CN1304340C - Process for preparing amine propyl functional porous material - Google Patents
Process for preparing amine propyl functional porous material Download PDFInfo
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- CN1304340C CN1304340C CN 200510012772 CN200510012772A CN1304340C CN 1304340 C CN1304340 C CN 1304340C CN 200510012772 CN200510012772 CN 200510012772 CN 200510012772 A CN200510012772 A CN 200510012772A CN 1304340 C CN1304340 C CN 1304340C
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- amine propyl
- porous material
- carrier
- ultrasonic wave
- 50khz
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Abstract
The present invention relates to a process for preparing an amino propyl functional porous material with amino propyl trimethyl silane, cyclohexane and carrier in the mass ratio of 5: 30 to 40: 3 to 4. The amino propyl trimethyl silane is made into cyclohexane solution, after dispersion is homogeneous under the action of ultrasonic wave in 20 to 50KHz work frequency, the carrier is immersed into the solution, and sealing is done. After oscillation is done for 1-2 h at room temperature and under the action of the ultrasonic wave in work frequency of 20 to 50KHz, the extraction of toluene is carried out for 8-12 h, and vacuum drying at 80 to 100 DEG C is carried out for 8-12 h to obtain the amino propyl functional porous material. The present invention has the advantages of simple preparation process, easy operation and mild preparation condition.
Description
Technical field
The invention belongs to a kind of preparation method who is used for amine propyl group 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 group 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 group 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 group.
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 group 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 group 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 amine propyl group 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 amine propyl group 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 amine propyl group 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 (1)
1, a kind of preparation method of amine propyl group 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 group;
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 CN1749225A (en) | 2006-03-22 |
| CN1304340C true 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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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104117343B (en) * | 2014-07-14 | 2016-02-03 | 中国人民解放军国防科学技术大学 | A kind of renewable low concentration CO 2the preparation method of efficient adsorption material |
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