CN114196066B - Thermal response type intelligent sponge and preparation method and application thereof - Google Patents
Thermal response type intelligent sponge and preparation method and application thereof Download PDFInfo
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/208—Off-grid powered water treatment
- Y02A20/212—Solar-powered wastewater sewage treatment, e.g. spray evaporation
Abstract
The invention relates to a thermal response type intelligent sponge, and a preparation method and application thereof, wherein the thermal response type intelligent sponge comprises the following components: step one: preparing PDMS/CNT sponge by an improved hard template method, and treating the PDMS/CNT sponge by oxygen plasma to introduce hydroxyl groups on the surface of the PDMS/CNT sponge; step two: immersing PDMS/CNT sponge in toluene solution added with aminopropyl triethoxysilane to introduce amino; step three: putting PDMS/CNT sponge into a mixed solution of dichloromethane and triethylamine, and dropwise adding 2-bromoisobutyl bromide into an ice bath to introduce active bromine groups; step four: and (3) putting the PDMS/CNT sponge into a mixed solution of methanol, N-isopropyl acrylamide, cuBr and pentamethyl divinyl triamine (PMDETA), and reacting under the protection of nitrogen to obtain the thermally-responsive intelligent sponge. The PNIPAM is grafted on the PDMS/CNT sponge by adopting a surface initiated atom transfer radical polymerization method, so that the thermal response intelligent sponge material is prepared, and the purposes of directionally transporting and recovering liquid and continuously evaporating solar seawater are achieved, so that the purposes of purifying sewage and producing fresh water are achieved.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a thermally-responsive intelligent sponge, and a preparation method and application thereof.
Background
Water resource shortages are one of the most serious challenges faced by many areas of the world. For how clean fresh water resources are obtained, it is necessary to establish directional transportation of petroleum or organic solvents, water purification by adsorption of liquids, and solar-driven evaporation of seawater. In the applications, the porous material is widely applied due to the characteristics of high adsorption capacity and rapid evaporation, and the design and synthesis of the novel low-cost porous material have important significance for various applications such as recoverable solar seawater desalination, liquid recovery and the like.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a thermally responsive intelligent sponge capable of being used for transporting and recycling liquid and evaporating continuous solar seawater, and a preparation method and application thereof.
The technical solution for realizing the purpose of the invention is as follows:
a preparation method of a thermally responsive intelligent sponge comprises the following steps:
step one: preparing PDMS/CNT sponge by an improved hard template method, and treating the PDMS/CNT sponge by oxygen plasma to introduce hydroxyl groups on the surface of the PDMS/CNT sponge;
step two: immersing PDMS/CNT sponge with hydroxyl group into toluene solution with aminopropyl triethoxysilane added to introduce amino group;
step three: putting the PDMS/CNT sponge with the amino group into a mixed solution of dichloromethane and triethylamine, and dropwise adding 2-bromoisobutyl bromide into an ice bath to introduce active bromine groups;
step four: and (3) putting the PDMS/CNT sponge with the active bromine group into a mixed solution of methanol, N-isopropyl acrylamide, cuBr and pentamethyl diethylenetriamine (PMDETA), and reacting under the protection of nitrogen to prepare the thermally-responsive intelligent sponge.
Further, the second step specifically comprises: the hydroxyl-introduced PDMS/CNT sponge was immersed in a toluene solution to which aminopropyl triethoxysilane was added, reacted at room temperature for 12 hours to introduce an amino group, and then washed with toluene and dried.
Further, the third step specifically comprises: putting the PDMS/CNT sponge with the amino group into a mixed solution of dichloromethane and triethylamine, dropwise adding 2-bromoisobutyl bromide into an ice bath to react at 0 ℃ for 1-2 h, introducing active bromine groups, washing the PDMS/CNT sponge with dichloromethane, and then putting into an oven for drying, wherein the volume ratio of the dichloromethane solvent to the triethylamine solution is 50:1.
Further, the fourth step specifically comprises: and (3) putting the PDMS/CNT sponge into a mixed solution of methanol, N-isopropyl acrylamide, cuBr and pentamethyl diethylenetriamine (PMDETA), reacting for 2-3 hours at room temperature under the protection of nitrogen, and finally thoroughly cleaning the obtained substance by using methanol and water to obtain the thermally responsive intelligent sponge, wherein the volume ratio of the methanol to the water in the mixed solution is 1:1, the dosage of the N-isopropyl acrylamide is 5-g, the dosage of the initiator CuBr is 0.2-g, and the dosage of the pentamethyl diethylenetriamine (PMDETA) is 1-mL.
Further, the first step specifically comprises: mixing PDMS (Sylgard 184) and a curing agent according to the mass ratio of 10:1, carrying out ultrasonic treatment for 20-30 minutes until the mixture is uniformly mixed to obtain a mixture, then removing bubbles in the mixture by using a vacuum pump, adding Carbon Nanotubes (CNTs) into the mixture, carrying out ultrasonic mixing uniformly, putting square sugar into the mixture, continuously vacuumizing to allow liquid mixture to permeate into a square sugar frame, then curing for 5-10 minutes in a blast furnace at 100-120 ℃, then putting the cured product into hot water for ultrasonic treatment for 1-2 h, dissolving square sugar, drying to obtain a series of different PDMS/CNT sponges, and carrying out oxygen plasma treatment on the PDMS/CNT sponges for 5-10 minutes to introduce hydroxyl groups on the surface of the PDMS/CNT sponges.
The thermal response type intelligent sponge is prepared by the method.
A method for preparing clean water adopts the thermal response type intelligent sponge to treat sewage so as to obtain clean water.
A method for preparing clean fresh water adopts the thermal response type intelligent sponge to evaporate sea water so as to obtain fresh water.
Compared with the prior art, the invention has the remarkable advantages that:
1. in the preparation method of the intelligent sponge material for directional transportation and recycling of liquid and continuous solar brine evaporation, adopted raw materials are easy to obtain, the synthetic route is simple, precise and expensive instruments are not used in the whole process, and the product of reversible switching wettability, high adsorption performance, high evaporation rate, high photo-thermal conversion efficiency, real-time regeneration, high efficiency and stable solar brine evaporation is prepared by using a very simple method;
2. the invention is used for the directional transportation and recycling of liquid and the continuous brine evaporation of solar energy, carbon Nanotubes (CNTs) are added to effectively enhance the mechanical properties of the sponge such as toughness, compression resistance and the like and excellent light absorption performance, and poly (N-isopropyl acrylamide) is a temperature responsive material, so that the prepared intelligent sponge can effectively carry out the directional transportation and recycling of liquid and continuous efficient seawater evaporation, and meanwhile, the polymers have high stability, good reusability and the like, so that the intelligent sponge has good application prospects in the aspects of energy and environmental protection;
3. the invention takes sponge as a carrier, carbon Nanotubes (CNTs) as a doping material, temperature responsive poly (N-isopropyl acrylamide) as a surface modifier, and combines the respective excellent performances of the two to prepare the intelligent sponge with directional transportation, automatic liquid recovery and continuous efficient seawater evaporation, which can directionally transport and automatically desorb organic solvents and oil, and the continuous efficient seawater evaporation, and mainly can realize industrial production of products so as to achieve the purposes of purifying sewage and producing fresh water.
Drawings
FIG. 1 is an SEM image of PDMS and PDMS/CNT sponge.
FIG. 2 is an SEM image of a CNT-PNIPAM sponge.
FIG. 3 is a graph showing reversible switching behavior of temperature responsive smart sponges to water wettability after PNIPAM modification on PDMS/CNT sponge.
Fig. 4 is a graph of directional delivery and automatic release performance of a sponge adsorbing an organic phase in response to adsorbing a liquid.
Fig. 5 is a graph of uv-vis spectral testing for characterizing the photothermal conversion performance of a smart sponge.
Fig. 6 is a solar seawater evaporation performance test chart of the intelligent sponge.
Fig. 7 is a graph of continuous solar seawater evaporation performance test of an intelligent sponge.
Description of the embodiments
The invention will be further described with reference to the accompanying drawings.
A preparation method of a thermally responsive intelligent sponge comprises the following steps:
step one: preparing PDMS/CNT sponge by an improved hard template method, and treating the PDMS/CNT sponge by oxygen plasma to introduce hydroxyl groups on the surface of the PDMS/CNT sponge;
step two: immersing PDMS/CNT sponge with hydroxyl group into toluene solution with aminopropyl triethoxysilane added to introduce amino group;
step three: putting the PDMS/CNT sponge with the amino group into a mixed solution of dichloromethane and triethylamine, and dropwise adding 2-bromoisobutyl bromide into an ice bath to introduce active bromine groups;
step four: and (3) putting the PDMS/CNT sponge with the active bromine group into a mixed solution of methanol, N-isopropyl acrylamide, cuBr and pentamethyl diethylenetriamine (PMDETA), and reacting under the protection of nitrogen to prepare the thermally-responsive intelligent sponge.
The substrate material is PDMS/CNT sponge, and although the substrate material has excellent compressibility and high adsorption capacity, the PDMS/CNT sponge is unfavorable for surface modification and does not have the hydrophilic-hydrophobic conversion capacity. After 15 times of liquid adsorption-desorption, the surface and adsorption performance of the material are not changed greatly. More importantly, the continuous solar energy evaporating brine for 5 days, the intelligent sponge keeps good photo-thermal conversion capability and high evaporation rate, the performance is basically unchanged, and the intelligent sponge has good reusability.
The second step is specifically as follows: the PDMS/CNT sponge with the hydroxyl group is immersed in toluene solution added with aminopropyl triethoxysilane (1-wt%) for reaction for 12 hours at room temperature to introduce amino group, and then washed with toluene and dried.
The third step is specifically as follows: putting the PDMS/CNT sponge with the amino group into a mixed solution of anhydrous dichloromethane and triethylamine, dropwise adding 2-bromoisobutyl bromide into an ice bath, reacting at 0 ℃ for 1-2 h, introducing active bromine groups, washing the PDMS/CNT sponge with dichloromethane, and then putting into an oven for drying, wherein the volume ratio of the solvent dichloromethane to the triethylamine is 50:1.
The fourth step is specifically as follows: the PDMS/CNT sponge with the active bromine group is put into a mixed solution of methanol, N-isopropyl acrylamide, cuBr and pentamethyl diethylenetriamine (PMDETA), the mixed solution reacts for 2 to 3 hours at room temperature under the protection of nitrogen, finally, the obtained substance is thoroughly cleaned by methanol and water to obtain the thermally responsive intelligent sponge, the thermally responsive intelligent sponge is dried in vacuum to obtain the intelligent sea water desalination material, the volume ratio of the methanol to the water in the mixed solution is 1 to 1, the dosage of the N-isopropyl acrylamide is 5 to g, the dosage of the initiator CuBr is 0.2 to g, the cuprous bromide can effectively initiate the polymerization of the monomer, the polymerization uniformity is maintained, the uneven distribution of the polymer on the surface of the net is avoided, the surface of the net obtained polymer is covered by the initiator of the invention, the polymer is quite uniform respectively, the wettability conversion, the directional transportation and the improvement of the solar evaporation performance are facilitated, and the dosage of the pentamethyl diethylenetriamine (PMDETA) is 1 to mL. FIGS. 2a, b and c are SEM images of different multiples of the PDMS/CNT-PNIPAM sponge described above, from which successful modification of the sponge surface with PNIPAM can be seen. And d, infrared spectrograms of PDMS, PDMS/CNT and PDMS/CNT-PNIPAM sponge.
The invention adopts different polymerization temperatures and time aiming at different monomers (aminopropyl triethoxysilane, 2-bromoisobutyl bromide, N-isopropyl acrylamide and PMDETA), can better control the quantity of the polymer on the sponge and the uniformity of the polymer so as to achieve controllable temperature wettability reversible conversion, can better polymerize on the sponge and can be modified on the surface of the sponge more uniformly by adjusting the proportion of the monomers and the initiator.
The preparation method of the PDMS sponge comprises the following steps: mixing PDMS (Sylgard 184) and a curing agent according to the mass ratio of 10:1, carrying out ultrasonic treatment for 20-30 minutes until the mixture is uniformly mixed to obtain a mixture, then removing bubbles in the mixture by a vacuum pump, putting the square sugar into a liquid mixture under vacuum, allowing the liquid mixture to permeate into a square sugar frame, then curing in a blast furnace at 100-120 ℃ for 5-10 minutes, then putting the cured product into hot water for ultrasonic treatment for 1-2 h, dissolving the square sugar, drying to obtain a three-dimensional interconnected porous PDMS sponge, adding different numbers of CNTs into the mixture of PDMS and the curing agent by the same hard template method, carrying out ultrasonic mixing uniformly, putting the square sugar into the mixture, continuously vacuumizing to allow the liquid mixture to permeate into the square sugar frame, then curing in the blast furnace at 100-120 ℃ for 5-10 minutes, then putting the cured product into hot water for ultrasonic treatment for 1-2 h, drying to obtain a series of different PDMS/CNT sponges, and carrying out oxygen treatment for 5-10 minutes on the PDMS/CNT sponges, and introducing hydroxyl groups on the surface of the PDMS/sponge. FIG. 1 is an SEM image of the PDMS sponge (part a of FIG. 1) and PDMS/CNT sponge (part b of FIG. 1) described above.
The invention discloses a simple template method for preparing a PDMS/CNT sponge from a PDMS/CNTs composite, and then modifying PNIPAM to the sponge through surface atom transfer radical polymerization to prepare an intelligent sponge with temperature response, liquid adsorption-desorption, directional transportation and seawater evaporation, which is widely applied to intelligent equipment, sewage purification, clean water regeneration and other aspects; and in continuous efficient evaporation of seawater.
The wettability behavior of the modified smart sponge is described in connection with fig. 3-4: fig. 3 shows reversible switching behavior of temperature response intelligent sponge after PNIPAM is modified on PDMS/CNT sponge, and by comparison, the sponge shows super-hydrophobicity at 40 ℃, and water drops immediately diffuse into the sponge at 28 ℃ to have super-hydrophilicity.
The intelligent sponge temperature response adsorption liquid directional conveying and automatic release performance test comprises the following specific steps: three-phase system is designed, which mainly comprises water, chloroform and oil red-oxygen dyed n-hexane. The adsorption-dyed PDMS/CNT-PNIPAM sponge is put into water, and bubbles gradually appear on the surface of the PDMS/CNT-PNIPAM sponge along with the temperature rising to 45 ℃, so that the surface state of the sponge is changed from hydrophilicity to super-hydrophobicity. When the sponge was contacted with water, the chloroform gradually changed from colorless to dark red. Thus, the n-hexane adsorbed in the sponge was successfully transferred and diffused into chloroform. In addition, after the intelligent sponge for adsorbing and dyeing chloroform is immersed in water at 15 ℃, the dyed chloroform is immediately released from the sea surface, which indicates that the intelligent sponge can automatically desorb the adsorption liquid.
PNIPAM modified intelligent sponge photo-thermal conversion and solar seawater evaporation performance test: FIG. 5 ultraviolet-visible spectrum test, used to characterize the absorbance properties of the intelligent sponge. From the graph, it can be seen that the pure polydimethylsiloxane sponge has almost no light absorption performance, however, as the amount of CNTs added increases, the light absorption performance of the sponge gradually increases. More importantly, the light absorption performance of the intelligent sponge formed by modifying PNIPAM is equivalent to that of PDMS/CNT-5, and the intelligent sponge is more than 95% and shows excellent light absorption performance.
Figures 6 and 7 are solar seawater evaporation performance tests of intelligent sponges, and from figure 6 it can be seen that different sponges have brine evaporation rates under 1 sun irradiation, and PDMS/CNT-PNIPAM sponges have the highest evaporation rates. More importantly, the brine evaporated for 5 consecutive days, with substantially no change in evaporation rate (fig. 7). Through the analysis, PNIPAM is successfully modified on PDMS/CNT sponge by a surface initiated atom transfer radical polymerization method to prepare the intelligent sponge, so that the intelligent sponge has good temperature response liquid directional transportation and automatic release performances. And under the synergistic effect of excellent photo-thermal conversion performance, wettability conversion and salt resistance, the intelligent sponge has the advantages of high evaporation efficiency, continuous and stable seawater evaporation and the like, and more importantly, the preparation method is simple. Therefore, the method has good application prospect in the aspects of intelligent equipment, sewage treatment and clean water regeneration.
A method for preparing clean water adopts the thermal response type intelligent sponge to treat sewage so as to obtain clean water.
According to the invention, PNIPAM is grafted onto PDMS/CNT sponge by adopting a surface initiated atom transfer radical polymerization method, so that the thermal response intelligent sponge material is prepared, liquid can be transported and recovered in a directional manner, continuous solar seawater evaporation can be realized, and the purposes of purifying sewage and producing fresh water are achieved.
The foregoing has outlined and described the basic principles, features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. The preparation method of the thermal response type intelligent sponge is characterized by comprising the following steps of:
step one: preparing PDMS/CNT sponge by an improved hard template method, and treating the PDMS/CNT sponge by oxygen plasma to introduce hydroxyl groups on the surface of the PDMS/CNT sponge;
step two: immersing PDMS/CNT sponge with hydroxyl group into toluene solution with aminopropyl triethoxysilane added to introduce amino group;
step three: putting the PDMS/CNT sponge with the amino group into a mixed solution of dichloromethane and triethylamine, and dropwise adding 2-bromoisobutyl bromide into an ice bath to introduce active bromine groups;
step four: and (3) putting the PDMS/CNT sponge with the active bromine group into a mixed solution of methanol, N-isopropyl acrylamide, cuBr and pentamethyl diethylenetriamine, and reacting under the protection of nitrogen to prepare the thermally responsive intelligent sponge.
2. The method for preparing the thermally responsive type intelligent sponge according to claim 1, wherein,
the second step is specifically as follows: the hydroxyl-introduced PDMS/CNT sponge was immersed in a toluene solution to which aminopropyl triethoxysilane was added, reacted at room temperature for 12 hours to introduce an amino group, and then washed with toluene and dried.
3. The method for preparing the thermally responsive type intelligent sponge according to claim 2, wherein,
the third step is specifically as follows: putting the PDMS/CNT sponge with the amino group into a mixed solution of dichloromethane and triethylamine, dropwise adding 2-bromoisobutyl bromide into an ice bath to react at 0 ℃ for 1-2 h, introducing active bromine groups, washing the PDMS/CNT sponge with dichloromethane, and then putting into an oven for drying, wherein the volume ratio of the dichloromethane to the triethylamine is 50:1.
4. The method for preparing the thermally responsive type intelligent sponge as claimed in claim 3, wherein,
the fourth step is specifically as follows: and (3) putting the PDMS/CNT sponge into a mixed solution of methanol, N-isopropyl acrylamide, cuBr and pentamethyldiethylenetriamine, reacting for 2-3 hours at room temperature under the protection of nitrogen, and finally thoroughly cleaning the obtained substance by using methanol and water to obtain the thermally responsive intelligent sponge, wherein the volume ratio of the methanol to the water in the mixed solution is 1:1, the dosage of the N-isopropyl acrylamide is 5 g, the dosage of the initiator CuBr is 0.2 g, and the dosage of the pentamethyldiethylenetriamine is 1 mL.
5. The method for preparing a thermally responsive type intelligent sponge as claimed in claim 4, wherein the first step is as follows: mixing PDMS and a curing agent according to the mass ratio of 10:1, carrying out ultrasonic treatment for 20-30 minutes until the mixture is uniformly mixed to obtain a mixture, then removing bubbles in the mixture by using a vacuum pump, adding carbon nano tube CNTs into the mixture, carrying out ultrasonic mixing uniformly, putting square sugar into the mixture, continuously vacuumizing to allow liquid mixture to permeate into a square sugar frame, then curing in a blast furnace at 100-120 ℃ for 5-10 minutes, then putting the cured product into hot water for ultrasonic treatment for 1-2 h to dissolve the square sugar, drying to prepare a series of different PDMS/CNT sponges, and carrying out oxygen plasma treatment on the PDMS/CNT sponges for 5-10 minutes to introduce hydroxyl groups on the surface of the PDMS/CNT sponges.
6. A thermally responsive smart sponge, wherein the thermally responsive smart sponge is prepared by the method of any one of claims 1-5.
7. A method for preparing clean water, characterized in that the heat-responsive intelligent sponge according to claim 6 is used for treating sewage to obtain clean water.
8. A method for preparing clean fresh water, characterized in that the heat-responsive intelligent sponge according to claim 6 is used for evaporating sea water to obtain fresh water.
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| CN106955676A (en) * | 2017-03-18 | 2017-07-18 | 华南理工大学 | A kind of temperature-responsive water-oil separating foam and preparation method thereof |
| CN107759104B (en) * | 2017-10-31 | 2020-12-22 | 华南理工大学 | Quaternized polymer brush antibacterial material based on Si-ATRP method and preparation method thereof |
| CN108341989B (en) * | 2018-02-02 | 2020-02-18 | 华南理工大学 | Temperature-sensitive polyurethane sponge capable of controlling hydrophilic-hydrophobic conversion and preparation method and application thereof |
| CN111013199A (en) * | 2019-12-31 | 2020-04-17 | 常州大学 | Preparation method of intelligent pH response type melamine foam oil-water separation material |
| CN111138859A (en) * | 2020-01-09 | 2020-05-12 | 合肥工业大学 | Three-dimensional structure nano composite intelligent sponge, preparation method and application |
| CN113150371A (en) * | 2021-04-09 | 2021-07-23 | 华东师范大学 | PDMS sponge-based strain sensor and preparation method thereof |
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