CN114958095A - Super-hydrophobic bacterial cellulose and green preparation method and application thereof - Google Patents
Super-hydrophobic bacterial cellulose and green preparation method and application thereof Download PDFInfo
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- CN114958095A CN114958095A CN202210451269.6A CN202210451269A CN114958095A CN 114958095 A CN114958095 A CN 114958095A CN 202210451269 A CN202210451269 A CN 202210451269A CN 114958095 A CN114958095 A CN 114958095A
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Abstract
The invention relates to super-hydrophobic bacterial cellulose and a green preparation method and application thereof, belonging to the field of super-hydrophobic functional materials. Placing the bacterial cellulose hydrogel into water for swelling, and then soaking the bacterial cellulose hydrogel into absolute ethyl alcohol to replace the water in the bacterial cellulose hydrogel with the absolute ethyl alcohol so as to obtain the bacterial cellulose gel of an absolute ethyl alcohol phase; dispersing the silicon dioxide nano particles in absolute ethyl alcohol to obtain super-hydrophobic dispersion liquid; and adding the bacterial cellulose gel of an absolute ethyl alcohol phase into the super-hydrophobic dispersion liquid to enable the silicon dioxide nano particles and hydroxyl groups on the bacterial cellulose to form hydrogen bonds, so as to obtain the super-hydrophobic bacterial cellulose. The super-hydrophobic bacterial cellulose prepared by the method has excellent super-hydrophobic performance and acid, alkali and salt and other liquid corrosion resistance; the soaking time exceeds half a year and still shows excellent super-hydrophobic performance.
Description
Technical Field
The invention relates to the field of super-hydrophobic functional materials, in particular to super-hydrophobic bacterial cellulose and a green preparation method and application thereof.
Background
The super-hydrophobic material is a functional material with a contact angle between the surface of the material and water of more than 150 degrees and a rolling angle of less than 10 degrees, and therefore, the super-hydrophobic material can be widely applied to the fields of water resistance, ice resistance, fog resistance and the like.
The super-hydrophobic nano particles are prepared into the super-hydrophobic coating, and the super-hydrophobic coating is used as the simplest, rapid and low-cost method for preparing the super-hydrophobic material, so that the super-hydrophobic coating is widely applied, but the super-hydrophobic nano particles cannot be well adhered to the surface of the material by simple coating, and the prepared super-hydrophobic material is extremely easy to damage by external force. In order to solve the problem of adhesion of the superhydrophobic nanoparticles, scientists invented a chemical vapor deposition method and a self-assembly method to prepare the superhydrophobic material with firmer superhydrophobic performance, but the synthesis process involved in the preparation process is complicated, a large amount of organic reagents are used, the cost is high, and environmental pollution is easily caused. The firm super-hydrophobic material can be prepared by etching a firm microstructure on the surface of the material through a photoetching technology, and the preparation process does not have the pollution of chemical reagents to the environment, but needs a photoetching machine, and has high cost. In summary, the current superhydrophobic materials cannot combine strong superhydrophobic performance with low cost and the preparation process is environmentally friendly.
Disclosure of Invention
The invention solves the problems that the existing super-hydrophobic material cannot give consideration to firm super-hydrophobic performance, low cost and environment friendliness in the preparation process, and provides a method for preparing a bacterial cellulose nano-particle-reinforced silicon dioxide nano-particle by using bacterial cellulose as a base material and loading silicon dioxide nano-particles into a bacterial cellulose fiber network structure. The preparation process of the super-hydrophobic bacterial cellulose only relates to three materials of absolute ethyl alcohol, silicon dioxide nano particles and bacterial cellulose, the cost is low, and the preparation process hardly causes environmental pollution.
According to a first aspect of the invention, a preparation method of super-hydrophobic bacterial cellulose is provided, which comprises the following steps:
(1) placing the bacterial cellulose hydrogel into water for swelling, and then soaking the bacterial cellulose hydrogel into absolute ethyl alcohol to replace the water in the bacterial cellulose hydrogel with the absolute ethyl alcohol so as to obtain the bacterial cellulose gel of an absolute ethyl alcohol phase;
(2) dispersing the silicon dioxide nano particles in absolute ethyl alcohol to obtain super-hydrophobic dispersion liquid; and (2) adding the anhydrous ethanol phase bacterial cellulose gel obtained in the step (1) into the super-hydrophobic dispersion liquid, so that hydrogen bonds are formed between the silicon dioxide nanoparticles and hydroxyl groups on the bacterial cellulose, and the super-hydrophobic bacterial cellulose is obtained.
Preferably, in the step (1), the bacterial cellulose hydrogel is placed in boiling water to be boiled and swelled so as to accelerate the swelling speed of the bacterial cellulose hydrogel.
Preferably, the silica nanoparticles are 50 ± 10nm in size.
Preferably, the concentration of the silica nanoparticles in the superhydrophobic dispersion is 1 wt% to 5 wt%.
Preferably, in the step (2), the mass ratio of the bacterial cellulose gel of the anhydrous ethanol phase to the super-hydrophobic dispersion is (0.2-1): 1.
according to another aspect of the invention, the super-hydrophobic bacterial cellulose prepared by any one of the preparation methods is provided.
Preferably, the thickness of the super-hydrophobic bacterial cellulose is 20-40 um.
According to another aspect of the invention, the application of the super-hydrophobic bacterial cellulose in super-hydrophobic materials is provided.
Generally, compared with the prior art, the technical scheme conceived by the invention mainly has the following technical advantages:
(1) the average contact angle of the prepared super-hydrophobic bacterial cellulose to water can reach 163.98 degrees, the contact angles of the prepared super-hydrophobic bacterial cellulose to concentrated hydrochloric acid, a 5% NaOH solution, a 10% NaCl solution and a standard PBS solution are respectively 159.25 degrees, 159.00 degrees, 161.41 degrees and 160.23 degrees, and the super-hydrophobic bacterial cellulose shows excellent super-hydrophobic performance and performances of resisting corrosion of acid, alkali, salt and other liquids.
(2) After the super-hydrophobic bacterial cellulose prepared by the method is soaked in water for more than 6 months, the contact angles of water, concentrated hydrochloric acid, a 5% NaOH solution, a 10% NaCl solution and a standard PBS solution are 158.91 degrees, 158.13 degrees, 160 degrees, 157.48 degrees and 162.44 degrees respectively, and the super-hydrophobic bacterial cellulose still shows excellent super-hydrophobic performance after being soaked for more than half a year.
(3) The super-hydrophobic bacterial cellulose prepared by the method has an average contact angle of 158.87 degrees after being circularly rubbed for 100 times under the load of 10N.
(4) In the production process of the super-hydrophobic bacterial cellulose, only three substances, namely natural bacterial cellulose, absolute ethyl alcohol and silicon dioxide nanoparticles, are used, and are all harmless substances, so that the method is environment-friendly, and meanwhile, the natural bacterial cellulose can be naturally degraded without generating pollutants.
Drawings
FIG. 1 is a schematic diagram of a green preparation process of super-hydrophobic bacterial cellulose according to the present invention.
FIG. 2 is a graph representing the contact angle of superhydrophobic bacterial cellulose to water.
FIG. 3 is a statistical data of the contact angles of the superhydrophobic bacterial cellulose and the standard PBS after the superhydrophobic bacterial cellulose is soaked in water for more than 6 months.
FIG. 4 is a picture of the surface microstructure characterization of superhydrophobic bacterial cellulose.
FIG. 5 is a droplet of superhydrophobic bacterial cellulose surface.
FIG. 6 is a photograph of superhydrophobic bacterial cellulose prepared on a large scale.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention provides super-hydrophobic bacterial cellulose which is prepared by compounding natural bacterial cellulose with silicon dioxide nanoparticles and has the characteristics of excellent super-hydrophobic property and firmness.
The invention provides a novel super-hydrophobic material taking bacterial cellulose as a base material, which comprises nano fibers and silicon dioxide nano particles in a microstructure, wherein the silicon dioxide nano particles are attached to a fiber network structure of the bacterial cellulose and filled in pores of the fiber network structure.
The surface of the super-hydrophobic bacterial cellulose prepared by the method contains a large number of silicon dioxide nano-particles, and the fiber networks of the silicon dioxide nano-particles and the bacterial cellulose are obviously interwoven.
The thickness of the super-hydrophobic bacterial cellulose prepared by the method is 20-40 um.
In some embodiments, the preparation process of the superhydrophobic bacterial cellulose of the invention comprises:
(1) boiling and swelling the bacterial cellulose hydrogel with boiling water;
(2) soaking the boiled and swollen bacterial cellulose hydrogel in absolute ethyl alcohol;
(3) repeating the step (2) until the water content of the bacterial cellulose is completely replaced by the absolute ethyl alcohol to obtain the bacterial cellulose gel of an absolute ethyl alcohol phase, and taking out for later use;
(4) dispersing the silicon dioxide nano particles in an absolute ethyl alcohol solution to prepare a super-hydrophobic dispersion liquid for later use;
(5) putting the absolute ethyl alcohol phase bacterial cellulose into the super-hydrophobic dispersion liquid, and performing ultrasonic treatment and oscillation to obtain bacterial cellulose gel containing silicon dioxide nano-particles;
(6) and taking out the gel obtained in the last step, and placing the gel on a flat plate for drying to obtain the final super-hydrophobic bacterial cellulose.
In some embodiments, the bacterial cellulose hydrogel in step (1) of the present invention is a 1mm thick film, and has a thickness of 2mm after boiling, and the boiling is performed to sufficiently open the fiber network structure of the bacterial cellulose.
The steps (2) and (3) of the invention aim to obtain the bacterial cellulose gel of the absolute ethyl alcohol phase by repeatedly soaking the bacterial cellulose hydrogel in the absolute ethyl alcohol solution and diluting the water content of the cellulose hydrogel one step by one step.
In some embodiments, in each soaking step (2) and (3), when the mass ratio of the bacterial cellulose gel to the absolute ethyl alcohol is 0.5, the soaking step is repeated three times to replace the water in the bacterial cellulose sufficiently to obtain an absolute ethyl alcohol phase to obtain the bacterial cellulose gel. The water content of the solution after the last soaking was checked with anhydrous copper sulfate powder.
In some embodiments, the mass ratio of the silica nanoparticles to the absolute ethyl alcohol used in step (4) of the present invention is 1: 2, 25g of silica nanoparticles and 1L of absolute ethanol are generally used.
In some embodiments, in step (5) of the present invention, the mass ratio of the bacterial cellulose gel and the superhydrophobic dispersion of the anhydrous ethanol phase is 1: 2, performing ultrasonic operation when the cellulose gel is just put in, which is beneficial to the dispersion of the silicon dioxide nano particles, wherein the ultrasonic time is 1h, and the oscillation time is 12 h.
In some embodiments, the silica nanoparticles used in the present invention are 50 ± 10nm in size.
Example 1
The embodiment of the application also provides a preparation method of the super-hydrophobic bacterial cellulose, which specifically comprises the following steps as shown in fig. 1:
step 1: boiling and swelling natural bacterial cellulose gel (a)
And 2, step: soaking the boiled and swollen natural bacterial cellulose gel (a) in an absolute ethyl alcohol solution.
And step 3: and (c) repeating the step (2) until the water phase in the bacterial cellulose is changed into an alcohol phase, so as to obtain the bacterial cellulose gel (b) with an absolute alcohol phase.
And 4, step 4: dispersing the silica nanoparticles (e) in the anhydrous ethanol (f) to obtain a superhydrophobic dispersion (g).
And 5: and (3) placing the bacterial cellulose gel (b) of the absolute ethyl alcohol phase into the super-hydrophobic dispersion liquid (g), and performing ultrasonic oscillation treatment to obtain the bacterial cellulose gel (c) loaded with the silicon dioxide nanoparticles.
Step 6: and (3) placing the bacterial cellulose gel (c) loaded with the silicon dioxide nano particles on a flat plate for drying to obtain the final super-hydrophobic bacterial cellulose.
Example 2
On the other hand, the contact angle test of the prepared superhydrophobic bacterial cellulose is performed in the embodiment of the application, and as shown in fig. 2, the contact angle test result for water is 165.5 °.
According to the invention, the prepared super-hydrophobic bacterial cellulose can resist corrosion of acid-base salt and standard PBS, and contact angle data of water, concentrated hydrochloric acid, a 5% NaOH solution, a 10% NaCl solution and a standard PBS solution are measured on the super-hydrophobic bacterial cellulose in the embodiment of the application, as shown in FIG. 3.
In the examples of the present application, the contact angles of water, concentrated hydrochloric acid, 5% NaOH solution, 10% NaCl solution, and standard PBS solution were 163.98 °, 159.25 °, 159.00 °, 161.41 °, and 160.23 °, respectively.
Example 3
According to the invention, the prepared super-hydrophobic bacterial cellulose still has excellent super-hydrophobic performance after being soaked in an aqueous solution for more than 6 months. According to the embodiment of the application, the prepared super-hydrophobic bacterial cellulose is soaked in water for 6 months and then taken out, and contact angle data of water, concentrated hydrochloric acid, a 5% NaOH solution, a 10% NaCl solution and a standard PBS solution are measured on the super-hydrophobic bacterial cellulose, as shown in FIG. 3.
In the examples of the present application, the contact angles of water, concentrated hydrochloric acid, 5% NaOH solution, 10% NaCl solution, and standard PBS solution were 158.91 °, 158.13 °, 160 °, 157.48 °, and 162.44 °, respectively.
Example 4
According to the invention, the prepared superhydrophobic bacterial cellulose is subjected to SEM characterization to obtain a surface microstructure diagram, as shown in FIG. 4, the prepared superhydrophobic bacterial cellulose surface microstructure comprises nanofibers and silica nanoparticles, the silica nanoparticles are attached to a fiber network structure of the bacterial cellulose and fill gaps of the fiber network structure, the silica nanoparticles and the fiber network of the bacterial cellulose are interwoven to provide a guarantee for firm superhydrophobic performance, and the prepared superhydrophobic bacterial cellulose is distributed in the thickness of 20-40 um.
Example 5
According to the invention, the prepared super-hydrophobic bacterial cellulose has excellent super-hydrophobic performance, and in the embodiment of the application, the liquid drops are placed on the surface of the super-hydrophobic bacterial cellulose, as shown in fig. 5, the liquid drops are gathered into one piece on the surface of the super-hydrophobic bacterial cellulose but are not adhered to the surface of the super-hydrophobic bacterial cellulose, so that the excellent super-hydrophobic performance is shown.
Example 6
According to the present invention, the preparation method of the superhydrophobic bacterial cellulose is simple and suitable for mass production, and the present embodiment performs mass production of the superhydrophobic bacterial cellulose under laboratory conditions, as shown in fig. 6, the superhydrophobic bacterial cellulose produced in a laboratory within 4 days.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A preparation method of super-hydrophobic bacterial cellulose is characterized by comprising the following steps:
(1) placing the bacterial cellulose hydrogel into water for swelling, and then soaking the bacterial cellulose hydrogel into absolute ethyl alcohol to replace the water in the bacterial cellulose hydrogel with the absolute ethyl alcohol so as to obtain the bacterial cellulose gel of an absolute ethyl alcohol phase;
(2) dispersing the silicon dioxide nano particles in absolute ethyl alcohol to obtain super-hydrophobic dispersion liquid; and (2) adding the anhydrous ethanol phase bacterial cellulose gel obtained in the step (1) into the super-hydrophobic dispersion liquid, so that hydrogen bonds are formed between the silicon dioxide nanoparticles and hydroxyl groups on the bacterial cellulose, and the super-hydrophobic bacterial cellulose is obtained.
2. The method for preparing superhydrophobic bacterial cellulose according to claim 1, wherein in the step (1), the bacterial cellulose hydrogel is placed in boiling water to be boiled and swelled so as to increase the swelling speed of the bacterial cellulose hydrogel.
3. The method for preparing superhydrophobic bacterial cellulose of claim 1, wherein the silica nanoparticle size is 50 ± 10 nm.
4. The method for preparing superhydrophobic bacterial cellulose according to claim 1 or 3, wherein the concentration of the silica nanoparticles in the superhydrophobic dispersion is 1 wt% to 5 wt%.
5. The method for preparing superhydrophobic bacterial cellulose according to claim 1, wherein in the step (2), the mass ratio of the bacterial cellulose gel of the anhydrous ethanol phase to the superhydrophobic dispersion is (0.2-1): 1.
6. the superhydrophobic bacterial cellulose prepared by the preparation method according to any one of claims 1 to 5.
7. The superhydrophobic bacterial cellulose of claim 6, wherein the superhydrophobic bacterial cellulose has a thickness of 20-40 um.
8. Use of the superhydrophobic bacterial cellulose of claim 6 or 7 for a superhydrophobic material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210451269.6A CN114958095A (en) | 2022-04-26 | 2022-04-26 | Super-hydrophobic bacterial cellulose and green preparation method and application thereof |
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| CN202210451269.6A CN114958095A (en) | 2022-04-26 | 2022-04-26 | Super-hydrophobic bacterial cellulose and green preparation method and application thereof |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880410A (en) * | 2010-07-21 | 2010-11-10 | 武汉大学 | High-strength transparent cellulose material and preparation method thereof |
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- 2022-04-26 CN CN202210451269.6A patent/CN114958095A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880410A (en) * | 2010-07-21 | 2010-11-10 | 武汉大学 | High-strength transparent cellulose material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| JIAN HE等: ""Superelastic and superhydrophobic bacterial cellulose/silica aerogels with hierarchical cellular structure for oil absorption and recovery"", 《JOURNAL OF HAZARDOUS MATERIALS》 * |
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