CN115845813A - Elastic super-hydrophobic oleophylic MOF/SiO 2 Preparation method of composite aerogel - Google Patents
Elastic super-hydrophobic oleophylic MOF/SiO 2 Preparation method of composite aerogel Download PDFInfo
- Publication number
- CN115845813A CN115845813A CN202211297026.8A CN202211297026A CN115845813A CN 115845813 A CN115845813 A CN 115845813A CN 202211297026 A CN202211297026 A CN 202211297026A CN 115845813 A CN115845813 A CN 115845813A
- Authority
- CN
- China
- Prior art keywords
- mof
- sio
- elastic
- composite aerogel
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000004964 aerogel Substances 0.000 title claims abstract description 59
- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 36
- 229910004298 SiO 2 Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000002243 precursor Substances 0.000 claims abstract description 46
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 42
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 33
- 239000008367 deionised water Substances 0.000 claims abstract description 32
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 32
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 29
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 29
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 239000004094 surface-active agent Substances 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 20
- 239000011259 mixed solution Substances 0.000 claims abstract description 19
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims abstract description 18
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims abstract description 17
- WFNRNCNCXRGUKN-UHFFFAOYSA-N 2,3,5,6-tetrafluoroterephthalic acid Chemical compound OC(=O)C1=C(F)C(F)=C(C(O)=O)C(F)=C1F WFNRNCNCXRGUKN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 230000032683 aging Effects 0.000 claims abstract description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 16
- 239000010703 silicon Substances 0.000 claims abstract description 16
- 239000012298 atmosphere Substances 0.000 claims abstract description 14
- 238000001879 gelation Methods 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 11
- 238000000197 pyrolysis Methods 0.000 claims abstract description 11
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 238000013329 compounding Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 26
- 238000004108 freeze drying Methods 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 11
- 238000000352 supercritical drying Methods 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000007710 freezing Methods 0.000 claims description 8
- 230000008014 freezing Effects 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- AGFRTAFWXGPUDC-UHFFFAOYSA-M hexadecyl(trimethoxy)azanium chloride Chemical compound [Cl-].CO[N+](CCCCCCCCCCCCCCCC)(OC)OC AGFRTAFWXGPUDC-UHFFFAOYSA-M 0.000 claims description 3
- SNEFVJQHWBOIMY-UHFFFAOYSA-M hexadecyl(trimethoxy)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](OC)(OC)OC SNEFVJQHWBOIMY-UHFFFAOYSA-M 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- 241000764238 Isis Species 0.000 claims 1
- 239000012621 metal-organic framework Substances 0.000 abstract description 90
- 238000000034 method Methods 0.000 abstract description 8
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 239000012919 MOF-derived carbon material Substances 0.000 abstract description 3
- 230000002209 hydrophobic effect Effects 0.000 abstract description 3
- 239000003292 glue Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 28
- 239000003921 oil Substances 0.000 description 12
- 238000002791 soaking Methods 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000003344 environmental pollutant Substances 0.000 description 6
- 231100000719 pollutant Toxicity 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 229910021389 graphene Inorganic materials 0.000 description 5
- 238000005086 pumping Methods 0.000 description 5
- 238000002485 combustion reaction Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 238000006065 biodegradation reaction Methods 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229920002749 Bacterial cellulose Polymers 0.000 description 1
- 240000003826 Eichhornia crassipes Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 239000012917 MOF crystal Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000005016 bacterial cellulose Substances 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001924 cycloalkanes Chemical class 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000021384 green leafy vegetables Nutrition 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000008206 lipophilic material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012924 metal-organic framework composite Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention discloses an elastic super-hydrophobic oleophylic MOF/SiO 2 A preparation method of the composite aerogel. The method comprises the following steps: dissolving zinc nitrate hexahydrate and tetrafluoroterephthalic acid in deionized water, and dropwise adding ammonia water to form an MOF precursor; putting the MOF precursor into a tube furnace, carrying out high-temperature pyrolysis in an inert atmosphere, and carrying out acid washing to obtain MOF derived carbon; dissolving a mixture of MOF derived carbon and ethanol and a surfactant in deionized water, ultrasonically oscillating and uniformly stirring to form a mixed solution, which is marked as A; adding methyltrimethoxysilane and dimethyldimethoxysilane into the A as silicon sources, fully stirring, adding an alkali catalyst, and pouring into a mold to wait for gelation; aging and drying the gel to obtain the elastic super-hydrophobic oleophylic MOF/SiO 2 And (3) compounding the aerogel. The invention uses elastic hydrophobic oleophylic SiO 2 Air condensationThe glue is compounded with the MOF derived carbon material, the fragility of the MOF is overcome, and the prepared MOF/SiO 2 The composite aerogel can be restored after being compressed for many times, the water contact angle is as high as 153 degrees, the super-hydrophobic oleophylic performance is shown, and the composite aerogel is beneficial to repeated use.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to elastic super-hydrophobic oleophylic MOF/SiO 2 A preparation method of the composite aerogel.
Background
In recent years, frequent petroleum leakage and discharge of untreated wastewater, farmland sewage and the like cause a large amount of oily substances (including organic substances such as n-alkanes, cycloalkanes, aromatic hydrocarbons and the like) to enter rivers and oceans, which seriously pollutes water quality and ecological environment in areas, causes death of a large amount of aquatic animals, and seriously affects human living environment and physical health.
The common methods for treating oily pollutants in water at present comprise biodegradation, combustion, mechanical oil pumping, oleophilic material oil pumping and the like. The biodegradation method is to artificially culture oil-feeding microorganisms and then put the oil-feeding microorganisms into a polluted water area for biodegradation, but the method has slow degradation speed and long sewage treatment period, and cannot completely avoid the harm caused by oily pollutants. The combustion adopts various combustion improvers to burn a large amount of oily pollutants in a short time, but the oily pollutants can be burnt to generate CO and SO 2 And other harmful gases, and other products of combustion can also influence the growth and reproduction of aquatic animals and plants. The mechanical oil pumping speed is high, but the energy consumption is large, the cost is high, the mechanical oil pumping device is mostly suitable for sea level, and the oil pumping effect is not thorough.
The oleophylic material is used for oil absorption, so that the efficiency is high, the energy consumption is low, the environment is protected, and the policy of double carbon is met. Foams and sponges are lipophilic materials commonly used for oil absorption, but the foams and the sponges absorb part of water while absorbing oily substances, so that the subsequent oil-water separation is inconvenient. The aerogel has the advantages of super-large specific surface, super-high porosity, super-strong oil absorption capacity and the like, is considered as a novel high-efficiency oleophylic oil absorption material, and is particularly suitable for dirty oil treatment. The preparation method comprises the following steps of putting bacterial cellulose in deionized water, performing deacidification, liquid nitrogen freezing, freeze drying and high-temperature pyrolysis treatment to obtain carbon nanofiber aerogel, performing acid catalytic hydrolysis, gel forming and drying treatment to a silicon source containing methyl to obtain silicon dioxide aerogel, extracting cellulose from water hyacinth plants by CN 103333358A and CN 114394600A, preparing cellulose solution, adding a papermaking wet strength agent, uniformly mixing, and performing freeze drying to obtain cellulose aerogel. However, the aerogel prepared by the process has the advantages of small porosity, low specific surface area and insufficient adsorption capacity on oily substances.
Metal Organic Framework (MOF) has larger specific surface, higher porosity and better Hydrophobicity, so that the MOF and the Aerogel have stronger and more Efficient Oil absorption capacity than the Aerogel, and document Hydrophobicity-Adjustable MOF structures Superhydrophic MOF-rGO Aerogel for Efficient Oil Separation reports that a composite Aerogel prepared by compounding pre-prepared MOF microspheres with graphene after surface hydrophobic modification has ultrahigh adsorption capacity on oily pollutants; in patent CN 107215863B, mixing MOF crystal powder with graphene or graphene oxide according to a mass ratio of 1. However, the cost of graphene is too high, which is not beneficial to the large-scale production and application of the graphene/MOF composite aerogel.
Disclosure of Invention
The invention aims to solve the problems and provide an elastic super-hydrophobic oleophylic MOF/SiO with low production cost and convenient operation 2 A preparation method of the composite aerogel.
In order to solve the technical problems, the technical scheme of the invention is as follows: elastic super-hydrophobic oleophylic MOF/SiO 2 The preparation method of the composite aerogel comprises the following steps:
s1, dissolving zinc nitrate hexahydrate and tetrafluoro terephthalic acid in deionized water, and dropwise adding ammonia water to form an MOF precursor;
s2, putting the MOF precursor into a tube furnace, carrying out high-temperature pyrolysis in an inert atmosphere, and then carrying out acid washing to obtain MOF derived carbon;
s3, dissolving a mixture of the MOF derived carbon and ethanol and a surfactant in deionized water, and performing ultrasonic oscillation and uniform stirring to form a mixed solution marked as A;
s4, adding methyltrimethoxysilane and dimethyldimethoxysilane serving as silicon sources into the A, fully stirring, adding an alkali catalyst, and pouring into a mold to wait for gelation;
s5, aging, solvent replacement and drying treatment are carried out on the gel to obtain the elastic super-hydrophobic oleophylic MOF/SiO 2 And (3) compounding the aerogel.
Further, in the step S1, the molar ratio of zinc nitrate hexahydrate to tetrafluoroterephthalic acid is 0.5 to 4.0, and the volume ratio of deionized water to ammonia water is 10 to 60.
Further, the inert gas in the step S2 is Ar gas or N 2 The pyrolysis temperature of the gas is 500-1100 ℃, the pyrolysis time is 0.5-8 h, and the acid is soaked in acid with the concentration of 20% of any one of hydrochloric acid, sulfuric acid and nitric acid for 6-72 h.
Further, the mass ratio of the MOF-derived carbon, ethanol, and surfactant in step S3 is: 0.002-2.0.
Further, in the step S3, the surfactant is at least one of hexadecyl trimethoxy ammonium chloride and hexadecyl trimethoxy ammonium bromide.
Further, in the step S4, the molar ratio of the silane to the surfactant is 0.5 to 2.0.
Further, in the step S4, the alkali catalyst is at least one of sodium hydroxide, potassium hydroxide and ammonia water.
Further, the volume ratio of methyltrimethoxysilane to dimethyldimethoxysilane in step S4 is 0.5 to 2.0
Further, the aging process in the step S5 is carried out at 10-80 ℃.
Further, the drying in the step S5 comprises normal pressure drying, freeze drying and supercritical drying, wherein the temperature of the normal pressure drying is 80-150 ℃, and the time is 24-72 hours; s5, the freeze-drying pre-freezing temperature is-50-0 ℃, the pre-freezing time is 1-12 hours, and the freeze-drying time is 12-72 hours; and S5, the supercritical drying temperature is 35-45 ℃, the pressure is 9-14 MPa, and the time is 8-36 h.
The invention has the beneficial effects that:
1. the invention provides an elastic super-hydrophobic oleophylic MOF/SiO 2 The preparation method of the composite aerogel takes methyl trimethoxy silane and dimethyl dimethoxy silane with low cost as silicon sources and is compounded with MOF derived carbon materials, so that MOF/SiO is prepared 2 And (3) compounding the aerogel. The composite aerogel can be restored after being compressed for many times, and the limitation that the MOF derived carbon material is difficult to reuse due to poor mechanical property is overcome. The composite aerogel has a contact angle with water of 153 degrees, has super-hydrophobicity, can adsorb n-hexane (n-alkane) with the weight being tens of times of the weight of the composite aerogel, is particularly suitable for adsorbing oily pollutants in various water bodies, improves water quality, greens the environment and protects the ecology in an efficient, cheap and environment-friendly manner.
2. The invention uses high elasticity SiO 2 Aerogel is used as a carrier to load the MOF derived carbon with high specific surface. Prepared MOF/SiO 2 The composite aerogel has good hydrophobicity and lipophilicity, can adsorb various organic matters with the weight being several times or even tens of times of the weight of the composite aerogel, can still recover the original shape after being extruded for many times, and is beneficial to repeated use.
Drawings
FIG. 1 is a diagram of an elastic superhydrophobic oleophilic MOF/SiO 2 The flow diagram of the preparation method of the composite aerogel;
FIG. 2 is a diagram of the elastic superhydrophobic lipophilic MOF/SiO obtained in one embodiment of the invention 2 Schematic contact angle of complex aerogel and water;
FIG. 3 is the elastic superhydrophobic oleophilic MOF/SiO obtained in example six of the present invention 2 N of composite aerogel 2 A schematic diagram of a gas adsorption desorption curve;
FIG. 4 is the elastic superhydrophobic oleophilic MOF/SiO obtained in example six of the present invention 2 Schematic contact angle of complex aerogel and water;
FIG. 5 is the present inventionElastic super SiO obtained in the comparative example of the invention 2 N of aerogel 2 The gas adsorption and desorption curve is shown schematically.
Detailed Description
The invention is further described with reference to the following figures and specific examples:
example one
As shown in figure 1, the invention provides an elastic super-hydrophobic oleophilic MOF/SiO 2 The preparation method of the composite aerogel comprises the following steps:
s1, dissolving zinc nitrate hexahydrate and tetrafluoroterephthalic acid in deionized water, and dropwise adding ammonia water to form an MOF precursor.
The molar ratio of zinc nitrate hexahydrate to tetrafluoroterephthalic acid in the step S1 is 0.5-4.0, and the volume ratio of deionized water to ammonia water is 10-60.
In this example, 29.7363g of zinc nitrate hexahydrate and 11.9045g of tetrafluoroterephthalic acid were dissolved in 1000ml of deionized water, and 20ml of aqueous ammonia was added dropwise to form an MOF precursor.
S2, putting the MOF precursor into a tube furnace, performing high-temperature pyrolysis in an inert atmosphere, and then performing acid washing to obtain the MOF derived carbon.
In the step S2, the inert gas is Ar gas or N 2 The pyrolysis temperature of the gas is 500-1100 ℃, the pyrolysis time is 0.5-8 h, and the acid is soaked in acid with the concentration of 20% of any one of hydrochloric acid, sulfuric acid and nitric acid for 6-72 h.
In the embodiment, the MOF precursor is put into a tube furnace and pyrolyzed at 800 ℃ for 4h under Ar atmosphere, and then is soaked in hydrochloric acid with 20% concentration for 24h to obtain MOF-derived carbon.
And S3, dissolving the mixture of the MOF derived carbon and the ethanol and the surfactant in deionized water, and performing ultrasonic oscillation and uniform stirring to form a mixed solution, wherein the mixed solution is marked as A.
In the step S3, the mass ratio of the MOF derived carbon to the ethanol to the surfactant is as follows: 0.002 to 2.0. In the step S3, the surfactant is at least one of hexadecyl trimethoxy ammonium chloride and hexadecyl trimethoxy ammonium bromide.
In this example, a mixture of 0.01g of MOF-derived carbon and 0.2ml of ethanol, 1.5g of surfactant, was dissolved in 21.4ml of deionized water, sonicated and stirred uniformly to form a mixed solution, labeled A.
And S4, adding methyltrimethoxysilane and dimethyldimethoxysilane serving as silicon sources into the A, fully stirring, adding an alkali catalyst, and pouring into a mold to wait for gelation.
The molar ratio of the silane to the surfactant in the step S4 is 0.5-2.0. The alkali catalyst is at least one of sodium hydroxide, potassium hydroxide and ammonia water. In the step S4, the volume ratio of methyltrimethoxysilane to dimethyldimethoxysilane is 0.5-2.0.
In this example, 5ml methyltrimethoxysilane and 3.4ml dimethyldimethoxysilane were added as silicon source to A, ammonia was added after stirring well, the solution ph was adjusted to 9, and poured into molds to wait for gelation.
S5, aging, solvent replacement and drying treatment are carried out on the gel to obtain the elastic super-hydrophobic oleophylic MOF/SiO 2 And (3) compounding the aerogel.
The aging process in the step S5 is carried out at 10-80 ℃, and the drying in the step S5 comprises normal pressure drying, freeze drying and supercritical drying, wherein the temperature of the normal pressure drying is 80-150 ℃, and the time is 24-72 hours; s5, the freeze-drying pre-freezing temperature is-50-0 ℃, the pre-freezing time is 1-12 hours, and the freeze-drying time is 12-72 hours; and S5, the supercritical drying temperature is 35-45 ℃, the pressure is 9-14 MPa, and the time is 8-36 h.
In the actual use process, the atmospheric drying, the freeze drying and the supercritical drying in step S5 may be used sequentially, or only one or a combination of a plurality of drying methods may be selected according to actual needs. So as to be suitable for more using environments and increase the practicability of the invention.
In this example, a small amount of water was added to the gel, which was aged at 40 ℃ for 24h, pre-frozen at-40 ℃ for 5h, and freeze-dried for 48h to give the elastic superhydrophobic oleophilic MOF/SiO 2 Composite aerogel, labeled sample 1. Sample 1 had a contact angle with water of 154.886 deg., and exhibited superhydrophobicity.
The elastic superhydrophobic oleophilic MOF/SiO obtained in this example 2 The contact angles of the complex aerogel and water are shown in fig. 2.
Example two
S1, dissolving 29.7363g of zinc nitrate hexahydrate and 11.9045g of tetrafluoroterephthalic acid in 1000ml of deionized water, and dropwise adding 20ml of ammonia water to form an MOF precursor.
S2, putting the MOF precursor into a tube furnace, pyrolyzing the precursor at 800 ℃ for 4h in Ar atmosphere, and soaking the precursor in hydrochloric acid with the concentration of 20% for 24h to obtain the MOF derived carbon.
S3, dissolving 0.01g of a mixture of MOF derived carbon and 0.2ml of ethanol and 1.5g of a surfactant in 21.4ml of deionized water, and ultrasonically shaking and uniformly stirring to form a mixed solution, wherein the mixed solution is marked as A.
And S4, adding 5ml of methyltrimethoxysilane and 3.4ml of dimethyldimethoxysilane serving as silicon sources into the solution A, fully stirring, adding ammonia water, adjusting the pH of the solution to 9, and pouring the solution into a mold to wait for gelation.
S5, adding a small amount of water into the gel, aging the gel for 24h at 40 ℃, replacing the gel with an ethanol solvent, and performing supercritical drying at 40 ℃ and 14MPa for 12h to obtain the elastic super-hydrophobic oleophylic MOF/SiO 2 The composite aerogel, labeled sample 2.
EXAMPLE III
S1, dissolving 29.7363g of zinc nitrate hexahydrate and 11.9045g of tetrafluoroterephthalic acid in 1000ml of deionized water, and dropwise adding 20ml of ammonia water to form an MOF precursor.
S2, putting the MOF precursor into a tube furnace, pyrolyzing the precursor at 800 ℃ for 4h in Ar atmosphere, and soaking the precursor in hydrochloric acid with the concentration of 20% for 24h to obtain the MOF derived carbon.
S3, dissolving 0.02g of a mixture of MOF derived carbon and 0.4ml of ethanol and 1.5g of a surfactant in 21.4ml of deionized water, and ultrasonically oscillating and uniformly stirring to form a mixed solution, which is marked as A.
And S4, adding 5ml of methyltrimethoxysilane and 3.4ml of dimethyldimethoxysilane serving as silicon sources into the solution A, fully stirring, adding ammonia water, adjusting the pH of the solution to 9, and pouring the solution into a mold to wait for gelation.
S5, adding a small amount of water into the gel, aging the gel for 24 hours at 40 ℃, and then pre-aging the gel at-40 DEG CFreezing for 5h, and freeze-drying for 48h to obtain elastic super-hydrophobic oleophylic MOF/SiO 2 Composite aerogel, labeled sample 3.
Example four
S1, dissolving 29.7363g of zinc nitrate hexahydrate and 11.9045g of tetrafluoroterephthalic acid in 1000ml of deionized water, and dropwise adding 20ml of ammonia water to form an MOF precursor.
S2, putting the MOF precursor into a tube furnace, pyrolyzing the precursor at 800 ℃ for 4h in Ar atmosphere, and soaking the precursor in hydrochloric acid with the concentration of 20% for 24h to obtain the MOF derived carbon.
S3, dissolving 0.05g of a mixture of MOF derived carbon and 1ml of ethanol and 1.5g of a surfactant in 21.4ml of deionized water, and ultrasonically oscillating and uniformly stirring to form a mixed solution, wherein the mixed solution is marked as A.
S4, adding 5ml of methyltrimethoxysilane and 3.4ml of dimethyldimethoxysilane serving as silicon sources into the A, fully stirring, adding ammonia water, adjusting the ph of the solution to 9, pouring the solution into a mold, and waiting for gelation.
S5, adding a small amount of water into the gel, aging the gel for 24 hours at 40 ℃, pre-freezing the gel for 5 hours at-40 ℃, and freeze-drying the gel for 48 hours to obtain the elastic super-hydrophobic oleophylic MOF/SiO 2 Composite aerogel, labeled sample 4.
EXAMPLE five
S1, dissolving 29.7363g of zinc nitrate hexahydrate and 11.9045g of tetrafluoroterephthalic acid in 1000ml of deionized water, and dropwise adding 20ml of ammonia water to form an MOF precursor.
S2, putting the MOF precursor into a tube furnace, pyrolyzing the precursor at 800 ℃ for 4h in Ar atmosphere, and soaking the precursor in hydrochloric acid with the concentration of 20% for 24h to obtain the MOF derived carbon.
S3, dissolving 0.1g of a mixture of MOF derived carbon and 2ml of ethanol and 1.5g of a surfactant in 21.4ml of deionized water, and ultrasonically oscillating and uniformly stirring to form a mixed solution, wherein the mixed solution is marked as A.
And S4, adding 5ml of methyltrimethoxysilane and 3.4ml of dimethyldimethoxysilane serving as silicon sources into the solution A, fully stirring, adding ammonia water, adjusting the pH of the solution to 9, and pouring the solution into a mold to wait for gelation.
S5, adding a small amount of water into the gel, aging the gel for 24 hours at 40 ℃, pre-freezing the gel for 5 hours at-40 ℃, and freeze-drying the gel for 48 hours to obtain the gelElastic super-hydrophobic oleophilic MOF/SiO 2 Composite aerogel, labeled sample 5.
EXAMPLE six
S1, dissolving 29.7363g of zinc nitrate hexahydrate and 11.9045g of tetrafluoroterephthalic acid in 1000ml of deionized water, and dropwise adding 20ml of ammonia water to form an MOF precursor.
S2, putting the MOF precursor into a tube furnace, pyrolyzing the precursor at 800 ℃ for 4h under Ar atmosphere, and soaking the precursor in hydrochloric acid with the concentration of 20% for 24h to obtain MOF derived carbon, which is marked as a sample 6. The specific surface area of sample 6 was 1251.7139m 2 The contact angle with water is 152.652 DEG, which shows super-hydrophobicity.
EXAMPLE six N of MOF-derived carbons obtained 2 The gas adsorption desorption curve is shown in fig. 3, and the contact angle of the MOF-derived carbon and water is shown in fig. 4.
EXAMPLE seven
S1, dissolving 29.7363g of zinc nitrate hexahydrate and 11.9045g of tetrafluoroterephthalic acid in 1000ml of deionized water, and dropwise adding 20ml of ammonia water to form an MOF precursor.
S2, putting the MOF precursor into a tube furnace, pyrolyzing the precursor for 4 hours at 800 ℃ under Ar atmosphere, and soaking the precursor for 24 hours by using hydrochloric acid with the concentration of 20% to obtain the MOF derived carbon.
S3, dissolving 0.02g of a mixture of MOF derived carbon and 0.4ml of ethanol and 1.5g of a surfactant in 21.4ml of deionized water, and ultrasonically oscillating and uniformly stirring to form a mixed solution, which is marked as A.
And S4, adding 5ml of methyltrimethoxysilane and 3.4ml of dimethyldimethoxysilane serving as silicon sources into the solution A, fully stirring, adding ammonia water, adjusting the pH of the solution to 9, and pouring the solution into a mold to wait for gelation.
S5, adding a small amount of water into the gel, aging the gel for 24 hours at 40 ℃, replacing the gel by an ethanol solvent, and performing supercritical drying for 12 hours at 40 ℃ and 14MPa to obtain the elastic super-hydrophobic oleophylic MOF/SiO 2 Composite aerogel, labeled sample 7.
Example eight
S1, dissolving 29.7363g of zinc nitrate hexahydrate and 11.9045g of tetrafluoroterephthalic acid in 1000ml of deionized water, and dropwise adding 20ml of ammonia water to form an MOF precursor.
S2, putting the MOF precursor into a tube furnace, pyrolyzing the precursor at 800 ℃ for 4h in Ar atmosphere, and soaking the precursor in hydrochloric acid with the concentration of 20% for 24h to obtain the MOF derived carbon.
S3, dissolving 0.02g of a mixture of MOF derived carbon and 0.4ml of ethanol and 1.5g of a surfactant in 21.4ml of deionized water, and ultrasonically oscillating and uniformly stirring to form a mixed solution, which is marked as A.
And S4, adding 5ml of methyltrimethoxysilane and 3.4ml of dimethyldimethoxysilane serving as silicon sources into the solution A, fully stirring, adding ammonia water, adjusting the pH of the solution to 9, and pouring the solution into a mold to wait for gelation.
S5, adding a small amount of water into the gel, aging the gel for 24h at 40 ℃, performing solvent replacement by using ethanol, drying the gel for 12h at 80 ℃ under normal pressure, and drying the gel for 48h at 120 ℃ under normal pressure to obtain the elastic super-hydrophobic oleophylic MOF/SiO 2 Composite aerogel, labeled sample 8.
Example nine
S1, dissolving 29.7363g of zinc nitrate hexahydrate and 11.9045g of tetrafluoroterephthalic acid in 1000ml of deionized water, and dropwise adding 20ml of ammonia water to form an MOF precursor.
S2, putting the MOF precursor into a tube furnace, pyrolyzing the precursor for 4 hours at 800 ℃ under Ar atmosphere, and soaking the precursor for 24 hours by using hydrochloric acid with the concentration of 20% to obtain the MOF derived carbon.
S3, dissolving 0.1g of a mixture of MOF derived carbon and 2ml of ethanol and 1.5g of a surfactant in 21.4ml of deionized water, and performing ultrasonic oscillation and uniform stirring to form a mixed solution marked as A;
and S4, adding 5ml of methyltrimethoxysilane and 3.4ml of dimethyldimethoxysilane serving as silicon sources into the solution A, fully stirring, adding ammonia water, adjusting the pH of the solution to 9, and pouring the solution into a mold to wait for gelation.
S5, adding a small amount of water into the gel, aging the gel for 24h at 40 ℃, replacing the gel with an ethanol solvent, and performing supercritical drying at 40 ℃ and 14MPa for 12h to obtain the elastic super-hydrophobic oleophylic MOF/SiO 2 Composite aerogel, labeled sample 9.
EXAMPLE ten
S1, dissolving 29.7363g of zinc nitrate hexahydrate and 11.9045g of tetrafluoroterephthalic acid in 1000ml of deionized water, and dropwise adding 20ml of ammonia water to form an MOF precursor.
S2, putting the MOF precursor into a tube furnace, pyrolyzing the precursor at 800 ℃ for 4h in Ar atmosphere, and soaking the precursor in hydrochloric acid with the concentration of 20% for 24h to obtain the MOF derived carbon.
S3, dissolving 0.1g of a mixture of MOF-derived carbon and 2ml of ethanol and 1.5g of a surfactant in 21.4ml of deionized water, and ultrasonically oscillating and uniformly stirring to form a mixed solution, wherein the mixed solution is marked as A.
And S4, adding 5ml of methyltrimethoxysilane and 3.4ml of dimethyldimethoxysilane serving as silicon sources into the solution A, fully stirring, adding ammonia water, adjusting the pH of the solution to 9, and pouring the solution into a mold to wait for gelation.
S5, adding a small amount of water into the gel, aging the gel at 40 ℃ for 24 hours, replacing the solvent with ethanol, drying the gel at 80 ℃ for 12 hours, and drying the gel at 120 ℃ for 48 hours to obtain the elastic super-hydrophobic oleophylic MOF/SiO 2 Composite aerogel, labeled sample 10.
In the actual use process, the following method was used as a control:
in the first step, 1.5g of surfactant was dissolved in 21.4ml of deionized water, sonicated and stirred uniformly to form a mixed solution, labeled as A.
And secondly, adding 5ml of methyltrimethoxysilane and 3.4ml of dimethyldimethoxysilane serving as silicon sources into the solution A, fully stirring, adding ammonia water, adjusting the pH of the solution to 9, and pouring the solution into a mold to wait for gelation.
And thirdly, adding a small amount of water into the gel, aging the gel for 24 hours at 40 ℃, and finally performing freeze drying treatment to obtain the elastic SiO2 aerogel which is marked as a sample 11. The specific surface of sample 11 was 10.1706m2/g.
The N2 gas adsorption and desorption curve of the elastic hydrophobic oleophilic SiO2 aerogel obtained is shown in fig. 5. By comparison, the MOF/SiO prepared in the examples of the present invention 2 The composite aerogel has better hydrophobicity, lipophilicity and adsorbability.
It will be appreciated by those of ordinary skill in the art that the embodiments described herein are intended to assist the reader in understanding the principles of the invention and are to be construed as being without limitation to such specifically recited embodiments and examples. Those skilled in the art can make various other specific changes and combinations based on the teachings of the present invention without departing from the spirit of the invention, and these changes and combinations are within the scope of the invention.
Claims (10)
1. Elastic super-hydrophobic oleophylic MOF/SiO 2 The preparation method of the composite aerogel is characterized by comprising the following steps:
s1, dissolving zinc nitrate hexahydrate and tetrafluoro terephthalic acid in deionized water, and dropwise adding ammonia water to form an MOF precursor;
s2, putting the MOF precursor into a tube furnace, performing high-temperature pyrolysis in an inert atmosphere, and then performing acid washing to obtain MOF derived carbon;
s3, dissolving a mixture of MOF derived carbon and ethanol and a surfactant in deionized water, and performing ultrasonic oscillation and uniform stirring to form a mixed solution marked as A;
s4, adding methyltrimethoxysilane and dimethyldimethoxysilane serving as silicon sources into the A, fully stirring, adding an alkali catalyst, and pouring into a mold to wait for gelation;
s5, aging, solvent replacement and drying treatment are carried out on the gel to obtain the elastic super-hydrophobic oleophylic MOF/SiO 2 And (3) compounding the aerogel.
2. The elastic superhydrophobic oleophilic MOF/SiO of claim 1 2 The preparation method of the composite aerogel is characterized by comprising the following steps: the molar ratio of zinc nitrate hexahydrate to tetrafluoroterephthalic acid in the step S1 is 0.5-4.0, and the volume ratio of deionized water to ammonia water is 10-60.
3. The elastic superhydrophobic oleophilic MOF/SiO of claim 1 2 The preparation method of the composite aerogel is characterized by comprising the following steps: the inert gas in the step S2 is Ar gas or N 2 The pyrolysis temperature of the gas is 500-1100 ℃, the pyrolysis time is 0.5-8 h, and the acid is soaked in acid with the concentration of 20% of any one of hydrochloric acid, sulfuric acid and nitric acid for 6-72 h.
4. An elastic article according to claim 1Super-hydrophobic oleophilic MOF/SiO 2 The preparation method of the composite aerogel is characterized by comprising the following steps: in the step S3, the mass ratio of the MOF derived carbon to the ethanol to the surfactant is as follows: 0.002 to 2.0.
5. An elastic superhydrophobic lipophilic MOF/SiO according to claim 1 2 The preparation method of the composite aerogel is characterized by comprising the following steps: and in the step S3, the surfactant is at least one of hexadecyl trimethoxy ammonium chloride and hexadecyl trimethoxy ammonium bromide.
6. The elastic superhydrophobic oleophilic MOF/SiO of claim 1 2 The preparation method of the composite aerogel is characterized by comprising the following steps: the molar ratio of the silane to the surfactant in the step S4 is 0.5-2.0.
7. An elastic superhydrophobic lipophilic MOF/SiO according to claim 1 2 The preparation method of the composite aerogel is characterized by comprising the following steps: and in the step S4, the alkali catalyst is at least one of sodium hydroxide, potassium hydroxide and ammonia water.
8. The elastic superhydrophobic oleophilic MOF/SiO of claim 1 2 The preparation method of the composite aerogel is characterized by comprising the following steps: the volume ratio of methyltrimethoxysilane to dimethyldimethoxysilane in the step S4 is 0.5-2.0.
9. The elastic superhydrophobic oleophilic MOF/SiO of claim 1 2 The preparation method of the composite aerogel is characterized by comprising the following steps: the aging process in the step S5 is carried out at 10-80 ℃.
10. The elastic superhydrophobic oleophilic MOF/SiO of claim 1 2 The preparation method of the composite aerogel is characterized by comprising the following steps: the drying in the step S5 comprises normal pressure drying, freeze drying and supercritical drying, wherein the temperature of the normal pressure drying is 80-150 ℃, and the time isIs 24 to 72 hours; s5, pre-freezing at-50-0 ℃ for 1-12 h, and freeze-drying for 12-72 h; and S5, the supercritical drying temperature is 35-45 ℃, the pressure is 9-14 MPa, and the time is 8-36 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211297026.8A CN115845813B (en) | 2022-10-18 | 2022-10-18 | Elastic super-hydrophobic oleophylic MOF derived carbon/SiO2Preparation method of composite aerogel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211297026.8A CN115845813B (en) | 2022-10-18 | 2022-10-18 | Elastic super-hydrophobic oleophylic MOF derived carbon/SiO2Preparation method of composite aerogel |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115845813A true CN115845813A (en) | 2023-03-28 |
| CN115845813B CN115845813B (en) | 2024-07-09 |
Family
ID=85661734
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211297026.8A Active CN115845813B (en) | 2022-10-18 | 2022-10-18 | Elastic super-hydrophobic oleophylic MOF derived carbon/SiO2Preparation method of composite aerogel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115845813B (en) |
Citations (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090030131A (en) * | 2007-09-19 | 2009-03-24 | 주식회사 넵 | Method for preparing surface-modified transparent bead type aerogel and aerogel prepared therefrom |
| CN102125821A (en) * | 2011-01-13 | 2011-07-20 | 中国科学院生态环境研究中心 | Active carbon-silicon aerogel complex for removing volatile organic pollutants |
| US20120077006A1 (en) * | 2010-01-27 | 2012-03-29 | Lawrence Livermore National Security, Llc | High surface area silicon carbide-coated carbon aerogel |
| CN102773073A (en) * | 2011-11-30 | 2012-11-14 | 南京工业大学 | Hydrophobic SiO2Preparation method of aerogel-activated carbon composite material |
| CN104016360A (en) * | 2014-05-16 | 2014-09-03 | 厦门大学 | Hydrophobic lipophilic soft aerogel block and preparation method thereof |
| CN105688815A (en) * | 2016-03-22 | 2016-06-22 | 中国石油大学(华东) | Method for preparing multi-walled carbon nanotube-silicon dioxide compound aerogel |
| CN106032276A (en) * | 2015-03-13 | 2016-10-19 | 长春工业大学 | Preparation method of novel environment-friendly aerogel material used for oil-water separation |
| KR20170104914A (en) * | 2016-03-08 | 2017-09-18 | 주식회사 엘지화학 | Method for preparing aerogel blanket and aerogel blanket prepared by the same |
| WO2019070193A1 (en) * | 2017-10-03 | 2019-04-11 | Bronx Creative & Design Centre Pte Ltd | Method of manufacturing silica aerogel composite |
| CN109718727A (en) * | 2019-02-21 | 2019-05-07 | 西北大学 | Carbon aerogels and its method and its application in terms of environmental protection and energy storage based on the calcining preparation of MOFs disk |
| CN112625288A (en) * | 2020-12-08 | 2021-04-09 | 苏州启创新材料科技有限公司 | Organic-inorganic hybrid heat insulation film based on MOF/aerogel composite modification and preparation method thereof |
| CN112938930A (en) * | 2021-02-26 | 2021-06-11 | 宁波工程学院 | Bacterial cellulose composite metal organic framework material derived carbon aerogel and preparation method and application thereof |
| CN113304699A (en) * | 2021-06-03 | 2021-08-27 | 内蒙古科技大学 | Aerogel microsphere prepared by compounding coal gangue and agarose and preparation method thereof |
| CN113617331A (en) * | 2021-08-25 | 2021-11-09 | 华南农业大学 | Preparation method and application of graphite carbon-coated nano iron derived from double-layer metal organic framework material |
| CN114247425A (en) * | 2021-12-09 | 2022-03-29 | 南京大学 | Preparation method and application of carbon nanorod spherical superstructure material |
| CN114394600A (en) * | 2022-01-27 | 2022-04-26 | 华南理工大学 | Hydrophobic and oleophylic flexible silica aerogel and preparation method and application thereof |
| CN115124102A (en) * | 2022-07-04 | 2022-09-30 | 河海大学 | ZIF-8 derived carbon-wood sponge composite evaporation material and preparation method and application thereof |
-
2022
- 2022-10-18 CN CN202211297026.8A patent/CN115845813B/en active Active
Patent Citations (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090030131A (en) * | 2007-09-19 | 2009-03-24 | 주식회사 넵 | Method for preparing surface-modified transparent bead type aerogel and aerogel prepared therefrom |
| US20120077006A1 (en) * | 2010-01-27 | 2012-03-29 | Lawrence Livermore National Security, Llc | High surface area silicon carbide-coated carbon aerogel |
| CN102125821A (en) * | 2011-01-13 | 2011-07-20 | 中国科学院生态环境研究中心 | Active carbon-silicon aerogel complex for removing volatile organic pollutants |
| CN102773073A (en) * | 2011-11-30 | 2012-11-14 | 南京工业大学 | Hydrophobic SiO2Preparation method of aerogel-activated carbon composite material |
| CN104016360A (en) * | 2014-05-16 | 2014-09-03 | 厦门大学 | Hydrophobic lipophilic soft aerogel block and preparation method thereof |
| CN106032276A (en) * | 2015-03-13 | 2016-10-19 | 长春工业大学 | Preparation method of novel environment-friendly aerogel material used for oil-water separation |
| KR20170104914A (en) * | 2016-03-08 | 2017-09-18 | 주식회사 엘지화학 | Method for preparing aerogel blanket and aerogel blanket prepared by the same |
| CN105688815A (en) * | 2016-03-22 | 2016-06-22 | 中国石油大学(华东) | Method for preparing multi-walled carbon nanotube-silicon dioxide compound aerogel |
| WO2019070193A1 (en) * | 2017-10-03 | 2019-04-11 | Bronx Creative & Design Centre Pte Ltd | Method of manufacturing silica aerogel composite |
| CN109718727A (en) * | 2019-02-21 | 2019-05-07 | 西北大学 | Carbon aerogels and its method and its application in terms of environmental protection and energy storage based on the calcining preparation of MOFs disk |
| CN112625288A (en) * | 2020-12-08 | 2021-04-09 | 苏州启创新材料科技有限公司 | Organic-inorganic hybrid heat insulation film based on MOF/aerogel composite modification and preparation method thereof |
| CN112938930A (en) * | 2021-02-26 | 2021-06-11 | 宁波工程学院 | Bacterial cellulose composite metal organic framework material derived carbon aerogel and preparation method and application thereof |
| CN113304699A (en) * | 2021-06-03 | 2021-08-27 | 内蒙古科技大学 | Aerogel microsphere prepared by compounding coal gangue and agarose and preparation method thereof |
| CN113617331A (en) * | 2021-08-25 | 2021-11-09 | 华南农业大学 | Preparation method and application of graphite carbon-coated nano iron derived from double-layer metal organic framework material |
| CN114247425A (en) * | 2021-12-09 | 2022-03-29 | 南京大学 | Preparation method and application of carbon nanorod spherical superstructure material |
| CN114394600A (en) * | 2022-01-27 | 2022-04-26 | 华南理工大学 | Hydrophobic and oleophylic flexible silica aerogel and preparation method and application thereof |
| CN115124102A (en) * | 2022-07-04 | 2022-09-30 | 河海大学 | ZIF-8 derived carbon-wood sponge composite evaporation material and preparation method and application thereof |
Non-Patent Citations (6)
| Title |
|---|
| CHEN ZHI 等: "High loading of NiFe active sites on a melamine formaldehyde carbon-based aerogel towards efficient bi-functional electrocatalysis for water splitting", 《SUSTAINABLE ENERGY & FUELS》, vol. 5, no. 19, 7 October 2021 (2021-10-07), pages 4973 - 4980 * |
| PENG HAIHAO 等: "Advanced MOFs@aerogel composites: Construction and application towards environmental remediation", 《JOURNAL OF HAZARDOUS MATERIALS》, vol. 432, 15 June 2022 (2022-06-15), pages 1 - 26 * |
| SONG PIN 等: "Carbon Microtube Aerogel Derived from Kapok Fiber: An Efficient and Recyclable Sorbent for Oils and Organic Solvents", 《ACS NANO》, vol. 14, no. 1, 31 December 2019 (2019-12-31), pages 595 - 602 * |
| 任思佳 等: "高强度二氧化硅气凝胶的制备及性能研究", 《广州化工》, vol. 51, no. 11, 8 June 2023 (2023-06-08), pages 48 - 51 * |
| 唐腾飞 等: "SiO2气凝胶-活性炭复合材料的研究进展", 《炭素技术》, vol. 35, no. 6, 28 December 2016 (2016-12-28), pages 8 - 11 * |
| 王玮 等: "复合气凝胶的制备及对甲苯的吸附试验", 《消防科学与技术》, vol. 37, no. 10, 15 October 2018 (2018-10-15), pages 1396 - 1399 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115845813B (en) | 2024-07-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2019153619A1 (en) | Sulfur and nitrogen co-doped graphene-based aerogel and preparation method therefor | |
| CN112121766B (en) | Ramie fiber-based biochar and preparation method and application thereof | |
| CN106693898B (en) | Doping-degree-controllable porous reduced graphene oxide oil absorption material and preparation method thereof | |
| CN107857893B (en) | Preparation method of oil absorption material with hierarchical pore structure | |
| CN111318254B (en) | Preparation method of high-efficiency regenerated activated carbon | |
| CN109759132A (en) | The preparation method and composite photocatalyst gel ball of composite photocatalyst gel ball | |
| CN109513404A (en) | A kind of load TiO2The preparation method of the functional fiber element aerogel composite of nano particle | |
| CN108031447B (en) | Cellulose/silicon oxide composite aerogel elastomer, preparation method and application thereof in oil-water separation field | |
| CN107081127A (en) | A kind of preparation method of graphene/activated carbon composite porous microspheres | |
| CN106423100B (en) | Polyacrylonitrile/graphene-based composite aerogel adsorption material and preparation method thereof | |
| CN107935102A (en) | A kind of method that water removal moderate resistance life element is removed using persulfuric acid hydrogen salt and magnetic bismuth oxyiodide visible light catalytic | |
| CN115475604B (en) | Manufacturing method of composite multifunctional adsorbent based on cork activated carbon and amino carbon quantum dots | |
| CN110575794A (en) | super-hydrophobic cotton cellulose aerogel and preparation method and application thereof | |
| CN114452948A (en) | Modified cellulose aerogel and preparation method and application thereof | |
| CN107262051B (en) | Carboxymethyl Konjac Glucomannan microsphere adsorbing agent and preparation method thereof for dephosphorization | |
| CN108439373B (en) | Amphiphilic Janus structure graphene-based aerogel and preparation method thereof | |
| CN111298763A (en) | Modified silica gel CO2Adsorbent and preparation method and application thereof | |
| CN110327905A (en) | A kind of nitrogenous porous carbon nano-composite material preparation method of polyaniline carbon nanotube base | |
| Ma et al. | Preparation of 3D superhydrophobic porous g-C3N4 nanosheets@ carbonized kapok fiber composites for oil/water separation and treating organic pollutants | |
| CN115845813A (en) | Elastic super-hydrophobic oleophylic MOF/SiO 2 Preparation method of composite aerogel | |
| CN108837798B (en) | Hollow hierarchical core-shell structure biomass carbon aerogel, and preparation method and application thereof | |
| CN114700065B (en) | Waste resin carbon sphere composite ozone catalyst and preparation method and application thereof | |
| CN113926423B (en) | Modified biochar using water hyacinth, preparation method thereof and treatment method of organic pollutants | |
| CN113173665B (en) | ZnWO 4 /MgWO 4 Method for degrading organic wastewater by using composite semiconductor material | |
| CN115072845A (en) | Nano porous carbon modified graphite felt cathode material and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |