CN108911525B - Preparation method of hydrophobic sand core material - Google Patents
Preparation method of hydrophobic sand core material Download PDFInfo
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- CN108911525B CN108911525B CN201810878474.4A CN201810878474A CN108911525B CN 108911525 B CN108911525 B CN 108911525B CN 201810878474 A CN201810878474 A CN 201810878474A CN 108911525 B CN108911525 B CN 108911525B
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- sand core
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
- C03C17/30—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with silicon-containing compounds
Abstract
The invention discloses a preparation method of a hydrophobic sand core material, and belongs to the technical field of hydrophobic material preparation. The method comprises the following steps of exposing a sand core material to an organosilane reagent atmosphere, and carrying out condensation polymerization on the organosilane reagent and hydroxyl on the surface of the sand core material to form a hydrophobic silane coating, wherein the method comprises the following steps: and adding an organic silanization reagent into the container, placing the organic silanization reagent and the sand core material into the container, and heating the container in a closed manner to ensure that the organic silanization reagent is gasified and fully contacts and reacts with the sand core material to obtain the hydrophobic sand core material. The method has the advantages of simple process, no environmental pollution and low cost, and the hydrophobic modified sand core funnel obtained by the method has good hydrophobicity, can be used in the fields of wastewater treatment, oil-water separation, emulsion separation and the like, and has good industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of hydrophobic material preparation, and particularly relates to a preparation method of a hydrophobic sand core material.
Background
The sand core filter plate of the sand core funnel is formed by grinding, sieving and sintering glass materials, is composed of excellent hard high-boron glass, has higher physical and chemical properties, can filter acid liquor and is treated by acid, and is also called an acid-resistant funnel and a glass vertical melting funnel. The sand core funnel is a filtering device capable of realizing solid-liquid separation, has the advantages of simplicity, rapidness, low cost and the like, and is widely applied to aspects of chemical analysis, health monitoring, environment monitoring, biological products, scientific research and the like. Generally, a sand core filter plate of a sand core funnel mainly comprises silicon dioxide, the surface of the sand core filter plate contains a large number of hydroxyl groups, a high-energy and hydrophilic surface is formed, and the sand core filter plate has no selectivity on different solvents such as water, oil and the like during filtration. In order to expand the practical application of the sand core funnel, the sand core filter plate needs to be subjected to hydrophobic modification, so that a good oil-water separation effect is achieved. Methods commonly used for preparing materials with special wettability include biomimetic methods, chemical modification, layer-by-layer self-assembly, templating methods, chemical etching methods, spray coating methods, and czochralski methods, among others. Specifically, the water contact angle of the surface of the modified glass reaches over 90 degrees (Polymer. chem.,2017,8, 7457-7468) through surface grafting, click reaction and copper-initiated living radical polymerization. Silica nanospheres are synthesized by a sol-gel method and a superhydrophobic film is formed on the surface with a silica network (ACS appl. The silicon wafer is soaked in a mixed solution of a silane coupling agent and an organic solvent by a leaching method, and then a series of post-treatment processes such as cleaning and drying are carried out to obtain the super-hydrophobic surface (J.Am.chem.Soc.,2006,128, 9052-9053). Mesoporous silica particles are assembled into a coating with a hierarchical structure by a layer-by-layer self-assembly method, and a glass surface with super-hydrophobic property is obtained (Langmuir,2010,26, 13528-13534). The preparation of hydrophobic surfaces on silica surfaces currently presents the following technical difficulties: the existing method for preparing the hydrophobic silicon dioxide material has complex steps, complex construction of the material at the early stage, more complicated post-treatment process, higher production cost and less possibility of large-scale application. Importantly, the sand core filter plate has natural advantages, is composed of gravels with different sizes, is wide in formed aperture distribution range, is as large as hundreds of micrometers and less than 1 micrometer, forms surfaces with different roughness, and can meet the requirements of various oil-water mixing and separation after hydrophobic modification. The development of a simple, low cost and valuable hydrophobic core material is urgently needed.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention aims to provide the preparation method of the hydrophobic sand core material, the method is a chemical vapor deposition method, the hydrophobic sand core material can be prepared by adopting an in-situ one-step reaction, and the preparation method has the advantages of simple process, no environmental pollution and low cost. The invention also aims to provide application of the prepared hydrophobic sand core material.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a hydrophobic sand core material comprises the steps of exposing the sand core material to an organosilane reagent atmosphere, and enabling the organosilane reagent to be subjected to condensation polymerization with hydroxyl on the surface of the sand core material to form a hydrophobic silane coating, so that the hydrophobic sand core material is obtained. Wherein the organosilane reagent atmosphere is obtained by heating and vaporizing an organosilane reagent. The sand core material comprises a sand core funnel, a sand chip and the like.
Preferably, the organosilane reagent comprises hexamethyldisilazane, methyltrimethoxysilane, dodecyltrimethoxysilane, perfluorooctyltriethoxysilane, octadecyltrichlorosilane, and the like. Further preferably, the organosilane reagent is perfluorooctyltriethoxysilane.
More specifically, the preparation method of the hydrophobic sand core material comprises the following steps: and adding an organic silanization reagent and a sand core material (the sand core material is not contacted with the organic silanization reagent) into the container, closing the container, and heating the container to ensure that the organic silanization reagent is gasified and is fully contacted with the sand core material to obtain the hydrophobic sand core material. Preferably, the container is vacuumized before being heated, the heating temperature is 40-140 ℃, and the heating time is 10 min-24 h.
The hydrophobic sand core material is obtained by the preparation method.
The hydrophobic sand core material can be applied to the fields of oil-water separation, emulsion separation, wastewater treatment and the like.
The principle of the invention is as follows: the main component of the sand core material is silicon dioxide, the surface of the sand core material contains abundant silicon hydroxyl, a series of derivatization reactions related to the hydroxyl can be carried out, an organic silane reagent is gasified by heating, the sand core material is completely exposed in the silane reagent atmosphere and fully contacts with the silane reagent atmosphere, and the hydrophobic silane coating is formed by condensation polymerization of the organic silane reagent and the hydroxyl on the solid surface, so that the hydrophobic surface of the sand core material is constructed.
The invention has the following technical effects:
(1) the method has simple process, no environmental pollution and no need of any expensive equipment.
(2) The hydrophobic modified sand core funnel obtained by the method has good hydrophobicity, the water contact angle can reach 90-150 degrees, the funnel can resist acid and alkali salt solution, the cost is low, the funnel can be used in the fields of wastewater treatment, oil-water separation, emulsion separation and the like, and has good industrial application prospect.
Drawings
Fig. 1 is a schematic diagram of a dryer apparatus and a method for making a hydrophobically modified sand core funnel used in embodiments of the present invention.
Fig. 2 is a graph showing the results of water contact angles of the pre-modified sand core funnel (a) and the post-modified sand core funnel (b) in example 1 of the present invention.
Fig. 3 is a graph of the water contact angle results for pre-modified sand core funnel (a) and post-modified sand core funnel (b) of example 2 of the present invention.
FIG. 4 is a graph showing the results of separation of a toluene/water mixture (a) and a chloroform/water mixture (b) in the modified sand core funnel in example 2 of the present invention.
Fig. 5 is a graph of the water contact angle results for a modified sand core funnel of example 2 of the present invention for a pH 1 sulfuric acid solution (a), a pH 13 sodium hydroxide solution (b), and a 5 wt% sodium chloride solution (c).
Fig. 6 is a graph of the water contact angle results for pre-modification sand core funnel (a) and post-modification sand core funnel (b) of example 3 of the present invention.
Fig. 7 is a graph of the water contact angle results for pre-modified sand core funnel (a) and post-modified sand core funnel (b) of example 4 of the present invention.
Fig. 8 is a graph of the water contact angle results for pre-modified sand core funnel (a) and post-modified sand core funnel (b) of example 5 of the present invention.
Fig. 9 is a graph of the water contact angle results for pre-modified sand core funnel (a) and post-modified sand core funnel (b) of example 6 of the present invention.
Fig. 10 is a graph of the water contact angle results for pre-modified sand core funnel (a) and post-modified sand core funnel (b) of example 7 of the present invention.
Fig. 11 is a graph of the water contact angle results for pre-modified sand core funnel (a) and post-modified sand core funnel (b) of example 8 of the present invention.
Fig. 12 is a graph of the water contact angle results for pre-modified sand core funnel (a) and post-modified sand core funnel (b) of example 9 of the present invention.
Fig. 13 is a graph of the water contact angle results for pre-modification sand core funnel (a) and post-modification sand core funnel (b) of example 10 of the present invention.
Fig. 14 is a graph showing the results of water contact angles for the pre-modification sand core funnel (a) and the post-modification sand core funnel (b) of example 14 of the present invention.
Detailed Description
The invention is described in further detail below with reference to examples, it being understood that the examples are provided by way of illustration of the process of the invention only and are not intended to limit the remainder of the disclosure in any way.
[ example 1 ]
Firstly, ultrasonically cleaning a sand core funnel for 3 times by using absolute ethyl alcohol and acetone alternately, wherein the ultrasonic cleaning time is 5 minutes each time, cleaning the sand core funnel for 3 times by using deionized water, and then drying the sand core funnel by using hot air. The sand core funnel G1 is placed in a dryer, a small culture dish is placed at the bottom of the dryer, as shown in figure 1, 10mL of perfluorooctyl triethoxysilane is added, the dryer is vacuumized, placed in an oven at 140 ℃ for heating for 4 hours, taken out and cooled to room temperature to obtain the hydrophobically modified sand core funnel, the water/air contact angle of the hydrophobically modified sand core funnel is 131 degrees, and the contact angles of the sand core funnel before and after modification can be obviously changed from figure 2.
[ example 2 ]
Firstly, ultrasonically cleaning a sand core funnel for 3 times by using absolute ethyl alcohol and acetone alternately, wherein the ultrasonic cleaning time is 5 minutes each time, cleaning the sand core funnel for 3 times by using deionized water, and then drying the sand core funnel by using hot air. The sand core funnel G2 is placed in a dryer, a small culture dish is placed at the bottom of the dryer, as shown in figure 1, 10mL of perfluorooctyl triethoxysilane is added, the dryer is vacuumized, placed in an oven at 140 ℃ for heating for 4 hours, taken out and cooled to room temperature to obtain the hydrophobically modified sand core funnel, the water/air contact angle of the hydrophobically modified sand core funnel is 136 degrees, and the contact angles of the sand core funnel before and after modification can be obviously changed as shown in figure 3. The modified sand core funnel is used for oil-water separation, a graph of the separation of a toluene/water mixed solution and a chloroform/water mixed solution of the modified G2 funnel is shown in fig. 4, the oil-water mixed solution is successfully separated, all organic solvents pass through the modified G2 funnel, water is completely reserved on the water, the whole separation process is completed within ten seconds, the separation speed is high, and the separation effect is excellent. Fig. 5 shows the water contact angle of the modified sand core funnel G2 to acid and base salts, wherein the water contact angle to sulfuric acid solution at pH 1 is 129 °, the water contact angle to sodium hydroxide solution at pH 13 is 125 °, the water contact angle to sodium chloride solution at 5 wt% is 129 °, and excellent acid and alkali resistance is exhibited.
[ example 3 ]
Firstly, ultrasonically cleaning a sand core funnel for 3 times by using absolute ethyl alcohol and acetone alternately, wherein the ultrasonic cleaning time is 5 minutes each time, cleaning the sand core funnel for 3 times by using deionized water, and then drying the sand core funnel by using hot air. The sand core funnel G3 is placed in a dryer, a small culture dish is placed at the bottom of the dryer, as shown in figure 1, 10mL of perfluorooctyl triethoxysilane is added, the dryer is vacuumized, placed in an oven at 140 ℃ for heating for 4 hours, taken out and cooled to room temperature to obtain the hydrophobically modified sand core funnel, the water/air contact angle of the hydrophobically modified sand core funnel is 140 degrees, and the contact angles of the sand core funnel before and after modification can be obviously changed from figure 6.
[ example 4 ]
Firstly, ultrasonically cleaning a sand core funnel for 3 times by using absolute ethyl alcohol and acetone alternately, wherein the ultrasonic cleaning time is 5 minutes each time, cleaning the sand core funnel for 3 times by using deionized water, and then drying the sand core funnel by using hot air. The sand core funnel G4 is placed in a dryer, a small culture dish is placed at the bottom of the dryer, as shown in figure 1, 10mL of perfluorooctyl triethoxysilane is added, the dryer is vacuumized, placed in an oven at 140 ℃ for heating for 4 hours, taken out and cooled to room temperature to obtain the hydrophobically modified sand core funnel, the water/air contact angle of the hydrophobically modified sand core funnel is 145 degrees, and the contact angles of the sand core funnel before and after modification can be obviously changed from figure 7.
[ example 5 ]
Firstly, ultrasonically cleaning a sand core funnel for 3 times by using absolute ethyl alcohol and acetone alternately, wherein the ultrasonic cleaning time is 5 minutes each time, cleaning the sand core funnel for 3 times by using deionized water, and then drying the sand core funnel by using hot air. The sand core funnel G5 is placed in a dryer, a small culture dish is placed at the bottom of the dryer, as shown in figure 1, 10mL of perfluorooctyl triethoxysilane is added, the dryer is vacuumized, placed in an oven at 140 ℃ for heating for 4 hours, taken out and cooled to room temperature to obtain the hydrophobic modified glass, the water/air contact angle of the hydrophobic modified glass is 147 degrees, and the contact angle of the sand core funnel before and after modification can be obviously changed as shown in figure 8.
[ example 6 ]
Firstly, ultrasonically cleaning a sand core funnel for 3 times by using absolute ethyl alcohol and acetone alternately, wherein the ultrasonic cleaning time is 5 minutes each time, cleaning the sand core funnel for 3 times by using deionized water, and then drying the sand core funnel by using hot air. The sand core funnel G6 is placed in a dryer, a small culture dish is placed at the bottom of the dryer, as shown in figure 1, 10mL of perfluorooctyl triethoxysilane is added, the dryer is vacuumized, placed in an oven at 140 ℃ for heating for 4 hours, taken out and cooled to room temperature to obtain the hydrophobically modified sand core funnel, the water/air contact angle of the hydrophobically modified sand core funnel is 150 degrees, and the contact angles of the sand core funnel before and after modification can be obviously changed from figure 9.
[ example 7 ]
Firstly, ultrasonically cleaning a sand core funnel for 3 times by using absolute ethyl alcohol and acetone alternately, wherein the ultrasonic cleaning time is 5 minutes each time, cleaning the sand core funnel for 3 times by using deionized water, and then drying the sand core funnel by using hot air. Placing the sand core funnel G6 in a dryer, placing a small culture dish at the bottom of the dryer, adding 10mL hexamethyldisilazane as shown in figure 1, vacuumizing the dryer, placing the dryer in an oven at 140 ℃ for heating for 4 hours, taking out and cooling to room temperature to obtain the hydrophobically modified sand core funnel, wherein the water/air contact angle of the hydrophobically modified sand core funnel is 143 degrees, and the contact angle of the sand core funnel before and after modification can be obviously changed from figure 10.
[ example 8 ]
Firstly, ultrasonically cleaning a sand core funnel for 3 times by using absolute ethyl alcohol and acetone alternately, wherein the ultrasonic cleaning time is 5 minutes each time, cleaning the sand core funnel for 3 times by using deionized water, and then drying the sand core funnel by using hot air. The sand core funnel G6 is placed in a dryer, a small culture dish is placed at the bottom of the dryer, 10mL of methyltrimethoxysilane is added as shown in figure 1, the dryer is vacuumized, placed in an oven at 140 ℃ for heating for 4 hours, taken out and cooled to room temperature to obtain the hydrophobically modified sand core funnel, the water/air contact angle of the hydrophobically modified sand core funnel is 138 degrees, and the contact angles of the sand core funnel before and after modification can be obviously changed from figure 11.
[ example 9 ]
Firstly, ultrasonically cleaning a sand core funnel for 3 times by using absolute ethyl alcohol and acetone alternately, wherein the ultrasonic cleaning time is 5 minutes each time, cleaning the sand core funnel for 3 times by using deionized water, and then drying the sand core funnel by using hot air. The sand core funnel G6 is placed in a dryer, a small-sized culture dish is placed at the bottom of the dryer, 10mL of dodecyl trimethoxy silane is added as shown in figure 1, the dryer is vacuumized, placed in an oven at 140 ℃ for heating for 4 hours, taken out and cooled to room temperature to obtain the hydrophobically modified sand core funnel, the water/air contact angle of the hydrophobically modified sand core funnel is 141 degrees, and the contact angles of the sand core funnel before and after modification can be obviously changed from figure 12.
[ example 10 ]
Firstly, ultrasonically cleaning a sand core funnel for 3 times by using absolute ethyl alcohol and acetone alternately, wherein the ultrasonic cleaning time is 5 minutes each time, cleaning the sand core funnel for 3 times by using deionized water, and then drying the sand core funnel by using hot air. Placing the sand core funnel G6 in a dryer, placing a small culture dish at the bottom of the dryer, adding 10mL of octadecyl trichlorosilane as shown in figure 1, vacuumizing the dryer, placing the dryer in an oven at 140 ℃ for heating for 10min, taking out and cooling to room temperature to obtain the hydrophobically modified sand core funnel, wherein the water/air contact angle of the hydrophobically modified sand core funnel is 141 degrees, and the contact angles of the sand core funnel before and after modification can be obviously changed from figure 13.
[ example 11 ]
Firstly, ultrasonically cleaning a sand core funnel for 3 times by using absolute ethyl alcohol and acetone alternately, wherein the ultrasonic cleaning time is 5 minutes each time, cleaning the sand core funnel for 3 times by using deionized water, and then drying the sand core funnel by using hot air. Placing the sand core funnel G6 in a dryer, placing a small culture dish at the bottom of the dryer, adding 10mL perfluorooctyl triethoxysilane as shown in figure 1, vacuumizing the dryer, placing the dryer in a 40 ℃ oven for heating for 30min, taking out and cooling to room temperature to obtain the hydrophobically modified sand core funnel, wherein the water/air contact angle is 124 degrees.
[ example 12 ]
Firstly, ultrasonically cleaning a sand core funnel for 3 times by using absolute ethyl alcohol and acetone alternately, wherein the ultrasonic cleaning time is 5 minutes each time, cleaning the sand core funnel for 3 times by using deionized water, and then drying the sand core funnel by using hot air. Placing the sand core funnel G6 in a dryer, placing a small culture dish at the bottom of the dryer, adding 10mL perfluorooctyl triethoxysilane as shown in figure 1, vacuumizing the dryer, placing the dryer in an oven at 70 ℃ for heating for 30min, taking out and cooling to room temperature to obtain the hydrophobically modified sand core funnel, wherein the water/air contact angle is 134 degrees.
[ example 13 ]
Firstly, ultrasonically cleaning a sand core funnel for 3 times by using absolute ethyl alcohol and acetone alternately, wherein the ultrasonic cleaning time is 5 minutes each time, cleaning the sand core funnel for 3 times by using deionized water, and then drying the sand core funnel by using hot air. Placing the sand core funnel G6 in a dryer, placing a small culture dish at the bottom of the dryer, adding 10mL perfluorooctyl triethoxysilane as shown in figure 1, placing in a 70 ℃ oven for heating for 24 hours, taking out and cooling to room temperature to obtain the hydrophobically modified sand core funnel, wherein the water/air contact angle is 145 degrees.
[ example 14 ]
Firstly, ultrasonically cleaning a sand core funnel for 3 times by using absolute ethyl alcohol and acetone alternately, wherein the ultrasonic cleaning time is 5 minutes each time, cleaning the sand core funnel for 3 times by using deionized water, and then drying the sand core funnel by using hot air. The sand core funnel G6 is placed in a dryer, a small culture dish is placed at the bottom of the dryer, as shown in figure 1, 10mL of perfluorooctyl triethoxysilane is added, the dryer is placed in a drying oven at 140 ℃ for heating for 4 hours, the sand core funnel is taken out and cooled to room temperature, the hydrophobic modified sand core funnel is obtained, the water/air contact angle of the sand core funnel is 144 degrees, the contact angle of the sand core funnel before and after modification can be obviously changed, and the hydrophobic modified sand core funnel is successfully obtained through the method, so that an excellent hydrophobic effect is achieved.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. A preparation method of a hydrophobic sand core material is characterized by comprising the following steps: exposing the sand core material in an organosilane reagent atmosphere, and performing condensation polymerization on the organosilane reagent and hydroxyl on the surface of the sand core material to form a hydrophobic silane coating to obtain a hydrophobic sand core material; the sand core material is a sand core filter plate of a sand core funnel.
2. The method of claim 1, wherein: the organic silane reagent atmosphere is obtained by heating and vaporizing an organic silane reagent.
3. The method of claim 1, wherein: the organosilane reagent comprises hexamethyldisilazane, methyltrimethoxysilane, dodecyltrimethoxysilane, perfluorooctyltriethoxysilane, octadecyltrichlorosilane.
4. The production method according to claim 3, characterized in that: the organosilane reagent is perfluorooctyl triethoxysilane.
5. The method of claim 1, wherein: the method comprises the following steps: and adding an organic silanization reagent and a sand core material into the container, closing the container, and heating the container to ensure that the organic silanization reagent is gasified and fully contacted with the sand core material to obtain the hydrophobic sand core material.
6. The method of claim 5, wherein: the container is evacuated before being heated.
7. The method of claim 5, wherein: the heating temperature is 40-140 ℃, and the heating time is 10 min-24 h.
8. A hydrophobic sand core material is characterized in that: obtained by the production method according to any one of claims 1 to 7.
9. The use of the hydrophobic sand core material of claim 8 in the field of oil-water separation, emulsion separation or wastewater treatment.
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