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    • 专利摘要:
    The present invention discloses a preparation method of a lignin/resin superhydrophobic insulated corrosion-resistant coating, and relates to the technical field of coatings and polymeric functional materials; dissolving alkali lignin in a polar solvent, slowly adding an initiator to an obtained alkali lignin solution, heating to 90— 180°C under protection of nitrogen, slowly adding long-chain alkane methoxysilane to react to obtain a modified alkali lignin solution, settling the modified alkali lignin solution to separate out to obtain modified alkali lignin modifier, adding the modified lignin into hydrophobic resin, stirring and adding a curing agent to obtain a lignin/ resin composite coating, and spraying the coating to the surface of wood, ceramics or metal by using a spray gun to form a super-hydrophobic surface film layer; the super-hydrophobic surface film layer has strong hydrophobicity, corrosion resistance and insulativity, adopts raw materials which are cheap and rich in source, belongs to cyclic comprehensive application of biomass raw materials, and thus has good application prospect and economical benefit.
    公开号:NL2025892A
    申请号:NL2025892
    申请日:2020-06-23
    公开日:2021-01-26
    发明作者:Wang Shoujuan；Sun Haodong；Kong Fangong
    申请人:Univ Qilu Technology；
    IPC主号:
    专利说明:

    PREPARATION METHOD OF LIGNIN-RESIN SUPER-HYDROPHOBIC INSULATED CORROSION-RESISTANT COATING
    TECHNICAL FIELD The present invention discloses a preparation method of a ligninfresin super hydrophobic insulated corrosion-resistant coating, and relates to the {echnical field of coatings and polymeric functional materials.
    BACKGROUD Lignin is a natural resource, ranking only second to cellulose and chitin in the nature, and is one of three major components of plant cell walls. Lignin not only exists in wood raw materials, but also exits In herbage raw materials such as wheat straw and reed, and is one of important componenis for plants to keep upright and prevent corrosion. The reserves of lignin is huge, and if not being sufficiently utilized, not only resource is wasted, but also 18 environmental pollution is caused, The present invention provides a preparation method of a ligninfresin supsr-hydrophobic insulated corrosion-resistant coating, in which modified super-hydrophobic lignin is mixed with hydrophobic resin lo form a super-hydrophobic coating. A contact angle of the supser-hydrophobic coating is greater than 180° | a sliding angle is smaller than 10° and because the super-hydrophobic coating has superstrong hydrophobic and oleophilic properties, the super-hydrophobic surface coating of the present invention has a broad application prospect in the direction of organic coatings, especially in architectural engineering, the super-hydrophobic surface coating can be applied to painting outer walls and top layers, the coating disclosed by the present invention has excellent corrosion resistance, anti-poliution properly, and walerproof, seal-cleaning and surface protective effects, and can keep io bring lasting freshness io buildings, thereby reducing construction and saving cost.
    SUMMARY Directed to problems of the prior art, the present invention provides a preparation method of a lignin/resin super-hydrophobic insulated corrosion-resistant coating, and the super-hydrophobic coating has a strong hydrophobic capacity, is strong in durability and insulativity, also has a self-cleaning capacity, adopts the raw material, lignin, which is cheap and rich In source, and belongs to cyclic comprehensive application of biomass raw materials, and thus has good application prospect and economical benefit. A specific scheme provided by the present invention is: a preparation method of a lignin/resin supsr-hydrophobic insulated corrosion-resislant coating, comprising:
    dissolving alkali lignin in a polar solvent, slowly adding an initiator to an obtained alkali lignin solution, heating to 80-180 under protection of nitrogen, slowly adding long-chain alkane methoxysilane lo react to obtain a modified alkali lignin solution, selling and purifying the modified alkali lignin solution lo & separate out an alkali lignin modifier, and drying for later use, and adding the alkali lignin modifier to a hydrophobic resin solution, stirring, and adding a curing agent io obtain a nanometer lignin fluoride-free super-hydrophobic coating.
    According to the preparation method, dissolving alkali lignin in any polar solvent out of acetonsg, dioxane, N N-dimsthyliormamide (DMF) and dimethyisulfoxide DMSO, According to the preparation method, slowly adding a triethylamine or sodium alkoxide initiator with mass concentration of 194-107 To an obtained alkali lignin solution.
    According to the preparation method, slowly adding an initiator lo an oblained alkali fignin solution, healing lo 80-180°C under the protection of nitrogen, and slowly adding long- chain alkane methoxysilane with mass concentration of 19-20% to react to obtain a modified alkali lignin solution.
    According to the preparation method, reacting for 2-10h to oblain a modified alkali lignin solution.
    According to the preparation method, the long-chain alkane methoxysilane refers to that from dodecyl trimethylisilane lo ocladecy! trimethyisilans.
    According to the preparation method, dissolving alkali lignin in a polar solvent, to obtain an alkali lignin solution with mass concentration of 19%-15%.
    According to the preparation method, the hydrophobic resin refers to one or a mixture of several out of polyurethane rasin, epoxy resin, polysulfone resin, poly-methyi silicon resin, poly-sthyl silicone resin and poly-aryl organic silicon resin.
    According to the preparation method, the mass fraction of hydrophobic resin is 10-50%.
    According to the preparation method, a curing agent is one or a mixture of several out of water-based isocyanate, walerbome polyurethane resin, and waterborne acrylic resin, and the mass percent of the curing agent is 1-8%.
    The present invention also relates to a ligninfresin super-hydrophobic insulated corrosion-resistiant coating prepared by the preparation method, The present invention further relates to an application implemented by utilizing the fignindresin super-hyorophobic insulated corrosion-resistant coating.
    The present invention has the following benefits: the present invention provides a preparation method of a ligninfresin super-hydrophobic insulated corrosion-resistant coating, According to the present invention, alkali lignin is dissolved In a polar solvent to obtain a lignin solution, an initiator is added to the lignin solution, pretreatment is performed on lignin in the solution by utilizing strong bacisity to the initiator to increase the quantity of phenolic hydroxyl groups, heating is performed under the protection of nitrogen to generate hydrolysis reaction with long-chain alkane methoxysilane, so as to realize silylation of lignin and obtain modified lignin of a net stereostructure of a long-chain alkane methoxysilane framework, meanwhile, lignin contains a large quantity of hydroxide radicals and has certain rigidity, which lays good foundation for grafting reagents with low surface energy and constructing rough surfaces. Modified lignin is mixed with hydrophobic rein in an organic solvent to obtain a super-hydrophobic lignin coating, contact angles of the super- hydrophobic lignin coating all reach greater than 150° and a curing agent is added to improve the bonding strength of the super-hydrophobic coating, so that the coating is more uniform and dense, meanwhile, the water resistance, corrosion resistance, insulativity and thermal oxidation resistance of the coating are improved.
    BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a flow diagram of a method of the present invention; FIG. 2 is a schematic diagram of a contact angle of the surface of a coated board, a contact angle being 156°. FIG. 3 is a black-and-white photograph of water drops on a wood chip, wherein A is the form of water drops on a wood chip after being coated with the super-hydrophobic coating, coagulated as spherical water drops; B is the form of water drops on an original wood chip, dispersed as elliptical water stains; FIG. 4 is a hydrophobic property data graph of a wood chip coated with the coating of embodiment 1 after staying in strong acid, neutral salt and strong base for 12h respectively, wherein it is tested that a contact angle of a woof chip coated with the super-hydrophobic coating is not smaller than 151°, and it is shown in the drawing that the coating has good water resistance and corrosion resistance; FIG. 5 is a hydrophobic property data graph of a wood chip coated with the coating of embodiment 2 after staying in strong acid, neutral salt and strong base for 12h respectively, wherein it is tested that a contact angle of a woof chip coated with the super-hydrophobic coating is not smaller than 152°, and it is shown in the drawing that the coating has good water resistance and corrosion resistance; FIG. 6 is a hydrophobic property data graph of a wood chip coated with the coating of embodiment 3 after staying in strong acid, neutral salt and strong base for 12h respectively, wherein it is tested that a contact angle of a woof chip coated with the super-hydrophobic coating is not smaller than 151°, and it is shown in the drawing that the coating has good water resistance and corrosion resistance;
    FIG. 7 is a hydrophobic property data graph of a wood chip coated with the coating of embodiment 4 after staying in strong acid, neutral salt and strong base for 12h respectively, wherein it is lesied that a contact angle of a woof chip coaled with the super-hydrophobic coating is not smaller than 152°, and it is shown in the drawing that the coating has good water resistance and corrosion resistance; FIG, 8 is a hydrophobic property data graph of a wood chip coated with the coating of smbodiment 5 after staying in strong acid, neutral salt and strong base for 12h respectively, wherein i is tested that a contact angle of a wool chip coated with the super-hydrophobic coating is not smaller than 150° and il is shown in the drawing that the coating has good water resistance and corrosion resistance; and FIG. S is a hydrophobic property data graph of a wood chip coated with the coating of embodiment 8 after staying in strong acid, neutral sall and strong base 12h respectively, wherein i is tested that a contact angle of a woof chip coated with the super-hydrophobic coating is not smaller than 150° and it is shown in the drawing that the coating has good waler resistance and corrosion resistance.
    DESCRIPTION OF THE EMBODIMENTS The present invention provides a preparation method of a lignin/resin super-hydrophobic insulated corrosion~-resistant coating, comprising: dissolving alkali lignin in a polar solvent, slowly adding an initiator to an obtained alkali lignin solution, heating to 86-180°C under protection of nitrogen, slowly adding long-chain alkane methoxysilane to react lo oblain a modified alkali lignin solution, setting and purifying the modified alkali lignin solution to separate out an alkali lignin modifier, and drying for later use, and adding the alkali lignin modifier 10 a hydrophobic resin solution, stirring, and adding a curing agent to obtain a nanometer lignin fluoride-free super-hydrophobic coating.
    The present invention also relates to a ligninfresin super-hydrophobic insulated corrosion-resistant coating prepared by the preparation method.
    The present invention further relates io an application implemented by utilizing the ligninvresin super-nydrophobic insulated corrosion-resistant coating.
    Alkali lignin is processed with long-chain alkane methoxysilane to obtain modified alkali grin, and a chemical equation is as follows:
    & p AH RN af > RET Ha, ed 9 ite + i Lh ‘ a ben md EN | ¥ TT Tug | ; # § OOH, The following further describes the present invention in combination with drawings and specific embodiments, so that technicians of the field may better understand and implement the present invention, however, the embodiments should not be deemed as limitation to the 5 present invention.
    Embodiment 1 a. dissolving polysulfone resin in dichloromethane to prepare a polysulfone resin solution with mass fraction of 10%; b. dissolving alkali lignin in DMF to prepare an alkali lignin solution with mass fraction of 8%, dissolving sodium methoxide in ethanol to prepare a sodium methoxide solution with mass fraction of 1%, slowly mixing the alkali lignin solution with the sodium methoxide solution, heating to 110°C under the protection of nitrogen, then slowly adding dodecyl trimethoxy silane with mass fraction of 2%, reacting and stirring for 4h to form a steady modified alkali lignin solution; settling and separating out modified alkali lignin with ethanol to obtain an alkali lignin modifier which is then dried for later use; and c. dissolving the alkali lignin modifier in DMF to prepare an alkali lignin modifier solution with mass fraction of 20%, mixing the polysulfone resin after being processed in a with the alkali lignin modifier solution, stirring for 1h at room temperature and then adding water- based isocyanate with mass fraction of 5%, and stirring for 5min, to obtain the polysulfone resin/lignin super-hydrophobic coating.
    In all the embodiments, besides spraying, brush coating, spin coating and blade coating may be also adopted as a coating mode of the coating.
    Embodiment 2 a. dissolving polyurethane resin in thinner to prepare a polyurethane resin solution with mass fraction of 50%; b. dissolving alkali lignin in DMF to prepare an alkali lignin solution with mass fraction of
    10%, dissolving sodium methoxide in ethanol to prepare a sodium methoxide solution with mass fraction of 2%, slowly mixing the alkali lignin solution with the sodium methoxide solution, heating to 90°C under the protection of nitrogen, then slowly adding tetradecy! trimethoxy silane with mass fraction of 5.5%, reacting and stirring for 5h to form a steady modified alkali lignin solution; settling and separating out modified alkali lignin with ethanol to obtain an alkali lignin modifier which is then dried for later use; and c. dissolving the alkali lignin modifier in DMF to prepare an alkali lignin modifier solution with mass fraction of 25%, mixing the polyurethane resin after being processed in a with the alkali lignin modifier solution, stirring for 1.5h at room temperature and then adding water- based isocyanate with mass fraction of 4%, and stirring for 20min, to obtain the polyurethane resin/lignin super-hydrophobic coating.
    Embodiment 3 a. dissolving poly-methyl silicon resin in butyl acetate to prepare a poly-methyl silicon resin solution with mass fraction of 17%; b. dissolving alkali lignin in DMF to prepare an alkali lignin solution with mass fraction of 11%, dissolving sodium methoxide in ethanol to prepare a sodium methoxide solution with mass fraction of 3%, slowly mixing the alkali lignin solution with the sodium methoxide solution, heating to 100°C under the protection of nitrogen, then slowly adding cetyl trimethoxy silane with mass fraction of 7%, reacting and stirring for 6h to form a steady modified alkali lignin solution; settling and separating out modified alkali lignin with ethanol to obtain an alkali lignin modifier which is then dried for later use; and c. dissolving the alkali lignin modifier in DMF to prepare an alkali lignin modifier solution with mass fraction of 28%, mixing the poly-methyl silicon resin after being processed in a with the alkali lignin modifier solution, stirring for 3h at room temperature and then adding waterborne polyurethane resin with mass fraction of 10%, and stirring for 25min, to obtain the poly-methyt silicon resin/lignin super-hydrophobic coating.
    Embodiment 4 a. dissolving epoxy resin in butyl acetate to prepare an epoxy silicon resin solution with mass fraction of 21%; b. dissolving alkali lignin in DMF to prepare an alkali lignin solution with mass fraction of 12%, dissolving sodium methoxide in ethanol to prepare a sodium methoxide solution with mass fraction of 5%, slowly mixing the alkali lignin solution with the sodium methoxide solution, heating to 130°C under the protection of nitrogen, then slowly adding cetyl trimethoxy silane with mass fraction of 14%, reacting and stirring for 8h to form a steady modified alkali lignin solution; settling and separating out modified alkali lignin with ethanol to obtain an alkali lignin modifier which is then dried for later use; and c. dissolving the alkali lignin modifier in DMF to prepare an alkali lignin modifier solution with mass fraction of 26%, mixing the epoxy resin after being processed in a with the alkali lignin modifier solution, stirring for 2h at room temperature and then adding waterborne polyurethane resin with mass fraction of 8%, and stirring for 21min, to obtain the epoxy resin/lignin super-hydrophobic coating.
    Embodiment 5 a. dissolving poly-ethyl silicone resin in butyl acetate to prepare a poly-ethyl silicone resin solution with mass fraction of 28%; b. dissolving alkali lignin in DMF to prepare an alkali lignin solution with mass fraction of 15%, dissolving sodium methoxide in ethanol to prepare a sodium methoxide solution with mass fraction of 7%, slowly mixing the alkali lignin solution with the sodium methoxide solution, heating to 150°C under the protection of nitrogen, then slowly adding cetyl trimethoxy silane with mass fraction of 18%, reacting and stirring for 2h to form a steady modified alkali lignin solution; settling and separating out modified alkali lignin with ethanol to obtain an alkali lignin modifier which is then dried for later use; and c. dissolving the alkali lignin modifier in DMF to prepare an alkali lignin modifier solution with mass fraction of 30%, mixing the poly-ethyl silicone resin after being processed in a with the alkali lignin modifier solution, stirring for 4h at room temperature and then adding waterborne acrylic resin with mass fraction of 7%, and stirring for 18min, to obtain the poly- ethyl silicone resin/lignin super-hydrophobic coating.
    Embodiment 6 a. dissolving poly-aryl organic silicon resin in thinner to prepare a poly-aryl organic silicon resin solution with mass fraction of 35%; b. dissolving alkali lignin in DMF to prepare an alkali lignin solution with mass fraction of 5%, dissolving sodium methoxide in ethanol to prepare a sodium methoxide solution with mass fraction of 10%, slowly mixing the alkali lignin solution with the sodium methoxide solution, heating to 180°C under the protection of nitrogen, then slowly adding octadecyl trimethoxy silane with mass fraction of 1%, reacting and stirring for 10h to form a steady modified alkali lignin solution; settling and separating out modified alkali lignin with ethanol to obtain an alkali lignin modifier which is then dried for later use; and c. dissolving the alkali lignin modifier in DMF to prepare an alkali lignin modifier solution with mass fraction of 26%, mixing the poly-aryl organic silicon resin after being processed in a with the alkali lignin modifier solution, stirring for 3.5h at room temperature and then adding waterborne acrylic resin with mass fraction of 1%, and stirring for 40min, to obtain the poly-
    aryl organic silicon resin/lignin super-hydrophobic coating.
    The coating obtained in embodiments 1-6 are respectively coated at two ends of a wood chip to perform a waterproof test, referring to FIG, 3, wherein A is the form of water drops on a wood chip after being coaled with the super-hydrophobic coating, coagulated as spherical water drops; B is the form of water drops on an original wood chip, dispersed as effiptical water stains; and after a wood chip coated with the coating oblained In embodiments 1-6 is immersed in strong acid, neutral sal and strong base for 12h, referring to hydrophobic property test diagrams of FIG. 4-9, il is tested that after staying in strong acid, neutral salt and strong base for 12h, contact angles of a wood chip coated with the super-hydrophobic coating are still not smaller than 1817 | indicating that the coating of the present invention has good water resistance and corrosion resistance, Application of a polar solvent and an initiator of alkali lignin are flexibly combined according Io actual conditions on the premise of not departing from the {echnical scheme of the present invention, hydrophobic resin and curing agent can be added as a selection according to conditions, and the adding mass is properly adjusted, to obtain a lignin Huorde- free super-hydrophobic insulated durable coating, and il is test by hydrophobic property test after a coated wood chip is immersed in strong acid, neutral salt and strong base for 12h, contact angles of the wood chips coated with the super-hydrophobic coating are not smaller than 151° | indicating thal the coating of the present invention has good waler resistance and corrosion resistance, According to the present invention, lignin extracted from soda pulping black liquor can be utilized to perform lignin modification, and cheap alkali lignin rich in content is utilized 10 construct a super-hydrophobic rough surface and used as a carrier of low-surface-energy substances, thereby being economical and environment-friendly, Other reagents used in the present invention are all reagents that may be purchased or prepared in the prior art, and are not further described hersin.
    The foregoing embodiments ars merely preferred embodiments for sufficiently describing the present invention, and the protection scope of the present invention is not limited herein, Equivalent substitution or transformation made by technicians of the technical Held on the basis of the present invention all fall within the protection scope of the present invention.
    The protection scope of the present invention should be subject to the claims.
    权利要求:
    Claims (10)
    [1]
    A method of manufacturing a superhydrophobic insulated corrosion resistant lignin / resin coating comprising: dissolving an alkaline lignin in a polar solvent, slowly adding an initiator to a obtained alkaline lignin solution, heating to 90-180 ° C under a protecting nitrogen, slowly adding a long chain methoxysilane alkane to react and obtain a modified alkaline lignin solution, stabilizing and purifying the modified alkaline lignin solution to separate an alkaline lignin modifier, and drying for later use, and adding the alkaline lignin modifier to a hydrophobic solution of resin, stirring it, and adding a curing agent to obtain a fluoride-free and superhydrophobic coating of nanometer scale lignin.
    [2]
    Manufacturing method according to claim 1, comprising dissolving alkaline lignin in a polar solvent such as acetone, dioxane, N, N-dimethylformamide and DMSO.
    [3]
    Manufacturing method according to claim 1 or 2, comprising slowly adding a triethylamine or sodium alkoxide initiator in a mass concentration of 1% -10% with respect to a obtained alkaline lignin solution.
    [4]
    The method of manufacture according to claim 3, comprising slowly adding an initiator to a obtained alkaline lignin solution, heating to 90-180 ° C under a protection of nitrogen, and slowly adding a methoxysilane long chain alkane in a mass concentration of 1% -20% in order to react and obtain a modified alkaline lignin solution.
    [5]
    The method of manufacture according to claim 4, wherein the methoxysilane long chain alkane has the meaning of a dodecyltrimethylsilane to an octadecyltrimethylsilane.
    [6]
    Manufacturing method according to claim 4 or 5, wherein the mass fraction of hydrophobic resin is 0.01% - 0.2%.
    [7]
    Manufacturing method according to claim 1 or 6, wherein the hydrophobic resin has the meaning of a polyurethane resin, an epoxy resin, a polysulfone resin, a polymethyl silicone resin, a polyethyl silicone resin, an organic polyaryl silicone resin, or a mixture of some of these. fabrics.
    [8]
    8. Manufacturing method according to claim 1 or 7, wherein the mass fraction of hardener is 1% to 8%.
    [9]
    A superhydrophobic insulated corrosion resistant lignin / resin coating made by a manufacturing method according to any one of claims 1-8.
    [10]
    The use of a superhydrophobic insulated corrosion resistant lignin / resin coating according to claim 9.
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    法律状态:
    优先权:
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