CN115304748A - Preparation method of porous polymer material - Google Patents
Preparation method of porous polymer material Download PDFInfo
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- CN115304748A CN115304748A CN202211069860.1A CN202211069860A CN115304748A CN 115304748 A CN115304748 A CN 115304748A CN 202211069860 A CN202211069860 A CN 202211069860A CN 115304748 A CN115304748 A CN 115304748A
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G61/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G61/02—Macromolecular compounds containing only carbon atoms in the main chain of the macromolecule, e.g. polyxylylenes
- C08G61/025—Polyxylylenes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G2261/10—Definition of the polymer structure
- C08G2261/11—Homopolymers
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G2261/30—Monomer units or repeat units incorporating structural elements in the main chain
- C08G2261/31—Monomer units or repeat units incorporating structural elements in the main chain incorporating aromatic structural elements in the main chain
- C08G2261/312—Non-condensed aromatic systems, e.g. benzene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G2261/30—Monomer units or repeat units incorporating structural elements in the main chain
- C08G2261/33—Monomer units or repeat units incorporating structural elements in the main chain incorporating non-aromatic structural elements in the main chain
- C08G2261/332—Monomer units or repeat units incorporating structural elements in the main chain incorporating non-aromatic structural elements in the main chain containing only carbon atoms
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Abstract
The invention discloses a preparation method of a porous polymer material, which comprises the following steps: and (2) taking a sodium-potassium alloy as a metal reducing agent, taking hexachloro-p-xylene as a precursor, stirring at room temperature, and controlling the reaction time to adjust the pore structure of the porous polymer material, thereby finally preparing the porous polymer material. The preparation method provided by the invention has advanced process and full and precise data, does not need additional template agent and high-temperature roasting, greatly shortens the preparation time and reduces the energy consumption of reaction; the product obtained by the method is yellow powder, has a porous pore channel structure, has a product yield of 81.2 percent, and can be used as CO after being modified by organic matters 2 The catalyst of cycloaddition reaction is an ideal method for preparing porous polymer material.
Description
Technical Field
The invention relates to the technical field of preparation and application of porous materials, in particular to a preparation method of a porous polymer material.
Background
The porous polymer material has the advantages of good structure adjustability, adsorption performance, higher specific surface area, larger pore volume and the like, and is widely applied to the fields of adsorption, catalysis, gas separation and the like.
The synthesis method and the process of the porous polymer material directly influence the structural characteristics and the performance of the material, the selection of the synthesis method and the template is a decisive influence factor, and the reaction temperature and the reaction time also have important influence on the pore channel structure of the porous polymer material.
The template is a basic component for preparing the porous polymer material, and the precursor and the template form a porous structure through supermolecular force or chemical action. The structure and kind of the template will affect the channel structure of the porous polymer material, and therefore the selection and use of the template is very important.
In the process of synthesizing the porous polymer material by taking an organic matter as a precursor, a soft template or a hard template is mostly needed to be used as a structure directing agent, and due to the fact that different selected chemical substances, different synthesis parameters and different synthesis processes exist, the synthesis temperature is from 100 ℃ to 200 ℃, the obtained porous polymer material has large difference in chemical and physical properties, and the requirements of the synthesized substances are difficult to meet, so that the application of the material is greatly limited.
Disclosure of Invention
In view of this, the present invention discloses a preparation method of a porous polymer material, which provides a new reaction path for the preparation of the porous polymer material.
The technical scheme provided by the invention is specifically that a preparation method of a porous polymer material comprises the following steps: and (2) taking a sodium-potassium alloy as a metal reducing agent, taking hexachloro-p-xylene as a precursor, stirring at room temperature, and controlling the reaction time to adjust the pore structure of the porous polymer material, thereby finally preparing the porous polymer material.
Further, the method comprises the following reactants: metal sodium, metal potassium, hexachloro-p-xylene, tetrahydrofuran, ethanol and deionized water;
the combined dosage is as follows: taking g and ml as the measurement unit,
the method comprises the following steps:
(1) Preparing a sodium-potassium alloy: weighing 0.1g +/-0.01 g of metal sodium, weighing 0.4g +/-0.02 g of metal potassium, and stirring for 1 minute to prepare a sodium-potassium alloy;
(2) Synthesis of porous polymer materials: weighing 0.6g +/-0.02 g of hexachloro-p-xylene under the protection of nitrogen, dissolving the hexachloro-p-xylene in 10mL +/-0.5 mL of tetrahydrofuran, stirring for 5 minutes, adding the prepared sodium-potassium alloy, stirring and reducing at room temperature, reacting for 24 hours, adding 20mL +/-1 mL of ethanol, continuously stirring for 30 minutes, and filtering to obtain a solid to obtain an intermediate product;
(3) Washing and suction filtration:
(4) And (3) vacuum drying: drying to obtain the porous polymer material;
(5) Detection, analysis and characterization: the morphology, the components and the chemical and physical properties of the prepared porous polymer material are detected, analyzed and characterized.
Further, the specific steps of washing and suction filtration in the step (3) are as follows: placing the filtered product in a beaker, adding 100mL of deionized water, and stirring and washing for 5 minutes; placing the washing liquid in a Buchner funnel of a filter flask, performing suction filtration by using a microporous filter membrane, reserving a product filter cake on the filter membrane, pumping the washing liquid into the filter flask, and performing washing and suction filtration for 2 times; adding tetrahydrofuran 100mL, stirring and washing for 5 minutes, washing and filtering for 2 times.
Further, the vacuum drying in the step (4) comprises the following specific steps: and (3) placing the washed product filter cake into a glass container, and then placing the glass container into a vacuum drying oven for drying at the drying temperature of 50 +/-1 ℃ under the vacuum degree of 50Pa for 10 hours.
The preparation method of the porous polymer material provided by the invention has the advantages of advanced preparation method and process, full and precise data, no need of additional template agent and high-temperature roasting, and great improvement on the preparation methodThe preparation time is shortened, and the reaction energy consumption is reduced; the product obtained by the method is yellow powder, has a porous pore channel structure, has a product yield of 81.2 percent, and can be used as CO after being modified by organic matters 2 The catalyst of cycloaddition reaction is an ideal method for preparing porous polymer material.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments or prior art solutions of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a diagram illustrating a state of synthesis and preparation of a porous polymer material provided in an embodiment of the present disclosure;
FIG. 2 is an X-ray diffraction pattern of a porous polymeric material provided in accordance with an embodiment of the present disclosure;
FIG. 3 is a graph illustrating nitrogen adsorption and desorption for a porous polymer material according to an embodiment of the present disclosure;
FIG. 4 is a transmission electron micrograph of a porous polymeric body material provided in accordance with an embodiment of the disclosure.
Detailed Description
Reference will now be made in detail to the exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The implementations described in the following exemplary examples do not represent all implementations consistent with the present invention. Rather, they are merely examples of systems consistent with certain aspects of the invention, as detailed in the appended claims.
In order to solve the problems that in the prior art, in the process of synthesizing the porous polymer material by taking an organic matter as a precursor, a soft template or a hard template is mostly needed to be used as a structure directing agent, so that the obtained porous polymer material has large difference of chemical and physical properties, the requirement of a synthetic substance is difficult to meet and the like 2 Catalysts for cycloaddition reactions.
Specifically, the method comprises the following chemical substance materials: metal sodium, metal potassium, hexachloro-p-xylene, tetrahydrofuran, ethanol and deionized water;
the combined dosage is as follows: taking g and ml as the measurement unit,
the preparation method comprises the following steps:
(1) Preparing a sodium-potassium alloy: weighing 0.1g +/-0.01 g of metal sodium, weighing 0.4g +/-0.02 g of metal potassium, and stirring for 1 minute to prepare a sodium-potassium alloy;
(2) Synthesis of porous polymer materials: weighing 0.6g +/-0.02 g of hexachloro-p-xylene under the protection of nitrogen, dissolving the hexachloro-p-xylene in 10mL +/-0.5 mL of tetrahydrofuran, stirring for 5 minutes, adding the prepared sodium-potassium alloy, stirring and reducing at room temperature, reacting for 24 hours, adding 20mL +/-1 mL of ethanol, continuously stirring for 30 minutes, and filtering to obtain a solid to obtain an intermediate product;
(3) Washing and suction filtration:
(4) And (3) vacuum drying: drying to obtain the porous polymer material;
(5) Detection, analysis and characterization: the morphology, the components and the chemical and physical properties of the prepared porous polymer material are detected, analyzed and characterized.
The step (2) specifically comprises the following steps:
A. preparing a mixed reaction mixture: weighing 0.6g +/-0.02 g of hexachloro-p-xylene and 0.5g +/-0.03 g of sodium-potassium alloy, weighing 10mL +/-0.5 mL of tetrahydrofuran, and adding into a round-bottom flask to obtain a mixed reaction solution;
B. starting magnetic stirring, stirring for 24 hours, and reacting the mixed reaction solution at room temperature.
C. After the reaction is finished, adding 20mL +/-1 mL of ethanol, continuously stirring for 30 minutes at room temperature, and stopping stirring; and (3) suction filtration: and placing the reacted mixture into a Buchner funnel of a filter flask, carrying out suction filtration by using a microporous filter membrane, and pumping the residual product filter cake waste liquid on the filter membrane into the filter flask.
The concrete steps of washing and suction filtration in the step (3) are as follows: placing the filtered product in a beaker, adding 100mL of deionized water, and stirring and washing for 5 minutes; placing the washing liquid in a Buchner funnel of a filter flask, performing suction filtration by using a microporous filter membrane, reserving a product filter cake on the filter membrane, pumping the washing liquid into the filter flask, and performing washing and suction filtration for 2 times; adding tetrahydrofuran 100mL, stirring and washing for 5 minutes, washing and filtering for 2 times.
The vacuum drying in the step (4) comprises the following specific steps: and (3) placing the washed product filter cake into a glass container, and then placing the glass container into a vacuum drying oven for drying at the drying temperature of 50 +/-1 ℃ under the vacuum degree of 50Pa for 10 hours.
The porous polymer material prepared by the preparation method can be used as CO after being modified by organic matters 2 Catalysts for cycloaddition reactions.
FIG. 1 is a diagram showing the state of the synthesis and preparation of a porous polymer material, in which the positions of the components are correct, proportioned by weight and operated sequentially; the amount of chemical substance used for preparation is determined in a preset range, and the measured unit is gram and milliliter.
The synthesis of the porous polymer material is carried out in a glass round-bottom flask and is completed under the condition of stirring at room temperature;
the stirrer is rectangular, the round-bottom flask 2 is fixed on a fixing rod 4 of the stirring table 3 by using an iron clamp 1, the magnetic stirrer 5 is arranged at the bottom of the conical flask, and the mouth of the conical flask is sealed by a plastic rubber plug 6. The stirrer base 7 is provided with a display screen 8, an indicator light 9, a power switch 10 and a rotating speed regulator 11.
The invention will now be further illustrated with reference to specific examples, which are not intended to limit the scope of the invention.
The preparation method comprises the following steps:
(1) Selecting chemical materials
The chemical material used for preparation is selected and subjected to quality purity control:
(2) Preparation of sodium-potassium alloy
Weighing 0.1g +/-0.01 g of metal sodium, weighing 0.4g +/-0.02 g of metal potassium, and stirring for 1 minute to prepare a sodium-potassium alloy;
(3) Synthetic porous polymer material
The synthesis of the porous polymer material was carried out under nitrogen protection, reduced with stirring at room temperature, and then filtered to give a solid.
(1) Preparing a mixed reaction mixture
Weighing 0.6g +/-0.02 g of hexachloro-p-xylene, 0.1g +/-0.01 g of sodium-potassium alloy and 10mL +/-0.5 mL of tetrahydrofuran;
adding the mixture into a round-bottom flask to obtain a mixed reaction solution;
(2) starting magnetic stirring for 24 hours, mixing the reaction solution for reaction,
(3) after the reaction is finished, adding 20mL +/-1 mL of ethanol, continuing stirring for 30 minutes, and stopping stirring;
(4) Suction filtration
Placing the reacted mixture into a Buchner funnel of a filter flask, carrying out suction filtration by using a microporous filter membrane, remaining a product filter cake on the filter membrane, and pumping the waste liquid into the filter flask;
(5) Washing and suction filtering
Placing the filtered product in a beaker, adding 100mL of deionized water, and stirring and washing for 5 minutes;
placing the washing liquid in a Buchner funnel of a filter flask, carrying out suction filtration by using a microporous filter membrane, reserving a product filter cake on the filter membrane, and pumping the washing liquid into the filter flask;
washing and filtering for 2 times;
putting the product filter cake into a beaker, adding 100mL of deionized water, and stirring and washing for 5 minutes;
adding 100mL of ethanol, stirring and washing for 5 minutes,
washing and suction filtering are carried out for 2 times.
(6) Vacuum drying
Putting the washed product filter cake into a glass container, and then putting the glass container into a vacuum drying oven for drying at the drying temperature of 50 +/-1 ℃ and the vacuum degree of 50Pa for 10 hours;
drying to obtain the porous polymer material;
(7) Detection, analysis, characterization
Detecting, analyzing and characterizing the morphology, the components and the chemical and physical properties of the prepared porous polymer material;
carrying out structural analysis on the material by using an X-ray diffractometer; the results are shown in fig. 2, which is an X-ray diffraction pattern of the porous polymeric material, and it can be seen in fig. 2 that the resulting material has an amorphous crystalline structure.
Analyzing the pore structure of the material by using a nitrogen physical adsorption instrument; as shown in fig. 3, which is a graph showing nitrogen adsorption and desorption of the porous polymer material, it can be seen that the obtained porous polymer material has a porous channel structure.
Carrying out microstructure analysis on the material by using a transmission electron microscope; results fig. 4 shows a transmission electron micrograph of the porous polymer body material, in which it can be seen that the resulting porous polymer body material has a channel structure. The figures are all processed by a material studio software program;
the conclusion is that: the material for synthesizing the porous polymer body at room temperature is yellow powder, the material has a mesoporous channel structure, and the product yield is 81.2%;
(8) Product storage
The prepared porous polymer material is stored in a brown transparent glass container, is stored in a closed and dark place, and needs to be waterproof, moistureproof, sun-proof and acid, alkali and salt corrosion resistant, the storage temperature is 20 +/-2 ℃, and the relative humidity is less than or equal to 10%.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. This application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.
It will be understood that the invention is not limited to the precise arrangements described above and shown in the drawings and that various modifications and changes may be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.
Claims (4)
1. A method of preparing a porous polymeric material, comprising: and (2) taking a sodium-potassium alloy as a metal reducing agent, taking hexachloro-p-xylene as a precursor, stirring at room temperature, and controlling the reaction time to adjust the pore structure of the porous polymer material, thereby finally preparing the porous polymer material.
2. The method of claim 1, comprising the reactants of: metal sodium, metal potassium, hexachloro-p-xylene, tetrahydrofuran, ethanol and deionized water;
the combined dosage is as follows: taking g and ml as the measurement unit,
the method comprises the following steps:
(1) Preparing a sodium-potassium alloy: weighing 0.1g +/-0.01 g of metal sodium, weighing 0.4g +/-0.02 g of metal potassium, and stirring for 1 minute to prepare a sodium-potassium alloy;
(2) Synthesis of porous polymer materials: weighing 0.6g +/-0.02 g of hexachloro-p-xylene under the protection of nitrogen, dissolving the hexachloro-p-xylene in 10mL +/-0.5 mL of tetrahydrofuran, stirring for 5 minutes, adding the prepared sodium-potassium alloy, stirring and reducing at room temperature, reacting for 24 hours, adding 20mL +/-1 mL of ethanol, continuously stirring for 30 minutes, and filtering to obtain a solid to obtain an intermediate product;
(3) Washing and suction filtration:
(4) And (3) vacuum drying: drying to obtain the porous polymer material;
(5) Detection, analysis and characterization: the morphology, the components and the chemical and physical properties of the prepared porous polymer material are detected, analyzed and characterized.
3. The method for preparing the porous polymer material according to claim 1, wherein the washing and suction filtration in the step (3) comprises the following specific steps: placing the filtered product in a beaker, adding 100mL of deionized water, and stirring and washing for 5 minutes; placing the washing liquid in a Buchner funnel of a filter flask, performing suction filtration by using a microporous filter membrane, remaining a product filter cake on the filter membrane, pumping the washing liquid into the filter flask, and performing washing and suction filtration for 2 times; adding tetrahydrofuran 100mL, stirring and washing for 5 minutes, washing and filtering for 2 times.
4. The method for preparing a porous polymer material according to claim 1, wherein the vacuum drying in step (4) comprises the following steps: and (3) placing the washed product filter cake into a glass container, and then placing the glass container into a vacuum drying oven for drying at the drying temperature of 50 +/-1 ℃ under the vacuum degree of 50Pa for 10 hours.
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