CN103275286A - Preparation method and application of selective adsorptive separation porous organic polymer material - Google Patents
Preparation method and application of selective adsorptive separation porous organic polymer material Download PDFInfo
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Abstract
Provided is a preparation method of a selective adsorptive separation porous organic polymer material. The polymer material is a porous organic polymer material condensed from melamine and 2,4,6-trihydroxy isophthalaldehyde and is obtained through the condensation reaction between the melamine and 2,4,6-trihydroxy isophthalaldehyde and removal of micro-molecular polymers and low-molecular polymers through Soxhlet extraction. The preparation method has the advantages that the organic porous polymer material has a relatively good adsorption performance on the carbon dioxide under the conditions of ordinary pressures of 273K and 298K, but barely adsorbs methane or nitrogen, so that the selective adsorptive separation porous organic polymer material can serve as an adsorptive separation material in the application.
Description
Technical field
The present invention relates to the porous organo polysilica laminate material, particularly a kind of selective adsorption separates preparation and the application thereof of porous organo polysilica laminate material.
Background technology
In recent years, environment and energy problem become the focus that international community pays close attention to gradually, also are one of the severeest problems of facing of current mankind.Utilize porous material to separate and stored energy source gas hydrogen, methane etc., the capturing ambient atmospheric carbon dioxide, and multifunction research has become chemistry and one of the focus of materialogy research and field, forward position.The porous organo polysilica laminate material has higher thermostability and chemical stability, such material is because of its synthetic diversity in addition, can modify its hole surface by the construction unit that choose reasonable connects, thereby change performances such as its absorption, separation, catalysis, consult: Dawson, R. Cooper, A. I. Adams, D. J. Prog. Polym. Sci. 2012,37,530; Zhang, Y. Riduan, S. N. Chem. Soc. Rev., 2012,41,2083; Xiang, Z. Cao, D. J. Mater. Chem. A, 2013,1,2691; Chang, Z. Zhang, D.-S. Chen, Q. Bu, X.-H. Phys. Chem. Chem. Phys., 2013,15,5430.This makes it be expected to be used and develop in the Application Areas of traditional molecular screen material, especially separates in gas adsorption, and fields such as the purification of Sweet natural gas, separation have broad prospect of application.
Summary of the invention
The objective of the invention is at above-mentioned technical Analysis, provide a kind of selective adsorption to separate preparation and the application thereof of porous organo polysilica laminate material, this material is based on trimeric cyanamide and 2,4, the porous organo polysilica compound of 6-trihydroxy-m-terephthal aldehyde condensation, carbonic acid gas is had stronger adsorption function, and adsorbed methane and nitrogen hardly.
Technical scheme of the present invention:
A kind of selective adsorption separates the preparation method of porous organo polysilica laminate material, and described polymer materials is that its preparation method comprises the steps: based on the porous organo polysilica compound of trimeric cyanamide and the condensation of 2,4,6-trihydroxy-m-terephthal aldehyde
1) trimeric cyanamide and 2,4,6-trihydroxy-m-terephthal aldehyde are dissolved in the methyl-sulphoxide, are stirred to solid and dissolve fully;
2) reacted 72 hours at 433-458 K under argon shield, the agitation condition; filter then; use methyl-sulphoxide volume and washed with dichloromethane solid respectively; then the sorrel solid that obtains was extracted 48 hours with methylene dichloride and tetrahydrofuran (THF) in apparatus,Soxhlet's successively, obtain pulverous organic porous polymer material.
The mol ratio of described trimeric cyanamide and 2,4,6-trihydroxy-m-terephthal aldehyde is 1:1-3, and the amount ratio of trimeric cyanamide and methyl-sulphoxide is 2 mmoles: 25 milliliters.
The volume ratio of methyl-sulphoxide is 0.4:1 in the methyl-sulphoxide of described washing solid and the step 1), and the volume ratio of methyl-sulphoxide is 0.8:1 in the methylene dichloride of washing solid and the step 1).
A kind of prepared selective adsorption separates the application of porous organo polysilica laminate material, this polymkeric substance all has stronger absorption property to carbonic acid gas under 273K, 298K condition of normal pressure, and adsorbed methane and nitrogen hardly, thereby can be used as the carbon dioxide adsorption and separation material.
Advantage of the present invention is: this organic porous polymer material all has stronger absorption property to carbonic acid gas under 273K, 298K condition of normal pressure, and adsorbed methane and nitrogen hardly are applied thereby can be used as adsorption and separation material.
Description of drawings
Carbonic acid gas, methane and the nitrogen adsorption figure of organic porous polymer material that accompanying drawing makes for embodiment.
Embodiment
Embodiment:
A kind of selective adsorption separates the preparation method of porous organo polysilica laminate material, and described polymer materials is that its preparation method comprises the steps: based on the porous organo polysilica compound of trimeric cyanamide and the condensation of 2,4,6-trihydroxy-m-terephthal aldehyde
1) in 50 milliliters there-necked flask, with 2 mmole trimeric cyanamides and 3 mmoles 2,4,6-trihydroxy-m-terephthal aldehyde is dissolved in the dimethylsulfoxide solvent that 25 milliliters of drying treatment cross, and is stirred to solid and dissolves fully;
2) reacted 72 hours at 433-458K under argon shield, the agitation condition; filter then and remove solution; use 10 milliliters of methyl-sulphoxides and 20 milliliters of washed with dichloromethane solids respectively; then the sorrel solid that obtains was extracted 48 hours with methylene dichloride and tetrahydrofuran (THF) in apparatus,Soxhlet's successively, obtain pulverous organic porous polymer material.
Prepared selective adsorption separates the porous organo polysilica laminate material, can be used as the carbon dioxide adsorption and separation material, and it all has stronger absorption property to carbonic acid gas under 273K, 298K condition of normal pressure, and adsorbed methane and nitrogen hardly.
Carbonic acid gas, methane and the nitrogen adsorption figure of organic porous polymer material that accompanying drawing makes for this embodiment, show among the figure: this material has highly selective to carbonic acid gas/methane separation or carbonic acid gas/nitrogen separation.
Claims (4)
1. a selective adsorption separates the preparation method of porous organo polysilica laminate material, it is characterized in that: described polymer materials is based on trimeric cyanamide and 2,4, the porous organo polysilica compound of 6-trihydroxy-m-terephthal aldehyde condensation, and its preparation method comprises the steps:
1) trimeric cyanamide and 2,4,6-trihydroxy-m-terephthal aldehyde are dissolved in the methyl-sulphoxide, are stirred to solid and dissolve fully;
2) reacted 72 hours at 433-458 K under argon shield, the agitation condition; filter then; use methyl-sulphoxide volume and washed with dichloromethane solid respectively; then the sorrel solid that obtains was extracted 48 hours with methylene dichloride and tetrahydrofuran (THF) in apparatus,Soxhlet's successively, obtain pulverous organic porous polymer material.
2. described selective adsorption separates the preparation method of porous organo polysilica laminate material according to claim 1, it is characterized in that: described trimeric cyanamide and 2, the mol ratio of 4,6-trihydroxy-m-terephthal aldehyde is 1:1-3, and the amount ratio of trimeric cyanamide and methyl-sulphoxide is 2 mmoles: 25 milliliters.
3. described selective adsorption separates the preparation method of porous organo polysilica laminate material according to claim 1, it is characterized in that: the volume ratio of methyl-sulphoxide is 0.4:1 in the methyl-sulphoxide of described washing solid and the step 1), and the volume ratio of methyl-sulphoxide is 0.8:1 in the methylene dichloride of washing solid and the step 1).
4. the prepared selective adsorption of claim 1 separates the application of porous organo polysilica laminate material, it is characterized in that: this polymkeric substance all has stronger absorption property to carbonic acid gas under 273K, 298K condition of normal pressure, and adsorbed methane and nitrogen hardly, thereby can be used as the carbon dioxide adsorption and separation material.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910379A (en) * | 2014-03-12 | 2015-09-16 | 周卫星 | Preparation method of amino group-containing porous material, and application of amino group-containing porous material in recover of waste electric appliance precious metals |
| CN106749286A (en) * | 2016-12-09 | 2017-05-31 | 北京理工大学 | NN-bond-connected organic porous polymer material and preparation method thereof |
| CN109517130A (en) * | 2018-10-31 | 2019-03-26 | 韶关市合众化工有限公司 | Melamine derivative modified aqueous polyurethane flame-proof antibiotic resin and preparation method thereof |
| CN109880032A (en) * | 2019-01-16 | 2019-06-14 | 大连理工大学 | Rich nitrogen micropore organic polymer containing functional group and preparation method thereof |
| CN110354702A (en) * | 2019-06-20 | 2019-10-22 | 郑州大学 | One kind being used for CO2/N2The mixed substrate membrane containing nano-grade molecular sieve and preparation method thereof of gas separation |
| CN111333836A (en) * | 2020-03-12 | 2020-06-26 | 江苏科技大学 | Porous covalent organic polymer based on melamine, preparation method and application thereof |
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| CN102430396A (en) * | 2011-09-16 | 2012-05-02 | 华东理工大学 | Synthetic method of spherical nitrogen-enriched micro-reticular resin for CO2 adsorption |
| CN102584902A (en) * | 2012-01-11 | 2012-07-18 | 南开大学 | Microporous cobalt coordination polymer and preparation method and application thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102430396A (en) * | 2011-09-16 | 2012-05-02 | 华东理工大学 | Synthetic method of spherical nitrogen-enriched micro-reticular resin for CO2 adsorption |
| CN102584902A (en) * | 2012-01-11 | 2012-07-18 | 南开大学 | Microporous cobalt coordination polymer and preparation method and application thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910379A (en) * | 2014-03-12 | 2015-09-16 | 周卫星 | Preparation method of amino group-containing porous material, and application of amino group-containing porous material in recover of waste electric appliance precious metals |
| CN106749286A (en) * | 2016-12-09 | 2017-05-31 | 北京理工大学 | NN-bond-connected organic porous polymer material and preparation method thereof |
| CN106749286B (en) * | 2016-12-09 | 2019-06-11 | 北京理工大学 | NN-bond-connected organic porous polymer material and preparation method thereof |
| CN109517130A (en) * | 2018-10-31 | 2019-03-26 | 韶关市合众化工有限公司 | Melamine derivative modified aqueous polyurethane flame-proof antibiotic resin and preparation method thereof |
| CN109880032A (en) * | 2019-01-16 | 2019-06-14 | 大连理工大学 | Rich nitrogen micropore organic polymer containing functional group and preparation method thereof |
| CN110354702A (en) * | 2019-06-20 | 2019-10-22 | 郑州大学 | One kind being used for CO2/N2The mixed substrate membrane containing nano-grade molecular sieve and preparation method thereof of gas separation |
| CN110354702B (en) * | 2019-06-20 | 2021-10-08 | 郑州大学 | For CO2/N2Mixed matrix membrane for gas separation and preparation method thereof |
| CN111333836A (en) * | 2020-03-12 | 2020-06-26 | 江苏科技大学 | Porous covalent organic polymer based on melamine, preparation method and application thereof |
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