CN113600143A - Super-hydrophobic magnetic biomass material based on beeswax and preparation method and application thereof - Google Patents
Super-hydrophobic magnetic biomass material based on beeswax and preparation method and application thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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Abstract
The invention discloses a preparation method of a super-hydrophobic magnetic biomass material based on beeswax, which takes the biomass material with adsorbability as a core, and sequentially wraps ferroferric oxide and beeswax on the surface of the biomass material by utilizing the adhesive action of a thermoplastic resin adhesive, so as to prepare the super-hydrophobic magnetic biomass material, wherein the contact angles of the super-hydrophobic magnetic biomass material prepared by the preparation method in a hydrophobic performance test are all larger than 150 degrees. The preparation method is simple and easy to implement, has low cost, can quickly adsorb a large amount of organic pollutants, can be recycled and reused through magnetism, and can be applied to environmental pollution treatment.
Description
Technical Field
The invention belongs to the technical field of preparation of biological functional materials, and particularly relates to a beeswax-based super-hydrophobic magnetic biomass material and a preparation method and application thereof.
Background
With the progress of human science and technology and the development of society, environmental pollution becomes a problem which needs to be paid attention more and more. Among the various pollutants, organic pollution is a problem that is closely related to human life. Such as leakage of various organic substances and crude oil, river and sea pollution. Adsorption materials capable of separating organic materials and crude oil from water have received much attention from researchers. A wide variety of adsorbent materials have been developed, such as superhydrophobic sponges, superhydrophobic cotton, superhydrophobic wood, and the like. Although these materials have been used, they have some drawbacks, more or less, in terms of ease of separation, biocompatibility and cost. Therefore, it is necessary to prepare an adsorbent having selective adsorption ability, large adsorption capacity, easy recovery, low cost and good reproducibility. The biomass material is a common adsorption material, can be prepared into super-hydrophobic oil absorption wood chips by modifying the surface of the biomass material, and has the advantages of low cost and recoverability. A method for preparing super-hydrophobic wood chips by using wood chips was published by redley of northeast forestry university in 2015. Before preparation, the wood chips are thoroughly washed by ultrapure water, absolute ethyl alcohol and ultrapure water, then the wood chips are subjected to lignin and hemicellulose removal by sodium hydroxide, and the lignocellulose is obtained after bleaching by hydrogen peroxide. Then, taking ethyl orthosilicate as a silicon source and ammonia water as a catalyst, preparing silica particles with uniform particle size by adopting a sol-gel technology, loading the silica particles on the surface of a wood fiber bundle, and obtaining the super-hydrophobic super-oleophylic wood chip fiber through self-assembly of a monomolecular layer of hexadecyl trimethoxy silane on the surface of the silica particles. The modified wood chips only have the function of absorbing oil, so that the wood chips adsorbed with pollutants need to be recovered in the actual pollution treatment application, and the wood chips only with super-hydrophobicity are difficult to recover in a wide application environment. And the coating silicon dioxide of the super-hydrophobic wood chips is not firm enough, the preparation time is long, and the process is complex. Therefore, a simple and feasible method is needed to prepare the green environment-friendly multifunctional super-hydrophobic biomass material, which not only has the oil absorption performance, but also is easy to recover and reuse.
Disclosure of Invention
The invention aims to provide a beeswax-based super-hydrophobic magnetic biomass material, and a preparation method and application thereof, aiming at the problems, the preparation cost of the super-hydrophobic magnetic biomass material is low, the process is simple, and the super-hydrophobic magnetic biomass material can quickly adsorb a large amount of organic pollutants and can be recycled and reused through magnetism.
The technical content of the invention is as follows:
a preparation method of a super-hydrophobic magnetic biomass material based on beeswax comprises the steps of taking a biomass material with adsorbability as a core, and sequentially coating ferroferric oxide and beeswax on the surface of the biomass material by utilizing the adhesive effect of a thermoplastic resin adhesive, so as to prepare the super-hydrophobic magnetic biomass material.
In some embodiments of the preparation method of the present invention, the preparation method comprises the steps of:
the method comprises the following steps: cleaning and drying the biomass material with adsorbability, and screening to obtain the biomass material with a certain uniform granularity;
step two: uniformly dispersing a thermoplastic resin adhesive in an organic solvent, adding the biomass material with a certain uniform granularity obtained in the step one, performing ultrasonic mixing uniformly in a closed space, adding a proper amount of ferroferric oxide, continuing performing ultrasonic treatment for a certain time, filtering, and removing the organic solvent through volatilization to obtain a ferroferric oxide-coated biomass material;
step three: and (3) thermally dissolving beeswax in ethanol, adding the ferroferric oxide coated biomass material obtained in the step two, maintaining the mixture for a certain time in a heating state, cooling the mixture to enable the beeswax to be gradually separated out and coated on the ferroferric oxide coated biomass material, and filtering and drying the mixture to obtain the beeswax coated ferroferric oxide super-hydrophobic biomass material.
In some embodiments of the methods of the present invention, the biomass material comprises one or more of corn stover, wheat straw, wood chips, corn cobs, and other crop stover and wood kernels and pericarp.
In some embodiments of the preparation method of the present invention, the thermoplastic resin binder is one or more of hydroxy acrylic resin, polyacrylic resin, polyvinyl acetate resin, polyvinyl alcohol and polyamide.
In some embodiments of the preparation method of the present invention, in the first step, the particle size of the sieved biomass material is 20 to 60 meshes; in the second step, the particle size of the ferroferric oxide is 40-80 nm.
In some embodiments of the preparation method of the present invention, in the second step, the organic solvent includes one or more of xylene, toluene, benzene and petroleum ether.
In some embodiments of the preparation method of the present invention, the raw materials are added in amounts by mass of the biomass material: thermoplastic resin binder: ferroferric oxide: beeswax = 1: 0.3-0.8: 0.05-0.2: 0.05 to 0.2.
The invention also discloses a super-hydrophobic magnetic biomass material prepared by the preparation method.
Further, the contact angle of the super-hydrophobic magnetic biomass material in a hydrophobic property test is larger than 150 degrees.
The invention also discloses an oil-water separation method, which comprises the step of putting the super-hydrophobic magnetic biomass material into an oil-water mixture for oil product adsorption to realize oil-water separation.
Due to the adoption of the scheme, the invention has the following technical effects: the mechanism of the invention is that the adhesive is firstly absorbed and dispersed on the surface of the biomass material by utilizing the action of hydrogen bonds formed by hydroxyl on the surface of the adhesive, lignin on the surface of the biomass and hydroxyl on cellulose, then the hydrogen bonds are formed by the hydroxyl on the surface of the adhesive and the hydroxyl on the surface of the nano ferroferric oxide, the nano ferroferric oxide is firmly absorbed on the surface of the adhesive, the free fatty acid in the beeswax and the hydroxyl in the free fatty alcohol compound can inwards form the hydrogen bonds with the adhesive and the hydroxyl on the surface of the ferroferric oxide, the free fatty acid in the beeswax and the alkyl of the free fatty alcohol are outwards directionally arranged to form a super-hydrophobic structure, the adhesive plays the role of fixing the ferroferric oxide and the beeswax, the ferroferric oxide has magnetism, and the carbon chains of the beeswax have the super-hydrophobic action after being directionally arranged outwards. In the process of the invention, beeswax is heated and dissolved in ethanol solution to react with the biomass material, so that a thermoplastic resin adhesive is adopted, and the adhesive is softened and bonded when being heated and is hardened after being cooled to have certain strength. Has the advantages of impact resistance, good peel strength and initial adhesion, convenient use and repeated adhesion.
Drawings
FIG. 1 is a contact angle diagram of super-hydrophobic magnetic corn stover;
FIG. 2 is a scanning electron micrograph of the surface of superhydrophobic magnetic corn stalk;
FIG. 3 is a photograph of oil-water separation using magnetism of super-hydrophobic magnetic corn stover.
Detailed Description
All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations of features and/or steps that are mutually exclusive.
Any feature disclosed in this specification may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.
Examples
The invention discloses a preparation method of a super-hydrophobic magnetic biomass material based on beeswax, which takes the biomass material with adsorbability as a core, and sequentially wraps ferroferric oxide and beeswax on the surface of the biomass material by using the adhesive action of a thermoplastic resin adhesive, thereby preparing the super-hydrophobic magnetic biomass material.
In some embodiments, the preparation method comprises the following steps:
the method comprises the following steps: cleaning and drying the biomass material with adsorbability, and screening to obtain the biomass material with a certain uniform granularity;
step two: uniformly dispersing a thermoplastic resin adhesive in an organic solvent, adding the biomass material with a certain uniform granularity obtained in the step one, performing ultrasonic mixing uniformly in a closed space, adding a proper amount of ferroferric oxide, continuing performing ultrasonic treatment for a certain time, filtering, and removing the organic solvent through volatilization to obtain a ferroferric oxide-coated biomass material;
step three: and (3) thermally dissolving beeswax in ethanol, adding the ferroferric oxide coated biomass material obtained in the step two, maintaining the mixture for a certain time in a heating state, cooling the mixture to enable the beeswax to be gradually separated out and coated on the ferroferric oxide coated biomass material, and filtering and drying the mixture to obtain the beeswax coated ferroferric oxide super-hydrophobic biomass material.
In some embodiments, the biomass material comprises one or more mixtures of stalks of agricultural crops such as corn stover, wheat straw, wood chips, and corn cobs, and wood kernels and pericarps. The biomass material is selected mainly on the basis of the characteristic that the biomass material is easy to obtain and has a porous adsorption structure, can well adsorb organic matters, and can be popularized in a large scale in application.
In some embodiments, the thermoplastic resin binder is one or more of hydroxy acrylic resin, polyacrylic resin, polyvinyl acetate resin, polyvinyl alcohol, polyamide, and the like. Thermoplastic resin adhesives are a class of adhesives that are softened by heating, have good adhesion, and solidify upon cooling.
In some embodiments, in the first step, the particle size of the sieved biomass material is 20-60 meshes; in the second step, the particle size of the ferroferric oxide is 40-80 nm, the biomass particles are large, the specific surface area is small, the particles are small, the specific surface area is large, the particles are too small to be operated easily, the particle size of the ferroferric oxide is 40-80 nm, the particles are large, the uniform adhesion is not easy, the particles are small, and the cost is high.
In some embodiments, in the second step, the organic solvent includes one or more of xylene, toluene, benzene and petroleum ether. The organic solvent is selected mainly on the basis of the function of being able to dissolve and disperse the corresponding thermoplastic resin binder on the one hand, without damaging the biomass material on the other hand, and of being subsequently easily removable by evaporation.
In some embodiments, the raw materials are added in amounts by mass of the biomass material: thermoplastic resin binder: ferroferric oxide: beeswax = 1: 0.3-0.8: 0.05-0.2: 0.05-0.2, the surface of the biomass is uneven, if the using amount of the adhesive is too much, the roughness of the surface of the biomass is reduced, the specific surface is reduced, the performance is reduced, the using amount is less, the coating is not uniform, a preferable range is obtained through experiments, the influence of other ferroferric oxides and beeswax is the same, and the determination of the preferable range can also be obtained through experiments.
The following specific example implementation was carried out using the preparation method of this example:
example 1
(1) Washing the crushed corn stalks with ethanol for 3 times, and drying for 24 hours at 50 ℃. Then sieving the corn straw particles by a screen to obtain corn straw particle materials with the particle size of 40-60 meshes;
(2) adding 50mL of dimethylbenzene and 0.3 g of hydroxyl acrylic resin adhesive into a cleaned and dried 250mL beaker, placing the beaker in an ultrasonic cleaner for 5 minutes, adding 1 g of 40-60-mesh corn straw material, sealing the beaker by using a preservative film to prevent dimethylbenzene from volatilizing, carrying out ultrasonic treatment for 10 minutes, adding 0.2 g of 60-80nm ferroferric oxide, continuing ultrasonic treatment for 20 minutes, filtering, and volatilizing dimethylbenzene in a fume hood to obtain the ferroferric oxide coated corn straw material.
(3) Adding 50mL of absolute ethyl alcohol and 0.2 g of beeswax into a beaker, heating to 75 ℃ under magnetic stirring, completely dissolving the beeswax in the absolute ethyl alcohol, adding 1.5 g of ferroferric oxide coated corn straw material prepared in the second step, maintaining for 5 minutes, gradually cooling to room temperature, gradually separating out the beeswax, coating the beeswax on the surface of the magnetic corn straw material, filtering, and drying the obtained material in a 50-DEG oven for 24 hours to obtain the beeswax coated ferroferric oxide super-hydrophobic corn straw material.
Example 2
(1) Washing the crushed wheat straws with ethanol for 3 times, and drying for 24 hours at 50 ℃. Then sieving with a screen to obtain wheat straw material with the particle size of 20-40 meshes;
(2) adding 50mL of benzene and 0.5 g of polypropylene resin adhesive into a cleaned and dried 250mL beaker, placing the beaker in an ultrasonic cleaner for ultrasonic treatment for 5 minutes, adding 1 g of 20-40 mesh wheat straw material, sealing the beaker by using a preservative film to prevent benzene from volatilizing, performing ultrasonic treatment for 10 minutes, adding 0.15 g of 40-60nm ferroferric oxide, continuing ultrasonic treatment for 20 minutes, filtering, and volatilizing the solvent benzene in a fume hood to obtain the ferroferric oxide coated wheat straw material.
(3) Adding 50mL of absolute ethyl alcohol and 0.09 g of beeswax into a beaker, heating to 75 ℃ under magnetic stirring, completely dissolving the beeswax in the absolute ethyl alcohol, adding 1.65 g of ferroferric oxide coated wheat straw material prepared in the second step, maintaining for 5 minutes, gradually cooling to room temperature, gradually separating out the beeswax, coating the beeswax on the surface of a magnetic wheat straw material, filtering, and drying the obtained material in a 50-DEG oven for 24 hours to obtain the beeswax coated ferroferric oxide super-hydrophobic wheat straw material.
Example 3
(1) And washing the crushed wood chips with ethanol for 3 times, and drying at 50 ℃ for 24 hours. Then screening by using a screen to obtain wood dust particle materials with the particle size of 40-60 meshes;
(2) adding 50mL of methylbenzene and 0.8 g of polyamide resin adhesive into a cleaned and dried 250mL beaker, placing the beaker in an ultrasonic cleaning instrument for ultrasonic treatment for 5 minutes, adding 1 g of wood chip material with 40-60 meshes, sealing the opening by using a preservative film to prevent the methylbenzene from volatilizing, performing ultrasonic treatment for 10 minutes, adding 0.09 g of 50-80nm ferroferric oxide, continuing ultrasonic treatment for 20 minutes, filtering, and volatilizing the methylbenzene in a fume hood to obtain the wood chip material wrapped by the ferroferric oxide.
(3) Adding 50mL of absolute ethyl alcohol and 0.15 g of beeswax into a beaker, heating to 75 ℃ under magnetic stirring, completely dissolving the beeswax in the absolute ethyl alcohol, adding 1.89 g of ferroferric oxide coated sawdust material prepared in the second step, maintaining for 5 minutes, gradually cooling to room temperature, gradually separating out the beeswax, coating the beeswax on the surface of a magnetic sawdust material, filtering, and drying the obtained material in a 50-DEG oven for 24 hours to obtain the beeswax coated ferroferric oxide super-hydrophobic sawdust material.
Example 4
(1) Washing the crushed corncobs with ethanol for 3 times, and drying at 50 ℃ for 24 hours. Then sieving by a screen to obtain corncob granular materials with the grain diameter of 30-50 meshes;
(2) adding 50mL of petroleum ether with the boiling point of 60-90 ℃ and 0.4 g of polyvinyl acetate resin adhesive into a cleaned and dried 250mL beaker, placing the beaker in an ultrasonic cleaner for ultrasonic treatment for 5 minutes, adding 1 g of corn core material with the granularity of 30-50 meshes, sealing the opening by using a preservative film to prevent the petroleum ether from volatilizing, performing ultrasonic treatment for 10 minutes, adding 0.16 g of 60-80nm ferroferric oxide, continuing ultrasonic treatment for 20 minutes, filtering, volatilizing the petroleum ether in a fume hood to obtain the ferroferric oxide coated corn core material.
(3) Adding 50mL of absolute ethyl alcohol and 0.2 g of beeswax into a beaker, heating to 75 ℃ under magnetic stirring, completely dissolving the beeswax in the absolute ethyl alcohol, adding 1.56 g of ferroferric oxide coated corncob material prepared in the second step, maintaining for 5 minutes, gradually cooling to room temperature, gradually separating out the beeswax, coating the beeswax on the surface of the magnetic corncob material, filtering, and drying the obtained material in a 50-DEG oven for 24 hours to obtain the beeswax coated ferroferric oxide super-hydrophobic wood chip material.
The super-hydrophobic magnetic biomass materials prepared in examples 1 to 4 are subjected to contact angle test on hydrophobic property, the contact angles of the obtained materials are all larger than 150 degrees, the materials have excellent super-hydrophobic property, and as shown in fig. 1, the contact angle of the super-hydrophobic magnetic corn straw obtained in example 1 is 160.1 degrees. In addition, fig. 2 is a scanning electron micrograph of example 1, and it can be seen from fig. 2 that the superhydrophobic magnetic biomass material has a rough surface, which also proves that it has a better hydrophobic property.
The super-hydrophobic magnetic biomass materials prepared in examples 1 to 4 respectively show excellent adsorption performance and magnetic effect after being subjected to oil-water separation tests. As shown in fig. 3, the super-hydrophobic magnetic biomass material of example 1 can well adsorb organic matters, has a good magnetic effect, and can be beneficial to material recovery, and such a material can be used in the field of environmental protection.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
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