CN116855174A - Anti-icing lignin super-hydrophobic coating and preparation method and application thereof - Google Patents
Anti-icing lignin super-hydrophobic coating and preparation method and application thereof Download PDFInfo
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- CN116855174A CN116855174A CN202310905612.4A CN202310905612A CN116855174A CN 116855174 A CN116855174 A CN 116855174A CN 202310905612 A CN202310905612 A CN 202310905612A CN 116855174 A CN116855174 A CN 116855174A
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- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 117
- 238000000576 coating method Methods 0.000 title claims abstract description 102
- 239000011248 coating agent Substances 0.000 title claims abstract description 100
- 229920005610 lignin Polymers 0.000 title claims abstract description 98
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 158
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 114
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 81
- 238000003756 stirring Methods 0.000 claims abstract description 72
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims abstract description 69
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 56
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 51
- 229910000077 silane Inorganic materials 0.000 claims abstract description 51
- 239000008367 deionised water Substances 0.000 claims abstract description 42
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 42
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 42
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 42
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 38
- 239000003822 epoxy resin Substances 0.000 claims abstract description 33
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 33
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 32
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 21
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 10
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 239000007921 spray Substances 0.000 claims description 68
- 238000001291 vacuum drying Methods 0.000 claims description 50
- 239000000203 mixture Substances 0.000 claims description 25
- 229920005611 kraft lignin Polymers 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 11
- 230000005540 biological transmission Effects 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 239000011268 mixed slurry Substances 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 3
- RCHUVCPBWWSUMC-UHFFFAOYSA-N trichloro(octyl)silane Chemical compound CCCCCCCC[Si](Cl)(Cl)Cl RCHUVCPBWWSUMC-UHFFFAOYSA-N 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 14
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 124
- 239000012496 blank sample Substances 0.000 description 39
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 35
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 22
- 239000002244 precipitate Substances 0.000 description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 18
- 239000011521 glass Substances 0.000 description 18
- 230000008014 freezing Effects 0.000 description 17
- 238000007710 freezing Methods 0.000 description 17
- 230000002209 hydrophobic effect Effects 0.000 description 17
- 230000003068 static effect Effects 0.000 description 15
- 239000000741 silica gel Substances 0.000 description 13
- 229910002027 silica gel Inorganic materials 0.000 description 13
- 239000002253 acid Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 12
- 238000007599 discharging Methods 0.000 description 12
- 238000007789 sealing Methods 0.000 description 12
- 239000002023 wood Substances 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 11
- 238000000643 oven drying Methods 0.000 description 11
- 239000006228 supernatant Substances 0.000 description 11
- 238000004140 cleaning Methods 0.000 description 9
- 238000002791 soaking Methods 0.000 description 9
- 229910000838 Al alloy Inorganic materials 0.000 description 6
- 239000000123 paper Substances 0.000 description 6
- 238000005498 polishing Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 238000005096 rolling process Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002352 surface water Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 241000533950 Leucojum Species 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 241001179707 Penthe Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D197/00—Coating compositions based on lignin-containing materials
- C09D197/005—Lignin
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/18—Materials not provided for elsewhere for application to surfaces to minimize adherence of ice, mist or water thereto; Thawing or antifreeze materials for application to surfaces
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- C—CHEMISTRY; METALLURGY
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Combustion & Propulsion (AREA)
- Materials Applied To Surfaces To Minimize Adherence Of Mist Or Water (AREA)
Abstract
The invention discloses an anti-icing lignin super-hydrophobic coating, a preparation method and application thereof, wherein the anti-icing lignin super-hydrophobic coating comprises the following components in parts by weight: 1-10 parts of silane modified lignin; 1-5 parts of nano silicon dioxide; 50-100 parts of acetone; 1-3 parts of polydimethylsiloxane; 1-3 parts of epoxy resin; 0.1 to 0.5 part of polydimethylsiloxane curing agent; 0.1 to 0.5 part of epoxy resin curing agent diethylenetriamine; the preparation method of the silane modified lignin comprises the following steps: adding imidazole into lignin solution in an inert atmosphere, and stirring for a set time to obtain a mixed solution; then dripping the acetone solution of the silane reagent into the mixed solution, heating and stirring for reaction; and after the reaction is finished, adding acetone into the reaction system, stirring, adding deionized water into the reaction system, precipitating, separating and drying the modified lignin to obtain the silane modified lignin. The coating prepared by the super-hydrophobic coating has excellent anti-icing performance.
Description
Technical Field
The invention relates to the field of hydrophobic coatings, in particular to an anti-icing lignin super-hydrophobic coating, and a preparation method and application thereof.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
The icing of the power transmission line means that raindrops or snowflakes are condensed on the power transmission line, the weight and wind resistance of the power transmission line are increased, the problem of ice flash and overload of the insulating part is caused, and even the tower body is collapsed when serious, so that the safe operation of a power grid is threatened.
Current deicing technologies mainly include active and passive categories. The active ice breaking method is mainly an electrothermal method, namely ice melting is carried out by utilizing short-circuit current or direct current and other methods, and the method is simple and efficient, but has high energy consumption, and when the ice is melted in continuous rainy and snowy weather, the line after ice melting is covered again, and the ice melting is needed to be heated again or for multiple times, so that the risk of accidents in the operation process is increased.
The passive ice breaking method mainly comprises the steps of constructing a super-hydrophobic surface, reducing or eliminating the adhesion force of ice on the surface of a coating by reducing the interaction between the surface of a power transmission line and water molecules, and enabling the surface of the power transmission line coated with the coating to have certain anti-icing capacity, so that excessive consumption of energy is avoided. The super-hydrophobic surface is constructed based on the 'lotus leaf effect' bionic, and the static contact angle on the surface of the matrix is larger than 150 degrees, and the rolling contact angle is smaller than 10 degrees. The existing preparation method has the problems of complex preparation process, high production cost, limited coating method, poor anti-icing performance and the like, and is difficult to widely apply.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide the anti-icing lignin super-hydrophobic coating, and the preparation method and application thereof, and solves the problems of reduced power transmission efficiency and service life caused by icing of the surface of a power transmission line.
In order to achieve the above object, the present invention is realized by the following technical scheme:
in a first aspect, the invention provides an anti-icing lignin superhydrophobic coating, which comprises the following components in parts by weight: 1-10 parts of silane modified lignin; 1-5 parts of nano silicon dioxide; 50-100 parts of acetone; 1-3 parts of polydimethylsiloxane; 1-3 parts of epoxy resin; 0.1 to 0.5 part of polydimethylsiloxane curing agent; 0.1 to 0.5 part of epoxy resin curing agent diethylenetriamine;
the preparation method of the silane modified lignin comprises the following steps: adding imidazole into lignin solution in an inert atmosphere, dissolving lignin, and stirring for a set time to obtain a mixed solution;
then, dripping the acetone solution containing the silane reagent into the mixed solution, heating and stirring to react:
and after the reaction is finished, adding acetone into the reaction system, stirring to dissolve the modified lignin agglomerates, adding deionized water into the mixture to precipitate, separate and dry the modified lignin, thus obtaining the silane modified lignin.
Silane modified lignin: the main raw materials and other supplementary raw materials form a coating.
Nano silicon dioxide: the secondary raw material reacts with polydimethylsiloxane to generate PDMS/SiO 2 A composite material.
Polydimethyl siloxane: PDMS/SiO with nano silicon dioxide 2 A nanocomposite.
Epoxy resin: improving silane modified lignin and PDMS/SiO 2 The bonding degree of the composite particles increases the adhesive force between the coating and the surface of the substrate, and enhances the mechanical strength of the coating.
Diethylenetriamine: and (3) an epoxy resin curing agent.
Imidazole action: dissolving lignin.
Inert atmosphere: the imidazole is protected from oxidation.
Acetone was added to dissolve the modified lignin pellet.
Reaction principle:
in a nitrogen atmosphere, imidazole is added into lignin solution to dissolve lignin, silane-containing reagents such as 1H, 2H-perfluorooctyl trichlorosilane and the like are dripped into the lignin to modify the lignin, reaction sites occur at hydroxyl positions on the surface of the lignin, hydroxyl groups are replaced by silane, and fluorine-containing branched chains are introduced to obtain silane modified lignin.
In some embodiments, the mass ratio of lignin, imidazole, and silane reagents is 1-3:2-4:1-5.
In some embodiments, the lignin is kraft lignin or alkali lignin.
In some embodiments, imidazole is added to the lignin solution for a period of 1-5 hours. The stirring function is to uniformly disperse the imidazole in the solution.
In some embodiments, the heating temperature of the heated agitation reaction is 45-55deg.C and the agitation time is 12-24 hours.
In some embodiments, the silane reagent is 1h,2 h-perfluorooctyl trichlorosilane (FOTS).
In some embodiments, the epoxy is E-44 or E-51.
In some embodiments, the epoxy curing agent is diethylenetriamine or ethylenediamine.
In some embodiments, the polydimethylsiloxane curative is dakaning DC184.
In a second aspect, the invention provides a preparation method of the anti-icing lignin super-hydrophobic coating, which comprises the following steps:
adding silane modified lignin, nano silicon dioxide, polydimethylsiloxane and epoxy resin into acetone according to a proportion, and stirring and uniformly mixing to obtain mixed slurry;
and then adding the polydimethylsiloxane curing agent and the epoxy resin curing agent into the mixed slurry according to a proportion, and uniformly mixing to obtain the super-hydrophobic coating.
In a third aspect, the invention provides a method for preparing an anti-icing lignin superhydrophobic coating, comprising the following steps: and adding the super-hydrophobic coating into a spray pen, spraying the coating on the surface of a substrate, and then placing the substrate into a vacuum drying oven for curing at 60-90 ℃ for 1-10 hours to obtain the super-hydrophobic coating.
In a fourth aspect, the invention provides an application of the anti-icing lignin super-hydrophobic coating in preparation of a power transmission line.
The beneficial effects achieved by one or more embodiments of the present invention described above are as follows:
1) The biomass lignin is used as a raw material to prepare the coating, and the coating has the advantages of being renewable, green, environment-friendly, pollution-free and the like;
2) The super-hydrophobic coating has no requirements on the type, size and shape of the substrate material, and expands the application range of the super-hydrophobic coating;
3) The coating prepared by the superhydrophobic coating has superhydrophobic performance, a static contact angle of 163 degrees, a dynamic contact angle of 1 degree, and excellent anti-icing performance, and icing time is three times that of a common surface.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is a graph of contact angles of the superhydrophobic coating prepared in example 1;
fig. 2 is an anti-icing effect graph of the superhydrophobic coating prepared in example 1, in which (a) a surface water droplet icing photograph of the superhydrophobic coating attached to the surface and (b) a surface water droplet icing photograph of the sample not attached to the superhydrophobic coating are shown.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The invention is further illustrated below with reference to examples.
Example 1
(1) Preparing an aluminum alloy sample with the specification of 76 x 26 x 1mm, polishing by using 600# abrasive paper, soaking in ethanol solution, ultrasonically cleaning, drying by using a vacuum drying oven at 60 ℃, and then placing into a dryer with silica gel for later use.
(2) 2g of kraft lignin is weighed by an electronic balance and dispersed in 60mL of deionized water, and the solution A is obtained by stirring at 300r/min for 5min at room temperature. Solution A was poured into a 250mL three-necked flask and stirring was continued at 0.5m 3 Nitrogen was introduced at a flow rate of/h, 3.5g of imidazole was weighed into solution A by means of an electronic balance and stirred for 1h. The acetone is measured by a measuring cylinder and poured into a beaker, 8mL of FOTS is measured by the measuring cylinder and poured into 30mL of acetone solution, the beaker is sealed by adopting a sealing film, and the solution B is obtained by stirring for 1h at 300 r/min. Dropwise adding the solution B into the solution A by using an acid buret, heating to 50 ℃, stirring for 24 hours, pouring 300mL of deionized water to precipitate lignin, standing for 30 minutes, pouring the solution A into a centrifuge tube, putting into the centrifuge to centrifugally precipitate for 10 minutes, pouring out supernatant, putting the precipitate into a vacuum drying oven, and vacuum drying at 85 ℃ for 12 hours to obtain silane modified lignin.
(3) 100mg of silane modified lignin and 100mg of nano silicon dioxide are respectively weighed by an electronic balance and blended in 10mL of acetone to obtain a solution C, 0.16mL of polydimethylsiloxane and 0.05mL of epoxy resin are removed by a pipette, discharged into the solution C, and stirred for 15min at room temperature of 500 r/min. And measuring 0.016mL of polydimethylsiloxane curing agent and 0.05mL of diethylenetriamine by using a pipette, discharging the mixture into the solution C, and stirring the mixture for 15min to obtain the super-hydrophobic coating.
(4) According to 0.0016g/cm 2 The spray amount of the super-hydrophobic coating is that the super-hydrophobic coating is poured into a spray pen, the caliber of the spray pen is adjusted to be 0.5mm, the distance between the spray pen and a sample is 15cm, the spray pen and the sample are placed into a vacuum drying oven after being sprayed on the surface of the sample, the spray pen is cured for 10 hours at 85 ℃ to obtain the super-hydrophobic coating, the static contact angle is 158 degrees, and the dynamic contact angle is 1 degree, as shown in figure 1.
(5) The blank sample and the super-hydrophobic sample are placed in a freezer at-18 ℃ for pre-freezing for 3min, 50 mu L of deionized water at 1 ℃ is dripped, the icing time of the water drop on the surface of the super-hydrophobic sample is 185s, and the icing time of the water drop on the surface of the blank sample is 62s, as shown in figure 2. The delay icing time of the super-hydrophobic sample is about three times that of the blank sample, which indicates that the super-hydrophobic sample has certain anti-icing performance.
Example 2
(1) Preparing an aluminum alloy sample with the specification of 76 x 26 x 1mm, polishing by using 600# abrasive paper, soaking in ethanol solution, ultrasonically cleaning, drying by using a vacuum drying oven at 60 ℃, and then placing into a dryer with silica gel for later use.
(2) 2g of kraft lignin is weighed by an electronic balance and dispersed in 60mL of deionized water, and the solution A is obtained by stirring at 300r/min for 5min at room temperature. Solution A was poured into a 250mL three-necked flask and stirring was continued at 0.5m 3 Nitrogen was introduced at a flow rate of/h, 3.5g of imidazole was weighed into solution A by means of an electronic balance and stirred for 1h. The acetone is measured by a measuring cylinder and poured into a beaker, 2mL of FOTS is measured by the measuring cylinder and poured into 36mL of acetone solution, the beaker is sealed by adopting a sealing film, and the solution B is obtained by stirring for 1h at 300 r/min. Dropwise adding the solution B into the solution A by using an acid buret, heating to 50 ℃, stirring for 24 hours, pouring 300mL of deionized water to precipitate lignin, standing for 30 minutes, pouring the solution A into a centrifuge tube, putting into the centrifuge to centrifugally precipitate for 10 minutes, pouring out supernatant, putting the precipitate into a vacuum drying oven, and vacuum drying at 85 ℃ for 12 hours to obtain silane modified lignin.
(3) 100mg of silane modified lignin and 100mg of nano silicon dioxide are respectively weighed by an electronic balance and blended in 10mL of acetone to obtain a solution C, 0.16mL of polydimethylsiloxane and 0.05mL of epoxy resin are removed by a pipette, discharged into the solution C, and stirred for 15min at room temperature of 500 r/min. And measuring 0.016mL of polydimethylsiloxane curing agent and 0.05mL of diethylenetriamine by using a pipette, discharging the mixture into the solution C, and stirring the mixture for 15min to obtain the super-hydrophobic coating.
(4) According to 0.0016g/cm 2 The super-hydrophobic paint is poured into a spray pen, the caliber of the spray pen is regulated to be 0.5mm, the distance between the spray pen and a sample is 15cm, and the spray pen is placed into a vacuum drying oven after being sprayed on the surface of the sample, and the temperature is 85 DEG CCuring for 10 hours to obtain the super-hydrophobic coating, wherein the static contact angle is 157 degrees, and the dynamic contact angle is 1 degree.
(5) And (3) placing the blank sample and the superhydrophobic sample into a freezer at the temperature of minus 18 ℃ for pre-freezing for 3min, and dripping 50 mu L of deionized water at the temperature of 1 ℃ to measure that the icing time of the water drops on the surface of the superhydrophobic sample is 178s and the icing time of the water drops on the surface of the blank sample is 61s. The delay icing time of the super-hydrophobic sample is about three times that of the blank sample, which indicates that the super-hydrophobic sample has certain anti-icing performance.
Example 3
(1) Preparing an aluminum alloy sample with the specification of 76 x 26 x 1mm, polishing by using 600# abrasive paper, soaking in ethanol solution, ultrasonically cleaning, drying by using a vacuum drying oven at 60 ℃, and then placing into a dryer with silica gel for later use.
(2) 2g of kraft lignin is weighed by an electronic balance and dispersed in 60mL of deionized water, and the solution A is obtained by stirring at 300r/min for 5min at room temperature. Solution A was poured into a 250mL three-necked flask and stirring was continued at 0.5m 3 Nitrogen was introduced at a flow rate of/h, 3.5g of imidazole was weighed into solution A by means of an electronic balance and stirred for 1h. The acetone is measured by a measuring cylinder and poured into a beaker, 4mL of FOTS is measured by the measuring cylinder and poured into 34mL of acetone solution, the beaker is sealed by adopting a sealing film, and the solution B is obtained by stirring for 1h at 300 r/min. Dropwise adding the solution B into the solution A by using an acid buret, heating to 50 ℃, stirring for 24 hours, pouring 300mL of deionized water to precipitate lignin, standing for 30 minutes, pouring the solution A into a centrifuge tube, putting into the centrifuge to centrifugally precipitate for 10 minutes, pouring out supernatant, putting the precipitate into a vacuum drying oven, and vacuum drying at 85 ℃ for 12 hours to obtain silane modified lignin.
(3) 100mg of silane modified lignin and 100mg of nano silicon dioxide are respectively weighed by an electronic balance and blended in 10mL of acetone to obtain a solution C, 0.16mL of polydimethylsiloxane and 0.05mL of epoxy resin are removed by a pipette, discharged into the solution C, and stirred for 15min at room temperature of 500 r/min. And measuring 0.016mL of polydimethylsiloxane curing agent and 0.05mL of diethylenetriamine by using a pipette, discharging the mixture into the solution C, and stirring the mixture for 15min to obtain the super-hydrophobic coating.
(4) According to 0.0016g/cm 2 The super-hydrophobic paint is poured into a spray pen according to the spraying amount of the paint, and the caliber of the spray penThe distance between the spray pen and the sample is adjusted to be 0.5mm, the distance between the spray pen and the sample is 15cm, the spray pen and the sample are placed into a vacuum drying oven after being sprayed on the surface of the sample, and the spray pen is cured for 10 hours at 85 ℃ to obtain the super-hydrophobic coating, wherein the static contact angle is 154 degrees, and the dynamic contact angle is 3 degrees.
(5) And (3) placing the blank sample and the super-hydrophobic sample into a freezer at the temperature of minus 18 ℃ for pre-freezing for 3min, and dripping 50 mu L of deionized water at the temperature of 1 ℃ to measure the icing time of the water drops on the surface of the super-hydrophobic sample to be 172s and the icing time of the water drops on the surface of the blank sample to be 62s. The delay icing time of the super-hydrophobic sample is about three times that of the blank sample, which indicates that the super-hydrophobic sample has certain anti-icing performance.
Example 4
(1) Preparing a glass sample with the specification of 76 x 26 x 1mm, soaking the glass sample in ethanol solution, ultrasonically cleaning the glass sample, flushing the glass sample with deionized water, drying the glass sample in a vacuum drying oven at 60 ℃, and then placing the glass sample in a dryer with silica gel for later use.
(2) 2g of kraft lignin is weighed by an electronic balance and dispersed in 60mL of deionized water, and the solution A is obtained by stirring at 300r/min for 5min at room temperature. Solution A was poured into a 250mL three-necked flask and stirring was continued at 0.5m 3 Nitrogen was introduced at a flow rate of/h, 3.5g of imidazole was weighed into solution A by means of an electronic balance and stirred for 1h. The acetone is measured by a measuring cylinder and poured into a beaker, 8mL of FOTS is measured by the measuring cylinder and poured into 30mL of acetone solution, the beaker is sealed by adopting a sealing film, and the solution B is obtained by stirring for 1h at 300 r/min. Dropwise adding the solution B into the solution A by using an acid buret, heating to 50 ℃, stirring for 24 hours, pouring 300mL of deionized water to precipitate lignin, standing for 30 minutes, pouring the solution A into a centrifuge tube, putting into the centrifuge to centrifugally precipitate for 10 minutes, pouring out supernatant, putting the precipitate into a vacuum drying oven, and vacuum drying at 85 ℃ for 12 hours to obtain silane modified lignin.
(3) 100mg of silane modified lignin and 100mg of nano silicon dioxide are respectively weighed by an electronic balance and blended in 10mL of acetone to obtain a solution C, 0.16mL of polydimethylsiloxane and 0.05mL of epoxy resin are removed by a pipette, discharged into the solution C, and stirred for 15min at room temperature of 500 r/min. And measuring 0.016mL of polydimethylsiloxane curing agent and 0.05mL of diethylenetriamine by using a pipette, discharging the mixture into the solution C, and stirring the mixture for 15min to obtain the super-hydrophobic coating.
(4) According to 0.0016g/cm 2 The super-hydrophobic coating is poured into a spray pen, the caliber of the spray pen is adjusted to be 0.5mm, the distance between the spray pen and a sample is 15cm, the spray pen is placed into a vacuum drying oven after being sprayed on the surface of the sample, the spray pen is cured for 10 hours at 85 ℃ to obtain the super-hydrophobic coating, the static contact angle is 157 degrees, and the dynamic contact angle is 1 degree.
(5) And (3) placing the blank sample and the super-hydrophobic sample into a freezer at the temperature of minus 18 ℃ for pre-freezing for 3min, and dripping 50 mu L of deionized water at the temperature of 1 ℃ to measure the icing time of the water drops on the surface of the super-hydrophobic sample to be 194s and the icing time of the water drops on the surface of the blank sample to be 63s. The delay icing time of the super-hydrophobic sample is about three times that of the blank sample, which indicates that the super-hydrophobic sample has certain anti-icing performance.
Example 5
(1) Preparing a glass sample with the specification of 76 x 26 x 1mm, soaking the glass sample in ethanol solution, ultrasonically cleaning the glass sample, flushing the glass sample with deionized water, drying the glass sample in a vacuum drying oven at 60 ℃, and then placing the glass sample in a dryer with silica gel for later use.
(2) 2g of kraft lignin is weighed by an electronic balance and dispersed in 60mL of deionized water, and the solution A is obtained by stirring at 300r/min for 5min at room temperature. Solution A was poured into a 250mL three-necked flask and stirring was continued at 0.5m 3 Nitrogen was introduced at a flow rate of/h, 3.5g of imidazole was weighed into solution A by means of an electronic balance and stirred for 1h. The acetone is measured by a measuring cylinder and poured into a beaker, 2mL of FOTS is measured by the measuring cylinder and poured into 36mL of acetone solution, the beaker is sealed by adopting a sealing film, and the solution B is obtained by stirring for 1h at 300 r/min. Dropwise adding the solution B into the solution A by using an acid buret, heating to 50 ℃, stirring for 24 hours, pouring 300mL of deionized water to precipitate lignin, standing for 30 minutes, pouring the solution A into a centrifuge tube, putting into the centrifuge to centrifugally precipitate for 10 minutes, pouring out supernatant, putting the precipitate into a vacuum drying oven, and vacuum drying at 85 ℃ for 12 hours to obtain silane modified lignin.
(3) 100mg of silane modified lignin and 100mg of nano silicon dioxide are respectively weighed by an electronic balance and blended in 10mL of acetone to obtain a solution C, 0.16mL of polydimethylsiloxane and 0.05mL of epoxy resin are removed by a pipette, discharged into the solution C, and stirred for 15min at room temperature of 500 r/min. And measuring 0.016mL of polydimethylsiloxane curing agent and 0.05mL of diethylenetriamine by using a pipette, discharging the mixture into the solution C, and stirring the mixture for 15min to obtain the super-hydrophobic coating.
(4) According to 0.0016g/cm 2 The super-hydrophobic coating is poured into a spray pen, the caliber of the spray pen is adjusted to be 0.5mm, the distance between the spray pen and a sample is 15cm, the spray pen and the sample are placed into a vacuum drying oven after being sprayed on the surface of the sample, and the spray pen is cured for 10 hours at 85 ℃ to obtain the super-hydrophobic coating, wherein the static contact angle is 152 degrees, and the dynamic contact angle is 4 degrees.
(5) And (3) placing the blank sample and the super-hydrophobic sample into a freezer at the temperature of minus 18 ℃ for pre-freezing for 3min, and dripping 50 mu L of deionized water at the temperature of 1 ℃ to measure the icing time of water drops on the surface of the super-hydrophobic sample to be 167s and the icing time of water drops on the surface of the blank sample to be 61s. The delay icing time of the super-hydrophobic sample is about three times that of the blank sample, which indicates that the super-hydrophobic sample has certain anti-icing performance.
Example 6
(1) Preparing a glass sample with the specification of 76 x 26 x 1mm, soaking the glass sample in ethanol solution, ultrasonically cleaning the glass sample, flushing the glass sample with deionized water, drying the glass sample in a vacuum drying oven at 60 ℃, and then placing the glass sample in a dryer with silica gel for later use.
(2) 2g of kraft lignin is weighed by an electronic balance and dispersed in 60mL of deionized water, and the solution A is obtained by stirring at 300r/min for 5min at room temperature. Solution A was poured into a 250mL three-necked flask and stirring was continued at 0.5m 3 Nitrogen was introduced at a flow rate of/h, 3.5g of imidazole was weighed into solution A by means of an electronic balance and stirred for 1h. The acetone is measured by a measuring cylinder and poured into a beaker, 4mL of FOTS is measured by the measuring cylinder and poured into 34mL of acetone solution, the beaker is sealed by adopting a sealing film, and the solution B is obtained by stirring for 1h at 300 r/min. Dropwise adding the solution B into the solution A by using an acid buret, heating to 50 ℃, stirring for 24 hours, pouring 300mL of deionized water to precipitate lignin, standing for 30 minutes, pouring the solution A into a centrifuge tube, putting into the centrifuge to centrifugally precipitate for 10 minutes, pouring out supernatant, putting the precipitate into a vacuum drying oven, and vacuum drying at 85 ℃ for 12 hours to obtain silane modified lignin.
(3) 100mg of silane modified lignin and 100mg of nano silicon dioxide are respectively weighed by an electronic balance and blended in 10mL of acetone to obtain a solution C, 0.16mL of polydimethylsiloxane and 0.05mL of epoxy resin are removed by a pipette, discharged into the solution C, and stirred for 15min at room temperature of 500 r/min. And measuring 0.016mL of polydimethylsiloxane curing agent and 0.05mL of diethylenetriamine by using a pipette, discharging the mixture into the solution C, and stirring the mixture for 15min to obtain the super-hydrophobic coating.
(4) According to 0.0016g/cm 2 The super-hydrophobic coating is poured into a spray pen, the caliber of the spray pen is adjusted to be 0.5mm, the distance between the spray pen and a sample is 15cm, the spray pen and the sample are placed into a vacuum drying oven after being sprayed on the surface of the sample, and the spray pen is cured for 10 hours at 85 ℃ to obtain the super-hydrophobic coating, wherein the static contact angle is 154 degrees, and the dynamic contact angle is 2 degrees.
(5) And (3) placing the blank sample and the super-hydrophobic sample into a freezer at the temperature of minus 18 ℃ for pre-freezing for 3min, and dripping 50 mu L of deionized water at the temperature of 1 ℃ to measure 173s of the freezing time of the water drops on the surface of the super-hydrophobic sample and 62s of the freezing time of the water drops on the surface of the blank sample. The delay icing time of the super-hydrophobic sample is about three times that of the blank sample, which indicates that the super-hydrophobic sample has certain anti-icing performance.
Example 7
(1) Preparing a wood block sample with the specification of 50 x 31 x 9mm, drying the wood block sample in a vacuum drying oven at 60 ℃, and then placing the wood block sample in a dryer with silica gel for later use.
(2) 2g of kraft lignin is weighed by an electronic balance and dispersed in 60mL of deionized water, and the solution A is obtained by stirring at 300r/min for 5min at room temperature. Solution A was poured into a 250mL three-necked flask and stirring was continued at 0.5m 3 Nitrogen was introduced at a flow rate of/h, 3.5g of imidazole was weighed into solution A by means of an electronic balance and stirred for 1h. The acetone is measured by a measuring cylinder and poured into a beaker, 8mL of FOTS is measured by the measuring cylinder and poured into 30mL of acetone solution, the beaker is sealed by adopting a sealing film, and the solution B is obtained by stirring for 1h at 300 r/min. Dropwise adding the solution B into the solution A by using an acid buret, heating to 50 ℃, stirring for 24 hours, pouring 300mL of deionized water to precipitate lignin, standing for 30 minutes, pouring the solution A into a centrifuge tube, putting into the centrifuge to centrifugally precipitate for 10 minutes, pouring out supernatant, putting the precipitate into a vacuum drying oven, and vacuum drying at 85 ℃ for 12 hours to obtain silane modified lignin.
(3) 100mg of silane modified lignin and 100mg of nano silicon dioxide are respectively weighed by an electronic balance and blended in 10mL of acetone to obtain a solution C, 0.16mL of polydimethylsiloxane and 0.05mL of epoxy resin are removed by a pipette, discharged into the solution C, and stirred for 15min at room temperature of 500 r/min. And measuring 0.016mL of polydimethylsiloxane curing agent and 0.05mL of diethylenetriamine by using a pipette, discharging the mixture into the solution C, and stirring the mixture for 15min to obtain the super-hydrophobic coating.
(4) According to 0.0016g/cm 2 The super-hydrophobic coating is poured into a spray pen, the caliber of the spray pen is adjusted to be 0.5mm, the distance between the spray pen and a sample is 15cm, the spray pen is placed into a vacuum drying oven after being sprayed on the surface of the sample, the spray pen is cured for 10 hours at 85 ℃ to obtain the super-hydrophobic coating, the static contact angle is 156 degrees, and the dynamic contact angle is 1 degree.
(5) And (3) placing the blank sample and the super-hydrophobic sample into a freezer at the temperature of minus 18 ℃ for pre-freezing for 3min, and dripping 50 mu L of deionized water at the temperature of 1 ℃ to measure that the icing time of the water drops on the surface of the super-hydrophobic sample is 189s and the icing time of the water drops on the surface of the blank sample is 63s. The delay icing time of the super-hydrophobic sample is about three times that of the blank sample, which indicates that the super-hydrophobic sample has certain anti-icing performance.
Example 8
(1) Preparing a wood block sample with the specification of 50 x 31 x 9mm, drying the wood block sample in a vacuum drying oven at 60 ℃, and then placing the wood block sample in a dryer with silica gel for later use.
(2) 2g of kraft lignin is weighed by an electronic balance and dispersed in 60mL of deionized water, and the solution A is obtained by stirring at 300r/min for 5min at room temperature. Solution A was poured into a 250mL three-necked flask and stirring was continued at 0.5m 3 Nitrogen was introduced at a flow rate of/h, 3.5g of imidazole was weighed into solution A by means of an electronic balance and stirred for 1h. The acetone is measured by a measuring cylinder and poured into a beaker, 2mL of FOTS is measured by the measuring cylinder and poured into 36mL of acetone solution, the beaker is sealed by adopting a sealing film, and the solution B is obtained by stirring for 1h at 300 r/min. Dropwise adding the solution B into the solution A by using an acid buret, heating to 50 ℃, stirring for 24 hours, pouring 300mL of deionized water to precipitate lignin, standing for 30 minutes, pouring the solution A into a centrifuge tube, putting into the centrifuge to centrifugally precipitate for 10 minutes, pouring out supernatant, putting the precipitate into a vacuum drying oven, and vacuum drying at 85 ℃ for 12 hours to obtain silane modified lignin.
(3) 100mg of silane modified lignin and 100mg of nano silicon dioxide are respectively weighed by an electronic balance and blended in 10mL of acetone to obtain a solution C, 0.16mL of polydimethylsiloxane and 0.05mL of epoxy resin are removed by a pipette, discharged into the solution C, and stirred for 15min at room temperature of 500 r/min. And measuring 0.016mL of polydimethylsiloxane curing agent and 0.05mL of diethylenetriamine by using a pipette, discharging the mixture into the solution C, and stirring the mixture for 15min to obtain the super-hydrophobic coating.
(4) According to 0.0016g/cm 2 The super-hydrophobic coating is poured into a spray pen, the caliber of the spray pen is adjusted to be 0.5mm, the distance between the spray pen and a sample is 15cm, the spray pen is placed into a vacuum drying oven after being sprayed on the surface of the sample, the spray pen is cured for 10 hours at 85 ℃ to obtain the super-hydrophobic coating, the static contact angle is 153 degrees, and the dynamic contact angle is 3 degrees.
(5) And (3) placing the blank sample and the super-hydrophobic sample into a freezer at the temperature of minus 18 ℃ for pre-freezing for 3min, and dripping 50 mu L of deionized water at the temperature of 1 ℃ to measure that the icing time of the water drops on the surface of the super-hydrophobic sample is 164s and the icing time of the water drops on the surface of the blank sample is 63s. The delay icing time of the super-hydrophobic sample is about three times that of the blank sample, which indicates that the super-hydrophobic sample has certain anti-icing performance.
Example 9
(1) Preparing a wood block sample with the specification of 50 x 31 x 9mm, drying the wood block sample in a vacuum drying oven at 60 ℃, and then placing the wood block sample in a dryer with silica gel for later use.
(2) 2g of kraft lignin is weighed by an electronic balance and dispersed in 60mL of deionized water, and the solution A is obtained by stirring at 300r/min for 5min at room temperature. Solution A was poured into a 250mL three-necked flask and stirring was continued at 0.5m 3 Nitrogen was introduced at a flow rate of/h, 3.5g of imidazole was weighed into solution A by means of an electronic balance and stirred for 1h. The acetone is measured by a measuring cylinder and poured into a beaker, 4mL of FOTS is measured by the measuring cylinder and poured into 34mL of acetone solution, the beaker is sealed by adopting a sealing film, and the solution B is obtained by stirring for 1h at 300 r/min. Dropwise adding the solution B into the solution A by using an acid buret, heating to 50 ℃, stirring for 24 hours, pouring 300mL of deionized water to precipitate lignin, standing for 30 minutes, pouring the solution A into a centrifuge tube, putting into the centrifuge to centrifugally precipitate for 10 minutes, pouring out supernatant, putting the precipitate into a vacuum drying oven, and vacuum drying at 85 ℃ for 12 hours to obtain silane modified lignin.
(3) 100mg of silane modified lignin and 100mg of nano silicon dioxide are respectively weighed by an electronic balance and blended in 10mL of acetone to obtain a solution C, 0.16mL of polydimethylsiloxane and 0.05mL of epoxy resin are removed by a pipette, discharged into the solution C, and stirred for 15min at room temperature of 500 r/min. And measuring 0.016mL of polydimethylsiloxane curing agent and 0.05mL of diethylenetriamine by using a pipette, discharging the mixture into the solution C, and stirring the mixture for 15min to obtain the super-hydrophobic coating.
(4) According to 0.0016g/cm 2 The super-hydrophobic coating is poured into a spray pen, the caliber of the spray pen is adjusted to be 0.5mm, the distance between the spray pen and a sample is 15cm, the spray pen is placed into a vacuum drying oven after being sprayed on the surface of the sample, the spray pen is cured for 10 hours at 85 ℃ to obtain the super-hydrophobic coating, the static contact angle is 155 degrees, and the dynamic contact angle is 1 degree.
(5) And (3) placing the blank sample and the super-hydrophobic sample into a freezer at the temperature of minus 18 ℃ for pre-freezing for 3min, and dripping 50 mu L of deionized water at the temperature of 1 ℃ to measure that the icing time of the water drops on the surface of the super-hydrophobic sample is 176s and the icing time of the water drops on the surface of the blank sample is 63s. The delay icing time of the super-hydrophobic sample is about three times that of the blank sample, which indicates that the super-hydrophobic sample has certain anti-icing performance.
Comparative example 1
(1) Preparing an aluminum alloy sample with the specification of 76 x 26 x 1mm, polishing by using 600# abrasive paper, soaking in ethanol solution, ultrasonically cleaning, drying by using a vacuum drying oven at 60 ℃, and then placing into a dryer with silica gel for later use.
(2) 2g of kraft lignin is weighed by an electronic balance and dispersed in 60mL of deionized water, and the solution A is obtained by stirring at 300r/min for 5min at room temperature. Solution A was poured into a 250mL three-necked flask and stirring was continued at 0.5m 3 Nitrogen was introduced at a flow rate of/h, 3.5g of imidazole was weighed into solution A by means of an electronic balance and stirred for 1h. The acetone is measured by a measuring cylinder and poured into a beaker, 8mL of n-octyl trichlorosilane is measured by the measuring cylinder and poured into 30mL of acetone solution, the beaker is sealed by adopting a sealing film, and the solution B is obtained by stirring for 1h at 300 r/min. Dropwise adding the solution B into the solution A by using an acid burette, heating to 50 ℃, stirring for 24 hours, pouring 300mL of deionized water to precipitate lignin, standing for 30 minutes, pouring the solution A into a centrifuge tube, putting into the centrifuge to centrifugally precipitate for 10 minutes, pouring out supernatant, putting the precipitate into a vacuum drying oven, and vacuum drying at 85 ℃ for 12 hours to obtain silane modified woodAnd (5) plain.
(3) 100mg of silane modified lignin and 100mg of nano silicon dioxide are respectively weighed by an electronic balance and blended in 10mL of acetone to obtain a solution C, 0.05mL of epoxy resin is removed by a pipette, the solution C is discharged, and the solution C is stirred for 15min at room temperature of 500 r/min. And measuring 0.016mL of polydimethylsiloxane curing agent and 0.05mL of diethylenetriamine by using a pipette, discharging the mixture into the solution C, and stirring the mixture for 15min to obtain the hydrophobic coating.
(4) According to 0.0016g/cm 2 The super-hydrophobic coating is poured into a spray pen, the caliber of the spray pen is adjusted to be 0.5mm, the distance between the spray pen and a sample is 15cm, the spray pen and the sample are placed into a vacuum drying oven after being sprayed on the surface of the sample, the spray pen is cured for 10 hours at 85 ℃ to obtain the hydrophobic coating, the static contact angle is 132 degrees, and the dynamic contact angle is 35 degrees.
(5) And (3) placing the blank sample and the super-hydrophobic sample into a freezer at the temperature of minus 18 ℃ for pre-freezing for 3min, and dripping 50 mu L of deionized water at the temperature of 1 ℃ to measure 86s of the freezing time of the water drops on the surface of the super-hydrophobic sample and 62s of the freezing time of the water drops on the surface of the blank sample. The delay icing time of the super-hydrophobic sample is smaller than that of the blank sample, which indicates that the anti-icing performance of the super-hydrophobic sample is common.
This comparative example replaces the components of the coating relative to example 1. In example 1, FOTS was used as a silane modifying agent, and was added dropwise to a lignin solution after being dissolved in acetone to modify the lignin solution; in comparative example 1, the modifying agent was changed to n-octyl trichlorosilane, and the modified agent was dissolved in acetone and then added dropwise to a lignin solution to modify the lignin solution. As the grafted silane branched chain does not contain fluorine, the surface energy of lignin cannot be effectively reduced, the hydrophobicity of the coating is reduced, the contact angle is reduced from 158 degrees to 132 degrees, the rolling angle is increased from 1 degree to 35 degrees, the anti-icing effect is reduced, and the icing time of water drops on the surface of the coating is shortened from 185s to 86s.
Comparative example 2
(1) Preparing an aluminum alloy sample with the specification of 76 x 26 x 1mm, polishing by using 600# abrasive paper, soaking in ethanol solution, ultrasonically cleaning, drying by using a vacuum drying oven at 60 ℃, and then placing into a dryer with silica gel for later use.
(2) 100mg of kraft lignin and 100mg of nano-silica were respectively weighed by an electronic balance and blended in 10mL of acetone to obtain solution A, which was stirred at 500r/min for 15min at room temperature. The acetone is measured by a measuring cylinder and poured into a beaker, 0.4mL of FOTS is measured by the measuring cylinder and poured into 1.5mL of acetone solution, the beaker is sealed by adopting a sealing film, the solution B is obtained by stirring for 1h at 300r/min, the solution B is dripped into the solution A by an acid burette, and the solution B is stirred for 15min at 300 r/min. 0.16mL of polydimethylsiloxane and 0.05mL of epoxy resin were removed using a pipette and placed in solution C and stirred at 500r/min for 15min at room temperature. And measuring 0.016mL of polydimethylsiloxane curing agent and 0.05mL of diethylenetriamine by using a pipette, discharging the solution A, and stirring the solution for 15min to obtain the hydrophobic coating.
(4) According to 0.0016g/cm 2 The super-hydrophobic coating is poured into a spray pen, the caliber of the spray pen is adjusted to be 0.5mm, the distance between the spray pen and a sample is 15cm, the spray pen and the sample are placed into a vacuum drying oven after being sprayed on the surface of the sample, the spray pen is cured for 10 hours at 85 ℃ to obtain the hydrophobic coating, the static contact angle is 139 degrees, and the dynamic contact angle is 21 degrees.
(5) And (3) placing the blank sample and the superhydrophobic sample into a freezer at the temperature of minus 18 ℃ for pre-freezing for 3min, and dripping 50 mu L of deionized water at the temperature of 1 ℃ to measure that the icing time of the water drops on the surface of the superhydrophobic sample is 105s and the icing time of the water drops on the surface of the blank sample is 61s. The delay icing time of the super-hydrophobic sample is about twice that of the blank sample, which indicates that the super-hydrophobic sample has certain anti-icing performance.
The comparative example was modified with respect to example 1 with respect to the preparation of the coating. In example 1, after the kraft lignin is subjected to silane modification in a high-temperature and inert atmosphere, the kraft lignin and nano silicon dioxide are blended in acetone to prepare the coating, in the comparative example, firstly, the kraft lignin and the nano silicon dioxide are blended in acetone, an acetone solution containing a silane reagent is directly dripped under the conditions of room temperature and air, the reaction with hydroxyl groups on the surface of the lignin is insufficient, grafted silane branched chains are reduced, the hydrophobicity of the coating is reduced, the contact angle is reduced from 158 degrees to 139 degrees, the rolling angle is increased from 1 degree to 21 degrees, the anti-icing performance is reduced, and the icing time of water drops on the surface of the coating is shortened from 185s to 105s.
Comparative example 3
(1) Preparing an aluminum alloy sample with the specification of 76 x 26 x 1mm, polishing by using 600# abrasive paper, soaking in ethanol solution, ultrasonically cleaning, drying by using a vacuum drying oven at 60 ℃, and then placing into a dryer with silica gel for later use.
(2) 2g of kraft lignin is weighed by an electronic balance and dispersed in 60mL of deionized water, and the solution A is obtained by stirring at 300r/min for 5min at room temperature. Solution A was poured into a 250mL three-necked flask and stirring was continued at 0.5m 3 Nitrogen was introduced at a flow rate of/h, 3.5g of imidazole was weighed into solution A by means of an electronic balance and stirred for 1h. The acetone is measured by a measuring cylinder and poured into a beaker, 4mL of FOTS is measured by the measuring cylinder and poured into 34mL of acetone solution, the beaker is sealed by adopting a sealing film, and the solution B is obtained by stirring for 1h at 300 r/min. Dropwise adding the solution B into the solution A by using an acid buret, heating to 50 ℃, stirring for 24 hours, pouring 300mL of deionized water to precipitate lignin, standing for 30 minutes, pouring the solution A into a centrifuge tube, putting into the centrifuge to centrifugally precipitate for 10 minutes, pouring out supernatant, putting the precipitate into a vacuum drying oven, and vacuum drying at 85 ℃ for 12 hours to obtain silane modified lignin.
(3) 100mg of silane modified lignin and 100mg of nano silicon dioxide are respectively weighed by an electronic balance and blended in 10mL of acetone to obtain a solution C, 0.16mL of polydimethylsiloxane and 1.5mL of epoxy resin are removed by a pipette, discharged into the solution C, and stirred for 15min at room temperature of 500 r/min. And measuring 0.016mL of polydimethylsiloxane curing agent and 1.5mL of diethylenetriamine by using a pipette, discharging the mixture into the solution C, and stirring the mixture for 15min to obtain the hydrophobic coating.
(4) According to 0.0016g/cm 2 The super-hydrophobic coating is poured into a spray pen, the caliber of the spray pen is adjusted to be 0.5mm, the distance between the spray pen and a sample is 15cm, the spray pen and the sample are placed into a vacuum drying oven after being sprayed on the surface of the sample, the spray pen is cured for 10 hours at 85 ℃ to obtain the hydrophobic coating, the static contact angle is 129 degrees, and the dynamic contact angle is 32 degrees.
(5) And (3) placing the blank sample and the super-hydrophobic sample into a freezer at the temperature of minus 18 ℃ for pre-freezing for 3min, and dripping 50 mu L of deionized water at the temperature of 1 ℃ to measure the icing time of the water drops on the surface of the super-hydrophobic sample to be 117s and the icing time of the water drops on the surface of the blank sample to be 61s. The delay icing time of the super-hydrophobic sample is about twice that of the blank sample, which indicates that the super-hydrophobic sample has certain anti-icing performance.
This comparative example changed the process parameters of the coating preparation relative to example 3. In example 3, 10mL of acetone solvent was added with 0.05mL of epoxy resin and 0.05mL of curing agent diethylenetriamine thereof, while in comparative example 3, the addition amount of epoxy resin and curing agent diethylenetriamine thereof was increased, and 1.5mL of epoxy resin and 1.5mL of curing agent diethylenetriamine were added to 10mL of acetone solvent. The epoxy resin is used as a coating component, so that the mechanical strength of the coating is improved, but the balance point exists between the addition amount of the epoxy resin and the hydrophobic property of the coating, the hydrophobic property of the coating is reduced due to the excessive addition of the epoxy resin, the contact angle is reduced from 158 degrees to 129 degrees, the rolling angle is increased from 1 degree to 32 degrees, the anti-icing property is reduced, and the icing time of water drops on the surface of the coating is shortened from 172s to 117s.
Comparative example 4
(1) Preparing a wood block sample with the specification of 50 x 31 x 9mm, drying the wood block sample in a vacuum drying oven at 60 ℃, and then placing the wood block sample in a dryer with silica gel for later use.
(2) 100mg of kraft lignin and 100mg of nano silicon dioxide are respectively weighed by an electronic balance and blended in 10mL of acetone to obtain a solution A, 0.16mL of polydimethylsiloxane and 0.05mL of epoxy resin are removed by a pipette, discharged into the solution A, and stirred for 15min at room temperature of 500 r/min. And (3) transferring 0.016mL of polydimethylsiloxane curing agent and 0.05mL of diethylenetriamine into the C solution by using a pipette, and stirring for 15min to obtain the hydrophobic coating.
(3) According to 0.0016g/cm 2 The hydrophobic coating is poured into a spray pen, the caliber of the spray pen is adjusted to be 0.5mm, the distance between the spray pen and a sample is 15cm, the spray pen and the sample are placed into a vacuum drying oven after being sprayed on the surface of the sample, and the spray pen is cured for 10 hours at 85 ℃ to obtain the hydrophobic coating, wherein the static contact angle is 126 degrees, and the dynamic contact angle is 46 degrees.
(4) And (3) placing the blank sample and the hydrophobic sample into a freezer at the temperature of minus 18 ℃ for pre-freezing for 3min, and dripping 50 mu L of deionized water at the temperature of 1 ℃ to measure that the icing time of the water drops on the surface of the hydrophobic sample is 103s and the icing time of the water drops on the surface of the blank sample is 63s. The delay icing time of the hydrophobic sample is higher than that of the blank sample, which indicates that the hydrophobic sample has certain anti-icing performance.
This comparative example replaces the coating composition relative to example 7. In example 7, kraft lignin was added to deionized water, imidazole was added in an inert atmosphere at a high temperature, and an acetone solvent containing a silane reagent was used to modify lignin, and blended with nanosilica to prepare a coating, and in comparative example 4, kraft lignin was used as a raw material, and blended with nanosilica to prepare a coating. Although the kraft lignin is hydrophobic, the coating prepared after direct blending can not achieve the super-hydrophobic effect, the contact angle is reduced from 156 degrees to 126 degrees, the rolling angle is increased from 1 degree to 46 degrees, the anti-icing performance is reduced, and the icing time of water drops on the surface of the coating is shortened from 189s to 103s.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An anti-icing lignin super-hydrophobic coating is characterized in that: the composite material consists of the following components in parts by weight: 1-10 parts of silane modified lignin; 1-5 parts of nano silicon dioxide; 50-100 parts of acetone; 1-3 parts of polydimethylsiloxane; 1-3 parts of epoxy resin; 0.1 to 0.5 part of polydimethylsiloxane curing agent; 0.1 to 0.5 part of epoxy resin curing agent diethylenetriamine;
the preparation method of the silane modified lignin comprises the following steps: adding imidazole into lignin solution in an inert atmosphere, dissolving lignin, and stirring for a set time to obtain a mixed solution;
then, the acetone solution containing the silane reagent is dripped into the mixed solution, and the mixture is heated and stirred for reaction:
and after the reaction is finished, adding acetone into the reaction system, stirring to dissolve the modified lignin agglomerates, adding deionized water into the mixture to precipitate, separate and dry the modified lignin, thus obtaining the silane modified lignin.
2. The anti-icing lignin superhydrophobic coating according to claim 1, wherein: the mass ratio of lignin, imidazole and silane reagent is 1-3:2-4:1-5.
3. The anti-icing lignin superhydrophobic coating according to claim 1, wherein: the lignin is kraft lignin or alkali lignin.
4. The anti-icing lignin superhydrophobic coating according to claim 1, wherein: adding imidazole into lignin solution, and stirring for 1-5h.
5. The anti-icing lignin superhydrophobic coating according to claim 1, wherein: the heating temperature of the heating and stirring reaction is 45-55 ℃, and the stirring time is 12-24h.
6. The anti-icing lignin superhydrophobic coating according to claim 1, wherein: the silane reagent is 1H, 2H-perfluoro octyl trichlorosilane or n-octyl trichlorosilane.
7. The anti-icing lignin superhydrophobic coating according to claim 1, wherein: the epoxy resin is E-44 or E-51;
preferably, the epoxy resin curing agent is diethylenetriamine or ethylenediamine;
preferably, the polydimethylsiloxane curative is Dow Corning DC184.
8. The method for preparing the anti-icing lignin super-hydrophobic coating according to any one of claims 1 to 7, which is characterized in that: the method comprises the following steps:
adding silane modified lignin, nano silicon dioxide, polydimethylsiloxane and epoxy resin into acetone according to a proportion, and stirring and uniformly mixing to obtain mixed slurry;
and then adding the polydimethylsiloxane curing agent and the epoxy resin curing agent into the mixed slurry according to a proportion, and uniformly mixing to obtain the super-hydrophobic coating.
9. A preparation method of an anti-icing lignin super-hydrophobic coating is characterized by comprising the following steps of: the method comprises the following steps: adding the super-hydrophobic coating according to any one of claims 1-7 into a spray pen, spraying the coating on the surface of a substrate, and then placing the substrate into a vacuum drying oven for curing at 60-90 ℃ for 1-10 hours to obtain the super-hydrophobic coating.
10. Use of the superhydrophobic coating according to any one of claims 1-7 for the preparation of electric transmission lines.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190233675A1 (en) * | 2016-10-18 | 2019-08-01 | Siemens Gamesa Renewable Energy Innovation &Technology, S.L. | Polymeric composition with anti-icing and self-cleaning properties |
| CN110272682A (en) * | 2019-06-24 | 2019-09-24 | 齐鲁工业大学 | A kind of preparation method of the super-hydrophobic insulation corrosion resistant coating of lignin/resin |
| CN112608683A (en) * | 2020-11-03 | 2021-04-06 | 中南林业科技大学 | Lignin-based super-hydrophobic coating and preparation method thereof |
| CN115787306A (en) * | 2022-11-29 | 2023-03-14 | 西安交通大学 | Preparation method of high-robustness super-hydrophobic anti-icing fabric |
| CN116179047A (en) * | 2022-12-28 | 2023-05-30 | 中国人民解放军61699部队 | Wear-resistant super-hydrophobic nano composite coating and preparation method thereof |
-
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190233675A1 (en) * | 2016-10-18 | 2019-08-01 | Siemens Gamesa Renewable Energy Innovation &Technology, S.L. | Polymeric composition with anti-icing and self-cleaning properties |
| CN110272682A (en) * | 2019-06-24 | 2019-09-24 | 齐鲁工业大学 | A kind of preparation method of the super-hydrophobic insulation corrosion resistant coating of lignin/resin |
| CN112608683A (en) * | 2020-11-03 | 2021-04-06 | 中南林业科技大学 | Lignin-based super-hydrophobic coating and preparation method thereof |
| CN115787306A (en) * | 2022-11-29 | 2023-03-14 | 西安交通大学 | Preparation method of high-robustness super-hydrophobic anti-icing fabric |
| CN116179047A (en) * | 2022-12-28 | 2023-05-30 | 中国人民解放军61699部队 | Wear-resistant super-hydrophobic nano composite coating and preparation method thereof |
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