CN103143493A - Artificial cultivation method of super-amphiphobic self-cleaning surface fine nano-structure - Google Patents
Artificial cultivation method of super-amphiphobic self-cleaning surface fine nano-structure Download PDFInfo
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Abstract
An artificial cultivation method of a super-amphiphobic self-cleaning surface fine nano-structure utilizes the main body of surface fine nano-structure with super-amphiphobic property as a rodlike nano cellulose, controllable ordered directional planting of nano filaments of the rodlike nano cellulose is realized on the surface of a substrate in an electrostatic flocking manner, and the flocked surface is modified by a fluorine-containing reagent and self-assembled to form a layer of fluorine-containing long-chain alkylsilane molecules so as to obtain the super-amphiphobic self-cleaning surface fine nano-structure. The surface of the prepared nano cellulose and nano filament fine nano-structure has remarkable super-amphiphobic and super-oleophobic properties, as well as favorable chemical stability and self-cleaning capability, and the fine nano-structure has a broad application prospect in medicine, fine chemical engineering, textile, construction material and other aspects, and provides new thoughts for efficient utilization of wood and other recyclable resources.
Description
Technical field
The present invention relates to a kind of fine nanostructur material and artificial method for planting thereof with super-hydrophobic super oleophobic automatically cleaning characteristic.
Background technology
Super-double-hydrophobic surface typically refers to the contact angle of water and oil phase all greater than the surface of 150 °.1997, the Electronic Speculum picture of Germany biologist Neinhuis and Barthlott research lotus leaf surface is found, there is the mastoid process of meticulous micro nano structure in lotus leaf surface, and this existence by the formed rough surface of micron and nanometer composite structure mastoid process and the wax-like thing of lotus leaf surface hydrophobicity causes lotus leaf to have super two thin self_cleaning effects of " go out mud and do not dye " jointly.Many good characteristics such as anti-pollution, the rain and snow that causes based on super two thin phenomenons, anticorrosion, anti-oxidant and self-cleaning surface, super-double-hydrophobic surface has potential application foreground widely in many-sides such as yarn fabric, traffic signals, wheel barnacle, space shuttle, various pipes, construction material, vehicle glass, satellite antennas, in recent years, the super two thin materials of bionic preparation and super-double-hydrophobic surface have caused the huge interest of Many researchers.
Not only relevant with surface tension, more closely related with surface roughness with the contact angle on surface in view of drop, the fine nanostructur surface that utilizes the whole bag of tricks to build to have the nano-micro level roughness seems particularly important to preparing super two thin material.Microstructure in the surface construction nano-scale concaveconvex shape complementation of material, recessed adsorption air by nano-scale, be equivalent to the gas membrane that has one deck stable on macroscopic view, You Heshui can't directly be contacted with the surface fully, and the part solid liquid interface is replaced by gas-liquid interface, and contact angle is increased, roughness is higher, contact angle is larger, and greater than 150 °, the surface just will show the two thin characteristics of excess of export when solid-liquid contact angle.The method of bionic preparation super-double-hydrophobic surface is a lot of at present, mainly contains: plasma technique, self assembly layer by layer, phase separation method, electrochemical method etc.But above method all is not suitable for the large-area super-double-hydrophobic surface of preparation.
Summary of the invention
Technical problem solved by the invention is to provide a kind of artificial method for planting of super two thin self-cleaning surface fine nanostructurs, this is the artificial method for planting of the super two thin self-cleaning surface fine nanostructurs of a kind of large tracts of land preparation, can be in order to solve the shortcoming in the above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
A kind of artificial method for planting of super two thin self-cleaning surface fine nanostructurs utilizes the main body of the surface fine nanostructured with super two thin characteristics to be clubbed nano-cellulose; The clubbed nano-cellulose nanofibrils is realized controlled orderly directional planting in the mode of electrostatic spinning at substrate surface; Flocked surface is modified through fluorine-containing reagent, and self assembly forms the fluorine-containing long chain alkyl silane molecule of one deck, obtains super two thin self-cleaning surface fine nanostructur.
Its concrete operation step is as follows:
1), preparation clubbed nano-cellulose: adopt strong acid-hydrolyzed method to prepare the clubbed nano-cellulose nanofibrils: fibrous raw material is dispersed in aqueous sulfuric acid, the stirring reaction certain hour, add the ice cube cessation reaction and make system be down to room temperature at a certain temperature.Centrifuge washing is to neutral, and taking precipitate is removed impurity with one week of deionized water dialysis, and freeze drying obtains the clubbed nano-cellulose nanofibrils.
2), the artificial growth of nano-cellulose nanofibrils: the sheet material that the plate face is clean is put into flocking plant, pass through successively the coating of sheet material adhesive, flocking, drying procedure, sequencing control to realize the orderly directed artificial growth based on the fine nanostructur surface of nano-cellulose nanofibrils.
3), the super two thin functionalization of nanofibrils flocked surface: the nanofibrils flocked surface that obtains in step (2) soaking at room temperature certain hour in fluorine-containing decorating liquid, use successively subsequently toluene, the ethanol rinse, dry under certain condition after rinse, obtain having super two thin self-cleaning surfaces of fine nanostructur.
In the present invention, described fibrous raw material is wood pulp cellulose, paper pulp fiber, bamboo pulp fiber, any one in cotton fiber or flaxen fiber and combination thereof.
In the present invention, aqueous sulfuric acid concentration is 50～64wt%, and reaction temperature is 20 ℃～50 ℃, and the reaction time is 30～60min.
In the present invention, described sheet material is that thickness is 0.1～1mm, and width is aluminium alloy, copper alloy, zinc alloy plate or the alloy steel products of 500～1500mm.
In the present invention, described adhesive is the curing epoxy resin adhesive stick, and curing epoxy resin adhesive stick coating weight is: 80～100g/m
2
The present invention is when electrostatic spinning, and the operating voltage of flocking plant is: 35～50kV, and electric current is: 0.5～5mA, and flocked pile is the nano-cellulose nanofibrils, and the fine hair diameter is 10～50nm, and villus length is 100～500nm, and the flocking amount is: 10～12g/m
2
In the present invention, described fluorine-containing decorating liquid is the toluene solution of 17 fluorine decyl trimethoxy silanes, and concentration is 1～2wt%, and the modification time is 4～24h.
In the present invention, drying is carried out when processing in super two thin planting suedes surfaces, dry treatment temperature is 80～120 ℃, and the dry processing time is 5～10min.
Advantage of the present invention and beneficial effect are:
1), the nano-cellulose fiber material that adopts of the present invention is general wood pulp cellulose, paper pulp fiber, bamboo pulp fiber, cotton fiber, any one in flaxen fiber.The cellulolytic method of method for making-strong acid commonly used with nano-cellulose prepares the nano-cellulose nanofibrils, and technique is simple, and is easy to operate, and cost is low.
2), the nanostructured surface of the present invention's preparation has well super-hydrophobic, super oleophobic property, and have good chemical stability, place at ambient temperature after some months drop substantially remain unchanged at the contact angle of these super two thin nanostructured surfaces (＞150 °).The nanostructured surface of the present invention's preparation also has good automatically cleaning ability.
3), the present invention is used for the super two thin self-cleaning surface fine nanostructurs of large tracts of land artificial growth, has potential application foreground widely in each fields such as medical science, textile industry, fine chemistry industry, construction materials.
The specific embodiment
The below gives an actual example and describes the present invention.
Technical solution of the present invention is including, but not limited to the following cited specific embodiment.
The specific embodiment 1:
A kind of artificial method for planting of super two thin self-cleaning surface fine nanostructurs carries out as follows:
Acid hydrolysis prepares clubbed nano-cellulose: fibrous raw material is dispersed in the 50wt% aqueous sulfuric acid, at 50 ℃ of stirring reaction 30min, adds 500g ice cube cessation reaction and make system be down to room temperature.Centrifuge washing is to neutral, and taking precipitate is removed impurity with one week of deionized water dialysis, and freeze drying obtains the clubbed nano-cellulose nanofibrils.
The artificial growth of nano-cellulose nanofibrils: selecting thickness is 1mm, width be the aluminum alloy plate materials of 1000mm as base material, be that 80g/m2 is coated on aluminum alloy sheet material surface with the curing epoxy resin adhesive stick by coating weight; Then be 50kV with the nano-cellulose nanofibrils at voltage, electric current is 5mA, and the flocking amount is that condition servant's work post of 10g/m ° is implanted in aluminum alloy sheet material surface.
The self assembly of nanofibrils flocked surface forms fluorine-containing long chain alkyl silane molecular layer: the nanofibrils flocked surface that step (2) obtains is soaking at room temperature 24h in the toluene solution of the 17 fluorine decyl trimethoxy silanes of 1wt%, use successively subsequently toluene, the ethanol rinse, 100 ℃ of dry 10min after rinse, acquisition has super two thin self-cleaning surfaces of fine nanostructur.
The fine nanostructur surface of the present invention preparation has well super-hydrophobic, super oleophobic property, and have good chemical stability, place at ambient temperature the contact angle on this super two thin fine nanostructurs surfaces of drop after some months substantially remain unchanged (＞150 °).The fine nanostructur surface of the present invention preparation also has good automatically cleaning ability.
The specific embodiment 2:
A kind of artificial method for planting of super two thin self-cleaning surface fine nanostructurs carries out as follows:
Acid hydrolysis prepares clubbed nano-cellulose: fibrous raw material is dispersed in the 50wt% aqueous sulfuric acid, at 20 ℃ of stirring reaction 60min.Centrifuge washing is to neutral, and taking precipitate is removed impurity with one week of deionized water dialysis, and freeze drying obtains the clubbed nano-cellulose nanofibrils.
The artificial growth of nano-cellulose nanofibrils: selecting thickness is 0.5mm, width be the alloy steel products of 1000mm as base material, be 100g/m with the curing epoxy resin adhesive stick by coating weight
2Be coated on the alloy steel products surface; Then be 50kV with the nano-cellulose nanofibrils at voltage, electric current is 0.5mA, and the flocking amount is 12g/m
2Condition servant's work post be implanted in steel alloy sheet material surface.
The self assembly of nanofibrils flocked surface forms fluorine-containing long chain alkyl silane molecular layer: the nanofibrils flocked surface that step (2) obtains is soaking at room temperature 4h in the toluene solution of the 17 fluorine decyl trimethoxy silanes of 2wt%, use successively subsequently toluene, the ethanol rinse, 80 ℃ of dry 10min after rinse, acquisition has super two thin self-cleaning surfaces of fine nanostructur.
The fine nanostructur surface of the present invention preparation has well super-hydrophobic, super oleophobic property, and have good chemical stability, place at ambient temperature the contact angle on this super two thin fine nanostructurs surfaces of drop after some months substantially remain unchanged (＞150 °).The fine nanostructur surface of the present invention preparation also has good automatically cleaning ability.
The specific embodiment 3:
A kind of artificial method for planting of super two thin self-cleaning surface fine nanostructurs carries out as follows:
Acid hydrolysis prepares clubbed nano-cellulose: fibrous raw material is dispersed in the 64wt% aqueous sulfuric acid, at 50 ℃ of stirring reaction 60min, adds 500g ice cube cessation reaction and make system be down to room temperature.Centrifuge washing is to neutral, and taking precipitate is removed impurity with one week of deionized water dialysis, and freeze drying obtains the clubbed nano-cellulose nanofibrils.
The artificial growth of nano-cellulose nanofibrils: selecting thickness is 1mm, width be the zinc alloy plate of 1000mm as base material, be 90g/m with the curing epoxy resin adhesive stick by coating weight
2Be coated on the zinc alloy plate surface; Then be 35kV with the nano-cellulose nanofibrils at voltage, electric current is 3mA, and the flocking amount is 10g/m
2Condition servant's work post be implanted in the zinc alloy plate surface.
The self assembly of nanofibrils flocked surface forms fluorine-containing long chain alkyl silane molecular layer: the nanofibrils flocked surface that step (2) obtains is soaking at room temperature 24h in the toluene solution of the 17 fluorine decyl trimethoxy silanes of 1.5wt%, use successively subsequently toluene, the ethanol rinse, 120 ℃ of dry 5min after rinse, acquisition has super two thin self-cleaning surfaces of fine nanostructur.
The fine nanostructur surface of the present invention preparation has well super-hydrophobic, super oleophobic property, and have good chemical stability, place at ambient temperature the contact angle on this super two thin fine nanostructurs surfaces of drop after some months substantially remain unchanged (＞150 °).The fine nanostructur surface of the present invention preparation also has good automatically cleaning ability.
The specific embodiment 4:
A kind of artificial method for planting of super two thin self-cleaning surface fine nanostructurs carries out as follows:
Acid hydrolysis prepares clubbed nano-cellulose: fibrous raw material is dispersed in the 64wt% aqueous sulfuric acid, at 40 ℃ of stirring reaction 60min, adds 500g ice cube cessation reaction and make system be down to room temperature.Centrifuge washing is to neutral, and taking precipitate is removed impurity with one week of deionized water dialysis, and freeze drying obtains the clubbed nano-cellulose nanofibrils.
The artificial growth of nano-cellulose nanofibrils: selecting thickness is 0.5mm, width be the copper alloy plate of 500mm as base material, be 90g/m with the curing epoxy resin adhesive stick by coating weight
2Be coated on the copper alloy plate surface; Then be 35kV with the nano-cellulose nanofibrils at voltage, electric current is 5mA, and the flocking amount is 10g/m
2Condition servant's work post be implanted in the copper alloy plate surface.
The self assembly of nanofibrils flocked surface forms fluorine-containing long chain alkyl silane molecular layer: the nanofibrils flocked surface that step (2) obtains is soaking at room temperature 12h in the toluene solution of the 17 fluorine decyl trimethoxy silanes of 1wt%, use successively subsequently toluene, the ethanol rinse, dry 5min in 100 ℃ after rinse, acquisition has super two thin self-cleaning surfaces of fine nanostructur.
Has well super-hydrophobic, super oleophobic property by the fine nanostructur surface for preparing in above-mentioned four embodiment, and have good chemical stability, place at ambient temperature the contact angle on this super two thin fine nanostructurs surfaces of drop after some months substantially remain unchanged (＞150 °).The fine nanostructur surface of the present invention preparation also has good automatically cleaning ability.
Above demonstration and described basic principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; that describes in above-described embodiment and specification just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (6)
1. the artificial method for planting of super two thin self-cleaning surface fine nanostructurs, is characterized in that, utilizes the main body of the surface fine nanostructured with super two thin characteristics to be clubbed nano-cellulose; The clubbed nano-cellulose nanofibrils is realized controlled orderly directional planting in the mode of electrostatic spinning at substrate surface; Flocked surface is modified through fluorine-containing reagent, and self assembly forms the fluorine-containing long chain alkyl silane molecule of one deck, obtains super two thin self-cleaning surface fine nanostructur, and its concrete operation step is as follows:
1), preparation clubbed nano-cellulose: adopt strong acid-hydrolyzed method to prepare the clubbed nano-cellulose nanofibrils, fibrous raw material is dispersed in aqueous sulfuric acid, stirring reaction 30～60min under 20 ℃～50 ℃ conditions, add the ice cube cessation reaction and make system be down to room temperature, centrifuge washing is to neutral, taking precipitate is removed impurity with one week of deionized water dialysis, and freeze drying obtains the clubbed nano-cellulose nanofibrils;
2), the artificial growth of nano-cellulose nanofibrils: the sheet material that the plate face is clean is put into flocking plant, carry out flocking associative operation program through the sheet material adhesive successively, in this process, the operating voltage of flocking plant is: 35～50kV, electric current is: 0.5～5mA, and flocked pile is the nano-cellulose nanofibrils, the fine hair diameter is 10～50nm, villus length is 100～500nm, and the flocking amount is: 10～12g/m
2
3), the super two thin functionalization of nanofibrils flocked surface: the nanofibrils flocked surface that obtains in step (2) soaking at room temperature certain hour in fluorine-containing decorating liquid, use successively subsequently toluene, the ethanol rinse, dry under certain condition after rinse, dry treatment temperature is 80～120 ℃, the dry processing time is 5～10min, obtains having super two thin self-cleaning surfaces of fine nanostructur.
2. the artificial method for planting of a kind of super two thin self-cleaning surface fine nanostructurs according to claim 1 is characterized in that: described in described step 1) aqueous sulfuric acid concentration be 50～64wt%.
3. the artificial method for planting of a kind of super two thin self-cleaning surface fine nanostructurs according to claim 1, it is characterized in that: described fibrous raw material is wood pulp cellulose, paper pulp fiber, bamboo pulp fiber, any one in cotton fiber or flaxen fiber and combination thereof.
4. the artificial method for planting of a kind of super two thin self-cleaning surface fine nanostructurs according to claim 1, it is characterized in that: described sheet material is that thickness is 0.1～1mm, and width is aluminium alloy, copper alloy, kirsite or the steel alloy sheet material of 500～1500mm.
5. the artificial method for planting of a kind of super two thin self-cleaning surface fine nanostructurs according to claim 1, it is characterized in that: described adhesive is the curing epoxy resin adhesive stick, curing epoxy resin adhesive stick coating weight is 80～100g/m
2
6. the artificial method for planting of a kind of super two thin self-cleaning surface fine nanostructurs according to claim 1, it is characterized in that: described fluorine-containing decorating liquid is the toluene solution of 17 fluorine decyl trimethoxy silanes, concentration is 1～2wt%, and the modification time is 4～24h.
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| CN110467849A (en) * | 2019-08-16 | 2019-11-19 | 于素阁 | A kind of EPA modified nanometer cellulose-nano-ZnO super hydrophobic material and its preparation method |
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