CN109847709B - Luffa composite oil absorption material - Google Patents
Luffa composite oil absorption material Download PDFInfo
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- CN109847709B CN109847709B CN201811560045.9A CN201811560045A CN109847709B CN 109847709 B CN109847709 B CN 109847709B CN 201811560045 A CN201811560045 A CN 201811560045A CN 109847709 B CN109847709 B CN 109847709B
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- 238000010521 absorption reaction Methods 0.000 title claims abstract description 55
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 239000000463 material Substances 0.000 title claims abstract description 43
- 241000219138 Luffa Species 0.000 title description 2
- 235000003956 Luffa Nutrition 0.000 title description 2
- 244000280244 Luffa acutangula Species 0.000 claims abstract description 101
- 235000009814 Luffa aegyptiaca Nutrition 0.000 claims abstract description 101
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 42
- 239000007787 solid Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 18
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 12
- 239000012298 atmosphere Substances 0.000 claims description 10
- 238000003763 carbonization Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 238000010000 carbonizing Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 4
- 239000000779 smoke Substances 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- 239000002912 waste gas Substances 0.000 abstract description 3
- 238000013329 compounding Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 230000035699 permeability Effects 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 231100001234 toxic pollutant Toxicity 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 48
- 239000004519 grease Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Chemical compound CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- MSBXTPRURXJCPF-DQWIULQBSA-N cucurbit[6]uril Chemical compound N1([C@@H]2[C@@H]3N(C1=O)CN1[C@@H]4[C@@H]5N(C1=O)CN1[C@@H]6[C@@H]7N(C1=O)CN1[C@@H]8[C@@H]9N(C1=O)CN([C@H]1N(C%10=O)CN9C(=O)N8CN7C(=O)N6CN5C(=O)N4CN3C(=O)N2C2)C3=O)CN4C(=O)N5[C@@H]6[C@H]4N2C(=O)N6CN%10[C@H]1N3C5 MSBXTPRURXJCPF-DQWIULQBSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- JQCXWCOOWVGKMT-UHFFFAOYSA-N phthalic acid diheptyl ester Natural products CCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCC JQCXWCOOWVGKMT-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention relates to a loofah sponge composite oil absorption material, which has the advantages of no generation of harmful and toxic pollutants in the preparation process, simplicity and convenience in operation and high efficiency, and can be used repeatedly for many times by compounding loofah sponge and graphene to obtain a composite oil absorption material with a large pore structure and good air permeability. The loofah sponge composite oil absorption material with high oil absorption and recycling effects, which is prepared by the invention, can be applied to marine oil stain treatment and oil smoke waste gas purification.
Description
Technical Field
The invention relates to a loofah sponge composite oil absorption material, and belongs to the technical field of preparation and application of environment purification materials.
Background
The oil pollution of water body is easily caused in the process of oil exploitation and transportation and the discharge of oily sewage in factories and cities, the biological health is harmed, and the method becomes a major environmental problem concerned all over the world.
In addition, edible oil can form the oil smoke in giving off the air with the oil mist form during the culinary art, and its harm is not a little, and multiple toxic composition in the oil smoke not only directly threatens human health, still can increase city fine object content, lead to air pollution, aggravate the emergence of haze weather.
Therefore, a practical and efficient porous oil absorption material is researched, and besides high oil absorption performance, the porous oil absorption material needs to be provided with a macroporous structure, a through hole structure and a microporous structure, so that sewage or waste can rapidly pass through the material, oil can be efficiently absorbed, and the problem of pollution caused by the oil pollution in water or air can be rapidly and efficiently solved.
The nano carbon-based material, particularly the novel graphene material, has the advantages of large specific surface area and strong oil absorption capacity, but the graphene oil absorption material has the defect of poor mechanical strength due to poor binding force, is similar to sponge, has small pores, is easy to block, and is insufficient in current practical application. The natural loofah sponge is a porous material with a unique spatial structure and formed by macro macropores and micropores, has certain mechanical strength, and the oil absorption capacity of the natural loofah sponge needs to be further improved.
Disclosure of Invention
The invention aims to overcome the defects that the existing graphene oil absorption material is poor in binding force and easy to block, and provides a practical and efficient loofah sponge composite oil absorption material which can adsorb grease more quickly and efficiently.
In order to achieve the purpose, the invention adopts the following technical scheme:
the loofah sponge composite oil absorption material is prepared by the following method:
(1) slicing loofah sponge, and carbonizing at 200-450 ℃ for 0.5-6 h in an anaerobic atmosphere to obtain carbonized loofah sponge;
(2) mixing the carbonized loofah sponge obtained in the step (1), hexadecyl trimethyl ammonium bromide and water, stirring for 1.5-2.5 hours at the temperature of 80-100 ℃, taking out and washing loofah sponge solids, and drying the loofah sponge solids for 1-2 hours at the temperature of 95-105 ℃ to obtain modified loofah sponge;
(3) weighing graphene oxide, mixing the graphene oxide with water, and stirring for 10-35 min under ultrasound to obtain a graphene oxide suspension;
(4) and (3) mixing the graphene suspension obtained in the step (3) with the modified loofah sponge obtained in the step (2), placing the mixture at 120-180 ℃ for hydrothermal reaction for 10-18 h to obtain a porous composite material, and then placing the porous composite material at 40-90 ℃ for drying for 4-48 h to obtain the loofah sponge composite oil absorption material.
Preferably, in the step (1), the carbonization conditions are that the anaerobic atmosphere is vacuum and N is2Atmosphere or Ar atmosphere.
Preferably, in the step (1), the carbonization temperature is 200-280 ℃, and the carbonization time is 0.5-2 h.
Preferably, in the step (2), the carbonized loofah sponge, cetyl trimethyl ammonium bromide and water are mixed and stirred for 1.5-2 hours at the temperature of 80-95 ℃ to obtain the loofah sponge solid.
Preferably, in the step (2), the loofah sponge solid is dried at 100-105 ℃ for 1-2 hours to obtain the modified loofah sponge.
Preferably, in the step (2), the mass ratio of the carbonized loofah sponge to the cetyl trimethyl ammonium bromide to the water is 1: 0.08-0.1: 200-250.
Preferably, in the step (3), the mass ratio of the graphene to the water is 1: 250-1000.
Preferably, in the step (4), the hydrothermal reaction temperature is 120 to 160 ℃.
Preferably, in the step (4), the hydrothermal reaction time is 10-12 h.
Preferably, in the step (4), the drying process of the porous composite material is performed in a freeze drying oven or a vacuum drying oven.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method disclosed by the invention has the advantages of no generation of harmful and toxic pollutants, simplicity and convenience in operation and high efficiency, and the loofah sponge and the graphene are compounded, so that the composite oil absorption material with a large pore structure and good air permeability can be obtained, and the composite oil absorption material can be repeatedly used for many times;
(2) the loofah sponge is treated by an oxygen-free carbonization method, the carbonization process can promote the removal of water and volatile components in the loofah sponge, and the loofah sponge is accompanied with the decomposition of cellulose, hemicellulose and lignin in the loofah sponge when in use, so that the specific surface area of the loofah sponge can be increased, and the oil absorption performance can be improved;
(3) modifying carbonized loofah sponge by cetyl trimethyl ammonium bromide, so that the electropositivity of the surface of the carbonized loofah sponge can be improved, in the process of loading graphene by hydrothermal treatment, the carbonized loofah sponge with positive charges on the surface can increase the electrostatic attraction to negatively charged Graphene Oxide (GO), promote the uniform distribution of graphene on the surface of the loofah sponge, prevent the graphene from agglomerating and growing, thereby obtaining a loofah sponge composite material with uniformly loaded graphene oxide, and reducing the graphene oxide on the surface of the loofah sponge into reduced graphene by hydrothermal reaction, thereby obtaining a loofah sponge composite oil absorption material;
the main reactions are as follows:
modification of carbonized loofah sponge: cetyl trimethyl ammonium bromide + carbonized retinervus Luffae fructus → modified carbonized retinervus Luffae fructus (with positive electricity)
Compounding the oxidized graphene-modified carbonized graphite network: carbonized loofah sponge with positive charge on surface and graphene oxide (with negative charge) → graphene oxide uniformly dispersed loofah sponge composite material (electrostatic adsorption)
Hydrothermal reaction: loofah sponge composite material → loofah sponge composite oil absorption material with graphene uniformly dispersed
(4) The loofah sponge composite oil absorption material has high specific surface area and promotes uniform loading of graphene on the loofah sponge filamentous network through carbonization and surface modification treatment of the loofah sponge, so that the obtained loofah sponge composite oil absorption material has good oil absorption performance and an excellent three-dimensional through hole structure, and can efficiently treat oily sewage/waste gas.
The loofah sponge composite oil absorption material with high oil absorption and recycling effects, which is prepared by the invention, can be applied to marine oil stain treatment and oil smoke waste gas purification.
Drawings
Fig. 1 is an SEM photograph of the loofah sponge composite oil absorption material obtained in example 1 of the present invention.
Detailed Description
The present invention is further illustrated by the following specific examples, but the scope of the invention is not limited thereto.
The raw materials and reagents used in the invention are all available from the market.
Example 1:
(1) slicing retinervus Luffae fructus at 200 deg.C and N2Carbonizing for 4h in the atmosphere to obtain carbonized loofah sponge;
(2) weighing 0.05g of hexadecyl trimethyl ammonium bromide, adding the hexadecyl trimethyl ammonium bromide into 100ml of water, stirring and mixing, weighing 0.5g of carbonized loofah, adding the carbonized loofah into the solution, stirring and modifying at 80 ℃ for 2 hours, taking out loofah solids, washing, and drying the loofah solids at 100 ℃ for 1 hour to obtain modified loofah;
(3) weighing 50mg of graphene, adding the graphene into 50ml of water, and stirring and mixing for 10min under ultrasonic waves to obtain a graphene suspension;
(4) and mixing the graphene suspension with the modified loofah sponge, performing hydrothermal reaction for 10 hours at 140 ℃ to obtain a porous solid, and drying the porous solid at 90 ℃ for 4 hours to obtain the loofah sponge composite oil absorption material. The SEM photograph of the loofah sponge composite oil absorption material is shown in figure 1.
Example 2:
(1) slicing retinervus Luffae fructus, and heating at 450 deg.C and N2Carbonizing for 2h in the atmosphere to obtain carbonized loofah;
(2) weighing 0.05g of hexadecyl trimethyl ammonium bromide, adding the hexadecyl trimethyl ammonium bromide into 300ml of water, stirring and mixing, weighing 1g of carbonized loofah, adding the carbonized loofah into the solution, stirring and modifying at 100 ℃ for 1.5h, taking out loofah solids, washing, drying the loofah solids at 105 ℃ for 2h, and obtaining modified loofah;
(3) weighing 300mg of graphene, adding the graphene into 75ml of water, and stirring and mixing for 35min under ultrasonic to obtain a graphene suspension;
(4) and mixing the graphene suspension with the modified loofah sponge, performing hydrothermal reaction at 160 ℃ for 18h to obtain a porous solid, and drying the porous solid at 40 ℃ for 48h to obtain the loofah sponge composite oil absorption material.
Example 3:
(1) slicing retinervus Luffae fructus, and carbonizing at 280 deg.C under vacuum for 6 hr to obtain carbonized retinervus Luffae fructus;
(2) weighing 0.1g of hexadecyl trimethyl ammonium bromide, adding the hexadecyl trimethyl ammonium bromide into 400ml of water, stirring and mixing, weighing 2g of carbonized loofah, adding the carbonized loofah into the solution, stirring and modifying at 95 ℃ for 2.5h, taking out loofah solids, washing, drying the loofah solids at 95 ℃ for 1h, and obtaining modified loofah;
(3) weighing 330mg of graphene, adding the graphene into 105ml of water, and stirring and mixing for 30min under ultrasonic to obtain a graphene suspension;
(4) and mixing the graphene suspension with the modified loofah sponge, performing hydrothermal reaction for 12h at 180 ℃ to obtain a porous solid, and drying the porous solid at 50 ℃ for 30h to obtain the loofah sponge composite oil absorption material.
Example 4:
(1) slicing retinervus Luffae fructus at 400 deg.C and N2Carbonizing for 0.5h under atmosphere to obtain carbonized retinervus Luffae fructus;
(2) weighing 0.08g of hexadecyl trimethyl ammonium bromide, adding the hexadecyl trimethyl ammonium bromide into 250ml of water, stirring and mixing, weighing 1g of carbonized loofah, adding the carbonized loofah into the solution, stirring and modifying at 100 ℃ for 2.5 hours, taking out loofah solids, washing, drying the loofah solids at 95 ℃ for 2 hours, and obtaining modified loofah;
(3) weighing 100mg of graphene, adding the graphene into 80ml of water, and stirring and mixing for 35min under ultrasonic waves to obtain a graphene suspension;
(4) and mixing the graphene suspension with the modified loofah sponge, performing hydrothermal reaction at 120 ℃ for 18h to obtain a porous solid, and drying the porous solid at 90 ℃ for 12h to obtain the loofah sponge composite oil absorption material.
Performance test experiments:
adding 100ml of di-n-octyl phthalate (simulated grease) into a 250ml beaker, adding the loofah sponge composite oil absorption material prepared in the embodiment 1-4 into the simulated grease, adsorbing for 10min at room temperature, recovering the loofah sponge composite oil absorption material by using tweezers, and calculating the oil absorption multiplying power (Q), wherein the calculation formula is as follows: q ═ WAfter absorbing oil-WBefore oil absorption)/WBefore oil absorptionW is a filamentThe weight of the cucurbituril composite oil absorption material before and after oil absorption. The results of the experiment are shown in table 1.
TABLE 1 test and analysis results of examples 1-3 and comparative examples
| Sample (I) | Oil absorption multiplying power |
| Example 1 | 14.1 |
| Example 2 | 14.5 |
| Example 3 | 16.3 |
| Example 4 | 13.9 |
As can be seen from the oil absorption multiplying power detection and analysis results of the samples in the examples 1 to 4 in the table 1, the samples in the examples 1 to 4 have higher oil absorption multiplying power and better oil absorption performance.
Claims (10)
1. The loofah sponge composite oil absorption material is characterized by being prepared by the following method:
(1) slicing loofah sponge, and carbonizing at 200-450 ℃ for 0.5-6 h in an anaerobic atmosphere to obtain carbonized loofah sponge;
(2) mixing the carbonized loofah sponge obtained in the step (1), hexadecyl trimethyl ammonium bromide and water, stirring for 1.5-2.5 hours at the temperature of 80-100 ℃, taking out and washing loofah sponge solids, and drying the loofah sponge solids for 1-2 hours at the temperature of 95-105 ℃ to obtain modified loofah sponge;
(3) weighing graphene oxide, mixing the graphene oxide with water, and stirring for 10-35 min under ultrasound to obtain a graphene oxide suspension;
(4) and (3) mixing the graphene suspension obtained in the step (3) with the modified loofah sponge obtained in the step (2), placing the mixture at 120-180 ℃ for hydrothermal reaction for 10-18 h to obtain a porous composite material, and then placing the porous composite material at 40-90 ℃ for drying for 4-48 h to obtain the loofah sponge composite oil absorption material.
2. The loofah sponge composite oil absorption material as claimed in claim 1, wherein the oxygen-free atmosphere is vacuum, N2Atmosphere or Ar atmosphere.
3. The loofah sponge composite oil absorption material as claimed in claim 1 or 2, wherein in the step (1), the carbonization temperature is 200-280 ℃, and the carbonization time is 0.5-2 h.
4. The loofah sponge composite oil absorption material as claimed in claim 1, wherein in the step (2), the carbonized loofah sponge, cetyl trimethyl ammonium bromide and water are mixed and stirred at 80-95 ℃ for 1.5-2 h to obtain loofah sponge solid.
5. The loofah sponge composite oil absorption material as claimed in claim 1, wherein in the step (2), the loofah sponge solid is dried at 100-105 ℃ for 1-2 hours to obtain the modified loofah sponge.
6. The loofah sponge composite oil absorption material according to claim 1, 4 or 5, wherein in the step (2), the mass ratio of the carbonized loofah sponge to the cetyl trimethyl ammonium bromide and the water is 1: 0.08-0.1: 200 to 250.
7. The loofah sponge composite oil absorption material as claimed in claim 1, wherein in the step (3), the mass ratio of graphene to water is 1: 250 to 1000.
8. The loofah sponge composite oil absorption material as claimed in claim 1, wherein in the step (4), the hydrothermal reaction temperature is 120-160 ℃.
9. The loofah sponge composite oil absorption material as claimed in claim 1, wherein in the step (4), the hydrothermal reaction time is 10-12 h.
10. The loofah sponge composite oil absorption material as claimed in claim 1, wherein in step (4), the drying process of the porous composite material is performed in a vacuum drying oven.
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