CN111250061A - Preparation method of titanium dioxide/graphene oxide/stearic acid composite modified sponge - Google Patents
Preparation method of titanium dioxide/graphene oxide/stearic acid composite modified sponge Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 136
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 87
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 68
- 239000002131 composite material Substances 0.000 title claims abstract description 58
- 235000021355 Stearic acid Nutrition 0.000 title claims abstract description 49
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 title claims abstract description 49
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000008117 stearic acid Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 24
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000006185 dispersion Substances 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 238000002791 soaking Methods 0.000 claims abstract description 11
- 238000007865 diluting Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 230000002209 hydrophobic effect Effects 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 description 25
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 12
- 238000012360 testing method Methods 0.000 description 11
- 238000005303 weighing Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical group ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- PLZVEHJLHYMBBY-UHFFFAOYSA-N Tetradecylamine Chemical compound CCCCCCCCCCCCCCN PLZVEHJLHYMBBY-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 241000779819 Syncarpia glomulifera Species 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 239000001045 blue dye Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 238000012669 compression test Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- -1 graphite alkene Chemical class 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- QJAOYSPHSNGHNC-UHFFFAOYSA-N octadecane-1-thiol Chemical compound CCCCCCCCCCCCCCCCCCS QJAOYSPHSNGHNC-UHFFFAOYSA-N 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 239000001739 pinus spp. Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000001612 separation test Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229940036248 turpentine Drugs 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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Abstract
The invention relates to a preparation method of titanium dioxide/graphene oxide/stearic acid composite modified sponge, which comprises the following steps: (1) soaking sponge in pure water and absolute ethyl alcohol respectively, performing ultrasonic treatment, and drying to obtain pretreated sponge for later use; (2) taking the graphene oxide dispersion liquid, and diluting with absolute ethyl alcohol to obtain a graphene oxide solution; (3) adding titanium dioxide powder into the graphene oxide solution prepared in the step (2), adding stearic acid, and performing ultrasonic treatment to obtain a mixed solution; (4) and (3) finally, soaking the pretreated sponge obtained in the step (1) in the mixed solution, performing ultrasonic treatment, and drying to obtain the finished product. Compared with the prior art, the preparation process is simple, the obtained composite modified sponge has strong hydrophobic oil absorption, can be produced in a large scale, and has wide practical application.
Description
Technical Field
The invention belongs to the technical field of modified sponges, and relates to a titanium dioxide/graphene oxide/stearic acid composite modified sponge and a preparation method thereof.
Background
Water is an important resource on which humans live, but today our water resources are severely polluted. According to statistics, about 5 hundred million kilograms of oil substances flow into the sea every year due to ship failures worldwide, fatal and long-term influence is generated on the ecological environment, the oil substances can be suspended on the sea after leakage, oxygen is isolated, natural degradation is avoided, and the methods mainly include a combustion method, an adsorption method, chemical treatment and the like at present. Among these schemes, adsorption is considered to be the most efficient, least costly method, and produces less secondary pollution.
The melamine sponge has the characteristics of low density, high strength, high air gap, low cost and the like, and has been widely applied as an oil absorption material; however, the sponge has the characteristics of hydrophilicity and poor water-oil separation, can not well block organic matters and water, has the defects of low adsorption rate, poor reutilization rate and the like in the practical application process, and is difficult to meet the requirement of sewage treatment.
Graphene Oxide (GO), which is a carbon material widely researched and applied at present, has the properties of high electron mobility, high strength and high specific surface area of graphene itself, and has many oxygen-containing groups on the planes and edges after oxidation, wherein the oxygen-containing groups enable the graphene oxide to add active sites and adsorb many organic substances.
Titanium dioxide is a widely used material, the conventional usage is to degrade organic pollutants by utilizing the photocatalysis, water is decomposed by photocatalysis to inactivate bacteria, and the titanium dioxide serving as the photocatalyst is widely used in the field of pollution treatment due to the advantages of higher activity, hydrophobicity, low price, no toxicity and the like.
Patent CN108384049A provides a preparation method of titanium dioxide-graphene composite sponge, which improves the injection capability of titanium dioxide and graphene on the sponge through a reduction reaction under a sealed condition, and the modified sponge does not fall off in the use process, and has high photocatalytic efficiency and good photocatalytic stability; patent CN110180513A provides a titanium dioxide-graphene oxide composite sponge, and the composite sponge has a good adsorption catalysis effect on phenol-containing sewage, the adsorption amount of the composite sponge on phenol reaches 219mg/g, the photodegradation rate on phenol can reach 86%, and the composite sponge has a remarkable application effect in phenol-containing sewage treatment. The adhesion ability of titanium dioxide, graphite alkene on the sponge has been improved to above-mentioned patent, has improved the organic matter adsorption efficiency of single sponge, but its repeatability is relatively poor.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of a titanium dioxide/graphene oxide/stearic acid composite modified sponge.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of titanium dioxide/graphene oxide/stearic acid composite modified sponge comprises the following steps:
(1) soaking sponge in pure water and absolute ethyl alcohol respectively, performing ultrasonic treatment, and drying to obtain pretreated sponge for later use;
(2) taking the graphene oxide dispersion liquid, and diluting with absolute ethyl alcohol to obtain a graphene oxide solution;
(3) adding titanium dioxide powder into the graphene oxide solution prepared in the step (2), adding stearic acid, and performing ultrasonic treatment to obtain a mixed solution;
(4) and (3) finally, soaking the pretreated sponge obtained in the step (1) in the mixed solution, performing ultrasonic treatment, and drying to obtain the finished product.
Further, in the step (1), the time of ultrasonic treatment is 15-30 min.
Further, in the step (1), the drying process conditions are as follows: drying in a 30 ℃ thermostat for 12-18 h.
Further, in the step (2), the concentration of the graphene oxide solution is 2-4 mg/ml.
Further, in the step (3), the mass ratio of the titanium dioxide to the graphene oxide is 1-5: 2.
Further, in the step (3), the mass ratio of titanium dioxide to stearic acid is 1: 2-3: 1.
Further, in the step (3), the time of ultrasonic treatment is 15-30 min.
Further, in the step (4), the drying conditions are as follows: drying at 30-40 deg.C for 12-18 h.
Compared with the prior art, the invention has the following advantages:
1) the sponge can adsorb and degrade organic dye after being modified by titanium dioxide and graphene oxide;
2) after stearic acid is added for composite modification, the adsorption capacity of the sponge for hydrophobic and organic matters is obviously improved, the adsorption repeatability is good, and when stearic acid is not added, the adsorption repeatability is poor;
3) the preparation process is simple, the repeatability is good, the cost is low, the preparation process is green and environment-friendly, and the preparation method can be used for treating organic pollution on a large scale.
Drawings
Fig. 1 is an SEM of the titanium dioxide/graphene oxide/stearic acid composite modified sponge prepared by the present invention.
Fig. 2 is a water-oil separation diagram of the titanium dioxide/graphene oxide/stearic acid composite modified sponge prepared by the invention.
Fig. 3 is a test of adsorption repeatability of the titanium dioxide/graphene oxide/stearic acid composite modified sponge prepared by the invention on methylene blue dye under ultraviolet illumination.
FIG. 4 is a graph showing the repeatability of hexane adsorption of the titanium dioxide/graphene oxide composite modified sponge prepared by the invention, which is reduced from 32.4g/g at the first time to 18.93g/g at the fifth time, and shows that the prepared composite modified sponge has poor adsorption repeatability when no stearic acid is doped and modified.
Fig. 5 is a graph showing the repeatability of the titanium dioxide/graphene oxide/stearic acid composite modified sponge prepared by the invention on hexane adsorption.
Fig. 6 is a graph showing the adsorption repeatability of the titanium dioxide/graphene oxide/stearic acid composite modified sponge prepared by the invention on other organic matters.
Fig. 7 is a graph of compressive stress-strain test for pure sponge (MS) and composite modified sponge (TGMS), and a graph of cyclic compression test for composite modified sponge.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
In the following examples, unless otherwise specified, the starting materials or the treatment techniques are all conventional and commercially available materials or conventional treatment techniques in the art.
Example 1:
a preparation method of titanium dioxide/graphene oxide/stearic acid composite modified sponge comprises the following steps:
(1) cutting sponge into proper volume, ultrasonically cleaning with absolute ethyl alcohol and deionized water for 30min, and drying in a 30 ℃ thermostat for 12 h;
(2) taking the graphene oxide dispersion liquid, and diluting the graphene oxide dispersion liquid into a graphene oxide solution with the concentration of 2mg/ml by using absolute ethyl alcohol as a solvent;
(3) weighing titanium dioxide according to the mass ratio of the titanium dioxide to the graphene oxide of 1:2, weighing stearic acid according to the mass ratio of the titanium dioxide to the stearic acid of 1:2, mixing with the titanium dioxide, adding into the graphene oxide solution obtained in the step (2), and carrying out ultrasonic treatment for 15min to fully mix;
(4) soaking the sponge treated in the step (1) in the mixed solution obtained in the step (3), performing ultrasonic treatment for 30min, and taking out and drying in a 30 ℃ thermostat for 12 h.
Example 2:
a preparation method of titanium dioxide/graphene oxide/stearic acid composite modified sponge comprises the following steps:
(1) cutting sponge into proper volume, ultrasonically cleaning with absolute ethyl alcohol and deionized water for 30min, and drying in a 30 ℃ thermostat for 15 h;
(2) taking the graphene oxide dispersion liquid, and diluting the graphene oxide dispersion liquid into a graphene oxide solution with the concentration of 3mg/ml by using absolute ethyl alcohol as a solvent;
(3) weighing titanium dioxide according to the mass ratio of 3:2 of titanium dioxide to graphene oxide, weighing stearic acid according to the mass ratio of 1.5:1 of titanium dioxide to stearic acid, mixing with titanium dioxide, adding into the graphene oxide solution obtained in the step (2), and carrying out ultrasonic treatment for 20min to fully mix;
(4) soaking the sponge treated in the step (1) in the mixed solution obtained in the step (3), performing ultrasonic treatment for 40min, and taking out and drying in a 30 ℃ thermostat for 15 h.
Example 3
A preparation method of titanium dioxide/graphene oxide/stearic acid composite modified sponge comprises the following steps:
(1) cutting sponge into proper volume, ultrasonically cleaning with anhydrous ethanol and deionized water for 50min, and drying in a 30 ℃ thermostat for 18 h;
(2) taking the graphene oxide dispersion liquid, and diluting the graphene oxide dispersion liquid into a graphene oxide solution with the concentration of 4mg/ml by using absolute ethyl alcohol as a solvent;
(3) weighing titanium dioxide according to the mass ratio of 5:2 of titanium dioxide to graphene oxide, weighing stearic acid according to the mass ratio of 3:1 of titanium dioxide to stearic acid, mixing with titanium dioxide, adding into the graphene oxide solution obtained in the step (2), and carrying out ultrasonic treatment for 25min to fully mix;
(4) soaking the sponge treated in the step (1) in the mixed solution obtained in the step (3), performing ultrasonic treatment for 40min, and taking out and drying in a 30 ℃ thermostat for 17 h.
Comparative example 1:
a preparation method of titanium dioxide/graphene oxide composite modified sponge comprises the following steps:
(1) cutting sponge into proper volume, ultrasonically cleaning with absolute ethyl alcohol and deionized water for 30min, and drying in a 30 ℃ thermostat for 15 h;
(2) taking the graphene oxide dispersion liquid, and diluting the graphene oxide dispersion liquid into a graphene oxide solution with the concentration of 3mg/ml by using absolute ethyl alcohol as a solvent;
(3) weighing titanium dioxide according to the mass ratio of 3:2 of the titanium dioxide to the graphene oxide, adding the titanium dioxide into the graphene oxide solution obtained in the step (2), and carrying out ultrasonic treatment for 20min to fully mix the titanium dioxide and the graphene oxide;
(4) soaking the sponge treated in the step (1) in the mixed solution obtained in the step (3), performing ultrasonic treatment for 40min, and taking out and drying in a 30 ℃ thermostat for 15 h.
The titanium dioxide/graphene oxide/stearic acid composite modified sponges prepared in examples 1, 2 and 3 were subjected to contact angle measurement, and the contact angles thereof were 135 °, 141 ° and 148 °, respectively, and the titanium dioxide/graphene oxide composite modified sponge without stearic acid (comparative example 1) was subjected to contact angle measurement, and the contact angle thereof was 124 °, which indicates that the contact angle of the composite modified sponge was significantly increased after the addition of stearic acid, and good hydrophobicity was exhibited although superhydrophobicity (CA ≧ 150 °) was not achieved.
SEM characterization is performed on the titanium dioxide/graphene oxide/stearic acid composite modified sponges prepared in examples 1 and 2, as shown in fig. 1, a-b are SEM scan images of example 1, c-d are SEM scan images of example 2, titanium dioxide particles can be observed on graphene oxide plane and edge folds, and graphene oxide is combined with the sponge to generate a stable and fold-filled plane or edge, which effectively combines the three to coat the particles on the graphene oxide.
The water-oil separation test is performed on the titanium dioxide/graphene oxide/stearic acid composite modified sponge prepared in example 1, as shown in fig. 2, after the test is finished, the upper layer is methylene blue pure water, the lower layer is chloroform, and the water-oil separation is thorough, which indicates that the modified sponge has good hydrophobicity and strong adsorption to chloroform organic matters.
A repeated adsorption test is performed on the titanium dioxide/graphene oxide/stearic acid composite modified sponge prepared in example 1, and as shown in fig. 3, the titanium dioxide/graphene oxide/stearic acid composite modified sponge still has a high adsorption capacity after being subjected to adsorption degradation for 20 times under the ultraviolet illumination condition, which indicates that the composite modified sponge has an excellent adsorption degradation capacity.
Performing a repeated adsorption test on the titanium dioxide/graphene oxide composite modified sponge prepared in the comparative example 1, wherein when no stearic acid is added, the adsorption amount of the sponge to hexane is reduced from 32.4g/g at the first time to 18.93g/g at the fifth time; the composite modified sponge prepared in example 2 was subjected to a repeated adsorption test, and as shown in fig. 5, the composite modified sponge modified with stearic acid still had a good repeated effect after being repeatedly used for 30 times.
An adsorption repeatability test is performed on the titanium dioxide/graphene oxide/stearic acid composite modified sponge prepared in example 3, and as shown in fig. 6, the composite modified sponge has good adsorption repeatability on hexane, and also has good adsorption repeatability on petroleum ether and turpentine.
The titanium dioxide/graphene oxide/stearic acid composite modified sponge prepared in example 3 was cut into a predetermined size (10mm × 10mm × 10mm), and subjected to mechanical property test. Firstly, testing the mechanical properties of pure sponge, respectively setting the compression amounts to be 20%, 40%, 60% and 80%, and recording the relation between the deformation amount and the stress; then testing the mechanical properties of the sponge after the composite modification, setting the compression amounts to be 20%, 40%, 60% and 80% in the same way, and comparing the mechanical property changes of the pure sponge and the sponge after the composite modification; meanwhile, the fatigue resistance of the composite modified sponge is researched, the composite modified sponge is subjected to 80% deformation quantity test and repeated for 100 times, the influence of extrusion or use times on the mechanical property of the sponge material is observed and researched, and the result is shown in figure 7. As shown in fig. 7, it can be seen from the graph (a) that the mechanical properties of the composite modified sponge of the present invention are significantly improved compared with the pure sponge material under the condition of 80% deformation, which indicates that the mechanical properties of the sponge are significantly improved by the addition of materials such as titanium dioxide and graphene oxide; as can be seen from the graph (b), the mechanical properties of the composite modified sponge of the present invention remained substantially unchanged after being subjected to 100 pressure-compression cycles, indicating that TGMS has a high degree of fatigue resistance under a large compressive strain. The TGMS sponge has great advantages in practical application, and after organic matters are adsorbed, a large amount of adsorbate can be extruded in a squeezing mode without influencing the repeated use of the sponge.
Comparative example 2:
a preparation method of titanium dioxide/graphene oxide/n-octadecyl mercaptan composite modified sponge comprises the following steps:
(1) cutting sponge into proper volume, ultrasonically cleaning with absolute ethyl alcohol and deionized water for 30min, and drying in a 30 ℃ thermostat for 15 h;
(2) taking the graphene oxide dispersion liquid, and diluting the graphene oxide dispersion liquid into a graphene oxide solution with the concentration of 3mg/ml by using absolute ethyl alcohol as a solvent;
(3) weighing titanium dioxide according to the mass ratio of 3:2 of the titanium dioxide to the graphene oxide; weighing decatetramine according to the mass ratio of graphene oxide to decatetramine of 1.5:1, adding the decatetramine into the graphene oxide solution obtained in the step (2), and carrying out ultrasonic treatment for 20min to fully mix the mixture;
(4) soaking the sponge treated in the step (1) in the mixed solution obtained in the step (3), performing ultrasonic treatment for 40min, and taking out and drying in a 30 ℃ thermostat for 15 h.
The contact angle of the titanium dioxide/graphene oxide/tetradecylamine composite modified sponge obtained in the comparative example 2 is measured to be 120 degrees, while the contact angles of the titanium dioxide/graphene oxide/stearic acid composite modified sponges adopted in the examples 1 to 3 are 135 degrees, 141 degrees and 148 degrees respectively, which shows that the composite modification effect of stearic acid is better than that of the conventional modifier, namely tetradecylamine.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (8)
1. A preparation method of titanium dioxide/graphene oxide/stearic acid composite modified sponge is characterized by comprising the following steps:
(1) soaking sponge in pure water and absolute ethyl alcohol respectively, performing ultrasonic treatment, and drying to obtain pretreated sponge for later use;
(2) taking the graphene oxide dispersion liquid, and diluting with absolute ethyl alcohol to obtain a graphene oxide solution;
(3) adding titanium dioxide powder into the graphene oxide solution prepared in the step (2), adding stearic acid, and performing ultrasonic treatment to obtain a mixed solution;
(4) and (3) finally, soaking the pretreated sponge obtained in the step (1) in the mixed solution, performing ultrasonic treatment, and drying to obtain the finished product.
2. The preparation method of the titanium dioxide/graphene oxide/stearic acid composite modified sponge according to claim 1, wherein in the step (1), the ultrasonic treatment time is 15-30 min.
3. The preparation method of the titanium dioxide/graphene oxide/stearic acid composite modified sponge according to claim 1, wherein in the step (1), the drying process conditions are as follows: drying in a 30 ℃ thermostat for 12-18 h.
4. The method for preparing the titanium dioxide/graphene oxide/stearic acid composite modified sponge according to claim 1, wherein in the step (2), the concentration of the graphene oxide solution is 2-4 mg/ml.
5. The preparation method of the titanium dioxide/graphene oxide/stearic acid composite modified sponge according to claim 1, wherein in the step (3), the mass ratio of the titanium dioxide to the graphene oxide is 1-5: 2.
6. The preparation method of the titanium dioxide/graphene oxide/stearic acid composite modified sponge according to claim 1, wherein in the step (3), the mass ratio of titanium dioxide to stearic acid is 1: 2-3: 1.
7. The preparation method of the titanium dioxide/graphene oxide/stearic acid composite modified sponge according to claim 1, wherein in the step (3), the ultrasonic treatment time is 15-30 min.
8. The preparation method of the titanium dioxide/graphene oxide/stearic acid composite modified sponge according to claim 1, wherein in the step (4), the drying conditions are as follows: drying at 30-40 deg.C for 12-18 h.
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