CN110947359A - Low-density high-elasticity hydrophobic/oleophylic carbon sponge and preparation method and application thereof - Google Patents
Low-density high-elasticity hydrophobic/oleophylic carbon sponge and preparation method and application thereof Download PDFInfo
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- CN110947359A CN110947359A CN201811121991.3A CN201811121991A CN110947359A CN 110947359 A CN110947359 A CN 110947359A CN 201811121991 A CN201811121991 A CN 201811121991A CN 110947359 A CN110947359 A CN 110947359A
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- 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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- 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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
Abstract
The invention provides a low-density high-elasticity hydrophobic/oleophylic carbon sponge and a preparation method and application thereof. The hydrophobic/oleophylic carbon sponge provided by the invention has a good adsorption effect on oil substances, can efficiently recover oil from water by an adsorption-extrusion desorption method, can be recycled, and has a wide application prospect in the fields of adsorption and separation treatment of oil stains on the surface of a water body and the like. Meanwhile, the preparation method of the hydrophobic/oleophylic carbon sponge with low density and high elasticity is simple and economic, is convenient to operate and is suitable for large-scale preparation.
Description
Technical Field
The invention relates to a low-density high-elasticity hydrophobic/oleophylic carbon sponge and a preparation method and application thereof, belonging to the technical field of functional material preparation.
Background
The porous carbon material has high specific surface area, high porosity, good electrical and thermal conductivity, and controllable pore size and surface performance, and is widely applied in the fields of catalyst carriers, supercapacitors, catalysts, adsorbents, gas storage and the like. At present, the variety of precursors for preparing the porous carbon material in the field is diversified, and the cost is low. The melamine derivative carbon sponge has the advantages of low cost, convenience in operation, low density, high elasticity and the like. However, melamine-derived carbon sponges are water-oil amphiphilic materials, which limits their use in oil-water separation.
Therefore, it has become an urgent technical problem to be solved in the art to provide a hydrophobic/oleophilic carbon sponge with low density and high elasticity, and a preparation method and application thereof.
Disclosure of Invention
To solve the above disadvantages and shortcomings, it is an object of the present invention to provide a hydrophobic/oleophilic carbon sponge having low density and high elasticity. The hydrophobic/oleophylic carbon sponge with low density and high elasticity provided by the invention is a hydrophobic oleophylic adsorption material with low density and high elasticity, and can realize high-efficiency adsorption and recovery of oil when being used for adsorbing the oil in a water body.
The invention also aims to provide a preparation method of the hydrophobic/oleophilic carbon sponge with low density and high elasticity.
The invention also aims to provide the application of the hydrophobic/oleophilic carbon sponge with low density and high elasticity in adsorbing oil in water.
In order to achieve the above objects, in one aspect, the present invention provides a low-density high-elasticity hydrophobic/oleophylic carbon sponge, wherein the low-density high-elasticity hydrophobic/oleophylic carbon sponge is prepared by soaking a melamine-derived carbon sponge in a surface modifier solution and modifying the surface of the melamine-derived carbon sponge with a surface modifier.
According to a specific embodiment of the invention, the hydrophobic/oleophilic carbon sponge is prepared by a preparation method comprising the following steps:
1) soaking the melamine derived carbon sponge in a surface modifier solution, taking out the melamine derived carbon sponge, and washing the melamine derived carbon sponge by using a solvent;
2) heating the carbon sponge obtained in the step 1) to enable the carbon sponge and the surface modifier to generate a cross-linking reaction, and obtaining the hydrophobic/oleophilic carbon sponge with low density and high elasticity after the reaction is finished.
According to a specific embodiment of the invention, in the low-density high-elasticity hydrophobic/oleophilic carbon sponge, the melamine-derived carbon sponge is obtained by calcining melamine sponge at 600-800 ℃ for 0.5-2h in an inert atmosphere.
The high-temperature calcination process of the melamine sponge in the inert atmosphere is a carbonization process, and most of oxygen-containing functional groups of the melamine sponge are lost in the calcination process, and only a carbon-nitrogen skeleton and a few oxygen-containing functional groups are left.
The melamine-derived carbon sponge is a water-oil amphiphilic material with low density and high elasticity and contains hydroxyl groups (formed in the calcining process of the melamine sponge), and the hydroxyl groups in the melamine-derived carbon sponge can be grafted with a surface modifier, such as alkyl trichlorosilane. Typically, the melamine-derived carbon sponge has a density of 6 to 8mg/cm3The recovery amount of the extrusion deformation is more than 92%.
In a particular embodiment of the invention, the melamine sponge used is a substance customary in the art and commercially available.
According to a specific embodiment of the present invention, in the hydrophobic/oleophilic carbon sponge with low density and high elasticity, the surface modifier solution is an alkyl trichlorosilane toluene solution.
According to a specific embodiment of the present invention, in the hydrophobic/oleophilic carbon sponge with low density and high elasticity, the concentration of the toluene solution of alkyltrichlorosilane is 0.5 wt% to 5 wt% based on the total weight of the toluene solution of alkyltrichlorosilane being 100%.
According to an embodiment of the present invention, in the hydrophobic/oleophilic carbon sponge with low density and high elasticity, the alkyl trichlorosilane includes one or more of dodecyl trichlorosilane, tetradecyl trichlorosilane, hexadecyl trichlorosilane and octadecyl trichlorosilane.
According to an embodiment of the invention, the low-density, high-resilience hydrophobic/oleophilic carbon sponge has a density of 6-9mg/cm3The recovery amount of the extrusion deformation is 92-96%.
According to a particular embodiment of the invention, the hydrophobic/oleophilic carbon sponge of low density and high resilience has a water contact angle of more than 90 °;
preferably, the hydrophobic/oleophilic carbon sponge of low density high resilience has a water contact angle of greater than 140 °.
In another aspect, the present invention further provides a method for preparing the hydrophobic/oleophilic carbon sponge with low density and high elasticity, wherein the method comprises the following steps:
1) soaking the melamine derived carbon sponge in a surface modifier solution, taking out the melamine derived carbon sponge, and washing the melamine derived carbon sponge by using a solvent;
2) heating the carbon sponge obtained in the step 1) to enable the carbon sponge and the surface modifier to generate a cross-linking reaction, and obtaining the hydrophobic/oleophilic carbon sponge with low density and high elasticity after the reaction is finished.
According to the specific embodiment of the present invention, in the preparation process of the hydrophobic/oleophylic carbon sponge with low density and high elasticity, the dosage ratio between the melamine-derived carbon sponge and the surface modifier solution is not specifically required, as long as the melamine-derived carbon sponge can be completely soaked in the surface modifier solution.
According to a specific embodiment of the invention, in the preparation method, the melamine-derived carbon sponge is obtained by calcining melamine sponge at 600-800 ℃ for 0.5-2h in an inert atmosphere.
According to a specific embodiment of the present invention, in the preparation method, the temperature increase rate of the calcination is 5 to 10 ℃/min.
According to an embodiment of the present invention, in the preparation method, the inert gas atmosphere includes argon, nitrogen and helium.
According to a specific embodiment of the invention, in step 1) of the preparation method, the soaking time is 5-60 min.
According to a particular embodiment of the invention, in step 1) of the preparation process, the solvent is toluene.
In step 1), the purpose of the solvent wash is to wash away excess unadsorbed surface modifier. According to a specific embodiment of the invention, in the preparation method, the step 2) is to heat the carbon sponge obtained in the step 1) to above 110 ℃, so that the carbon sponge and the surface modifier are subjected to a crosslinking reaction at above 110 ℃.
The crosslinking reaction process is a dehydration condensation reaction, the reaction is very rapid, the reaction time of the crosslinking reaction is not specifically required, and only the complete reaction is ensured, and in the specific implementation mode of the invention, the crosslinking reaction time is generally 1-2 h.
According to the specific embodiment of the present invention, in the step 2), the carbon sponge obtained in the step 1) is heated to 160 ℃ at 110-.
According to an embodiment of the present invention, the preparation method of the hydrophobic/oleophilic carbon sponge with low density and high elasticity further comprises the operations of washing the melamine sponge before calcination, and drying the melamine sponge after washing (for example, drying in an oven at 80 ℃ for 2 h). In the embodiment of the present invention, the solvent used for washing may be deionized water and ethanol, and one skilled in the art may set the number of washing times reasonably according to the operation requirement to remove impurities in the obtained sample.
According to an embodiment of the present invention, the preparation method of the hydrophobic/oleophilic carbon sponge with low density and high elasticity further comprises the operation of washing the product obtained after calcination, and drying (for example, drying in an oven at 80 ℃ for 2 hours) after washing. In the embodiment of the present invention, the solvent used for washing may be deionized water and ethanol, and one skilled in the art may set the number of washing times reasonably according to the operation requirement to remove impurities in the obtained sample.
According to the embodiment of the invention, no other components are added in the process of soaking, heating and crosslinking reaction of the carbon sponge and the surface modifier in the preparation method of the hydrophobic/oleophylic carbon sponge with low density and high elasticity.
According to embodiments of the present invention, the method of preparing the low-density, high-elasticity hydrophobic/oleophilic carbon sponge does not include a process of forming a hard template, a soft template, or activation.
According to the invention, the surface of the melamine-derived carbon sponge is modified with a hydrophobic substance, so that the surface of the melamine-derived carbon sponge can be changed from hydrophobic/oleophilic to hydrophilic through water-oil amphiphilic regulation, and oil substances can be efficiently adsorbed from water, and the melamine-derived carbon sponge has a wide application prospect in the aspect of oil-water separation.
In another aspect, the invention also provides the application of the hydrophobic/oleophilic carbon sponge with low density and high elasticity in absorbing oil in water.
The invention takes melamine derived carbon sponge as a substrate, and the surface modifier is modified on the surface of the melamine derived carbon sponge in a simple soaking way to prepare the hydrophobic/oleophylic carbon sponge with low density and high elasticity. The preparation method is simple and economical, convenient to operate and suitable for large-scale preparation, the prepared hydrophobic/oleophylic carbon sponge has a good adsorption effect on oil substances, oil can be efficiently recovered from water by an adsorption-extrusion desorption method, the oil can be recycled, and the preparation method has a wide application prospect in the fields of adsorption and separation treatment of oil stains on the surface of a water body and the like.
Drawings
FIG. 1 is a scanning electron microscope image of a low-density, high-elasticity hydrophobic/oleophilic carbon sponge prepared in example 1 of the present invention;
FIG. 2 is a schematic diagram showing the contact angle of the hydrophobic/oleophilic carbon sponge with low density and high elasticity prepared in example 1 of the present invention to water;
FIG. 3 is a schematic diagram showing the process of adsorbing toluene by using the hydrophobic/oleophilic carbon sponge prepared in example 1 of application example 1;
fig. 4 is a graph showing the relationship between the number of cycles of the low-density high-elasticity hydrophobic/oleophilic carbon sponge absorbing and desorbing toluene and the amount of toluene absorbed and desorbed by the sponge according to the present invention, which was prepared in example 1 of application example 2.
Detailed Description
In order to clearly understand the technical features, objects and advantages of the present invention, the following detailed description of the technical solutions of the present invention will be made with reference to the following specific examples, which should not be construed as limiting the implementable scope of the present invention.
Example 1
This example provides a hydrophobic/oleophilic carbon sponge (octadecyltrichlorosilane modified carbon sponge) with low density and high elasticity, which is prepared by the following steps:
1) washing melamine sponge with deionized water and ethanol for 3 times, and drying in an oven at 80 ℃ for 2 h;
2) calcining the melamine sponge obtained in the step 1) at 800 ℃ for 2h in an argon atmosphere at the heating rate of 5 ℃/min to obtain a low-density high-elasticity carbon sponge (melamine-derived carbon sponge), wherein the density of the melamine-derived carbon sponge is 7.8mg/cm3The recovery amount of the extrusion deformation is 96 percent, then the mixture is washed for 3 times by deionized water and ethanol and dried for 2 hours in an oven at the temperature of 80 ℃;
3) completely soaking the melamine derived carbon sponge obtained in the step 2) in a toluene solution of 2 wt% octadecyl trichlorosilane for 30min, taking out, and washing with toluene for 5 times;
4) heating the carbon sponge obtained in the step 3) at 120 ℃ for 2h to obtain the octadecyl trichlorosilane modified hydrophobic/oleophilic carbon sponge.
The scanning electron microscope analysis of the low-density high-elasticity hydrophobic/oleophilic carbon sponge prepared in this example is shown in fig. 1, and it can be seen from fig. 1 that the low-density high-elasticity hydrophobic/oleophilic carbon sponge prepared in this example has a good porous network structure,the density of the powder is 8.2mg/cm3The recovery amount of the extrusion deformation was 96%.
The schematic contact angle of the low-density high-elasticity hydrophobic/oleophilic carbon sponge prepared in this example is shown in fig. 2, and it can be seen from fig. 2 that the contact angle of the low-density high-elasticity hydrophobic/oleophilic carbon sponge to water is 142 °.
Example 2
This example provides a hydrophobic/oleophilic carbon sponge (hexadecyl trichlorosilane modified carbon sponge) with low density and high elasticity, which is prepared by the following steps:
1) washing melamine sponge with deionized water and ethanol for 3 times, and drying in an oven at 80 ℃ for 2 h;
2) calcining the melamine sponge obtained in the step 1) at 800 ℃ for 2h in an argon atmosphere at the heating rate of 5 ℃/min to obtain a low-density high-elasticity carbon sponge (melamine-derived carbon sponge), wherein the density of the melamine-derived carbon sponge is 7.8mg/cm3The recovery amount of the extrusion deformation is 96 percent, then the mixture is washed for 3 times by deionized water and ethanol and dried for 2 hours in an oven at the temperature of 80 ℃;
3) completely soaking the melamine derived carbon sponge obtained in the step 2) in a toluene solution of hexadecyl trichlorosilane with the concentration of 2 wt% for 30min, taking out and washing for 5 times by using toluene;
4) heating the carbon sponge obtained in the step 3) at 120 ℃ for 2h to obtain the hexadecyl trichlorosilane modified hydrophobic/oleophylic carbon sponge.
Example 3
This example provides a hydrophobic/oleophilic carbon sponge (tetradecyltrichlorosilane modified carbon sponge) with low density and high elasticity, which is prepared by the following steps:
1) washing melamine sponge with deionized water and ethanol for 3 times, and drying in an oven at 80 ℃ for 2 h;
2) calcining the melamine sponge obtained in the step 1) for 2h at 800 ℃ in an argon atmosphere at the heating rate of 5 ℃/min to obtain the low-density high-elasticity carbon sponge (melamine-derived carbon sponge), wherein the melamine-derived carbon sponge is prepared from melamineThe density of the sponge was 7.8mg/cm3The recovery amount of the extrusion deformation is 96 percent, then the mixture is washed for 3 times by deionized water and ethanol and dried for 2 hours in an oven at the temperature of 80 ℃;
3) completely soaking the melamine derived carbon sponge obtained in the step 2) in a toluene solution of tetradecyltrichlorosilane with the concentration of 2 wt% for 30min, taking out, and washing for 5 times by using toluene;
4) heating the carbon sponge obtained in the step 3) at 120 ℃ for 2h to obtain the tetradecyl trichlorosilane modified hydrophobic/oleophilic carbon sponge.
Application example 1
The toluene is adsorbed by the hydrophobic/oleophilic carbon sponge with low density and high elasticity prepared in example 1 of the present invention, the schematic diagram of the adsorption process is shown in FIG. 3, and it can be seen from FIG. 3 that the hydrophobic/oleophilic carbon sponge with low density and high elasticity can completely absorb toluene within 200ms, and the toluene adsorption capacity is 95 g/g.
Application example 2
The relationship between the number of cycles and the amount of toluene absorbed and desorbed is shown in fig. 4, and it can be seen from fig. 4 that the low-density high-elasticity hydrophobic/oleophilic carbon sponge prepared in example 1 can recycle and recover oil by the method of absorption-extrusion desorption.
The reason why the toluene adsorption amount is reduced in the process of circulating adsorption and desorption of toluene is explained as follows: after the first extrusion and desorption, part of oil remains in the sponge, and the theoretical limit of reabsorption at this time is the first oil output, so that the oil is considered to have cyclicity when the value is close to the value; after a plurality of squeezes, the deformation is hard to recover, so the oil absorption is further reduced, and the number of cycles close to the first oil discharge is considered to be the optimum number of cycles, specifically, in this application example, the optimum number of cycles of the hydrophobic/oleophilic carbon sponge with low density and high elasticity is 5.
The above detailed description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention. While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (20)
1. The hydrophobic/oleophylic carbon sponge with low density and high elasticity is characterized in that the hydrophobic/oleophylic carbon sponge with low density and high elasticity is prepared by soaking melamine derivative carbon sponge in a surface modifier solution and modifying the surface of the melamine derivative carbon sponge with a surface modifier.
2. The low-density high-elasticity hydrophobic/oleophilic carbon sponge according to claim 1, which is prepared by a preparation method comprising the following steps:
1) soaking the melamine derived carbon sponge in a surface modifier solution, taking out the melamine derived carbon sponge, and washing the melamine derived carbon sponge by using a solvent;
2) heating the carbon sponge obtained in the step 1) to enable the carbon sponge and the surface modifier to generate a cross-linking reaction, and obtaining the hydrophobic/oleophilic carbon sponge with low density and high elasticity after the reaction is finished.
3. The low-density high-elasticity hydrophobic/oleophilic carbon sponge as claimed in claim 1, wherein the melamine-derived carbon sponge is obtained by calcining melamine sponge at 600-800 ℃ for 0.5-2h under inert atmosphere.
4. The low-density, high-elasticity hydrophobic/oleophilic carbon sponge as in claim 1, wherein the surface modifier solution is an alkyltrichlorosilane toluene solution.
5. The hydrophobic/oleophilic carbon sponge as in claim 4, wherein the toluene alkyl trichlorosilane solution has a concentration of 0.5 wt% to 5 wt% based on the total weight of the toluene alkyl trichlorosilane solution taken as 100%.
6. The hydrophobic/oleophilic carbon sponge as in claim 5, wherein the alkyl trichlorosilane comprises one or a combination of dodecyl trichlorosilane, tetradecyl trichlorosilane, hexadecyl trichlorosilane and octadecyl trichlorosilane.
7. The low-density, high-elasticity hydrophobic/oleophilic carbon sponge as in any one of claims 1 to 6, wherein the density of the hydrophobic/oleophilic carbon sponge is from 6 to 9mg/cm3The recovery amount of the extrusion deformation is 92-96%.
8. The low-density, high-elasticity hydrophobic/oleophilic carbon sponge according to any one of claims 1 to 6, wherein the hydrophobic/oleophilic carbon sponge has a water contact angle of greater than 90 °.
9. The low-density, high-elasticity hydrophobic/oleophilic carbon sponge according to claim 7, wherein the hydrophobic/oleophilic carbon sponge has a water contact angle of greater than 90 °.
10. The low density, high elasticity hydrophobic/oleophilic carbon sponge according to claim 8, wherein the hydrophobic/oleophilic carbon sponge has a water contact angle of greater than 140 °.
11. The low density, high elasticity hydrophobic/oleophilic carbon sponge according to claim 9, wherein the hydrophobic/oleophilic carbon sponge has a water contact angle of greater than 140 °.
12. The method for preparing a low-density high-elasticity hydrophobic/oleophilic carbon sponge as claimed in any one of claims 1 to 11, wherein the method comprises the steps of:
1) soaking the melamine derived carbon sponge in a surface modifier solution, taking out the melamine derived carbon sponge, and washing the melamine derived carbon sponge by using a solvent;
2) heating the carbon sponge obtained in the step 1) to enable the carbon sponge and the surface modifier to generate a cross-linking reaction, and obtaining the hydrophobic/oleophilic carbon sponge with low density and high elasticity after the reaction is finished.
13. The method as claimed in claim 12, wherein the melamine-derived carbon sponge is obtained by calcining melamine sponge at 600-800 ℃ for 0.5-2h under an inert atmosphere.
14. The method of claim 13, wherein the temperature increase rate of the calcination is 5 to 10 ℃/min.
15. The method of claim 13 or 14, wherein the inert atmosphere comprises argon, nitrogen and helium.
16. The method of claim 12, wherein the soaking time in step 1) is 5-60 min.
17. The method according to claim 12, wherein the solvent in step 1) is toluene.
18. The method according to claim 12, wherein the step 2) comprises heating the carbon sponge obtained in the step 1) to a temperature of 110 ℃ or higher, so that the carbon sponge and the surface modifier undergo a crosslinking reaction at a temperature of 110 ℃ or higher.
19. The method as claimed in claim 18, wherein the step 2) comprises heating the carbon sponge obtained in the step 1) to 160 ℃ to cause the carbon sponge and the surface modifier to perform a crosslinking reaction at 160 ℃ to 110 ℃.
20. Use of the low density, high elasticity hydrophobic/oleophilic carbon sponge of any one of claims 1-11 to adsorb oil in water.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113385046A (en) * | 2021-06-24 | 2021-09-14 | 中国矿业大学 | Preparation method and application of sponge-based filter membrane adsorbing material for mercury adsorption removal |
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| CN113385046A (en) * | 2021-06-24 | 2021-09-14 | 中国矿业大学 | Preparation method and application of sponge-based filter membrane adsorbing material for mercury adsorption removal |
| CN113385046B (en) * | 2021-06-24 | 2022-05-10 | 中国矿业大学 | Preparation method and application of sponge-based filter membrane adsorbing material for mercury adsorption removal |
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