CN115286894B - Epoxy resin block-shaped super-hydrophobic material with photo-thermal effect and abrasion resistance - Google Patents
Epoxy resin block-shaped super-hydrophobic material with photo-thermal effect and abrasion resistance Download PDFInfo
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- CN115286894B CN115286894B CN202111452179.0A CN202111452179A CN115286894B CN 115286894 B CN115286894 B CN 115286894B CN 202111452179 A CN202111452179 A CN 202111452179A CN 115286894 B CN115286894 B CN 115286894B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/17—Amines; Quaternary ammonium compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention belongs to the field of super-hydrophobic materials, and in particular relates to an epoxy resin block-shaped super-hydrophobic material with a photo-thermal effect and abrasion resistance, and the preparation process comprises the following steps: dissolving bisphenol A epoxy resin, a curing agent and dopamine hydrochloride into a hydrophobic silica sol solution together to obtain an epoxy mixed solution; placing the epoxy mixed solution in a reaction container, and heating to a reflux state for reaction to obtain an undried superhydrophobic bulk material; and drying the undried superhydrophobic block material to obtain the epoxy resin block superhydrophobic material with photo-thermal effect and abrasion resistance. The obtained blocky super-hydrophobic material also has a photo-thermal effect through the blending reaction of dopamine hydrochloride and epoxy resin, and the surface temperature of the material is rapidly increased within 3 min under the irradiation of infrared light with the wave band of 808nm, so that the material has wide application prospect in photo-thermal sterilization, anti-icing and deicing, heavy oil separation and the like.
Description
Technical Field
The invention belongs to the field of super-hydrophobic materials, and particularly relates to an epoxy resin block-shaped super-hydrophobic material with a photo-thermal effect and abrasion resistance.
Background
Superhydrophobic materials refer to materials that have a contact angle of greater than 150 ° with a solid surface, and if they have a roll angle of less than 10 °, then the materials can be referred to as superhydrophobic surfaces in a low adhesion state. Two requirements, i.e., micro-nano coarse structure and low surface energy characteristics, are required for artificially preparing the super-hydrophobic material. However, the micro-nano coarse structure and the low surface energy property of which the superhydrophobic property is highly dependent are easily damaged by the influence of the outside, and the superhydrophobic property is easily lost. Therefore, how to improve the durability of materials and extend their life cycle is a critical problem that is urgently needed to be solved by current superhydrophobic materials.
Based on the special wettability of the surface, the super-hydrophobic material has good application potential in the fields of ice resistance, oil-water separation and the like. Although the materials have better capability of delaying icing and oil-water separation at the initial stage of use due to the unique micro-nano structure and micro-pores inside the materials. However, in a complex environment in nature, tiny water mist inevitably nucleates in micro-nano pores, and then icing occurs. The heating method is a safe and reliable deicing method with simple operation, but the externally-added heating deicing equipment is often limited by the space, the ambient temperature and other aspects, and the energy consumption cost is increased. In addition, the super-hydrophobic material has poor adsorption capacity to high-viscosity crude oil and low recovery rate when adsorbing oily liquid. Therefore, the common super-hydrophobic material is difficult to be an ideal material for efficiently absorbing crude oil.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art and provides an epoxy resin block-shaped super-hydrophobic material with photo-thermal effect and abrasion resistance.
In order to achieve the above object, the present invention provides the following technical solutions:
the preparation process of the epoxy resin block-shaped super-hydrophobic material with the photo-thermal effect and abrasion resistance comprises the following steps:
dissolving bisphenol A epoxy resin, a curing agent and dopamine hydrochloride into a hydrophobic silica sol solution together to obtain an epoxy mixed solution;
placing the epoxy mixed solution in a reaction container, and heating to a reflux state for reaction to obtain an undried superhydrophobic bulk material;
and drying the undried superhydrophobic block material to obtain the epoxy resin block superhydrophobic material with photo-thermal effect and abrasion resistance.
As a preferred embodiment of the present invention, the preparation process of the hydrophobic silica sol solution is as follows: dropwise adding tetraethoxysilane into ethanol, stirring, dropwise adding hexamethyldisilazane, stirring, adding distilled water, and continuously stirring to obtain a hydrophobic silica sol solution.
As a preferred scheme of the invention, the newly prepared hydrophobic silica sol solution is used for preparing the epoxy mixed solution after being kept stand for 5-10d at room temperature.
As a preferable scheme of the invention, the volume ratio of the tetraethoxysilane to the hexamethyldisilazane to the water to the ethanol is 1:1:1.5:15.
As a preferred embodiment of the present invention, the curing agent is a low molecular weight polyamide curing agent.
As a preferred embodiment of the present invention, the mass ratio of the bisphenol A type epoxy resin to the low molecular weight polyamide curing agent is 3:1.
As a preferable scheme of the invention, the mass of the dopamine hydrochloride contained in each 1mL of hydrophobic silica sol is 0.20 mg-12 mg.
As a preferable scheme of the invention, the reaction temperature of the epoxy mixed solution in the reaction container is 70-95 ℃, and the temperature exceeds the boiling point of ethanol, so that a large amount of bubbles are generated to impact the reaction product. The reaction time is 6-24 h.
As a preferable scheme of the invention, after bisphenol A epoxy resin, a curing agent and dopamine hydrochloride are added into a hydrophobic silica sol solution, the bisphenol A epoxy resin, the curing agent and the dopamine hydrochloride are heated to 40-60 ℃ to dissolve the bisphenol A epoxy resin, the curing agent and the dopamine hydrochloride into the hydrophobic silica sol solution.
As a preferred embodiment of the present invention, the undried superhydrophobic bulk material is soft and is placed in a mold for drying. The undried superhydrophobic block material can also be directly placed in an oven for drying, the obtained round block superhydrophobic material is the blocky superhydrophobic material, if the blocky superhydrophobic material with other shapes is expected to be obtained, the product undried superhydrophobic block material is dried in a mold with a mold cavity with a corresponding shape, the materials with different shapes are obtained after drying, and the photo-thermal effect, the wear resistance and the superhydrophobic property of the material are not influenced by the shapes.
Compared with the prior art, the invention has the following beneficial effects:
(1) The super-hydrophobic material prepared by the invention uses ethanol as a reaction solvent, does not involve solvents with larger toxicity, does not use expensive and toxic fluorine-containing low-surface-energy modifier, is friendly and environment-friendly, has simple preparation process, is cheap and easily obtained in raw materials, and is easy to realize large-scale production;
(2) According to the invention, a large amount of reaction products generated by new reaction of bubble impact can be generated in the process of the reflux reaction of the epoxy mixed solution by a bubble impact method, and the super-hydrophobic material generated by combining the synchronous epoxy curing reaction and the chemical bonding action of the epoxy resin between the cured products has uniform structure and clear pores, and the dried super-hydrophobic material has excellent wear resistance and chemical corrosion resistance, can bear serious mechanical wear, such as abrasive paper friction, finger belly friction, knife scraping, adhesive tape tearing, ultrasonic vibration and the like, and has good wear resistance;
(3) The epoxy cured product has the property of hydrophobic, the hydrophobicity of the silica sol further strengthens the hydrophobicity of the product, and the micro-nano porous coarse structure generated by the impact of bubbles is combined, so that the obtained super-hydrophobic material has the super-hydrophobic property with the same surface and inner side, and has the chemical stability of high temperature resistance and ultraviolet irradiation resistance;
(4) The super-hydrophobic material prepared by the invention has the advantages that on the basis of mechanical and chemical abrasion resistance, the photo-thermal conversion performance is also increased, the air cushion structure of the micro-nano pore of the super-hydrophobic material is combined with photo-thermal conversion to improve the temperature of the super-hydrophobic material, and the anti-icing effect can be well realized; in addition, from the perspective of crude oil absorption, the fluidity of the crude oil is greatly improved due to the increase of the temperature of the crude oil, which is favorable for realizing high-efficiency oil-water separation of the super-hydrophobic material, so that the super-hydrophobic material has very good application potential in the fields of ice resistance, oil-water separation and the like;
(5) The temperature rising capability of the material can be regulated by changing the addition amount of the dopamine hydrochloride, and in addition, the appearance color of the prepared superhydrophobic material can also change along with the change of the consumption amount of the dopamine hydrochloride, so that the color of the superhydrophobic material can be regulated and controlled.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are required in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that it is within the scope of the invention to one skilled in the art to obtain other drawings from these drawings without inventive faculty.
Fig. 1 is a physical diagram and a contact angle diagram of a block-shaped super-hydrophobic material of an epoxy resin with photo-thermal effect and abrasion resistance prepared in example 1;
FIG. 2 is a photo-thermal conversion temperature rise diagram of the epoxy resin block-shaped superhydrophobic material with photo-thermal effect and abrasion resistance prepared in example 1;
FIG. 3 is a physical diagram and a contact angle diagram of the epoxy resin block superhydrophobic material with photo-thermal effect and abrasion resistance prepared in example 2;
FIG. 4 is a photo-thermal conversion temperature rise diagram of the epoxy resin block-shaped superhydrophobic material with photo-thermal effect and abrasion resistance prepared in example 2;
fig. 5 is a physical diagram and a contact angle diagram of the epoxy resin block superhydrophobic material with photo-thermal effect and abrasion resistance prepared in example 3;
fig. 6 is a photo-thermal conversion temperature rise diagram of the epoxy resin block superhydrophobic material with photo-thermal effect and abrasion resistance prepared in example 3.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings, for the purpose of making the objects, technical solutions and advantages of the present invention more apparent.
Example 1
Ethyl orthosilicate 2.0. 2.0 mL is added into 30 mL ethanol drop by drop, stirring is continued, 2.0 mL hexamethyldisilazane is added dropwise after 10 min, stirring is performed for 30 min, then 3.0mL distilled water is added, stirring is continued for 120 min, and the reaction is closed. Standing for 6 d at room temperature to obtain hydrophobic silica sol solution. Bisphenol A type epoxy resin 1.25 g, low molecular weight polyamide curing agent 0.46 g and dopamine hydrochloride 0.02 g are added into a 20.0 mL hydrophobic silica sol solution together, and the mixture is slightly heated and dissolved to obtain epoxy mixed solution. Placing the epoxy mixed solution in a round-bottom flask, building a reflux device, increasing the reaction temperature to 80 ℃, stopping the reaction after 10 and h, obtaining an undried superhydrophobic block material, placing the undried superhydrophobic block material in a cylindrical mold, and drying at 60 ℃ to obtain the cylindrical wear-resistant block epoxy resin superhydrophobic material with a photo-thermal effect.
The contact angle of the prepared super-hydrophobic material is 157.3 degrees, and the rolling angle is 5.2 degrees. Under the load condition of 100 g, after 3000 cm is worn by 1000-mesh sand paper, the material still maintains good superhydrophobic performance, the contact angle is 155.3 degrees, and the rolling angle is 4.1 degrees. The abrasion rate of the material is low, and the mass retention rate of the material after the abrasive paper is abraded by 3000 cm is 97.37%. The photo-thermal conversion capability of the epoxy resin super-hydrophobic material is detected by using a thermal infrared imager, the irradiation wavelength is 808 and nm, and the power is 1W/cm 2 Under the irradiation of the light source, the material is heated rapidly, but the super-hydrophobic material has limited heating capacity due to the small addition amount of dopamine, and the highest temperature rising in 300 s time is 37.8 ℃. Nevertheless, the prepared epoxy resin super-hydrophobic block material has certain wear resistance and photothermal conversion capability, and is expected to improve the application potential of the super-hydrophobic material in the fields of anti-icing, heavy crude oil separation and the like.
Example 2
Ethyl orthosilicate 2.0. 2.0 mL is added into 30 mL ethanol drop by drop, stirring is continued, 2.0 mL hexamethyldisilazane is added dropwise after 10 min, stirring is performed for 30 min, then 3.0mL distilled water is added, stirring is continued for 120 min, and the reaction is closed. Standing for 8-d at room temperature to obtain hydrophobic silica sol solution. Bisphenol A type epoxy resin 1.25 g, low molecular weight polyamide curing agent 0.46 g and dopamine hydrochloride 0.08 g are added into 20.0 mL hydrophobic silica sol solution together, and the mixture is slightly heated and dissolved to obtain epoxy mixed solution. Placing the epoxy mixed solution in a round-bottom flask, building a reflux device, increasing the reaction temperature to 85 ℃, stopping the reaction after 16 and h, obtaining an undried superhydrophobic block material, placing the undried superhydrophobic block material in a round-table-shaped mold, and drying at 60 ℃ to obtain the round-table-shaped wear-resistant block-shaped epoxy resin superhydrophobic material with a photo-thermal effect.
The contact angle of the prepared super-hydrophobic material is 153.8 degrees, and the rolling angle is 7.8 degrees. Under the load condition of 100 g, after 3000 cm is worn by 1000-mesh sand paper, the material still maintains good superhydrophobic performance, the contact angle is 151.3 degrees, and the rolling angle is 9.3 degrees. The abrasion rate of the material is low, and the mass retention rate of the material after the abrasive paper is abraded by 3000 cm is 96.23%. The photo-thermal conversion capability of the epoxy resin super-hydrophobic material is detected by using a thermal infrared imager, the irradiation wavelength is 808 and nm, and the power is 1W/cm 2 Under the irradiation of the light source of (2), the material rapidly increased in temperature, and the maximum temperature increased in 300 and s was 50.7 ℃. Therefore, by increasing the addition amount of dopamine hydrochloride, the prepared epoxy resin super-hydrophobic block material has better wear resistance and photothermal conversion capability, and is expected to increase the application potential of the super-hydrophobic material in the fields of anti-icing, heavy crude oil separation and the like.
Example 3
Ethyl orthosilicate 2.0. 2.0 mL is added into 30 mL ethanol drop by drop, stirring is continued, 2.0 mL hexamethyldisilazane is added dropwise after 10 min, stirring is performed for 30 min, then 3.0mL distilled water is added, stirring is continued for 120 min, and the reaction is closed. Standing for 10 times d at room temperature to obtain the hydrophobic silica sol solution. Bisphenol A type epoxy resin 1.90 g, low molecular weight polyamide curing agent 0.65 g and dopamine hydrochloride 0.24 g are added into 30.0 mL hydrophobic silica sol solution together, and the epoxy mixed solution is obtained by slightly heating and dissolving. Placing the epoxy mixed solution in a round-bottom flask, building a reflux device, increasing the reaction temperature to 90 ℃, stopping the reaction after 24 and h to obtain an undried superhydrophobic block material, placing the undried superhydrophobic block material in a cylindrical mold, and drying at 60 ℃ to obtain the cylindrical wear-resistant blocky epoxy resin superhydrophobic material with a photo-thermal effect.
The contact angle of the prepared super-hydrophobic material is 152.1 degrees, and the rolling angle is 8.2 degrees. Under the load condition of 100 g, after 3000 cm is worn by 1000-mesh sand paper, the material still maintains good superhydrophobic performance, the contact angle is 150.6 degrees, and the rolling angle is 9.8 degrees. The abrasion rate of the material is slightly improved, and the mass retention rate of the material after the sand paper is abraded by 3000 cm is 95.80%. By infraredThe thermal imager detects the photo-thermal conversion capability of the epoxy resin super-hydrophobic material, and the power is 1W/cm when the irradiation wavelength is 808nm 2 Under the irradiation of the light source of (2), the material rapidly increased in temperature, and the maximum temperature increased in 300 and s was 64.9 ℃. Therefore, the prepared epoxy resin super-hydrophobic block material has excellent wear resistance and photothermal conversion capability, and is expected to improve the application potential of the super-hydrophobic material in the fields of anti-icing, heavy crude oil separation and the like.
Through the change of the reaction conditions and the comparison of the material properties in the above examples, it was found that the superhydrophobic materials with different shapes can be prepared by selecting different shapes of molds during drying. The color of the prepared super-hydrophobic material is obviously changed by changing the addition amount of dopamine hydrochloride, and the color of the prepared material is changed from white to light yellow and yellow. In addition, the temperature rising capability of the super-hydrophobic material is rapidly improved through the regulation and control of the addition amount of the dopamine. Therefore, the wear-resistant super-hydrophobic material obtained by the preparation technology can regulate and control the appearance shape, the color and the photo-thermal conversion capability of the material.
The foregoing disclosure is illustrative of the present invention and is not to be construed as limiting the scope of the invention, which is defined by the appended claims.
Claims (6)
1. The preparation process of the epoxy resin block-shaped super-hydrophobic material with the photo-thermal effect and abrasion resistance is characterized by comprising the following steps of:
dissolving bisphenol A epoxy resin, a curing agent and dopamine hydrochloride into a hydrophobic silica sol solution together to obtain an epoxy mixed solution;
placing the epoxy mixed solution in a reaction container, and heating to a reflux state for reaction to obtain an undried superhydrophobic bulk material;
drying the undried superhydrophobic block material to obtain an epoxy resin block superhydrophobic material with photo-thermal effect and abrasion resistance;
the preparation process of the hydrophobic silica sol solution is as follows: dropwise adding tetraethoxysilane into ethanol, stirring, dropwise adding hexamethyldisilazane, stirring, adding distilled water, and continuously stirring to obtain a hydrophobic silica sol solution;
the volume ratio of the tetraethoxysilane to the hexamethyldisilazane to the water to the ethanol is 1:1:1.5:15;
the mass of the dopamine hydrochloride contained in each 1mL of hydrophobic silica sol is 0.20 mg-12 mg.
2. The photo-thermal effect wear-resistant epoxy resin block superhydrophobic material according to claim 1, wherein: the newly prepared hydrophobic silica sol solution is kept stand for 5-10d at room temperature and then is used for preparing the epoxy mixed solution.
3. The photo-thermal effect wear-resistant epoxy resin block superhydrophobic material according to claim 1, wherein: the curing agent is a low molecular weight polyamide curing agent.
4. The photo-thermal effect wear-resistant epoxy resin block superhydrophobic material according to claim 1, wherein: the mass ratio of the bisphenol A type epoxy resin to the low molecular weight polyamide curing agent is 3:1.
5. The photo-thermal effect wear-resistant epoxy resin block superhydrophobic material according to claim 1, wherein: after bisphenol A epoxy resin, a curing agent and dopamine hydrochloride are added into the hydrophobic silica sol solution, heating to 40-60 ℃ to dissolve the bisphenol A epoxy resin, the curing agent and the dopamine hydrochloride into the hydrophobic silica sol solution.
6. The photo-thermal effect wear-resistant epoxy resin block superhydrophobic material according to claim 1, wherein: the undried superhydrophobic bulk material is soft and is placed in a mold for drying.
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| CN108659257A (en) * | 2018-05-21 | 2018-10-16 | 温州生物材料与工程研究所 | A kind of high intensity, anti abrasive super-hydrophobic composite material and preparation method |
| CN110743200A (en) * | 2018-07-23 | 2020-02-04 | 中国石油化工股份有限公司 | Super-hydrophobic and super-oleophilic three-dimensional porous material and preparation method and application thereof |
| CN112898593A (en) * | 2021-03-24 | 2021-06-04 | 温州医科大学 | Acid and alkali resistant and wear resistant fluoride-free blocky super-hydrophobic material based on epoxy microspheres |
| CN113480913A (en) * | 2021-07-02 | 2021-10-08 | 武汉理工大学 | Super-hydrophobic coating with photo-thermal effect, coating and preparation method |
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2021
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| CN105295698A (en) * | 2015-11-25 | 2016-02-03 | 中国科学院兰州化学物理研究所 | Aqueous coating material capable of performing super-hydrophobicity repair through photothermal method, and preparation method thereof |
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