CN109158094B - Preparation method of paper-based adsorption material based on MOF material - Google Patents
Preparation method of paper-based adsorption material based on MOF material Download PDFInfo
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- 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
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- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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- 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
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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- B01D2258/06—Polluted air
Abstract
The invention relates to the field of papermaking and materials, in particular to a preparation method of a paper-based adsorption material based on an MOF material, which comprises the following steps: adding nickel nitrate, terephthalic acid and wood pulp fiber into N, N-dimethylformamide, heating and reacting to obtain a wood pulp fiber-based MOF material, and drying to obtain an oven-dried fiber-based MOF material; and then dispersing the paper base adsorbing material in water, adding cationic polyacrylamide, stirring, adding graphene, stirring, sheet making, squeezing and drying to obtain the paper base adsorbing material based on the MOF material. The material obtained by the invention has better adsorption performance, and the preparation process is environment-friendly and harmless to the environment.
Description
Technical Field
The invention relates to a preparation method of a paper-based adsorption material based on an MOF material, belonging to the field of materials.
Background
With the increasing weight of air pollution, pollutants in the air, particularly fine particulate pollutants (PM2.5), are one of the important factors causing haze. Because the specific surface area of the fine particle pollutants is very large, harmful substances in the air such as bacteria, viruses and the like are easily adsorbed on the surfaces of the fine particle pollutants, and the health and the life quality of people are seriously influenced. With the continuous development and improvement of the dust removal and purification technology and the expansion of the application range of the dust removal and purification technology, new requirements on the air filter material in terms of quantity, variety and quality are provided.
In 2018, the country writes 'ecological civilization' into constitution, and can say that the country has mentioned ecological civilization and green development to an unprecedented political height.
The air filtering material can remove harmful dust, smoke, toxic fog and the like from gas, and can also obstruct bacteria, microorganisms and viruses, which is essential to environmental protection and human health guarantee and has important significance to social development. With the rapid development of national economy, the demand of air filtering materials is getting larger and larger, and the air filtering materials are more and more in variety, especially used in the aspect of indoor air purification.
At present, most air purification materials are prepared into non-woven fabrics or paper-based filter materials by adopting a dry method or a wet method forming process, and the selected synthetic fibers comprise polyolefin fibers, polyester fibers, polyphenylene sulfide fibers and the like; the natural fiber includes needle wood fiber, broad leaf wood fiber, hemp fiber, cotton fiber, etc. and has excellent physical filtering and retaining effect, high air permeability and high degradability.
Metal-organic frameworks (MOFs) are hybrid organic-inorganic materials with intramolecular pores formed by self-assembly of organic ligands and metal ions or clusters through coordination bonds. In the MOFs, the arrangement of organic ligands and metal ions or clusters has obvious directionality, and different framework pore structures can be formed, thereby showing different adsorption performance, optical properties and electromagnetic properties. The method has the advantages of high porosity, low density, large specific surface area, regular pore channels, adjustable pore diameter, diversity and tailorability of topological structures and the like.
Therefore, the environmental deterioration phenomenon caused by economic development is becoming more serious, especially the haze phenomenon, and the development of an air filter material having high adsorption performance is urgently needed.
Disclosure of Invention
The invention aims to provide a preparation method of a paper-based adsorption material based on an MOF material, which aims to solve the problem of low adsorption performance of an air adsorption material.
The purpose of the invention is realized by the following technical scheme: a preparation method of a paper-based adsorption material based on an MOF material comprises the following steps: adding nickel nitrate, terephthalic acid and wood pulp fiber into N, N-dimethylformamide, heating and reacting to obtain a wood pulp fiber-based MOF material, and drying to obtain an oven-dried fiber-based MOF material; and then dispersing the paper base adsorbing material in water, adding cationic polyacrylamide, stirring, adding graphene, stirring, sheet making, squeezing and drying to obtain the paper base adsorbing material based on the MOF material.
Further, the nickel nitrate: terephthalic acid: wood pulp fiber: the mass ratio of N, N-dimethylformamide is (20-40): (20-30): 1-5): 600-800.
Further, the wood pulp fiber comprises needle pulp and broad leaf pulp, wherein the mass ratio of the needle pulp to the broad leaf pulp is (2-4): 6-8), and the beating degree is 40-50 DEG SR.
Further, the mixture of nickel nitrate, terephthalic acid, wood pulp fiber and N, N-dimethylformamide was heated to 120-140 ℃.
Further, the drying temperature to obtain an oven dried fiber-based MOF material was 100-110 ℃.
Furthermore, the molecular weight of the cationic polyacrylamide is 55000-80000, and the addition amount of the cationic polyacrylamide is 0.3-0.5% of the mass of the oven-dried fiber-based MOF material.
Furthermore, the diameter of the graphene is 100 nm-10 μm, and the adding amount of the graphene is 4-6% of the mass of the absolutely dry fiber MOF material.
Further, the pressing pressure is 0.3-0.5 MPa.
Further, the temperature at which drying is performed after pressing is 100-110 ℃.
The paper-based adsorption material based on the MOF material is obtained by the preparation method of the paper-based adsorption material based on the MOF material.
The paper-based adsorption material based on the MOF material is used for adsorbing harmful substances in air and wastewater and catalyzing degradation.
Compared with the prior art, the invention has the following advantages:
the preparation method of the MOF paper-based adsorption material is simple, the process flow is short, and the MOF paper-based adsorption material can be used for adsorbing toxic gas in the air and generating catalytic degradation; when the MOF paper-based adsorption material is used for saturated adsorption, the adsorption capacity of the MOF paper-based adsorption material to formaldehyde can reach 80-92% of the self weight, and the degradation rate can reach 5-20%.
The MOF paper-based adsorption material is used for catalyzing and degrading harmful organic matters in air and wastewater.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic representation of the adsorption stripping of a paper-based adsorption material based on MOF material of example 1 of the present invention;
FIG. 2 is a drawing showing the desorption of a paper-based adsorbent material based on MOF material according to example 2 of the present invention;
FIG. 3 is a drawing showing the desorption of a paper-based adsorbent material based on MOF material according to example 3 of the present invention;
FIG. 4 is a schematic representation of the desorption of the paper-based adsorption material based on MOF material of comparative example 1 of the present invention;
figure 5 is a graph showing the desorption of the MOF material based paper-based adsorbent material of comparative example 2 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation method of the paper-based adsorption material based on the MOF material comprises the following steps: adding nickel nitrate, terephthalic acid and wood pulp fiber into N, N-dimethylformamide, heating and reacting to obtain a wood pulp fiber-based MOF material, and drying to obtain an oven-dried fiber-based MOF material; and then dispersing the paper base adsorbing material in water, adding cationic polyacrylamide, stirring, adding graphene, stirring, sheet making, squeezing and drying to obtain the paper base adsorbing material based on the MOF material.
The paper-based adsorption material based on the MOF material can effectively adsorb nitrogen molecules, the adsorption effect of the nitrogen mainly comes from Van der Waals force and electrostatic force, and the optimal adsorption position is at a metal position.
Preferably, the ratio of nickel nitrate: terephthalic acid: wood pulp fiber: the mass ratio of N, N-dimethylformamide is (20-40): (20-30): 1-5): 600-800.
Preferably, the wood pulp fiber comprises needle pulp and broad leaf pulp, wherein the mass ratio of the needle pulp to the broad leaf pulp is (2-4): 6-8), and the beating degree is 40-50 DEG SR.
Preferably, the mixture of nickel nitrate, terephthalic acid, wood pulp fiber and N, N-dimethylformamide is warmed to 120-140 ℃.
Preferably, the drying temperature to obtain an oven dried fiber-based MOF material is 100-110 ℃.
Preferably, the molecular weight of the cationic polyacrylamide is 55000-80000, and the addition amount is 0.3-0.5% of the mass of the oven-dried fiber-based MOF material.
Preferably, the diameter of the graphene is 100 nm-10 μm, and the addition amount is 4-6% of the mass of the oven dry fiber-based MOF material.
Preferably, the pressing pressure is 0.3-0.5 MPa.
Preferably, the temperature at which drying is carried out after pressing is 100-110 ℃.
The paper-based adsorption material based on the MOF material is obtained by the preparation method of the paper-based adsorption material based on the MOF material.
The paper-based adsorption material based on the MOF material is used for adsorbing harmful substances in air and wastewater and catalyzing degradation.
The beating is to make the fiber generate cutting, devillicating, brooming, swelling and other actions, then the fiber is further refined, the surface generates fuzzing to increase the evenness and fineness of the finished paper, improve the appearance quality of the paper and improve the internal strength of the paper. The pulp is endowed with papermaking performance and paper forming performance through mechanical action on the pulp, so that the quality requirement of paper is met.
Oven drying the fiber-based MOF material at 100-110 deg.C to constant weight.
The polyacrylamide functions as a retention aid, flocculating the fibers and fines together, and may be replaced by some low charge density high molecular weight material, such as cationic starch.
The graphene or the calcium carbonate is used as a filler and fine components, and the effect is different after the graphene or the calcium carbonate is added, namely the adsorption performance is different; it has an increased specific surface area, an enhanced adsorption property, and improved smoothness and opacity as compared to wood pulp fibers.
The wood pulp fibers include hardwood pulp fibers and softwood pulp fibers.
Example 1
Adding 30g of nickel nitrate, 25g of terephthalic acid and 1g of pulped wood pulp fiber (broad-leaf pulp: needle-leaf pulp 7:3, beating degree of 45 DEG SR) into 700g of N, N-dimethylformamide, placing the mixture into a hydrothermal reaction kettle, heating to 120 ℃, reacting for 24 hours, washing the obtained wood pulp fiber-based MOF material with absolute ethyl alcohol for 5 times, filtering, and drying in the air to obtain the oven-dried fiber-based MOF material.
Dispersing 1g of the obtained wood pulp fiber-based MOF material in 400g of water, adding 0.0004g of cationic polyacrylamide, stirring for 5min, adding 0.05g of graphene powder, stirring for 1min, carrying out sheet making on a sheet making machine, then pressing for 5min under the pressure of 0.4MPa, and then drying for 10min at 105 ℃ to obtain the paper-based adsorbing material based on the MOF material.
FIGS. 1 to 5 show the measurement of the adsorption amount of adsorbate molecule (N2) by a sample loaded in a sample tube according to the change of gas concentration before and after adsorption, as measured by a BET specific surface area tester.
As shown in figure 1, the adsorption and desorption diagram of the paper-based adsorption material shows that the adsorption curve and the desorption curve show that the adsorption quantity and the desorption quantity are gradually increased along with the increase of the pressure, and when the pressure reaches 1, the adsorption quantity reaches 45cm3/g。
Example 2
Adding 20g of nickel nitrate, 30g of terephthalic acid and 3g of pulped wood pulp fiber (broad-leaf pulp: needle-leaf pulp: 6:4, beating degree is 40 DEG SR) into 800g of N, N-dimethylformamide, placing the mixture into a hydrothermal reaction kettle, heating to 130 ℃, reacting for 30h, washing the obtained wood pulp fiber-based MOF material with absolute ethyl alcohol for 5 times, filtering, and drying in the air to obtain the oven-dried fiber-based MOF material.
Dispersing 1g of the obtained wood pulp fiber-based MOF material in 400g of water, adding 0.0003g of cationic polyacrylamide, stirring for 5min, adding 0.04g of graphene powder, stirring for 1min, sheet-making on a sheet-making machine, pressing for 5min under the pressure of 0.3MPa, and drying for 10min at 100 ℃ to obtain the paper-based adsorbing material based on the MOF material.
As shown in figure 2, the adsorption and desorption diagram of the paper-based adsorption material shows that the adsorption curve and the desorption curve show that the adsorption quantity and the desorption quantity are gradually increased along with the increase of the pressure, and when the pressure reaches 1, the adsorption quantity reaches 70cm3/g。
Example 3
Adding 40g of nickel nitrate, 20g of terephthalic acid and 5g of pulped wood pulp fiber (broad-leaf pulp: 8:2, beating degree is 50 DEG SR) into 600g of N, N-dimethylformamide, placing the mixture into a hydrothermal reaction kettle, heating to 140 ℃, reacting for 36h, washing the obtained wood pulp fiber-based MOF material with absolute ethyl alcohol for 5 times, filtering, and drying in the air to obtain the oven-dried fiber-based MOF material.
Dispersing 1g of the obtained wood pulp fiber-based MOF material in 400g of water, adding 0.0005g of cationic polyacrylamide, stirring for 5min, adding 0.06g of graphene powder, stirring for 1min, sheet-making on a sheet-making machine, then pressing under 0.5MPa for 5min, and then drying at 110 ℃ for 10min to obtain the paper-based adsorbing material based on the MOF material.
As shown in FIG. 3, the adsorption-desorption diagram of the paper-based adsorption material shows that the adsorption curve and the desorption curve show that the adsorption amount and the desorption amount are gradually increased along with the increase of the pressure, and when the pressure reaches 1, the adsorption amount reaches 66cm3/g。
Comparative example 1
Dispersing 1g of oven-dried pulp (broad-leaf pulp: needle-leaf pulp: 7:3, beating degree of 45 ° SR) in 400g of water, adding 0.0004g of cationic polyacrylamide, stirring for 5min, adding 0.3g of calcium carbonate, stirring for 1min, sheet-making on a sheet-making machine, squeezing under 0.4MPa for 5min, and drying at 105 ℃ for 10min to obtain the final paper sheet.
As shown in FIG. 4, the adsorption-desorption diagram of the paper-based adsorption material shows that the adsorption curve and the desorption curve show that the adsorption amount and the desorption amount are gradually increased along with the increase of the pressure, and when the pressure reaches 1, the adsorption amount reaches 22cm3/g。
Comparative example 2
Dispersing 1g of oven-dried pulp (broad-leaf pulp: needle-leaf pulp of 7:3, beating degree of 45 ° SR) in 400g of water, adding 0.0004g of cationic polyacrylamide, stirring for 5min, adding 0.3g of graphene, stirring for 1min, sheet-making on a sheet-making machine, pressing under 0.4MPa for 5min, and drying at 105 ℃ for 10min to obtain the final paper sheet.
As shown in FIG. 5, the adsorption-desorption diagram of the paper-based adsorption material shows that the adsorption curve and the desorption curve show that the adsorption amount and the desorption amount are gradually increased along with the increase of the pressure, and when the pressure reaches 1, the adsorption amount reaches 40cm3/g。
And (4) conclusion: the adsorption performance of the paper added with the MOF material is obviously better than that of the paper without the MOF material, so that the paper added with the MOF material can effectively adsorb toxic and harmful gases in the air and can be used as a functional adsorption material.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. A preparation method of a paper-based adsorption material based on an MOF material is characterized by comprising the following steps:
adding nickel nitrate, terephthalic acid and wood pulp fiber into N, N-dimethylformamide, heating and reacting to obtain a wood pulp fiber-based MOF material, and drying to obtain an oven-dried fiber-based MOF material;
dispersing the obtained product in water, adding cationic polyacrylamide, stirring, adding graphene, stirring, sheet making, squeezing and drying to obtain a paper-based adsorption material based on the MOF material; the nickel nitrate: terephthalic acid: wood pulp fiber: the mass ratio of N, N-dimethylformamide is (20-40): (20-30): 1-5): 600-800);
the diameter of the graphene is 100 nm-10 mu m, and the adding amount of the graphene is 4-6% of the mass of the oven dry fiber-based MOF material.
2. The preparation method of the paper-based adsorption material based on the MOF material, according to claim 1, characterized in that the wood pulp fibers comprise needle pulp and broad leaf pulp, wherein the mass ratio of the needle pulp to the broad leaf pulp is (2-4): 6-8), and the beating degree is 40-50 ° SR.
3. The method for preparing a paper-based adsorption material based on MOF material according to claim 2, characterized in that the mixture of nickel nitrate, terephthalic acid, wood pulp fiber and N, N-dimethylformamide is heated up to 120-140 ℃.
4. The method for preparing a paper-based adsorption material based on MOF material according to claim 3, wherein the drying temperature to obtain an absolutely dry fiber-based MOF material is 100-110 ℃.
5. The preparation method of the paper-based adsorption material based on the MOF material, according to claim 4, characterized in that the molecular weight of the cationic polyacrylamide is 55000-80000, and the addition amount is 0.3-0.5% of the mass of the absolutely dry fiber-based MOF material.
6. The method for preparing a paper-based adsorption material based on MOF material according to claim 5, characterized in that the pressing pressure is 0.3-0.5 MPa.
7. The method for preparing a paper-based adsorption material based on MOF material according to claim 6, wherein the temperature for drying after pressing is 100-110 ℃.
8. A MOF material based paper-based adsorption material obtained by the method of preparation of a MOF material based paper-based adsorption material according to any one of claims 1 to 7.
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| CN112755997B (en) * | 2021-01-29 | 2022-01-18 | 福州大学 | Mn/Fe-MOF-loaded polyphenylene sulfide denitration sulfur-resistant filter material and preparation method thereof |
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