CN110760030A - Preparation method and application of hydrophobic material based on nanoparticles - Google Patents
Preparation method and application of hydrophobic material based on nanoparticles Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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- 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
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- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
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- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
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- C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
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Abstract
The invention relates to a preparation method of a hydrophobic material based on nanoparticles, which comprises the following steps: adding a hole nano-particle material AlTz-68-C18 into the divinylbenzene solution, and uniformly stirring to obtain a dispersion liquid; taking a mixed solution of cyclohexanol and 1-dodecanol, adding a monomer containing a methacrylic acid group and diethylene glycol dimethacrylate, and uniformly mixing to obtain a hydrophilic material; and pouring the hydrophilic material into the dispersion, adding an initiator, and carrying out microwave reaction for 1 min. The preparation method is simple, the hydrophobic material does not need to adopt a matrix when being used as the oil-water separation material, the oil-water separation effect is good, the hydrophobic material can be repeatedly used, and the hydrophobic material can be made into different specifications and forms according to the requirements of different application occasions.
Description
Technical Field
The invention belongs to the technical field of oil-water separation materials, and particularly relates to a preparation method and application of a hydrophobic material based on nanoparticles.
Background
The oil leakage pollution generated in the processes of crude oil exploitation, transportation and processing is a serious problem faced by global water pollution at present. Crude oil leakage events, such as those occurring in the gulf of mexico in the united states in 2010, are historically the most serious oil leakage incidents in the united states, causing devastating environmental and ecological disasters in addition to significant economic losses.
The traditional oil pollution treatment method, such as the adoption of chemical dispersants, incineration, oil skimmers and the like, not only wastes time and energy, but also brings about the problem of secondary pollution, and is gradually eliminated. However, the organic matter causing oil pollution includes not only light oil floating on the water surface and deposited heavy oil, but also various oil-containing emulsions, so that a great deal of difficulties and challenges are faced in developing a simple, efficient and low-cost oil stain treatment strategy. The super-hydrophobic/oleophilic or super-oleophobic/hydrophilic material developed based on the bionic strategy can effectively realize oil-water separation through filtration, and becomes the hot research in the field of oil pollution treatment.
At present, most of super-hydrophobic/oleophilic or super-oleophobic/hydrophilic materials are modified by using sponge as a matrix to achieve the aim of hydrophobicity, so that oil-water separation is realized, for example, Chinese patent publication No. CN107020068B discloses a preparation method of carbon nanotube reinforced super-hydrophobic ethyl cellulose sponge for oil-water separation, ethyl cellulose is used as an oil-water separation material, and the sponge matrix is synergistically enhanced by crosslinking and introducing carbon nanotubes.
In view of the above, it is necessary to design a new method for preparing an oil-water separation material to solve the above problems.
Disclosure of Invention
A first object of the present invention is to provide a method for preparing a hydrophobic nanoparticle-based material.
The second object of the present invention is to provide a hydrophobic material obtained by the above-mentioned preparation method.
The third purpose of the invention is to provide the oil-water separation filter plate prepared by the hydrophobic material.
The fourth purpose of the invention is to provide an oil-water separation column prepared from the hydrophobic material.
In a first aspect of the present invention, there is provided a method for preparing a hydrophobic nanoparticle-based material, comprising the steps of:
s1 preparation of dispersion of porous nanoparticle material AlTz-68-C18
Adding 0.5-2.0 parts by weight of porous nano-particle material AlTz-68-C18 into 0.1-1 part by weight of divinylbenzene solution, stirring to uniformly disperse the porous nano-particle material AlTz-68-C18 in the divinylbenzene solution, thus obtaining the dispersion liquid;
s2 preparation of hydrophilic material
Taking 1.5-3.5 parts by weight of cyclohexanol and 1.5-3.5 parts by weight of 1-dodecanol, uniformly mixing, adding 0.5-3.0 parts by weight of monomer containing methacrylic acid group and 0.5-3.0 parts by weight of diethylene glycol dimethacrylate, and uniformly mixing to obtain the hydrophilic material;
s3 preparation of hydrophobic material
And (3) pouring the hydrophilic material prepared in the step (S2) into the dispersion prepared in the step (S1), adding 0.01-0.1 part by weight of an initiator, and carrying out microwave reaction at 50-100 ℃ for 1min to obtain the hydrophobic material.
The methacrylic acid group monomer is a monomer containing a methacrylic acid group, and further is one of glycidyl methacrylate, butyl methacrylate, 2-ethylhexyl acrylate, 2-hydroxyethyl methacrylate, methyl methacrylate and methacrylic acid.
Further, the mass ratio of the methacrylic group-containing monomer to diethylene glycol dimethacrylate was in agreement with the density ratio thereof.
The initiator is also called initiator, and refers to a compound which is easily decomposed into free radicals (namely primary free radicals) by heating, can be used for initiating free radical polymerization and copolymerization of alkene and diene monomers, and can also be used for crosslinking curing and macromolecular crosslinking of unsaturated polyester, and further, the initiator is azobisisobutyronitrile.
Further, the temperature of the microwave reaction is 80 ℃.
In a second aspect of the invention, there is provided a hydrophobic material obtained by the above-described preparation method.
Further, the contact angle value of the hydrophobic material and water is 140 +/-5 degrees.
The third aspect of the present invention provides an oil-water separation filter plate made of the hydrophobic material.
The fourth aspect of the invention provides an oil-water separation column prepared from the hydrophobic material.
Compared with the prior art, the invention has the following beneficial effects and advantages: the hydrophobic material is prepared by adding the nanoparticle dispersion liquid and the initiator into the hydrophilic material and then performing microwave reaction, the preparation method is simple and quick, no sponge is needed to be used as a matrix, the oil-water separation effect is good when the hydrophobic material is used in the field of oil-water separation, and after more than ten oil-water separation tests, the oil-water separation efficiency is almost the same, so that the hydrophobic material has better reusability; and can be made into different specifications and forms such as filter plates, pipe columns and the like according to the requirements of different application occasions.
Drawings
FIG. 1 is a picture of the appearance of a filter plate prepared in example 1 of the present invention;
FIG. 2 is a first picture of the appearance of a pipe string according to example 7 of the present invention;
FIG. 3 is a second picture of the appearance of a pipe string according to example 7 of the present invention;
FIG. 4 is a schematic diagram showing the hydrophobicity of the surface of the oil-water separation filter plate in example 1 of the present invention, wherein water droplets are located on the left side of the surface of the filter plate, and an organic solvent is located on the right side of the surface of the filter plate;
FIG. 5 shows the contact angle value with water of 140 ° in example 1 of the present invention;
FIG. 6 is a graph of the efficiency of repeated separations for examples 1-7 of the present invention;
FIG. 7 shows a filter device used in the oil-water separation test according to the present invention.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
At present, most of oil-water separation materials are sponges, have poor characteristic mechanical properties, low repeatable utilization rate and limited application occasions, and the hydrophobic materials can be manufactured by complicated steps.
The raw materials used in the examples of the present invention are shown in table 1 below, but not limited thereto:
TABLE 1
The porous nanoparticle material AlTz-68-C18 shown in Table 1 is prepared by self-making a modified porous organic framework and a preparation method thereof, a porous organic framework compound and a preparation method thereof, which are patent inventions with the patent publication number TWI641613B, and the specific steps are as follows:
a. preparation of a porous organic framework AlTz53
0.235mmol of aluminum chloride, 0.18mmol of 1,2,4, 5-tetrazine-3, 6-dicarboxylic acid and 5.0mL of diethylformamide are mixed, reacted for 1 day at 120 ℃, and washed for 3 times by 2.0mL of dimethylformamide to obtain the porous organic framework AlTz 53.
b. Preparation of porous organic framework AlTz53-C18
Mixing 10.0mg of porous organic framework AlTz53, 3.0mL of dimethylformamide and 2.0mL of 1-octadecene, reacting at 50 ℃ for 1 hour, reacting at 80 ℃ for 12 hours, and drying the dimethylformamide to obtain the porous organic framework AlTz 53-C18.
c. Preparation of porous nanoparticle material AlTz-68-C18
And (b) carrying out solvent replacement on the porous organic framework AlTz53-C18 obtained in the step (b) by using 3.0mL of diethyl ether for 3 times, soaking AlTz53-C18 in the diethyl ether, wherein the height of the diethyl ether is 0.5cm higher than that of AlTz53-C18, putting the whole into an oven, and heating at 75 ℃ for 1 hour to obtain the nano-porous particle material AlTz 68-C18.
Example 1
The preparation method of the oil-water separation material based on the nano particles comprises the following steps:
s1 preparation of dispersion of porous nanoparticle material AlTz-68-C18
Sequentially adding 0.25g of Divinylbenzene (DVB) liquid and 0.9g of porous nanoparticle material (AlTz-68-C18) into a 100ml beaker, and stirring by using a magnet to uniformly disperse and mix the nanoparticles;
s2 preparation of hydrophilic material
Adding 2.340mL of cyclohexanol and 2.710mL of 1-dodecanol into a 20mL beaker, uniformly mixing, adding 1.425mL of Glycidyl Methacrylate (GMA) and 1.425mL of diethylene glycol dimethacrylate (DEGDMA) into the beaker, and uniformly mixing;
s3 preparation of hydrophobic material
Pouring the hydrophilic material of S2 into the dispersion of S1, adding 50mg of Azobisisobutyronitrile (AIBN), reacting at 80 ℃ for 1min by microwave to obtain an oil-water separation material, and removing the oil-water separation material from the beaker to obtain the oil-water separation filter plate shown in figure 1.
As shown in fig. 4, when a drop of water and an organic solvent is respectively dropped on the surface of the oil-water separation filter plate, the organic solvent on the right side is absorbed by the oil-water separation filter plate, and the drop of water on the left side forms a contact angle with the surface of the filter plate, and the contact angle value is 140 ° as shown in fig. 5.
Example 2
The same procedure as in example 1 was repeated except that an equal volume of Butyl Methacrylate (BMA) was used in place of Glycidyl Methacrylate (GMA) in example 1.
Example 3
The same procedure as in example 1 was repeated except that an equal volume of 2-ethylhexyl acrylate (2-EHA) was used in place of Glycidyl Methacrylate (GMA) in example 1.
Example 4
An equal volume of 2-hydroxyethyl methacrylate (HEMA) was used in place of Glycidyl Methacrylate (GMA) in example 1, and the procedure was otherwise the same as in example 1.
Example 5
An equal volume of Methyl Methacrylate (MMA) was used in place of Glycidyl Methacrylate (GMA) in example 1, and the rest was the same as in example 1.
Example 6
An equal volume of Methacrylic Acid (MA) was used in place of Glycidyl Methacrylate (GMA) in example 1, and the procedure was otherwise the same as in example 1.
Example 7
The only difference from example 1 is: example 7 after 50mg of Azobisisobutyronitrile (AIBN) was added, the solution was poured into a column mold (made of teflon, 5cm long, 1.5cm outer diameter and 0.5cm inner diameter) for microwave reaction for 1min, and the oil-water separation column shown in fig. 2 and 3 was obtained after taking out and releasing the mold.
Separation efficiency test of examples 1 to 7
According to the oil-water separation efficiency test method shown in "modified super hydrophilic/super oleophobic material for anti-fog, self-cleaning and oil-water separation" published in journal of the American chemical society-applied materials and interfaces "at 21021-21029 of 2015, 8ml of distilled water and 8ml of soybean oil are uniformly mixed in a beaker, and then poured into a filter device shown in FIG. 7, the weight of the collected filtrate (i.e. distilled water) is measured, and the oil-water separation is repeated 10 times (the repeated separation efficiency is shown in FIG. 6), the test data are shown in the following Table 2:
TABLE 2
As can be seen from table 2: the hydrophobic materials of examples 1-7 all have good oil-water separation effect, and after ten oil-water separation tests, the oil-water separation efficiency is only slightly reduced, so that the hydrophobic materials of the invention have good reusability; as can be seen from the test results of examples 1-6, esters containing methacrylic groups; by comparing the embodiment 1 with the embodiment 7, the same hydrophobic material is prepared into different specification forms, the oil-water separation effect is not greatly different, and the oil-water separation material with different specification forms can be conveniently prepared according to the requirements of different application occasions.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, and that various changes and modifications may be made without departing from the spirit and scope of the invention as defined by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. The preparation method of the hydrophobic material based on the nano-particles is characterized by comprising the following steps:
s1 preparation of dispersion of porous nanoparticle material AlTz-68-C18
Adding 0.5-2.0 parts by weight of porous nano-particle material AlTz-68-C18 into 0.1-1 part by weight of divinylbenzene solution, stirring to uniformly disperse the porous nano-particle material AlTz-68-C18 in the divinylbenzene solution, thus obtaining the dispersion liquid;
s2 preparation of hydrophilic material
Taking 1.5-3.5 parts by weight of cyclohexanol and 1.5-3.5 parts by weight of 1-dodecanol, uniformly mixing, adding 0.5-3.0 parts by weight of monomer containing methacrylic acid group and 0.5-3.0 parts by weight of diethylene glycol dimethacrylate, and uniformly mixing to obtain the hydrophilic material;
s3 preparation of hydrophobic material
And (3) pouring the hydrophilic material prepared in the step (S2) into the dispersion prepared in the step (S1), adding 0.01-0.1 part by weight of an initiator, and carrying out microwave reaction at 50-100 ℃ for 1min to obtain the hydrophobic material.
2. The method of claim 1, wherein the methacrylate group monomer is one of glycidyl methacrylate, butyl methacrylate, 2-ethylhexyl acrylate, 2-hydroxyethyl methacrylate, methyl methacrylate, and methacrylic acid.
3. The method of claim 1, wherein the mass ratio of the methacrylate group-containing monomer to diethylene glycol dimethacrylate is in accordance with the density ratio thereof.
4. The method of claim 1, wherein the initiator is azobisisobutyronitrile.
5. The method of claim 1, wherein the microwave reaction is at a temperature of 80 ℃.
6. The hydrophobic material obtained by the production method according to any one of claims 1 to 5.
7. The hydrophobic material of claim 6, wherein the hydrophobic material has a contact angle value with water of 140 ± 5 °.
8. An oil-water separation filter plate made of the hydrophobic material according to claim 6.
9. An oil-water separation column prepared from the hydrophobic material according to claim 6.
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