sample is transferred to rapidly and is equipped with in the autoclave that volume is the 420mL absolute ethyl alcohol, install still after, use high-purity N
2Catch up with air residual in the most still repeatedly, under 18 ℃, 6MPa, use CO then
2Fluid exchange absolute ethyl alcohol, flow rate of liquid are controlled at about 6mL/min, and the content of ethanol is lower than 10 * 10 in the gas of discharging
-6The time, think exchange fully, whole exchange process needs 7 hours.(2) heat up: the control heating rate is warming up to 45 ℃ with the speed of 0.5 ℃ of per minute.(3) venting: under 45 ℃ of constant temperature, slowly exit less than the speed of 0.5MPa, drop to 0.1MPa, take out sample after being cooled to room temperature until pressure with per minute.
The non-supercritical drying means is as follows: 1, will make TiO
2/ SiO
2Gelled pill needs 12-36 hour with soaked in absolute ethyl alcohol washing 1-5 time at every turn, and soaking temperature is 0-70 ℃; 2, then with the alcohol solution dipping of ethyl orthosilicate or trim,ethylchlorosilane 1-5 time, need 12-36 hour, soaking temperature is 0-70 ℃ at every turn; 3, then use absolute ethanol washing 1-5 time, need 12-36 hour at every turn, soaking temperature is 0-70 ℃; 4, at last directly with TiO
2/ SiO
2The drier inner drying that gelled pill is placed under 40-78 ℃ can make TiO
2/ SiO
2Gas gel small ball.
TiO of the present invention
2/ SiO
2Gas gel small ball, therefore good except that having absorption property because it is a graininess, the photocatalysis efficiency advantages of higher also has advantages such as easy to use, easy recovery, difficult loss.
The specific embodiment
The knot specific embodiment further specifies the present invention and how to realize below:
Embodiment 1
Take by weighing 16 grams, 98% titanyl sulfate, be dissolved in the 500ml deionized water, place separatory funnel to drop to titanyl sulfate solution in 2 hours the ammoniacal liquor of 50ml, vigorous stirring makes abundant reaction simultaneously, treats to react 1 hour after ammoniacal liquor dropwises again.
The solution suction filtration of above-mentioned reaction gained is got white precipitate, and spending deionised water does not have SO to filtrate
4 2-Till.Then this white depositions is disperseed with the 70ml deionized water, add the aqueous solution of nitric acid of the 1.6mol/l of 31ml again, stir down at 70 ℃ and made the precipitation peptization in 10 hours, promptly obtain the titanium colloidal sol of stable uniform.
The percent concentration of the titanium colloidal sol that detection obtains is 4.8%, and molar concentration is 0.63 mol.
With 40ml industry silicasol 2.5ml30%HNO
3Transfer to acidity, the pH value is 2.Measure the titanium colloidal sol of 14ml0.6 mol, under agitation add the Ludox (molar concentration is 0.42 mol) of the above-mentioned processing of 6ml, make TiO
2/ SiO
2Colloidal sol.
The ammoniacal liquor of adding 25% highly is 8cm in the drum type reaction kit of the high about 40cm of 500ml, adds 2ml cetyl ammonium bromide saturated solution then, and highly be the kerosene of 24cm last the adding in measuring tank.
With above-mentioned TiO
2/ SiO
2Colloidal sol drips in flexible reactor, can obtain TiO
2/ SiO
2Gelled pill.
To make TiO
2/ SiO
2Gelled pill needs 20-36 hour with soaked in absolute ethyl alcohol washing 3-5 time at every turn, and soaking temperature is 10-30 ℃; Then use alcohol solution dipping 3-5 time of ethyl orthosilicate, need 20-36 hour at every turn, soaking temperature is 10-30 ℃; Then use absolute ethanol washing 3-5 time, need 20-36 hour at every turn, soaking temperature is 10-30 ℃.At last directly with TiO
2/ SiO
2The drier inner drying that gel is placed under 40-78 ℃ can make TiO
2/ SiO
2Make TiO
2/ SiO
2Gas gel small ball.
Prepared TiO
2/ SiO
2The gas gel small ball diameter is the 2-3 millimeter.
Embodiment 2
Take by weighing 16 grams, 98% titanyl sulfate, be dissolved in the 500ml deionized water, place separatory funnel to drop to titanyl sulfate solution in 2 hours the ammoniacal liquor of 50ml, vigorous stirring makes abundant reaction simultaneously.Treat to react again 1 hour after ammoniacal liquor dropwises.
The solution suction filtration of above-mentioned reaction gained is got white precipitate, and spending deionised water does not have SO to filtrate
4 2-Till.Then this white depositions is disperseed with the 70ml deionized water, add the aqueous solution of nitric acid of the 1.6mol/l of 31ml again, stir down at 70 ℃ and made the precipitation peptization in 10 hours, promptly obtain the titanium colloidal sol of stable uniform.
The percent concentration of the titanium colloidal sol that detection obtains is 4.8%, and molar concentration is 0.63 mol.
With 40ml industry silicasol 2.5ml30%HNO
3Transfer to acidity, the pH value is 2.Measure the titanium colloidal sol of 14ml0.6 mol, under agitation add the Ludox (molar concentration is 0.42 mol) of the above-mentioned processing of 6ml, make TiO
2/ SiO
2Colloidal sol.
The ammoniacal liquor of adding 25% highly is 8cm in the drum type reaction kit of the high about 40cm of 500ml, adds 2ml cetyl ammonium bromide saturated solution then, and highly be the kerosene of 24cm last the adding in measuring tank.
With above-mentioned TiO
2/ SiO
2Colloidal sol drips in flexible reactor, can obtain TiO
2/ SiO
2Gelled pill.
To make TiO
2/ SiO
2Gelled pill needs 20-36 hour with soaked in absolute ethyl alcohol washing 3-5 time at every turn, and soaking temperature is 10-30 ℃; Then use alcohol solution dipping 3-5 time of trim,ethylchlorosilane, need 20-36 hour at every turn, soaking temperature is 10-30 ℃; Then use absolute ethanol washing 3-5 time, need 20-36 hour at every turn, soaking temperature is 10-30 ℃.At last directly with TiO
2/ SiO
2The drier inner drying that gel is placed under 40-78 ℃ can make TiO
2/ SiO
2Gas gel small ball.
Prepared TiO
2/ SiO
2The gas gel small ball diameter is the 1-3 millimeter.
Embodiment 3
Take by weighing 16 grams, 98% titanyl sulfate, be dissolved in the 500ml deionized water, place separatory funnel to drop to titanyl sulfate solution in 2 hours the ammoniacal liquor of 50ml, vigorous stirring makes abundant reaction simultaneously.Treat to react again 1 hour after ammoniacal liquor dropwises.
The solution suction filtration of above-mentioned reaction gained is got white precipitate, and spending deionised water does not have SO to filtrate
4 2-Till.Then this white depositions is disperseed with the 70ml deionized water, add the aqueous solution of nitric acid of the 1.6mol/l of 31ml again, stir down at 70 ℃ and made the precipitation peptization in 10 hours, promptly obtain the titanium colloidal sol of stable uniform.
The percent concentration of the titanium colloidal sol that detection obtains is 4.8%, and molar concentration is 0.63 mol.
With 40ml industry silicasol 2.5ml30%HNO
3Transfer to acidity, the pH value is 2.Measure the titanium colloidal sol of 14ml0.6 mol, under agitation add the Ludox (molar concentration is 0.42 mol) of the above-mentioned processing of 6ml, make TiO
2/ SiO
2Colloidal sol.
The ammoniacal liquor of adding 25% highly is 8cm in the drum type reaction kit of the high about 40cm of 500ml, adds 2ml cetyl ammonium bromide saturated solution then, and highly be the kerosene of 24cm last the adding in measuring tank.
With above-mentioned TiO
2/ SiO
2Colloidal sol drips in flexible reactor, can obtain TiO
2/ SiO
2Gelled pill.
To make TiO
2/ SiO
2Gelled pill adopts the supercritical drying drying method to carry out drying, and the device that is adopted is the CO 2 supercritical drying system, is broadly divided into high-pressure liquid CO
2Generation, autoclave, control system and 4 parts of gas blow-off system, the autoclave volume is 500mL, and design pressure is 30Mpa, and the supercritical drying process is undertaken by following 4 steps: (1) exchange of solvent: will be immersed in the TiO in the absolute ethyl alcohol
2/ SiO
2Gel sample is transferred to rapidly in the autoclave that absolute ethyl alcohol is housed, install still after, use high-purity N
2Catch up with air residual in the most still repeatedly, use CO then
2Fluid exchange absolute ethyl alcohol, flow rate of liquid are controlled at about 6mL/min, and the content of ethanol is lower than 10 * 10 in the gas of discharging
-6The time, think that exchange is fully.(2) heat up: the control heating rate is warming up to 45 ℃ with the speed of 0.5 ℃ of per minute.(3) venting: under 45 ℃ of constant temperature, slowly exit, drop to 0.1MPa, make TiO after being cooled to room temperature until pressure with the speed of 0.2MPa/min-0.5MPa/min
2/ SiO
2Gas gel small ball.
Prepared TiO
2/ SiO
2The gas gel small ball diameter is the 1-4 millimeter.
Claims (8)
1, a kind of TiO
2/ SiO
2Gas gel small ball is characterized in that: described TiO
2/ SiO
2Gas gel small ball is the SiO of 5-90% by percentage by weight
2With percentage by weight be the TiO of 10-95%
2Form TiO
2/ SiO
2The gas gel small ball diameter is the 1-5 millimeter.
2, according to the described a kind of TiO of right claim 1
2/ SiO
2Gas gel small ball is characterized in that: described TiO
2/ SiO
2Gas gel small ball is the SiO of 50%-80% by percentage by weight
2With weight percentage be the TiO of 20%-50%
2Form TiO
2/ SiO
2The gas gel small ball diameter is the 2-3 millimeter.
3, according to right claim 1 or 2 described a kind of TiO
2/ SiO
2Gas gel small ball, its preparation method comprise following three steps successively:
A, TiO
2/ SiO
2The preparation of colloidal sol;
B, TiO
2/ SiO
2The preparation of gelled pill;
C, TiO
2/ SiO
2The preparation of gas gel small ball;
It is characterized in that: described c step TiO
2/ SiO
2The preparation method of gas gel small ball is: 1, will make TiO
2/ SiO
2Gelled pill washs with soaked in absolute ethyl alcohol; 2, again with the alcohol solution dipping of ethyl orthosilicate or trim,ethylchlorosilane; 3, then wash with soaked in absolute ethyl alcohol; 4, at last directly with TiO
2/ SiO
2Gelled pill is placed on the drier inner drying can make TiO
2/ SiO
2Gas gel small ball.
4, a kind of TiO according to claim 3
2/ SiO
2The preparation method of gas gel small ball is characterized in that: the temperature of washing by soaking is 5-70 ℃ in described 1,2,3 each step, and each required time is 12-36 hour, and 1,2,3 each step washing by soaking number of times are 1-5 time.
5, a kind of TiO according to claim 3
2/ SiO
2The preparation method of aeroge is characterized in that: the temperature of drier is 40-78 ℃ in described 4 steps.
6, according to right claim 1 or 2 described a kind of TiO
2/ SiO
2Gas gel small ball, its preparation method comprise following three steps successively: (1) will be immersed in the TiO in the absolute ethyl alcohol
2/ SiO
2Gelled pill is transferred to rapidly in the autoclave that absolute ethyl alcohol is housed, and uses high-purity N
2Catch up with air residual in the most still repeatedly, use CO then
2The fluid exchange absolute ethyl alcohol; (2) the control heating rate is warming up to 45 ℃ with the speed of 0.5 ℃ of per minute.(3) slowly venting under 45 ℃ of constant temperature drops to 0.1MPa until pressure, makes TiO after being cooled to room temperature
2/ SiO
2Gas gel small ball.
7, a kind of TiO according to claim 6
2/ SiO
2The preparation method of gas gel small ball is characterized in that: CO in the described step (1)
2Flow rate of liquid is controlled at about 6mL/min.
8, a kind of TiO according to claim 6
2/ SiO
2The preparation method of gas gel small ball is characterized in that: the venting speed in the described step (3) is less than 0.5MPa/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2003101094987A CN1546225A (en) | 2003-12-17 | 2003-12-17 | TiO2/SiO2 aerogel globule and method for making same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2003101094987A CN1546225A (en) | 2003-12-17 | 2003-12-17 | TiO2/SiO2 aerogel globule and method for making same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1546225A true CN1546225A (en) | 2004-11-17 |
Family
ID=34335236
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2003101094987A Pending CN1546225A (en) | 2003-12-17 | 2003-12-17 | TiO2/SiO2 aerogel globule and method for making same |
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|---|---|
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100417439C (en) * | 2006-06-05 | 2008-09-10 | 同济大学 | Method for preparing TiO2/SiO2 aerogel microsphere |
| CN100586850C (en) * | 2005-05-30 | 2010-02-03 | 同济大学 | Method for preparing micron SiO2 gas gel small ball |
| CN101274246B (en) * | 2007-12-26 | 2010-06-02 | 中国科学院上海硅酸盐研究所 | Sol-gel method for preparing earth silicon/titanic oxide hollow microballoon |
| CN102441370A (en) * | 2010-09-30 | 2012-05-09 | 中国石油化工股份有限公司 | Aerogel catalyst and preparation method thereof |
| CN102613245A (en) * | 2012-03-22 | 2012-08-01 | 陕西盟创纳米新型材料股份有限公司 | Preparation method of nano-silica aerogels |
| CN104001470A (en) * | 2014-05-21 | 2014-08-27 | 华南理工大学 | Ti-Si-O difunctional photocatalysis adsorbent as well as preparation method and application thereof in fuel oil desulphurization |
| CN105801156A (en) * | 2016-02-19 | 2016-07-27 | 厦门纳美特新材料科技有限公司 | Porous alumina-silicon oxide aerogel balls and quick preparation method thereof |
| CN106215917A (en) * | 2016-07-18 | 2016-12-14 | 长春工业大学 | A kind of TiO2/ SiO2the preparation method and applications of aerogel microball |
| CN107376828A (en) * | 2017-08-08 | 2017-11-24 | 西安工程大学 | A kind of preparation method of zirconium dioxide silica composite adsorbing material |
-
2003
- 2003-12-17 CN CNA2003101094987A patent/CN1546225A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100586850C (en) * | 2005-05-30 | 2010-02-03 | 同济大学 | Method for preparing micron SiO2 gas gel small ball |
| CN100417439C (en) * | 2006-06-05 | 2008-09-10 | 同济大学 | Method for preparing TiO2/SiO2 aerogel microsphere |
| CN101274246B (en) * | 2007-12-26 | 2010-06-02 | 中国科学院上海硅酸盐研究所 | Sol-gel method for preparing earth silicon/titanic oxide hollow microballoon |
| CN102441370B (en) * | 2010-09-30 | 2013-08-14 | 中国石油化工股份有限公司 | Aerogel catalyst and preparation method thereof |
| CN102441370A (en) * | 2010-09-30 | 2012-05-09 | 中国石油化工股份有限公司 | Aerogel catalyst and preparation method thereof |
| CN102613245B (en) * | 2012-03-22 | 2014-06-04 | 陕西盟创纳米新型材料股份有限公司 | Preparation method of nano-silica aerogels |
| CN102613245A (en) * | 2012-03-22 | 2012-08-01 | 陕西盟创纳米新型材料股份有限公司 | Preparation method of nano-silica aerogels |
| CN104001470A (en) * | 2014-05-21 | 2014-08-27 | 华南理工大学 | Ti-Si-O difunctional photocatalysis adsorbent as well as preparation method and application thereof in fuel oil desulphurization |
| CN104001470B (en) * | 2014-05-21 | 2016-10-05 | 华南理工大学 | Difunctional photocatalytic adsorbent of a kind of Ti-Si-O and preparation method thereof and its application in fuel desulfuration |
| CN105801156A (en) * | 2016-02-19 | 2016-07-27 | 厦门纳美特新材料科技有限公司 | Porous alumina-silicon oxide aerogel balls and quick preparation method thereof |
| CN105801156B (en) * | 2016-02-19 | 2019-02-19 | 厦门纳美特新材料科技有限公司 | A kind of porous aluminas-silica aerogel bead and its fast preparation method |
| CN106215917A (en) * | 2016-07-18 | 2016-12-14 | 长春工业大学 | A kind of TiO2/ SiO2the preparation method and applications of aerogel microball |
| CN106215917B (en) * | 2016-07-18 | 2019-04-12 | 长春工业大学 | A kind of TiO2/SiO2The preparation method and applications of aerogel microball |
| CN107376828A (en) * | 2017-08-08 | 2017-11-24 | 西安工程大学 | A kind of preparation method of zirconium dioxide silica composite adsorbing material |
| CN107376828B (en) * | 2017-08-08 | 2020-06-19 | 西安工程大学 | Preparation method of zirconium dioxide-silicon dioxide composite adsorption material |
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