CN114561039A - Preparation method of polysiloxane modified super-hydrophobic sponge for oil-water separation - Google Patents
Preparation method of polysiloxane modified super-hydrophobic sponge for oil-water separation Download PDFInfo
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Abstract
The invention discloses a preparation method of polysiloxane modified super-hydrophobic sponge for oil-water separation, and belongs to the technical field of preparation and application of functional materials. The invention uses proper amount of hydrophobic gas phase nano SiO2Dispersing the mixture into a solution of hydroxyl-terminated polydimethylsiloxane and ethyl orthosilicate, and preparing the super-hydrophobic melamine sponge by a dipping method, wherein the super-hydrophobic melamine sponge has a good pore structure and hydrophobic and oleophilic properties. When used for oil-water separation, the composite material has excellent compression resistance and recycling performance. The invention has simple and convenient process, low cost, nontoxic and harmless main raw materials and green colorThe method is environment-friendly, is a commercial industrial product, is easy to realize large-scale production, and has wide application prospect in separation and recovery of oil-containing or organic solvent and water mixture.
Description
Technical Field
The invention relates to a preparation method of polysiloxane modified super-hydrophobic sponge for oil-water separation, belonging to the technical field of preparation and application of functional materials.
Background
With the development of petrochemical industry, oil spill accidents in oceans frequently occur, which has adverse effects on the natural environment and human life. Therefore, the development of convenient and effective oil-absorbing materials is imminent. Three-dimensional porous materials with oversized internal spaces become one of the candidates for oil-water separation materials, such as high molecular materials, carbonaceous fibers, graphene, tobacco ash, aerogel and the like. Most of the hydrophobic oleophilic porous materials are prepared with the problems of high cost, large energy consumption and complex production process.
Currently, melamine sponges with high porosity, low density, elasticity, low cost are available for the absorption of oil phases or organic liquids through hydrophobic modification. The common melamine sponge has oil-water amphipathy, and can be made to have hydrophobicity and lipophilicity through modification modes such as introducing low surface energy substances, increasing surface roughness and the like. Generally, the introduction of low surface energy materials can realize the goal of enabling the sponge framework to have good hydrophobic and oleophilic properties, and meanwhile, a proper amount of nano particles can increase the surface roughness of the sponge framework and enhance the oil-water separation capability of the sponge. CN201810372973.6 discloses a preparation method of a flame-retardant super-hydrophobic melamine sponge, which comprises the steps of sequentially placing the sponge in a trihydroxymethyl aminomethane solution containing silicon dioxide particles, tannic acid and silver nitrate and an ethanol solution of perfluorododecanethiol to obtain the super-hydrophobic sponge. The method has complex process, and the introduction of fluorine-containing substances is not beneficial to environmental protection. CN201910955095.5 discloses a simple method for modifying melamine sponge with super-hydrophobicity, which comprises the steps of immersing commercial melamine sponge in a nitric acid solution in a one-step manner, and then simply washing and drying to realize the super-hydrophobic modification of amphiphilic melamine sponge. The method is simple and easy to implement, but the introduction of a strong oxidant brings experimental risks, and the heat resistance and the mechanical stability of the oxidized and etched sponge are reduced. Therefore, the method for preparing the super-hydrophobic oleophylic sponge through modification, which has the advantages of environmental friendliness, simplicity, convenience, low cost, easiness in realizing large-scale production and the like, is urgently needed to be developed.
Disclosure of Invention
Aiming at the problems and the defects in the prior art, the invention provides a simple, convenient and low-cost method for preparing the super-hydrophobic oleophylic sponge which has high adsorption capacity and good physical and chemical stability and is easy to realize large-scale production.
In order to solve the technical problems, the first object of the invention is to provide a preparation method of a modified super-hydrophobic sponge. The adopted technical scheme comprises the following steps:
step one, cutting off commercially available melamine sponge into blocks, washing and drying for later use.
Dissolving hydroxyl-terminated polydimethylsiloxane, ethyl orthosilicate and dibutyltin dilaurate in n-hexane, and adding hydrophobic gas phase nano SiO2After ultrasonic dispersion, stirring on a magnetic stirrer to obtain PDMS/SiO2And (4) compounding the solution.
Step three, completely immersing the pretreated sponge in PDMS/SiO2And taking out the composite solution after a period of time, and curing and drying the composite solution in an oven to obtain the super-hydrophobic oleophylic sponge.
Furthermore, the commercially available melamine sponge is a commercial melamine sponge with the characteristics of low cost, light weight, strong adsorption, good mechanical property and the like, the porosity is 98-99%, and the density is 7-10 kg/m3。
Further, the hydroxyl-terminated polydimethylsiloxane is commercially pure, chemically stable, colorless, transparent, flowing liquid with viscosity (25 ℃) of 5000-.
Further, the washing in the first step is washing with deionized water and ethanol for several times.
Further, the hydrophobic gas phase nano SiO2The addition amount is 0.3-0.5 of the total mass of the hydroxyl-terminated polydimethylsiloxane and the tetraethoxysilane. WhereinHydrophobic gas phase nano SiO2The comprehensive performance is optimal when the adding amount is 0.3 of the total mass of the hydroxyl-terminated polydimethylsiloxane and the tetraethoxysilane.
Furthermore, the mass ratio of the hydroxyl-terminated polydimethylsiloxane to the tetraethoxysilane is 5: 1.
Furthermore, the dibutyltin dilaurate is used as a catalyst, and the mass ratio of the dibutyltin dilaurate to the total mass of the hydroxyl-terminated polydimethylsiloxane and the tetraethoxysilane is 1: 60-1: 30. The catalyst dosage is small, the reaction is too slow, the catalyst dosage is large, the reaction is too fast, the coating cannot be carried out, and the catalyst residue exists.
Furthermore, the ultrasonic time is 10-20 min, the stirring time is 20-40 min, and the soaking time is 20-40 min.
Further, the drying temperature is 25-65 ℃.
The second purpose of the invention is to provide the modified super-hydrophobic sponge prepared by the method.
The third purpose of the invention is to provide an oil-water separation method, which uses the modified super-hydrophobic sponge of the invention as an adsorbent for adsorption.
Further, the oil in the oil-water separation can be any one or more of toluene, dichloromethane, n-hexane, petroleum ether and corn oil.
Further, the oil-water separation method further comprises the steps of extruding the modified super-hydrophobic sponge adsorbed with the oil, discharging the adsorbed oil, and recycling the modified super-hydrophobic sponge.
The fourth purpose of the invention is to provide the application of the modified super-hydrophobic sponge in the separation and recovery of oil-containing or organic solvent and water mixture.
Further, the separation and recovery may be performed in a high temperature environment, such as a high temperature environment below 300 ℃.
Further, the separation and recovery may be performed in a saline environment, such as a saline environment of 10 to 50% sodium chloride.
Further, the application comprises recycling the modified super-hydrophobic sponge.
The invention has the advantages and effects that:
the invention uses proper amount of hydrophobic gas phase nano SiO2Dispersing the mixture into a solution of hydroxyl-terminated polydimethylsiloxane and tetraethoxysilane, and soaking and curing the sponge to obtain the modified melamine sponge. The invention effectively controls the hydrophobic gas phase nano SiO2The addition amount is 0.3 of the total mass of the hydroxyl-terminated polydimethylsiloxane and the tetraethoxysilane, and the high-performance super-hydrophobic sponge is obtained.
The super-hydrophobic melamine sponge prepared by the invention has the following characteristics:
(1) the thermal stability is excellent: the temperature when the quality loss of the modified sponge is5 percent is about 300 ℃, and the obvious weight loss temperature is about 380 ℃;
(2) the compression resistance is excellent: the extrusion test result shows that the original appearance is kept after repeated extrusion for 100 times, and the water contact angle is still kept about 150 degrees;
(3) the weather resistance is good: the modified sponge keeps stable hydrophobicity in seawater with different concentrations simulated by 10-50 thousandths of sodium chloride solution;
(4) strong adsorption capacity to organic matters: the oil absorption capacity K values of the modified sponge p-toluene, dichloromethane, n-hexane, petroleum ether and corn oil are 68, 83, 42, 40 and 56 respectively.
(5) The recycling stability is good: after 10 times of adsorption and extrusion cycles, the absorption capacity of the modified sponge for various oils is basically not changed.
In addition, the super-hydrophobic modification process is simple and convenient, has low cost, has no toxicity and harm of main raw materials, is green and environment-friendly, is a commercially available industrial product, is easy to realize large-scale production, and has wide application prospect in separation and recovery of oil-containing or organic solvent and water mixture.
Drawings
FIG. 1 is a graph showing the water contact angle of a modified sponge prepared in example 1 of the present invention.
FIG. 2 is a scanning electron microscope before and after modification of a modified sponge prepared in example 1 of the present invention; wherein, fig. 2A is an unmodified sponge, and fig. 2B is a modified sponge.
FIG. 3 is a thermogravimetric plot of a modified sponge made in accordance with example 1 of the present invention;
FIG. 4 is a schematic diagram showing the hydrophobic-lipophilic properties of the modified sponge prepared in example 1 of the present invention;
FIG. 5 is a graph showing the oil absorption capacity and recycling performance of the modified sponge prepared in example 1 of the present invention.
Detailed Description
Reagents and instrumentation:
hydroxy-terminated polydimethylsiloxane, industrial pure, Shandong Yue chemical Co., Ltd; ethyl orthosilicate, dibutyltin dilaurate and hydrophobic gas phase nano SiO2Analytically pure, alatin chemical reagents ltd; n-hexane, toluene, dichloromethane, petroleum ether, ethanol, analytically pure, Tianjin Kemiou chemical reagent, Inc.; melamine sponge, commercially available from melamine technologies, ltd; corn oil, Shandongxiwang food Co., Ltd.
Nicolet-is5 Fourier transform Infrared Spectroscopy, Sammer Feishel technologies, USA; ZRY-2P high-temperature comprehensive thermal analyzer, Shanghai Jing Ke instruments and Equipment Co., Ltd; TM3030 desktop scanning electron microscope, japanese zerk institute of advanced technology, natake; JC2000D1 contact angle measuring instrument, shanghai midmorning digital technology equipment ltd; WT-C10002 electronic balance (precision 0.01g), Hangzhou Wan Temp weighing apparatus Co., Ltd; RCT basic IKA magnetic stirrer, ericardin instruments ltd.
The test method comprises the following steps:
1. performance and characterization of the samples: analyzing the composite solution by a Nicolet-is5 Fourier transform infrared spectrometer, preparing a sample by a potassium bromide tabletting method, and testing the wave number range of 400-4000cm-1Resolution of 4cm-1The number of scans was 16. ZRY-2P high-temperature comprehensive thermal analyzer, air is introduced, and the heating rate is 10 ℃/min. Preparing a sample into small blocks of 5 multiplied by 2mm, carrying out surface gold spraying treatment, and observing the surface structure and the appearance of the sponge by adopting a TM3030 desktop scanning electron microscope at a standard voltage of 5 kv. The wettability of the sponge is represented by using a JC2000D type contact angle measuring instrument, the liquid drop amount is 5uL, and the image processing is an automatic fitting mode。
2. Physical and chemical stability test
And (3) extrusion testing: loading 100g of modified sponge on the top, and repeatedly compressing, wherein the compression ratio is 50% each time; chemical durability test: the modified sponge is placed in a sodium chloride solution (simulated seawater) with the mass fraction of 10 per mill, 20 per mill, 30 per mill, 40 per mill and 50 per mill for 24 hours. The appearance of the sponge was observed and its contact angle change was recorded.
3. Sponge oil absorption ability and cyclic usability: weighing the modified sponge W0Soaking in oil for 5min, taking out, sucking excessive oil with filter paper, and weighing1The oil absorption capacity (K) of the sponge is calculated by the following formula:
wherein, W0Is the mass of the sponge before oil absorption, W1Is the mass of the sponge after oil absorption.
Soaking the modified sponge in oil for 5min, taking out after saturation absorption, manually extruding to discharge the absorbed oil, fully washing with ethanol, drying in an oven, and testing the oil absorption performance to investigate the circulating oil absorption capacity of the sponge material.
The following description of the preferred embodiments of the present invention is provided for the purpose of better illustrating the invention and is not intended to limit the invention thereto.
Example 1
Cutting melamine sponge into blocks of 2 × 2 × 2cm, washing with deionized water and ethanol for several times, and oven drying. 0.5g of hydroxyl-terminated polydimethylsiloxane, 0.1g of ethyl orthosilicate and 0.02g of dibutyltin dilaurate were dissolved in 15g of n-hexane, and 0.18g of hydrophobic gas-phase nano SiO2After ultrasonic dispersion for 10min, stirring for 60min on a magnetic stirrer to obtain PDMS/SiO2And (4) compounding the solution. Completely immersing the pretreated sponge in PDMS/SiO2Taking out the composite solution after 30min, and curing and drying the composite solution in an oven at the temperature of 55 ℃ to obtain PDMS/SiO2A modified sponge.
The modified sponge prepared according to example 1 was tested by a contact angle tester to have an average water contact angle of 151 ± 1.0 ° (fig. 1), and it can be seen that the modified sponge has excellent hydrophobicity.
As can be seen from the sem photographs of the modified sponge prepared according to example 1, the modified substance was firmly attached to the sponge skeleton, and the modified sponge (fig. 2B) maintained good porosity relative to the unmodified sponge (fig. 2A).
According to the thermogravimetric plot (fig. 3) of the modified sponge prepared in example 1, it can be seen that the sponge before and after modification has a large difference in thermal stability. The temperature when the unmodified sponge loses 5% of the mass is about 100 ℃, the obvious weight loss temperature is about 370 ℃, the temperature when the modified sponge loses 5% of the mass is about 300 ℃, and the obvious weight loss temperature is about 380 ℃. This is because the skeleton structure of the modified sponge is coated with polysiloxane having good thermal stability, and thus the rate of thermal weight loss is low. Therefore, the modified sponge has good thermal stability.
A schematic of the hydrophobic-oleophilic properties of the modified sponge prepared according to example 1 (fig. 4). As shown in fig. 4A, the unmodified sponge absorbs water and sinks to the bottom of the water, while the modified sponge floats on the surface of the water. As shown in fig. 4B, when the modified sponge is pressed into water by external force, the surface of the sponge is densely covered with small bubbles and quickly floats on the water surface after the pressure is released. As shown in fig. 4C, the lower part of the beaker is methylene blue dyed deionized water, the upper part is n-hexane, and the modified sponge is immersed in the n-hexane and floats on the oil-water separation interface, which proves that the modified sponge has excellent selective adsorption capacity. When the modified sponge was cut as shown in fig. 4D, the methylene blue-stained water droplets appeared spherical on the surface of the sponge and slid down with a slight inclination, demonstrating that the inner structure thereof also had hydrophobic properties.
After the modified sponge prepared according to the embodiment 1 is subjected to extrusion test for 20-100 times, the water contact angle is still kept about 150 degrees, the appearance is not obviously changed, and PDMS/SiO can be seen2The compound is firmly attached to the sponge skeleton. And the modified sponge keeps stable hydrophobicity in seawater with different concentrations simulated by 10-50 thousandths of sodium chloride solution, which is benefited by good weather resistance of polysiloxane. Can be seen, modifiedThe physical and chemical properties of the sponge are very stable and can continuously maintain the hydrophobic property of the sponge under various conditions.
According to the adsorption rate chart (fig. 5) of the modified sponge prepared in example 1 for different organic matters, the oil absorption capacity K values of the modified sponge are 68, 83, 42, 40 and 56 for toluene, dichloromethane, n-hexane, petroleum ether and corn oil, respectively. In addition, the modified sponge has good recycling performance, and as can be seen from fig. 5B, after 10 times of adsorption and extrusion cycles, the absorption capacity of the modified sponge for various oils is not substantially changed, and the K value can be maintained above 35, which indicates that the modified sponge has good recycling stability, and the material also has good mechanical properties and can be repeatedly extruded for use. The sponge has very high adsorption capacity and cycle performance for different oils or organic matters, and is an ideal adsorption material.
Comparative example 1
A modified sponge was prepared in a similar manner to example 1. The preparation procedure of this example is substantially the same as that of example 1, except that: in the step, hydrophobic gas phase nano SiO is added2The mass was changed from 0.18g to 0.06 g. The water contact angle of the modified sponge prepared according to the method is reduced compared with that of the modified sponge in example 1, and at the moment, the water contact angle is 145 +/-1.0 degrees, and the super-hydrophobic effect is not achieved. The modified sponge prepared by the method has high porosity.
Comparative example 2
A modified sponge was prepared in a similar manner to example 1. The preparation procedure of this example is substantially the same as that of example 1, except that: in the step, hydrophobic gas phase nano SiO is added2The mass was changed from 0.18g to 0.30 g. The water contact angle of the modified sponge prepared according to the method is increased compared with that of example 1, and the water contact angle is 153 +/-1.0 degrees. However, electron microscope observation and experimental results show that the porosity of the modified sponge prepared by the method is greatly reduced, and the adsorption effect on different organic matters is obviously reduced.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A preparation method of a modified super-hydrophobic sponge is characterized by comprising the following steps:
cutting off commercially available melamine sponge into blocks, washing and drying for later use;
dissolving hydroxyl-terminated polydimethylsiloxane, ethyl orthosilicate and dibutyltin dilaurate in n-hexane, and adding hydrophobic gas phase nano SiO2After ultrasonic dispersion, stirring on a magnetic stirrer to obtain PDMS/SiO2Compounding the solution;
step three, completely immersing the pretreated sponge in PDMS/SiO2And taking out the composite solution after a period of time, and curing and drying to obtain the super-hydrophobic oleophylic sponge.
2. The method of claim 1, wherein the hydrophobic gas phase nano SiO2The addition amount is 0.3-0.5 of the total mass of the hydroxyl-terminated polydimethylsiloxane and the tetraethoxysilane.
3. The method of claim 1, wherein the hydrophobic gas phase nano SiO2The addition amount is 0.3 of the total mass of the hydroxyl-terminated polydimethylsiloxane and the tetraethoxysilane.
4. The production method according to any one of claims 1 to 3, wherein the mass ratio of the hydroxyl-terminated polydimethylsiloxane to the tetraethoxysilane is 5: 1; the dibutyltin dilaurate is used as a catalyst, and the mass ratio of the dibutyltin dilaurate to the total mass of the hydroxyl-terminated polydimethylsiloxane and the tetraethoxysilane is 1: 60-1: 30.
5. The preparation method according to any one of claims 1 to 3, wherein the ultrasonic treatment is carried out for 10 to 20min, the stirring is carried out for 20 to 40min, and the soaking is carried out for 20 to 40 min.
6. A modified superhydrophobic sponge prepared according to the method of any of claims 1-5.
7. A method for oil-water separation, which comprises using the modified superhydrophobic sponge of claim 6 as an adsorbent for adsorption.
8. The method as claimed in claim 7, wherein the oil in the oil-water separation is any one or more of toluene, dichloromethane, n-hexane, petroleum ether, and corn oil.
9. Use of the modified superhydrophobic sponge of claim 6 in the separation and recovery of oil-containing or organic solvent and water mixtures.
10. Use according to claim 9, wherein the separation and recovery can be carried out in any one or more of the following environments: a high temperature environment below 300 ℃, and a salt-containing environment of 10-50 per mill sodium chloride.
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