CN107469776A - A kind of mesoporous silicon materials of KIT 6 of phenyl load and its preparation and application - Google Patents
A kind of mesoporous silicon materials of KIT 6 of phenyl load and its preparation and application Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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Abstract
The present invention discloses the mesoporous silicon materials of KIT 6 and its preparation and the application of a kind of phenyl load, P123 is used as template, add tetraethyl orthosilicate and organic silicon source containing phenyl, copolycondensation is hydrolyzed by hydro-thermal reaction in acid condition, prepares a kind of mesoporous silicon materials of KIT 6 of phenyl load.The material has high specific surface area and pore volume, compared with pure KIT 6, VOCs adsorption capacities (the 1.44mmol g under high humidity conditions of KIT 6 of phenyl load‑1) and hydrophobicity (Qwet/Qdry=77.8%) dramatically increase, therefore the sorbing material has great application potential in the field such as chemical industry and environmental protection.
Description
Technical field
The invention belongs to organo-mineral complexing porous material, sorbing material and its preparing technical field, it is related to chemical industry and ring
Protect the adsorption cleaning of benzene series VOCs under dry or high humidity in industry, more particularly to a kind of preparation side of KIT-6 mesoporous silicons
Method and absorption VOCs in terms of application.
Background technology
Artificial source volatile organic matter (VOCs) in air is mainly derived from petrochemical industry, oil product transport, printing and building materials dress
The industries such as decorations, directly can be sucked by human body, and and NOxGeneration photochemical reaction forms secondary particulate and O3, seriously endanger
The living environment of the mankind, therefore VOCs improvement is one of mostly important study hotspot of current field of Environment Protection.Common
In VOCs administering methods, solid absorption method has the advantage of the low cost of low energy consumption easy to operate, recyclable, is widely used in VOCs
Removal.Activated carbon is most common adsorbent, but the moisture under most of atmospheric conditions all containing the degree that is bound to, activity
The hydrophily of charcoal limits it in high humidity (RH>40%, 25 DEG C) under VOCs adsorption applications.
KIT-6 is a kind of three-dimensional ordered mesoporous silicon materials, has high specific surface area, high pore volume and good thermal stability etc.
Feature, and KIT-6 has the mesopore orbit of connection, is easy to modify hydrophobic organic groups, can solve high humility VOCs suctions with this
This attached great difficult problem.At present, there is researcher by rear grafting in a variety of mesoporous silicon surface graft phenyl, but only in low humidity
There is certain hydrophobic performance under the conditions of degree (RH=13%, 25 DEG C), this is due to that the phenyl quantity of rear grafting grafting is excessive
Easily formed and blocked in duct, therefore the limitation of phenyl grafting quantity also improves the limitation of material absorption property.
The content of the invention
The shortcomings that in order to overcome above-mentioned prior art, it is an object of the invention to provide a kind of preparation of KIT-6 mesoporous silicons
Method and absorption VOCs in terms of application, using copolycondensation method one-step synthesis phenyl load KIT-6, the adsorbent is in high humility
Under the conditions of there is high VOCs adsorption capacities and high hydrophobicity.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of KIT-6 mesoporous silicon materials of phenyl load, silicon phenyl base is uniformly modified with KIT-6 mesoporous silicon materials surface
Group, specific surface area is 700~1000m2/ g, pore volume are 0.4~1.1cm3/ g, aperture are 2~10nm, and drying condition Toluene is inhaled
Attached capacity is 1.5~2.1mmol g-1, it is wet under the conditions of toluene adsorption capacity be 0.3~1.5mmol g-1, hydrophilicity value
(Qwet/Qdry) it is 10%~80%.
The present invention also invented the preparation method of the KIT-6 mesoporous silicon materials of phenyl load, comprise the following steps：
(1) a certain amount of block copolymer P123 is dissolved in hydrochloric acid solution, the n-butanol of the quality such as addition and P123, stirred
Mix；
(2) keep element silicon total mole number constant, according to organic silicon source and the mol ratio 1 of tetraethyl orthosilicate containing phenyl：
The two is added hydrochloric acid solution, stirring by the ratio of (6~36)；
(3) slowly the uniform mixed liquor in step (2) is added dropwise in the mixed liquor obtained by step (1), after stirring, entered
Water-filling thermal response, only filter and do not clean, obtain white depositions；
(4) sediment obtained by step (3) is placed in 150~200 DEG C of baking oven and heated, obtain white powder thing, used
The ethanol solution of hydrochloric acid cleans 2 times, then is cleaned with deionized water, filter, dry, that is, obtains the KIT-6 mesoporous silicons of phenyl load
Material.
In the step (2), the mol ratio of organic silicon source and tetraethyl orthosilicate containing phenyl is 1:6、1:12、1:18 or 1:
36, preferably 1:6.
In the step (2), organic silicon source of phenyl is phenyl triethoxysilane, diphenyl diethoxy silane, three
Any one of phenyl ethoxy silane.
In the step (3), the uniform mixed liquor of step (2) and hydrochloric acid solution equivalent used in step (1), and gained mixes
The mol ratio of each material is P123 in liquid:The total silicon source of organic/inorganic:N-butanol:HCl:H2O=0.017:1:1.33:1.83:
195。
In the step (1), 4h is stirred at a temperature of 35~40 DEG C；
In the step (2), 3h is stirred at a temperature of 35~40 DEG C；
In the step (3), 20h is stirred, hydrothermal reaction condition is 100 DEG C, 24h；
In the step (4), sediment heats 5h in 150~200 DEG C of baking oven.
The KIT-6 mesoporous silicon materials of phenyl load can be applied under dry or high humidity adsorb VOCs.Including
The benzene homologues such as benzene, toluene and dimethylbenzene.
The condition of adsorption process is：Relative humidity 40%~80%, 25 DEG C of temperature.
Specifically：Measurement atmosphere is the nitrogen stream of the 100mL/min toluene concentration containing 1000ppm, and air speed is
60000mL/ (g h), temperature are 25 DEG C, and the relative humidity of aqueous adsorption process is 60%.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention compared with normal activated carbon and other modified porous silicon materials there is high VOCs under high humidity to inhale
Attached ability and high hydrophobicity.(the 1 of the present invention:6) KIT-6 sorbing materials under high humidity conditions (RH=60%, 25 DEG C), to first
The adsorption capacity of benzene reaches 1.44mmol/g, and hydrophobicity (aqueous/drying condition Toluene adsorbance ratio) is up to 77.8%.
Brief description of the drawings
Fig. 1 is the infrared spectrogram of the KIT-6 mesoporous silicons of the phenyl load prepared.
Fig. 2 is the nitrogen adsorption desorption curve map of the KIT-6 mesoporous silicons of the phenyl load prepared.
Fig. 3 is the graph of pore diameter distribution of the KIT-6 mesoporous silicons of the phenyl load prepared.
Fig. 4 is the KIT-6 mesoporous silicons of the phenyl load prepared in drying (solid dot) and RH=60% (hollow dots) bar
The breakthrough curve figure of toluene is adsorbed under part.
Embodiment
Describe embodiments of the present invention in detail with reference to the accompanying drawings and examples.
Embodiment 1
4g block copolymer P123 and 3.7g hydrochloric acid (37wt%) is added in 72mL deionized waters, 3h is stirred, adds
4g n-butanols, 1h is stirred at a temperature of 35 DEG C；1.40g phenyl triethoxysilanes and 7.29g tetraethyl orthosilicates are added
In 72mL deionized water, 3.7g hydrochloric acid (37wt%) is added, 3h is stirred at a temperature of 35 DEG C；By above-mentioned the latter's mixed liquor
It is added dropwise in the former mixed liquor, after stirring 20h at a temperature of 35 DEG C, loads the stainless steel reaction that liner is polytetrafluoroethylene (PTFE)
In kettle, 24h hydro-thermal reaction is carried out at 100 DEG C, only filters and does not clean, obtain white depositions；The sediment of gained is put
The 5h in 160 DEG C of baking oven, white powder thing is obtained, with the ethanol solution (hydrochloric acid containing 5mL (37wt%)) of 150mL hydrochloric acid 40
Cleaned 2 times at DEG C, then cleaned with deionized water, filter, dry, that is, obtained the KIT-6 mesoporous silicon materials of phenyl load, be designated as
(1:6)KIT-6。
It will be seen from figure 1 that increasing with addition organic precursor, in 1433,740 and 698cm-1The peak intensity at place is gradual
Enhancing, this phenyl quantity for showing successfully to be supported on KIT-6 also gradually increase.Fig. 2 and Fig. 3 is the adsorbent prepared respectively
Nitrogen adsorption desorption figure and graph of pore diameter distribution, it can be seen that all adsorbents from two figures and all contain meso-hole structure, but as phenyl is born
The increase of carrying capacity, mesoporous pore size and quantity gradually decrease.The specific surface area of the adsorbent is 761.4m2/ g, pore volume are
0.468cm3/ g, aperture 5.086nm.Its toluene absorption test condition be：Atmosphere is 100mL/min first containing 1000ppm
The nitrogen stream of benzene concentration, air speed are 60000mL/ (g h), and temperature is 25 DEG C, and the relative humidity of aqueous adsorption process is 60%.Property
Can result figure as shown in figure 4, the toluene adsorption capacity under its drying condition is 1.85mmol/g, the toluene under the conditions of RH=60%
Adsorption capacity is 1.44mmol/g, and hydrophilicity value (aqueous/drying condition Toluene adsorbance ratio) is 77.8%.
Embodiment 2
As different from Example 1：The quality for adding phenyl triethoxysilane and tetraethyl orthosilicate is changed into respectively
0.75g and 7.85g, remaining process are constant.The KIT-6 mesoporous silicon materials of obtained phenyl load, are designated as (1:12)KIT-6.
The specific surface area of the adsorbent is 838.4m2/ g, pore volume 0.606cm3/ g, aperture 5.086nm.Its toluene is inhaled
Attached test condition is：Atmosphere is the nitrogen stream of the 100mL/min toluene concentration containing 1000ppm, and air speed is 60000mL/ (g
H), temperature is 25 DEG C, and the relative humidity of aqueous adsorption process is 60%.Results of property figure is as shown in figure 4, under its drying condition
Toluene adsorption capacity is 2.01mmol/g, and the toluene adsorption capacity under the conditions of RH=60% is 1.16mmol/g, and hydrophilicity value (contains
Water/drying condition Toluene adsorbance ratio) it is 57.7%.
Embodiment 3
As different from Example 1：The quality for adding phenyl triethoxysilane and tetraethyl orthosilicate is changed into respectively
0.52g and 8.05g, remaining process are constant.The KIT-6 mesoporous silicon materials of obtained phenyl load, are designated as (1:18)KIT-6.
The specific surface area of the adsorbent is 842.0m2/ g, pore volume 0.841cm3/ g, aperture 6.317nm.Its toluene is inhaled
Attached test condition is：Atmosphere is the nitrogen stream of the 100mL/min toluene concentration containing 1000ppm, and air speed is 60000mL/ (g
H), temperature is 25 DEG C, and the relative humidity of aqueous adsorption process is 60%.Results of property figure is as shown in figure 4, under its drying condition
Toluene adsorption capacity is 1.85mmol/g, and the toluene adsorption capacity under the conditions of RH=60% is 0.98mmol/g, and hydrophilicity value (contains
Water/drying condition Toluene adsorbance ratio) it is 53.0%.
Embodiment 4
As different from Example 1：The quality for adding phenyl triethoxysilane and tetraethyl orthosilicate is changed into respectively
0.27g and 8.27g, remaining process are constant.The KIT-6 mesoporous silicon materials of obtained phenyl load, are designated as (1:36)KIT-6.
The specific surface area of the adsorbent is 898.6m2/ g, pore volume 1.067cm3/ g, aperture 7.032nm.Its toluene is inhaled
Attached test condition is：Atmosphere is the nitrogen stream of the 100mL/min toluene concentration containing 1000ppm, and air speed is 60000mL/ (g
H), temperature is 25 DEG C, and the relative humidity of aqueous adsorption process is 60%.Results of property figure is as shown in figure 4, under its drying condition
Toluene adsorption capacity is 1.86mmol/g, and the toluene adsorption capacity under the conditions of RH=60% is 0.36mmol/g, and hydrophilicity value (contains
Water/drying condition Toluene adsorbance ratio) it is 19.5%.
Comparative example 1
4g block copolymer P123 and 7.4g hydrochloric acid (37wt%) is added in 144mL deionized waters, 3h is stirred, adds
4g n-butanols, 1h is stirred at a temperature of 35 DEG C；8.50g tetraethyl orthosilicates are added dropwise in the former mixed liquor, at 35 DEG C
At a temperature of stir 20h after, is fitted into liner be polytetrafluoroethylene (PTFE) stainless steel cauldron in, at 100 DEG C progress 24h hydro-thermal it is anti-
Should, only filter and do not clean, obtain white depositions；The sediment of gained is placed in 5h in 160 DEG C of baking oven, obtains white powder
Thing, cleaned 2 times at 40 DEG C with the ethanol solution (hydrochloric acid containing 5mL (37wt%)) of 150mL hydrochloric acid, then cleaned with deionized water,
Filtering, drying, that is, obtain pure KIT-6 mesoporous silicon materials, be designated as KIT-6.
The specific surface area of the control sample adsorbent is 944.2m2/ g, pore volume 1.072cm3/ g, aperture 8.145nm.Its
Toluene absorption test condition be：Atmosphere is the nitrogen stream of the 100mL/min toluene concentration containing 1000ppm, and air speed is
60000mL/ (g h), temperature are 25 DEG C, and the relative humidity of aqueous adsorption process is 60%.Results of property figure as shown in figure 4, its
Toluene adsorption capacity under drying condition is 1.93mmol/g, and the toluene adsorption capacity under the conditions of RH=60% is 0.31mmol/
G, hydrophilicity value (aqueous/drying condition Toluene adsorbance ratio) are 16.1%.
To sum up, adsorbent (1 of the present invention is utilized:6) KIT-6, it is ensured that have higher toluene absorption under high humidity conditions
Capacity and higher hydrophobicity.
Applicant states that the present invention illustrates the method detailed of the present invention, but not office of the invention by above-described embodiment
It is limited to above-mentioned method detailed, that is, does not mean that the present invention has to rely on above-mentioned method detailed and could implemented.Art
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and disclosing.
Claims (10)
1. a kind of KIT-6 mesoporous silicon materials of phenyl load, it is characterised in that uniformly modified on KIT-6 mesoporous silicon materials surface
There is silicon phenyl group, specific surface area is 700~1000m2/ g, pore volume are 0.4~1.1cm3/ g, aperture are 2~10nm, dried strip
Part Toluene adsorption capacity is 1.5~2.1mmol g-1, it is wet under the conditions of toluene adsorption capacity be 0.3~1.5mmol g-1, dredge
Water-based value (Qwet/Qdry) it is 10%~80%.
2. a kind of preparation method of the KIT-6 mesoporous silicon materials of phenyl load, it is characterised in that comprise the following steps：
(1) a certain amount of block copolymer P123 is dissolved in hydrochloric acid solution, the n-butanol of the quality such as addition and P123, stirring；
(2) keep element silicon total mole number constant, according to organic silicon source and the mol ratio 1 of tetraethyl orthosilicate containing phenyl：(6~
36) the two is added hydrochloric acid solution, stirring by ratio；
(3) slowly the uniform mixed liquor in step (2) is added dropwise in the mixed liquor obtained by step (1), after stirring, enters water-filling
Thermal response, only filter and do not clean, obtain white depositions；
(4) sediment obtained by step (3) is placed in 150~200 DEG C of baking oven and heated, obtained white powder thing, use hydrochloric acid
Ethanol solution clean 2 times, then cleaned with deionized water, filter, dry, that is, obtain the KIT-6 mesoporous silicon materials of phenyl load.
3. the preparation method of the KIT-6 mesoporous silicon materials of phenyl load according to claim 2, it is characterised in that the step
Suddenly the mol ratio of each material of mixed liquor is P123 in (3):The total silicon source of organic/inorganic:N-butanol:HCl:H2O=0.017:1:
1.33:1.83:195。
4. the preparation method of the KIT-6 mesoporous silicon materials of phenyl load according to claim 2, it is characterised in that the step
Suddenly in (2), the mol ratio of organic silicon source and tetraethyl orthosilicate containing phenyl is 1:6、1:12、1:18 or 1:36.
5. the preparation method of the KIT-6 mesoporous silicon materials of phenyl load according to claim 2, it is characterised in that the step
Suddenly in (2), organic silicon source of phenyl is phenyl triethoxysilane, diphenyl diethoxy silane, triphenyl Ethoxysilane
Any one of.
6. the preparation method of the KIT-6 mesoporous silicon materials of phenyl load according to claim 2, it is characterised in that the step
Suddenly in (3), the uniform mixed liquor of step (2) and hydrochloric acid solution equivalent used in step (1).
7. the preparation method of the KIT-6 mesoporous silicon materials of phenyl load according to claim 2, it is characterised in that the step
Suddenly in (1), 4h is stirred at a temperature of 35~40 DEG C；
In the step (2), 3h is stirred at a temperature of 35~40 DEG C；
In the step (3), 20h is stirred, hydrothermal reaction condition is 100 DEG C, 24h；
In the step (4), sediment heats 5h in 150~200 DEG C of baking oven.
8. the KIT-6 mesoporous silicon materials that phenyl described in claim 1 loads are applied to adsorb under dry or high humidity
VZCs。
9. apply according to claim 8, it is characterised in that the VOCs includes benzene, toluene and dimethylbenzene.
10. apply according to claim 8, it is characterised in that the condition of adsorption process is：Relative humidity 40%~80%,
25 DEG C of temperature.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108187625A (en) * | 2018-01-19 | 2018-06-22 | 清华大学 | It a kind of organic mesoporous silicon adsorbent of high hydrophobicity and its prepares and the application of purifying VOCs |
| CN108499525A (en) * | 2018-03-28 | 2018-09-07 | 中触媒新材料股份有限公司 | A kind of preparation method of the adsorbent of purifying hydrogen peroxide solution and the method for purification of hydrogen peroxide |
-
2017
- 2017-08-24 CN CN201710733199.2A patent/CN107469776A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| SHUAI LIU ET AL.: ""Studies on toluene adsorption performance and hydrophobic property in phenyl functionalized KIT-6"", 《CHEMICAL ENGINEERING JOURNAL》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108187625A (en) * | 2018-01-19 | 2018-06-22 | 清华大学 | It a kind of organic mesoporous silicon adsorbent of high hydrophobicity and its prepares and the application of purifying VOCs |
| CN108187625B (en) * | 2018-01-19 | 2021-02-02 | 清华大学 | High-hydrophobicity organic mesoporous silicon adsorbent, preparation thereof and application of adsorbent in purifying VOCs |
| CN108499525A (en) * | 2018-03-28 | 2018-09-07 | 中触媒新材料股份有限公司 | A kind of preparation method of the adsorbent of purifying hydrogen peroxide solution and the method for purification of hydrogen peroxide |
| CN108499525B (en) * | 2018-03-28 | 2021-02-12 | 中触媒新材料股份有限公司 | Preparation method of adsorbent for purifying hydrogen peroxide solution and purification method of hydrogen peroxide |
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