CN1749225A - A kind of preparation method of amine propyl functional porous material - Google Patents
A kind of preparation method of amine propyl functional porous material Download PDFInfo
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- CN1749225A CN1749225A CN 200510012772 CN200510012772A CN1749225A CN 1749225 A CN1749225 A CN 1749225A CN 200510012772 CN200510012772 CN 200510012772 CN 200510012772 A CN200510012772 A CN 200510012772A CN 1749225 A CN1749225 A CN 1749225A
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- amine propyl
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- porous material
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- trimethoxy silicane
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Abstract
A kind of preparation method of amine propyl functional porous material, it is that mass ratio by amine propyl trimethoxy silicane, hexanaphthene and carrier is the amine propyl trimethoxy silicane: hexanaphthene: carrier=5: 30～40: 3～4, the amine propyl trimethoxy silicane is configured to cyclohexane solution, under the ultrasonic wave effect of operating frequency 20-50KHz, after being uniformly dispersed carrier is immersed wherein, and sealing; With it in vibration under the ultrasonic wave effect of room temperature, operating frequency 20-50KHz after 1-2 hour, toluene extracting 8-12 hour, 80-100 ℃ vacuum-drying 8-12 hour, promptly get the porous material of amine propyl functional.It is simple that the present invention has the preparation method, easy to operate, the advantage of preparation condition gentleness.
Description
Technical field
The invention belongs to a kind of preparation method who is used for amine propyl functional porous material.
Background technology
In the past ten years, with one of immobilized focus that has become researcher research of homogeneous phase organic amine, and obtained swift and violent development.Supported organic amine is widely used in the fields such as preparation of catalysis, absorption, separation, host-guest chemistry and functional materials, at present, preparation grafting-type organic solid alkali required raw material be mainly organo silane coupling agent and weak polar solvent (as, toluene, dimethylbenzene, methylene dichloride, trichloromethane and hexanaphthene etc.), carrier has the metal oxide of hydroxyl based on the surface of silicon-based mesoporous molecular sieve and silica gel.It is main that traditional preparation method mainly carries out the reflux stirring to reaction system, and in order to improve the condensation level of silane coupling agent and silica gel surface hydroxyl, temperature of reaction is had relatively high expectations.This method is operated loaded down with trivial details to reaction kit equipment requirements complexity.Therefore, it is extremely urgent to seek a kind of engrafting method of simple gentleness.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of reaction, the preparation method of the amine propyl functional porous material of reaction conditions gentleness.
The present invention utilizes the cavitation effect of ultrasonic technology that the amine propyl trimethoxy silicane is fully contacted with the hydroxyl of carrier surface and the material that condensation reaction prepares the different porous supports of amine propyl functional takes place fast.
The method for making of catalyzer of the present invention comprises the steps
Mass ratio by amine propyl trimethoxy silicane, hexanaphthene and carrier is the amine propyl trimethoxy silicane: hexanaphthene: carrier=5: 30～40: 3～4, the amine propyl trimethoxy silicane is configured to cyclohexane solution, under the ultrasonic wave effect of operating frequency 20-50KHz, after being uniformly dispersed carrier is immersed wherein, and sealing; With it in vibration under the ultrasonic wave effect of room temperature, operating frequency 20-50KHz after 1-2 hour, toluene extracting 8-12 hour, 80-100 ℃ vacuum-drying 8-12 hour, promptly get the porous material of amine propyl functional.
Carrier used in the present invention is: silica gel, mesopore molecular sieve, aluminium sesquioxide or mordenite
The present invention compared with prior art has following advantage:
(1) preparation method is simple, and is easy to operate.
(2) preparation condition gentleness.
Embodiment
Embodiment 1:
5.0g amine propyl trimethoxy silicane joined in the 30g hexanaphthene be configured to solution, ultrasonic wave (operating frequency 50KHz) is uniformly dispersed the back to wherein adding 3.0g silica gel, and sealing.With this reaction system ultrasonic wave (operating frequency 50KHz) vibration 1 hour.Toluene extracting sample 8 hours, 100 ℃ of vacuum-drying 8 hours.Promptly get amine propyl functional silica gel.Sample is measured its C through elemental analyser, H, the quality percentage composition of N element.The results are shown in Table 1.
Embodiment 2:
5.0g amine propyl trimethoxy silicane joined in the 32g hexanaphthene be configured to solution, ultrasonic wave (operating frequency 40KHz) is uniformly dispersed the back to wherein adding 3.2g silica gel, and sealing.With this reaction system ultrasonic wave (operating frequency 40KHz) vibration 1.25 hours.Toluene extracting sample 9 hours, 95 ℃ of vacuum-drying 9 hours.Promptly get amine propyl functional silica gel.Sample is measured its C through elemental analyser, H, the quality percentage composition of N element.The results are shown in Table 1.
Embodiment 3:
5.0g amine propyl trimethoxy silicane joined in the 35g hexanaphthene dispose solution, ultrasonic wave (operating frequency 33KHz) is uniformly dispersed the back to wherein adding the 3.5g mesopore molecular sieve, and sealing.With this reaction system ultrasonic wave (operating frequency 33KHz) vibration 1.5 hours.Toluene extracting sample 10 hours, 90 ℃ of vacuum-drying 10 hours.Promptly get the amine propyl functional mesopore molecular sieve.Sample is measured its C through elemental analyser, H, the quality percentage composition of N element.The results are shown in Table 1.
Embodiment 4:
5.0g amine propyl trimethoxy silicane joined in the 37g hexanaphthene dispose solution, ultrasonic wave (operating frequency 28KHz) is uniformly dispersed the back to wherein adding the 3.7g aluminium sesquioxide, and sealing.With this reaction system ultrasonic wave (operating frequency 28KHz) vibration 1.75 hours.Toluene extracting sample 11 hours, 85 ℃ of vacuum-drying 11 hours.Promptly get the amine propyl functional aluminium sesquioxide.Sample is measured its C through elemental analyser, H, the quality percentage composition of N element.The results are shown in Table 1.
Embodiment 5:
5.0g amine propyl trimethoxy silicane joined in the 40g hexanaphthene dispose solution, ultrasonic wave (operating frequency 20KHz) is uniformly dispersed the back to wherein adding the 4.0g mordenite, and sealing.With this reaction system ultrasonic wave (operating frequency 20KHz) vibration 2 hours.Toluene extracting sample 12 hours, 80 ℃ of vacuum-drying 12 hours.Promptly get the amine propyl functional mordenite.Sample is measured its C through elemental analyser, H, the quality percentage composition of N element.The results are shown in Table 1.
Table 1
| Embodiment | Ultimate analysis (wt.%) | N org.％ (mmol/g) | ||
| N％ | C％ | H％ | ||
| Embodiment 1 | 1.58 | 4.60 | 1.32 | 1.13 |
| Embodiment 2 | 1.44 | 4.21 | 1.22 | 1.03 |
| Embodiment 3 | 1.42 | 4.36 | 1.85 | 1.02 |
| Embodiment 4 | 0.65 | 2.01 | 0.86 | 0.47 |
| Embodiment 5 | 3.33 | 9.15 | 2.91 | 2.38 |
Claims (2)
1, a kind of preparation method of amine propyl functional porous material is characterized in that comprising the steps:
Mass ratio by amine propyl trimethoxy silicane, hexanaphthene and carrier is the amine propyl trimethoxy silicane: hexanaphthene: carrier=5: 30～40: 3～4, the amine propyl trimethoxy silicane is configured to cyclohexane solution, under the ultrasonic wave effect of operating frequency 20-50KHz, after being uniformly dispersed carrier is immersed wherein, and sealing; With it in vibration under the ultrasonic wave effect of room temperature, operating frequency 20-50KHz after 1-2 hour, toluene extracting 8-12 hour, 80-100 ℃ vacuum-drying 8-12 hour, promptly get the porous material of amine propyl functional.
2, the preparation method of a kind of amine propyl functional porous material as claimed in claim 1 is characterized in that described carrier is silica gel, mesopore molecular sieve, aluminium sesquioxide or mordenite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510012772 CN1304340C (en) | 2005-08-29 | 2005-08-29 | Process for preparing amine propyl functional porous material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510012772 CN1304340C (en) | 2005-08-29 | 2005-08-29 | Process for preparing amine propyl functional porous material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1749225A true CN1749225A (en) | 2006-03-22 |
| CN1304340C CN1304340C (en) | 2007-03-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200510012772 Expired - Fee Related CN1304340C (en) | 2005-08-29 | 2005-08-29 | Process for preparing amine propyl functional porous material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104117343A (en) * | 2014-07-14 | 2014-10-29 | 中国人民解放军国防科学技术大学 | Preparation method of renewable low concentration CO2 high efficient absorption material |
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2005
- 2005-08-29 CN CN 200510012772 patent/CN1304340C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104117343A (en) * | 2014-07-14 | 2014-10-29 | 中国人民解放军国防科学技术大学 | Preparation method of renewable low concentration CO2 high efficient absorption material |
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| CN1304340C (en) | 2007-03-14 |
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Granted publication date: 20070314 Termination date: 20170829 |