CN107998687B - Preparation method of intelligent oil-water separation material - Google Patents

Preparation method of intelligent oil-water separation material Download PDF

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CN107998687B
CN107998687B CN201711296548.5A CN201711296548A CN107998687B CN 107998687 B CN107998687 B CN 107998687B CN 201711296548 A CN201711296548 A CN 201711296548A CN 107998687 B CN107998687 B CN 107998687B
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separation material
water
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CN107998687A (en
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刘丁菡
李凌杰
雷惊雷
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Chongqing University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02Separation of non-miscible liquids
    • B01D17/0202Separation of non-miscible liquids by ab- or adsorption
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • B01D39/16Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
    • B01D39/1607Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
    • B01D39/1615Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of natural origin
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/10Filtering material manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4825Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
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  • Organic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Filtering Materials (AREA)

Abstract

The invention provides a preparation method of an intelligent oil-water separation material, and particularly relates to an intelligent oil-water separation material which is prepared by taking biomass loofah sponge as a raw material and through proper treatment and can conveniently and rapidly realize reversible conversion between different wetting states of super-hydrophobic/super-oleophilic and super-hydrophilic/underwater super-oleophobic. The natural three-dimensional reticular porous structure of the biomass loofah sponge is skillfully utilized and is used as a raw material, the cost is low, the material is easy to obtain, the prepared oil-water separation material has a good separation effect on an oil-water mixture, can be repeatedly utilized, has an intelligent characteristic, and can flexibly meet different oil-water separation requirements.

Description

Preparation method of intelligent oil-water separation material
Technical Field
The invention belongs to the technical field of oil-water separation, and particularly relates to a preparation method of an intelligent oil-water separation material.
Background
In recent years, water body pollution caused by leakage of petroleum and chemical substances frequently occurs, and the ecological environment and the living environment of human beings are seriously threatened, so that the research and development of an efficient and convenient oil-water separation technology are urgently needed, and an oil-water separation material is the key of the oil-water separation technology, wherein an adsorption type oil-water separation material and a filtration type oil-water separation material are considered to be ideal choices due to convenient operation, so that people develop a great deal of research around the adsorption type oil-water separation material and the filtration type oil-water separation material in recent years. Among the adsorption-type oil-water separation materials, the most representative ones are (super) hydrophobic/(super) oleophilic sponges prepared by appropriate treatment using sponges as raw materials, such as chinese patent CN 105688846A, "a preparation method of a high-efficiency oil-water separation sponge", CN 105797431a "a preparation method of a high-efficiency hydrophobic oil-absorption sponge", CN 106698583a "a preparation method of a super-hydrophobic melamine sponge adsorption-type oil-water separation material and a product and an application thereof", CN 107118386A "a super-hydrophobic sponge and a preparation method and an application thereof", CN 103626171B "a preparation method of an oil-water separation material", and the like. Among the filtration type oil-water separation materials, the most representative ones are a super-hydrophilic or super-hydrophobic porous structure prepared by appropriate treatment using a metal mesh or a foamed metal as a raw material, such as chinese patent CN 104874295B, "a preparation method of a super-hydrophilic self-cleaning multifunctional graded oil-water separation material", CN 106833340a "method for preparing a corrosion-resistant super-hydrophobic copper mesh by spray coating", CN 106630006A "a rapid oil-water separation material and a preparation method and application thereof", CN 106422423a "a super-hydrophobic metal mesh and a preparation method thereof", CN 106283133a "a preparation method of a bionic oil-water separation copper foam", CN 105879429a "a novel oil-water separation material and a use method thereof", and the like. It can be seen that these oil-water separation materials usually have only a certain wettability, i.e. superhydrophobic or superhydrophilic, and can not realize reversible switching between different wetting states, which means that these materials can only be used for separating water or oil, but can not flexibly select water or oil for separation according to different separation requirements; in addition, the materials realize oil-water separation in a single mode, namely only in an adsorption mode or a filtration mode, but not in a mode of flexibly changing the separation mode according to different separation requirements, which seriously influences the practical application of the oil-water separation materials.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of an intelligent oil-water separation material, the prepared material can conveniently and quickly realize reversible conversion between different wetting states of super-hydrophobic/super-oleophilic and super-hydrophilic/underwater super-oleophobic, and can be used as an adsorption type oil-water separation material and a filtration type oil-water separation material to meet different oil-water separation requirements.
The invention adopts the following technical scheme:
the preparation method of the intelligent oil-water separation material is characterized by comprising the following steps:
longitudinally compressing commercial vegetable sponge by 40-60 times and transversely compressing by 10-20 times to obtain a vegetable sponge compressed block with the height of about 1 cm and the diameter of about 1 cm, immersing the vegetable sponge compressed block in 0.5-2.0 mol/L dilute hydrochloric acid solution for ultrasonic treatment for 2-5 minutes, taking out, washing with pure water, and drying with compressed air;
immersing the sponge gourd pulp compressed block processed in the step one in 2.0-5.0 mol/L copper sulfate solution for ultrasonic treatment for 1-3 hours, taking out the sponge gourd pulp compressed block, pre-freezing the sponge gourd pulp compressed block at-20 to-40 ℃ for 1-3 hours, freeze-drying the sponge gourd pulp compressed block at-40 to-50 ℃ under the pressure of 1-3 Pa for 24-36 hours, taking out the sponge gourd pulp compressed block, and heating the sponge gourd pulp compressed block in air at 180-240 ℃ for 4-6 hours;
and thirdly, performing plasma treatment on the sponge gourd pulp compressed block treated in the second step for 5-15 minutes to obtain a super-hydrophobic/super-oleophylic oil-water separation material, wherein the super-hydrophobic/super-oleophylic oil-water separation material is used as an adsorption type oil-water separation material for adsorbing oil in water to realize oil-water separation.
And further, carrying out infrared radiation treatment on the super-hydrophobic/super-oleophylic oil-water separation material obtained in the step (III) for 15-30 minutes to obtain the super-hydrophilic/underwater super-oleophobic oil-water separation material, and using the super-hydrophilic/underwater super-oleophobic oil-water separation material as a filtering oil-water separation material for filtering and separating water and oil to realize oil-water separation.
And further, performing plasma treatment on the super-hydrophilic/underwater super-oleophobic oil-water separation material obtained in the step (iv) for 5-15 minutes to obtain a super-hydrophobic/super-oleophilic oil-water separation material which is used as an adsorption type oil-water separation material for adsorbing oil in water to realize oil-water separation.
Further, the third step, the fourth step and the fifth step can be repeated for a plurality of times, so that the prepared oil-water separation material can be reversibly converted between different wetting states of super-hydrophobic/super-oleophilic and super-hydrophilic/underwater super-oleophobic, and the intelligent oil-water separation material can be obtained.
As optimization, the plasma treatment takes high-purity nitrogen as a gas source, the vacuum degree is 20Pa, and the power is 50W. The light source for infrared radiation treatment is a 275W infrared lamp, and the distance from the surface of the material is 4 cm.
Compared with the prior art, the invention has the following beneficial effects:
1. the intelligent oil-water separation material prepared by the invention can conveniently and quickly realize reversible conversion between different wetting states of super-hydrophobic/super-oleophilic and super-hydrophilic/underwater super-oleophobic, can be used as an adsorption type oil-water separation material and a filtration type oil-water separation material, and overcomes the defect that the existing oil-water separation material can only be used for separating water or oil, can only be used for adsorption type separation or filtration type separation and cannot flexibly adapt to different separation requirements.
2. The invention skillfully utilizes the natural three-dimensional reticular porous structure of the biomass vegetable sponge as the raw material, is cheap and easy to obtain, and has relatively simple processing raw materials and process and lower cost.
3. The invention utilizes the characteristic that the vegetable sponge is insensitive to plasma and infrared radiation and the chemical deposition substances on the three-dimensional framework are sensitive to the plasma and the infrared radiation, and adopts the plasma treatment and the infrared radiation treatment to realize the reversible conversion of the prepared oil-water separation material between different wetting states for many times while keeping the three-dimensional framework stable.
4. The oil-water separation material prepared by the invention has good separation effect on oil-water mixture, can be repeatedly used, has intelligent characteristics, and can flexibly meet different oil-water separation requirements.
Detailed Description
First, preparation method
Example 1:
the method for preparing the intelligent oil-water separation material comprises the following specific steps:
longitudinally compressing the commercial vegetable sponge by 40 times and transversely compressing by 10 times to obtain a vegetable sponge compressed block with the height of about 1 cm and the diameter of about 1 cm, immersing the vegetable sponge compressed block in 0.5mol/L dilute hydrochloric acid solution for ultrasonic treatment for 2 minutes, taking out, washing with pure water, and drying with compressed air;
immersing the pressed sponge gourd block processed in the step one in 2.0mol/L copper sulfate solution for ultrasonic treatment for 3 hours, then taking out the pressed sponge gourd block, pre-freezing the pressed sponge gourd block for 3 hours at-20 ℃, freeze-drying the pressed sponge gourd block for 36 hours at-40 ℃ and 1Pa, taking out the pressed sponge gourd block, and heating the pressed sponge gourd block in air at 180 ℃ for 6 hours;
and thirdly, carrying out plasma treatment on the sponge gourd pulp compressed block treated in the second step for 15 minutes, wherein the plasma treatment uses high-purity nitrogen as a gas source, the vacuum degree is 20Pa and the power is 50W to obtain the super-hydrophobic/super-oleophylic oil-water separation material which is used as an adsorption type oil-water separation material for adsorbing oil in water to realize oil-water separation.
Example 2:
further, on the basis of the embodiment 1, the superhydrophobic/superoleophilic oil-water separation material obtained in the step (III) is subjected to infrared radiation treatment for 30 minutes, a 275W infrared lamp is used as a light source for the infrared radiation treatment, and the distance from the surface of the material is 4cm, so that the superhydrophilic/underwater superoleophobic oil-water separation material is obtained and is used as a filtering type oil-water separation material for filtering and separating water and oil to realize oil-water separation.
Example 3:
further, based on the example 2, the super-hydrophilic/underwater super-oleophobic oil-water separation material obtained in the step (iv) is subjected to plasma treatment for 15 minutes, wherein the plasma treatment uses high-purity nitrogen as a gas source, the vacuum degree is 20Pa, and the power is 50W, so that the super-hydrophobic/super-oleophilic oil-water separation material is obtained, and is used as an adsorption type oil-water separation material for adsorbing oil in water to realize oil-water separation.
The steps III, IV and V can be repeated for a plurality of times, so that the reversible conversion of the prepared oil-water separation material between different wetting states of super-hydrophobic/super-oleophilic and super-hydrophilic/underwater super-oleophobic is realized, and the intelligent oil-water separation material is obtained.
Example 4:
the method for preparing the intelligent oil-water separation material comprises the following specific steps:
longitudinally compressing commercial vegetable sponge by 50 times and transversely compressing by 15 times to obtain vegetable sponge compressed blocks with the height of about 1 cm and the diameter of about 1 cm, immersing the vegetable sponge compressed blocks in 1.0mol/L dilute hydrochloric acid solution for ultrasonic treatment for 3 minutes, taking out, washing with pure water, and drying with compressed air;
immersing the pressed sponge gourd block processed in the step one in 3.0mol/L copper sulfate solution for ultrasonic treatment for 2 hours, then taking out the pressed sponge gourd block, pre-freezing the pressed sponge gourd block for 2 hours at-30 ℃, freeze-drying the pressed sponge gourd block for 30 hours at-45 ℃ and under the pressure of 2Pa, taking out the pressed sponge gourd block, and heating the pressed sponge gourd block for 5 hours at 200 ℃ in the air;
thirdly, performing plasma treatment on the sponge gourd pulp compressed block treated in the second step for 10 minutes, wherein the plasma treatment uses high-purity nitrogen as a gas source, the vacuum degree is 20Pa and the power is 50W to obtain a super-hydrophobic/super-oleophylic oil-water separation material which is used as an adsorption type oil-water separation material for adsorbing oil in water to realize oil-water separation;
fourthly, further carrying out infrared radiation treatment on the super-hydrophobic/super-oleophilic oil-water separation material obtained in the third step for 25 minutes, wherein a light source of the infrared radiation treatment is a 275W infrared lamp, and the distance between the infrared radiation treatment and the surface of the material is 4cm, so that the super-hydrophilic/underwater super-oleophobic oil-water separation material is obtained and is used as a filtering type oil-water separation material for filtering and separating water and oil to realize oil-water separation;
fifthly, performing plasma treatment on the super-hydrophilic/underwater super-oleophobic oil-water separation material obtained in the step IV for 10 minutes, wherein the plasma treatment uses high-purity nitrogen as a gas source, the vacuum degree is 20Pa and the power is 50W to obtain a super-hydrophobic/super-oleophilic oil-water separation material which is used as an adsorption type oil-water separation material for adsorbing oil in water to realize oil-water separation;
the steps III, IV and V can be repeated for a plurality of times, so that the reversible conversion of the prepared oil-water separation material between different wetting states of super-hydrophobic/super-oleophilic and super-hydrophilic/underwater super-oleophobic is realized, and the intelligent oil-water separation material is obtained.
Example 5:
the method for preparing the intelligent oil-water separation material comprises the following specific steps:
longitudinally compressing commercial vegetable sponge by 60 times and transversely compressing by 20 times to obtain vegetable sponge compressed blocks with the height of about 1 cm and the diameter of about 1 cm, immersing the vegetable sponge compressed blocks in 1.5mol/L dilute hydrochloric acid solution for ultrasonic treatment for 4 minutes, taking out, cleaning with pure water, and drying with compressed air;
immersing the pressed sponge gourd block processed in the step one in 4.0mol/L copper sulfate solution for ultrasonic treatment for 1.5 hours, then taking out the pressed sponge gourd block, pre-freezing the pressed sponge gourd block for 1 hour at-40 ℃, freeze-drying the pressed sponge gourd block for 24 hours at-50 ℃ and 3Pa pressure, taking out the pressed sponge gourd block, and heating the pressed sponge gourd block in air at 240 ℃ for 4 hours;
thirdly, performing plasma treatment on the sponge gourd pulp compressed block treated in the second step for 10 minutes, wherein the plasma treatment uses high-purity nitrogen as a gas source, the vacuum degree is 20Pa and the power is 50W to obtain a super-hydrophobic/super-oleophylic oil-water separation material which is used as an adsorption type oil-water separation material for adsorbing oil in water to realize oil-water separation;
fourthly, the super-hydrophobic/super-oleophylic oil-water separation material obtained in the third step is further subjected to infrared radiation treatment for 20 minutes, a 275W infrared lamp is used as a light source of the infrared radiation treatment, the distance between the infrared radiation treatment and the surface of the material is 4cm, and the super-hydrophilic/underwater super-oleophobic oil-water separation material is obtained and can be used as a filtering type oil-water separation material for filtering and separating water and oil to realize oil-water separation;
fifthly, performing plasma treatment on the super-hydrophilic/underwater super-oleophobic oil-water separation material obtained in the step IV for 10 minutes, wherein the plasma treatment uses high-purity nitrogen as a gas source, the vacuum degree is 20Pa and the power is 50W to obtain a super-hydrophobic/super-oleophilic oil-water separation material which is used as an adsorption type oil-water separation material for adsorbing oil in water to realize oil-water separation;
the steps III, IV and V can be repeated for a plurality of times, so that the reversible conversion of the prepared oil-water separation material between different wetting states of super-hydrophobic/super-oleophilic and super-hydrophilic/underwater super-oleophobic is realized, and the intelligent oil-water separation material is obtained.
Example 6:
the preparation method of the intelligent oil-water separation material comprises the following specific steps:
longitudinally compressing the commercial vegetable sponge by 40 times and transversely compressing by 10 times to obtain a vegetable sponge compressed block with the height of about 1 cm and the diameter of about 1 cm, immersing the vegetable sponge compressed block in 2.0mol/L dilute hydrochloric acid solution for ultrasonic treatment for 5 minutes, taking out, washing with pure water, and drying with compressed air;
immersing the pressed sponge gourd block processed in the step one in 5.0mol/L copper sulfate solution for ultrasonic treatment for 1 hour, then taking out the pressed sponge gourd block, pre-freezing the pressed sponge gourd block for 1 hour at-40 ℃, freeze-drying the pressed sponge gourd block for 28 hours at-50 ℃ and 2Pa, taking out the pressed sponge gourd block, and heating the pressed sponge gourd block for 5 hours at 220 ℃ in air;
thirdly, performing plasma treatment on the sponge gourd pulp compressed block treated in the second step for 5 minutes, wherein the plasma treatment uses high-purity nitrogen as a gas source, the vacuum degree is 20Pa and the power is 50W to obtain a super-hydrophobic/super-oleophylic oil-water separation material which is used as an adsorption type oil-water separation material for adsorbing oil in water to realize oil-water separation;
fourthly, further carrying out infrared radiation treatment on the super-hydrophobic/super-oleophilic oil-water separation material obtained in the third step for 15 minutes, wherein a light source of the infrared radiation treatment is a 275W infrared lamp, and the distance between the infrared radiation treatment and the surface of the material is 4cm, so that the super-hydrophilic/underwater super-oleophobic oil-water separation material is obtained and is used as a filtering type oil-water separation material for filtering and separating water and oil to realize oil-water separation;
fifthly, performing plasma treatment on the super-hydrophilic/underwater super-oleophobic oil-water separation material obtained in the step IV for 5 minutes, wherein the plasma treatment uses high-purity nitrogen as a gas source, the vacuum degree is 20Pa and the power is 50W to obtain the super-hydrophobic/super-oleophilic oil-water separation material which is used as an adsorption type oil-water separation material for adsorbing oil in water to realize oil-water separation;
the steps III, IV and V can be repeated for a plurality of times, so that the reversible conversion of the prepared oil-water separation material between different wetting states of super-hydrophobic/super-oleophilic and super-hydrophilic/underwater super-oleophobic is realized, and the intelligent oil-water separation material is obtained.
Second, performance test
The performance test is carried out on the intelligent oil-water separation material prepared by the embodiment, and the method comprises the following steps:
(1) and (3) testing the wetting state: the wettability of the material is judged by measuring the static contact angle of 2 mu L of water drops (pure water) and oil drops (normal hexane) on the surface of the material by using a German Dataphysics OCA20 video optical contact angle measuring instrument, the contact angle is more than 150 degrees and is in a super-hydrophobic state, and the contact angle is less than 10 degrees and is in a super-hydrophilic state.
(2) Testing the oil absorption capacity: the prepared intelligent oil-water separation material is immersed in an oil phase medium (normal hexane) until the adsorption is saturated, then is quickly taken out and weighed, and the oil absorption capacity is calculated according to the weight change of the material before and after oil absorption, wherein the calculation formula is as follows:
oil absorption capacity ═ Mafter-Mbefore)/Mbefore
MbeforeAnd MafterThe weight of the material before and after oil absorption. It can be seen that the oil absorption capacity, i.e. the oil absorption of the material, is a multiple of its own weight.
(3) Testing the oil-water separation effect of the adsorption mode: the prepared intelligent oil-water separation material is placed in a mixture of 200 ml of oil (normal hexane, Sudan III dyed red, volume of 20 ml) and water (pure water, volume of 180 ml), the oil absorption process of the material is observed, and the time for complete adsorption of the oil is recorded. The adsorbed oil was squeezed off and the above oil absorption process test was repeated to investigate the repeated (10) use capacity of the material.
(4) Testing the oil-water separation effect of the filtering mode: the prepared intelligent oil-water separation material is longitudinally cut into a wafer with the thickness of about 1.5mm, the wafer is fixed between two glass tubes, an empty beaker is connected below the glass tubes, then 200 ml of a mixture of oil (normal hexane, Sudan III is dyed red and the volume of the mixture is 20 ml) and water (pure water and the volume of the mixture is 180 ml) is poured above the material, the oil-water separation process is observed, and the time for completely separating the oil from the water is recorded. The oil-water separation process test described above was repeated to examine the repeated (10 times) use ability of the material.
The results of the performance test of the samples prepared in the above examples are shown in table 1.
TABLE 1 Performance test results
As can be seen from Table 1, the intelligent oil-water separation material prepared by the invention can be reversibly switched between 2 different wetting states of super-hydrophobic/super-oleophilic and super-hydrophilic/underwater super-oleophobic, and has very good separation effect on oil-water mixtures as an adsorption oil-water separation material or a filtration oil-water separation material and can be repeatedly utilized.
In the above examples, n-hexane is used as an oil phase medium, and it should be noted that the intelligent oil-water separation material prepared by the present invention is also suitable for separation of oil-water mixtures when various organic solvents such as toluene, dichloromethane, carbon tetrachloride, isooctane, dodecane, etc. and diesel oil, engine oil, kerosene, edible oil, etc. are used as oil phase media.
Finally, the above embodiments are only used to illustrate the technical solutions of the present invention, and other modifications or equivalent substitutions made according to the technical solutions of the present invention should be covered by the scope of the claims of the present invention.

Claims (4)

1. The preparation method of the intelligent oil-water separation material is characterized by comprising the following steps:
longitudinally compressing the commercial vegetable sponge by 40 ~ 60 times and transversely compressing by 10 ~ 20 times to obtain a vegetable sponge compressed block with the height of about 1 cm and the diameter of about 1 cm, immersing the vegetable sponge compressed block in 0.5 ~ 2.0.0 mol/L dilute hydrochloric acid solution, carrying out ultrasonic treatment for 2 ~ 5 minutes, taking out, cleaning with pure water, and drying with compressed air;
immersing the pressed sponge gourd blocks processed in the step I in 2.0 ~ 5.0.0 mol/L copper sulfate solution for ultrasonic treatment for 1 ~ 3 hours, taking out the pressed sponge gourd blocks, pre-freezing the pressed sponge gourd blocks at the temperature of minus 20 ℃ and ~ -40 ℃ for 1 ~ 3 hours, then freeze-drying the pressed sponge gourd blocks at the temperature of minus 40 ℃ and ~ -50 ℃ and under the pressure of 1 ~ 3Pa for 24 ~ 36 hours, taking out the pressed sponge gourd blocks, and heating the pressed sponge gourd blocks in air at the temperature of 180 ~ 240 ℃ for 4 ~ 6 hours;
thirdly, performing plasma treatment on the sponge gourd pulp compressed block treated in the second step for 5 ~ 15 minutes to obtain a super-hydrophobic/super-oleophilic oil-water separation material which is used as an adsorption type oil-water separation material for adsorbing oil in water to realize oil-water separation;
fourthly, the super-hydrophobic/super-oleophilic oil-water separation material obtained in the third step is subjected to infrared radiation treatment for 15 ~ 30 minutes to obtain a super-hydrophilic/underwater super-oleophobic oil-water separation material which is used as a filtering type oil-water separation material for filtering and separating water and oil to realize oil-water separation;
fifthly, performing plasma treatment on the super-hydrophilic/underwater super-oleophobic oil-water separation material obtained in the step (iv) for 5 ~ 15 minutes to obtain a super-hydrophobic/super-oleophilic oil-water separation material which is used as an adsorption type oil-water separation material for adsorbing oil in water to realize oil-water separation.
2. The preparation method of the intelligent oil-water separation material according to claim 1, wherein the steps of the fourth step and the fifth step can be repeated for a plurality of times, so that the prepared oil-water separation material can be reversibly switched between different wetting states of super-hydrophobic/super-oleophilic and super-hydrophilic/underwater super-oleophobic, and the intelligent oil-water separation material can be obtained.
3. The method for preparing the intelligent oil-water separation material according to claim 1, wherein the plasma treatment uses high-purity nitrogen as a gas source, the vacuum degree is 20Pa, and the power is 50W.
4. The method for preparing the intelligent oil-water separation material as claimed in claim 1, wherein the light source for the infrared radiation treatment is a 275W infrared lamp, and the distance from the surface of the material is 4 cm.
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