CN108212119B - Preparation method of composite filter screen - Google Patents
Preparation method of composite filter screen Download PDFInfo
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- CN108212119B CN108212119B CN201711281249.4A CN201711281249A CN108212119B CN 108212119 B CN108212119 B CN 108212119B CN 201711281249 A CN201711281249 A CN 201711281249A CN 108212119 B CN108212119 B CN 108212119B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
Abstract
The invention discloses a preparation method of a composite filter screen, which specifically comprises the following steps: (1) mixing the two monomers; (2) adding a cross-linking agent solution into a reaction vessel, and adding a proper amount of acetic acid; (3) adding the well-aligned sub-micron fibers to a reaction vessel; (4) deoxidizing and sealing the reaction mixture, heating at constant temperature, and standing for reaction for several days; (5) after the reaction is finished, the product after being fully washed is dried in vacuum; (6) placing the dried porous polymer in an HF acid solution to corrode and remove fibers; (7) and depositing metal on the surface of the polymer porous structure by adopting an electroplating method to obtain the metal-polymer composite filter screen. The structure is controllable, the thermal stability is good, and the adsorption cycle performance is good; a plurality of nano holes exist in the molecule, so that the selective layer of the material is looser, and the high flux and the high retention rate of the material are kept under the lower operation pressure; green and pollution-free, simple operation, low energy consumption, high efficiency and multiple functions.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of a composite filter screen.
Background
Porous materials are widely found in nature, and zeolite, molecular sieve, sponge and the like are typical porous materials. The porous material is favored by people due to the unique advantages of large specific surface area and adjustable pore diameter, and people synthesize some functional porous materials on the basis of natural porous materials. The covalent organic porous polymer material is a novel porous material and is formed by connecting light elements such as carbon, hydrogen, oxygen, nitrogen, boron and the like through covalent bonds. Compared with common organic porous materials, the covalent organic porous polymer material has incomparable advantages: composed of light elements and therefore having a lower skeleton density; the structural units are connected through covalent bonds, so that the thermal stability and the chemical stability are excellent; the aperture and the function of the device can be designed in advance, and the device has structural controllability and functional adjustability; the synthesis method is numerous, the synthesis condition is simple, and the synthesis monomers are various. Based on the characteristics, the covalent organic porous polymer material has great potential in the aspects of energy, substance adsorption and separation, catalysis, chemical sensing, biomedicine and the like. The metal-polymer composite filter screen is a novel filter screen, can separate and filter substances, organisms and the like, and has important application in the fields of mining industry, petroleum, chemical industry, food, medicine, mechanical manufacturing and the like. In the pharmaceutical, chemical, beverage and other industries, filtration operations are often performed to separate some solids from liquids. The commonly used solid materials comprise filter cloth and filter paper, the filter paper is used most in the beverage industry, and the material has high breakage rate and short service life. How to develop a preparation method of a composite filter screen with good filtering effect has important practical significance.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of a composite filter screen.
The technical scheme adopted by the invention is as follows:
a preparation method of a composite filter screen specifically comprises the following steps:
(1) adding two monomers, namely 1, 5-diaminoanthracene and mesitylene trimethyl aldehyde, into a reaction vessel according to a certain proportion;
(2) dissolving a cross-linking agent in a 1, 4-dioxane solvent to prepare a solution with the concentration: 5X 10-3-8×l0-2Adding a proper amount of acetic acid into the cross-linking agent solution, and integrally adding the cross-linking agent solution into the reaction container;
(3) adding regularly arranged submicron fibers into a reaction vessel, wherein the addition amount of the submicron fibers is 2-3% of the reaction solution;
(4) deoxidizing the reaction mixture, sealing the reaction container, heating at constant temperature, and standing for several days;
(5) after the reaction is finished, cooling to room temperature, carrying out vacuum filtration on the product, fully washing the product with an organic solvent, and carrying out vacuum drying on the fully washed product;
(6) placing the dried porous polymer in an HF acid solution to corrode and remove fibers to form a hollow/solid controllable spherical porous structure of the polymer;
(7) and depositing metal on the surface of the polymer porous structure by adopting an electroplating method to obtain the metal-polymer composite filter screen.
Further, the cross-linking agent in the step (2) is a mixture of terephthalic acid and dihydroxy end group polyethylene glycol with the molecular weight of 200-2000 according to the weight ratio of 2: 3.
Further, the organic solvent in the step (5) is any one of dichloromethane, acetone, tetrahydrofuran or 1, 4-dioxane.
Further, the vacuum drying method in the step (5) is to control the drying temperature to be 80-120 ℃ in the vacuum drying oven for drying for 6-12 hours.
Further, the metal in the step (7) is any one or more of gold, silver, nickel, copper and iron.
The invention has the beneficial effects that:
the organic porous polymer material has the advantages of controllable structure, good thermal stability, good adsorption cycle performance, repeated use and good adsorption material; the polymer has a nearly spherical structure due to the crosslinking effect, and a plurality of nano holes exist in the molecule, so that a selective layer of the material is looser, and the high flux and the high retention rate of the material are kept under the lower operation pressure; the method is green and pollution-free, is simple to operate, low in energy consumption and high in efficiency, is suitable for industrial large-scale production, has multiple functions, can be used for capturing and storing volatile harmful substances such as iodine, and is high in adsorption efficiency; the obtained microstructure can be applied to the fields of mining industry, petroleum industry, chemical industry, food, medicine, mechanical manufacturing and the like.
Drawings
FIG. 1 is a Fourier transform-infrared spectrum of examples 1 and 2 of the present invention;
FIG. 2 is a thermogravimetric plot of examples 1 and 2 of the present invention in a nitrogen atmosphere.
Detailed Description
The present invention is further illustrated by the following examples.
Example 1
A preparation method of a composite filter screen specifically comprises the following steps:
(1) adding two monomers, namely 1, 5-diaminoanthracene and mesitylene trimethyl aldehyde, into a reaction vessel according to a certain proportion;
(2) dissolving a cross-linking agent in a 1, 4-dioxane solvent to prepare a solution with the concentration: 5X 10-3Adding a proper amount of acetic acid into the cross-linking agent solution, and integrally adding the cross-linking agent solution into the reaction container; the cross-linking agent is a mixture of terephthalic acid and dihydroxy end group polyethylene glycol with the molecular weight of 200-2000 in a weight ratio of 2: 3;
(3) adding regularly arranged submicron fibers into a reaction vessel, wherein the addition amount of the submicron fibers is 2-3% of the reaction solution;
(4) deoxidizing the reaction mixture, sealing the reaction container, heating at constant temperature, and standing for several days;
(5) after the reaction is finished, cooling to room temperature, carrying out vacuum filtration on the product, fully washing the product by using an organic solvent dichloromethane, and carrying out vacuum drying on the fully washed product; the vacuum drying method comprises controlling the drying temperature at 80 deg.C in a vacuum drying oven for 12 h;
(6) placing the dried porous polymer in an HF acid solution to corrode and remove fibers to form a hollow/solid controllable spherical porous structure of the polymer;
(7) and depositing metal gold on the surface of the polymer porous structure by adopting an electroplating method to obtain the metal-polymer composite filter screen.
Example 2
A preparation method of a composite filter screen specifically comprises the following steps:
(1) adding two monomers, namely 1, 5-diaminoanthracene and mesitylene trimethyl aldehyde, into a reaction vessel according to a certain proportion;
(2) dissolving a cross-linking agent in a 1, 4-dioxane solvent to prepare a solution with the concentration: 6 xl 0-2Adding a proper amount of acetic acid into the cross-linking agent solution, and integrally adding the cross-linking agent solution into the reaction container; the cross-linking agent is a mixture of terephthalic acid and dihydroxy end group polyethylene glycol with the molecular weight of 200-2000 in a weight ratio of 2: 3;
(3) adding regularly arranged submicron fibers into a reaction vessel, wherein the addition amount of the submicron fibers is 2-3% of the reaction solution;
(4) deoxidizing the reaction mixture, sealing the reaction container, heating at constant temperature, and standing for several days;
(5) after the reaction is finished, cooling to room temperature, carrying out vacuum filtration on the product, fully washing the product by using an organic solvent acetone, and carrying out vacuum drying on the fully washed product; the vacuum drying method comprises controlling the drying temperature at 100 deg.C for 10h in a vacuum drying oven;
(6) placing the dried porous polymer in an HF acid solution to corrode and remove fibers to form a hollow/solid controllable spherical porous structure of the polymer;
(7) and depositing metal nickel on the surface of the polymer porous structure by adopting an electroplating method to obtain the metal-polymer composite filter screen.
As shown in fig. 1, fourier transform-infrared spectrogram of the present invention in example 1 and example 2; wherein 1 represents monomer trimesic aldehyde, 2 represents monomer 1, 5-diaminoanthracene, and the spectrogram shows that 1627cm-1 in 2 is-N-H-bending vibration, 3400-.
As shown in fig. 2: thermogravimetric curves of examples 1 and 2 of the present invention in a nitrogen atmosphere;
example 3
A preparation method of a composite filter screen specifically comprises the following steps:
(1) adding two monomers, namely 1, 5-diaminoanthracene and mesitylene trimethyl aldehyde, into a reaction vessel according to a certain proportion;
(2) dissolving a cross-linking agent in a 1, 4-dioxane solvent to prepare a solution with the concentration: 8 xl 0-2Adding a proper amount of acetic acid into the cross-linking agent solution, and integrally adding the cross-linking agent solution into the reaction container; the cross-linking agent is a mixture of terephthalic acid and dihydroxy end group polyethylene glycol with the molecular weight of 200-2000 in a weight ratio of 2: 3;
(3) adding regularly arranged submicron fibers into a reaction vessel, wherein the addition amount of the submicron fibers is 2-3% of the reaction solution;
(4) deoxidizing the reaction mixture, sealing the reaction container, heating at constant temperature, and standing for several days;
(5) after the reaction is finished, cooling to room temperature, carrying out vacuum filtration on the product, fully washing the product by using an organic solvent tetrahydrofuran, and carrying out vacuum drying on the fully washed product; the vacuum drying method comprises controlling the drying temperature at 120 deg.C for 6h in a vacuum drying oven;
(6) placing the dried porous polymer in an HF acid solution to corrode and remove fibers to form a hollow/solid controllable spherical porous structure of the polymer;
(7) and depositing metal copper on the surface of the polymer porous structure by adopting an electroplating method to obtain the metal-polymer composite filter screen.
The above description is not meant to be limiting, it being noted that: it will be apparent to those skilled in the art that various changes, modifications, additions and substitutions can be made without departing from the true scope of the invention, and these improvements and modifications should also be construed as within the scope of the invention.
Claims (5)
1. The preparation method of the composite filter screen is characterized by comprising the following steps:
(1) adding two monomers, namely 1, 5-diaminoanthracene and mesitylene trimethyl aldehyde, into a reaction vessel according to a certain proportion;
(2) dissolving a cross-linking agent in a 1, 4-dioxane solvent to prepare a solution with the concentration: 5X 10-3-8×l0-2Adding a proper amount of acetic acid into the crosslinking agent solution of mol/L, and integrally adding the crosslinking agent solution into the reaction container;
(3) adding regularly arranged submicron fibers into a reaction vessel, wherein the addition amount of the submicron fibers is 2-3% of the reaction solution;
(4) deoxidizing the reaction mixture, sealing the reaction container, heating at constant temperature, and standing for several days;
(5) after the reaction is finished, cooling to room temperature, carrying out vacuum filtration on the product, fully washing the product with an organic solvent, and carrying out vacuum drying on the fully washed product;
(6) placing the dried porous polymer in an HF acid solution to corrode and remove fibers to form a hollow/solid controllable spherical porous structure of the polymer;
(7) and depositing metal on the surface of the polymer porous structure by adopting an electroplating method to obtain the metal-polymer composite filter screen.
2. The method for preparing the composite filter screen according to claim 1, wherein the cross-linking agent in the step (2) is a mixture of terephthalic acid and dihydroxyl terminated polyethylene glycol with the molecular weight of 200-2000 in a weight ratio of 2: 3.
3. The method for preparing a composite filter screen according to claim 1, wherein the organic solvent in the step (5) is any one of dichloromethane, acetone, tetrahydrofuran or 1, 4-dioxane.
4. The method for preparing the composite filter screen according to claim 1, wherein the vacuum drying method in the step (5) is to control the drying temperature to be 80-120 ℃ in the drying process of a vacuum drying oven, and the drying time to be 6-12 h.
5. The method for preparing the composite filter screen according to claim 1, wherein the metal in the step (7) is any one or more of gold, silver, nickel, copper and iron.
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| CN201711281249.4A CN108212119B (en) | 2017-12-07 | 2017-12-07 | Preparation method of composite filter screen |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101143705A (en) * | 2007-11-01 | 2008-03-19 | 南京大学 | Method for preparing micrometer and submicron probe arrays |
| CN103572270A (en) * | 2013-11-12 | 2014-02-12 | 无锡英普林纳米科技有限公司 | Preparation method of metal-polymer composite filter screen |
| CN105440058A (en) * | 2015-11-04 | 2016-03-30 | 兰州大学 | Synthesis method for benzothiazole unit-based covalent organic framework material |
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- 2017-12-07 CN CN201711281249.4A patent/CN108212119B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101143705A (en) * | 2007-11-01 | 2008-03-19 | 南京大学 | Method for preparing micrometer and submicron probe arrays |
| CN103572270A (en) * | 2013-11-12 | 2014-02-12 | 无锡英普林纳米科技有限公司 | Preparation method of metal-polymer composite filter screen |
| CN105440058A (en) * | 2015-11-04 | 2016-03-30 | 兰州大学 | Synthesis method for benzothiazole unit-based covalent organic framework material |
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Inventor after: Shao Bing Inventor after: Ma Shuangbin Inventor after: Wang Shenglei Inventor before: Wang Shenglei |
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Effective date of registration: 20201130 Address after: Room 1004, building 1, No. 555, Dongyang street, Sanjiang street, Wucheng District, Jinhua City, Zhejiang Province Applicant after: Shao Bing Address before: 266000 17th Floor, 168 Zhuzhou Road, Laoshan District, Qingdao City, Shandong Province Applicant before: QINGDAO ZHIXIN BIOTECHNOLOGY Co.,Ltd. |
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Effective date of registration: 20230105 Address after: No. 128, Taibo Avenue, Xintai Industrial Supporting Area, Meicun Village, Xinwu District, Wuxi City, Jiangsu Province, 214000 Patentee after: Wuxi Jingrun Sensing Technology Co.,Ltd. Address before: Room 1004, building 1, No. 555, Dongyang street, Sanjiang street, Wucheng District, Jinhua City, Zhejiang Province Patentee before: Shao Bing |
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