CN111518424A - Preparation method of bamboo wood waterproof and mildew-proof coating - Google Patents
Preparation method of bamboo wood waterproof and mildew-proof coating Download PDFInfo
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- CN111518424A CN111518424A CN202010451927.2A CN202010451927A CN111518424A CN 111518424 A CN111518424 A CN 111518424A CN 202010451927 A CN202010451927 A CN 202010451927A CN 111518424 A CN111518424 A CN 111518424A
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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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
- C09D1/02—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates
- C09D1/04—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates with organic additives
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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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
- C09D7/63—Additives non-macromolecular organic
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Abstract
The invention relates to a bamboo waterproof anticorrosive paint and a preparation method thereof, belonging to the technical field of bamboo protection. The invention utilizes the self-made swelling agent to generate swelling in the amorphous area of the cellulose, is beneficial to the penetration of the waterproof anticorrosive coating, after the paint infiltrates, the silica gel can firmly fix the metal silver ions in the bamboo wood, so that the anti-losing performance of the mildew inhibitor is improved, the protection performance of the bamboo wood to mould is improved through metal silver ions, the nanometer halloysite particles are used as carriers to further play a role in resisting the loss, in addition, the sodium silicate reacts with hydrochloric acid and is heated and decomposed to generate nanometer silicon dioxide particles, the nano silicon dioxide particles are embedded in the microstructure of the bamboo fiber, the compactness of the bamboo is improved, the infiltration of water is prevented, meanwhile, a large amount of nano silicon dioxide particles are bonded on the bamboo fiber, microscopic rough bulges are formed on the surface and inside of the bamboo fiber, so that the contact angle between the bamboo and water is increased, a hydrophobic interface is formed, and the corrosion resistance and the water resistance of the bamboo are improved.
Description
Technical Field
The invention relates to a preparation method of a bamboo wood waterproof and mildew-proof coating, and belongs to the technical field of bamboo wood protection.
Background
Along with the increasing scarcity of bamboo resources in China, the bamboo resources are rich, the production period is short and the bamboo resources can be regenerated
Are becoming an important source of wood based feedstocks. However, bamboo is rich in saccharide, starch and protein
The nutritional ingredients such as the texture, the fat and the like are easy to soak in water and generate mildew, color change, worm damage and decay in the processes of storage, transportation and use, thereby influencing the processing and utilization of the bamboo wood and even causing great economic loss.
However, the mildew-proof components in the common bamboo waterproof mildew-proof coating are easy to be soaked and run off, so that the mildew-proof performance cannot reach the estimated effect.
Therefore, in order to solve the technical problems, the invention provides a preparation method of a bamboo waterproof and mildewproof coating.
Disclosure of Invention
The invention mainly solves the technical problem, and provides a preparation method of a bamboo wood waterproof and mildew-proof coating, aiming at the defect that mildew-proof performance cannot be estimated due to the fact that mildew-proof components in the existing common bamboo wood waterproof and mildew-proof coating are easy to be soaked and run off.
In order to solve the technical problem, the technical scheme adopted by the application is as follows:
a preparation method of bamboo wood waterproof and mildew-proof coating comprises the following specific preparation steps:
(1) preparation of silica gel mildew-proof auxiliary agent:
mixing and heating ethyl orthosilicate, absolute ethyl alcohol and deionized water, adjusting the pH value by using hydrochloric acid, adding a silver nitrate solution and 3-aminopropyltriethoxysilane in a stirring state, and reacting to obtain a silica gel mildew-proof auxiliary agent;
(2) preparation of an anti-leaching mildew inhibitor:
stirring and reacting the nano halloysite and the silica gel mildew-proof auxiliary agent under a vacuum condition to obtain the anti-leaching mildew-proof agent;
(3) preparing a waterproof pre-emulsion:
mixing sodium silicate, propanedione, n-butanol and stearic acid, heating and reacting to obtain waterproof pre-emulsion;
(4) preparing a waterproof emulsion:
adding hydrochloric acid into the waterproof pre-emulsion, and stirring at a high temperature to react to obtain a waterproof emulsion;
(5) preparing a self-made swelling agent:
triethylamine hydrogen trifluoride and ammonium hexafluorophosphate are mixed and reacted to prepare a self-made swelling agent;
(6) preparing bamboo wood waterproof and mildew-proof coating:
mixing the anti-leaching mildew preventive, the waterproof emulsion, isophorone diisocyanate, maleic anhydride, glycerol and the self-made swelling agent, and heating to react to obtain the bamboo waterproof and mildew-proof coating.
Further, the preparation method comprises the following specific steps:
(1) preparation of silica gel mildew-proof auxiliary agent:
mixing ethyl orthosilicate, absolute ethyl alcohol and deionized water, then putting the mixture into a beaker, moving the beaker into a water bath kettle, heating, adding hydrochloric acid into the beaker to adjust the pH value, and stirring for reaction;
after the stirring reaction is finished, continuously stirring, slowly adding a silver nitrate solution and 3-aminopropyltriethoxysilane into a beaker in a stirring state, and continuously stirring for reaction to obtain a silica gel mildew-proof auxiliary agent;
(2) preparation of an anti-leaching mildew inhibitor:
weighing nano halloysite, filling the nano halloysite into a reaction eggplant-shaped bottle, vacuumizing the reaction eggplant-shaped bottle by using a vacuum pump, keeping the vacuum, adding a silica gel mildew-proof auxiliary agent into the eggplant-shaped bottle, stirring the mixture by using a magnetic stirrer for reaction, and discharging the mixture after the stirring reaction is finished to obtain a loss-resistant mildew-proof agent for later use;
(3) preparing a waterproof pre-emulsion:
weighing sodium silicate, propanedione, n-butanol and stearic acid, putting the beaker into a thermostat, raising the temperature of the thermostat, and stirring and reacting at constant temperature by using a stirrer to prepare waterproof pre-emulsion;
(4) preparing a waterproof emulsion:
dropwise adding hydrochloric acid into the beaker, adjusting the pH, mixing and stirring by using a stirrer, putting into a sand bath, heating, raising the temperature, and continuously stirring for reaction to obtain a waterproof emulsion;
(5) preparing a self-made swelling agent:
mixing triethylamine hydrogen trifluoride and ammonium hexafluorophosphate to obtain a self-made swelling agent;
(6) preparing bamboo wood waterproof and mildew-proof coating:
adding the standby anti-leaching mildew preventive, the waterproof emulsion, isophorone diisocyanate, maleic anhydride, glycerol and the self-made swelling agent into a reaction kettle, heating, stirring for reaction, and discharging to obtain the bamboo waterproof and mildew-proof coating.
Further, the preparation method comprises the following specific steps:
(1) preparation of silica gel mildew-proof auxiliary agent:
mixing ethyl orthosilicate, absolute ethyl alcohol and deionized water according to a mass ratio of 2:7:11, then putting the mixture into a beaker, then transferring the beaker into a water bath kettle, heating to 70-80 ℃, adding hydrochloric acid into the beaker to adjust the pH value to 3-4, and stirring and reacting for 30-40 min;
after the stirring reaction is finished, continuously stirring at 50-60 ℃, slowly adding 1mol/L silver nitrate solution with the mass of 2-3 times of that of the ethyl orthosilicate and 50% of 3-aminopropyltriethoxysilane with the mass of the ethyl orthosilicate into a beaker under the stirring state, and continuously stirring for reaction for 4-6 hours to obtain a silica gel mildew-proof auxiliary agent;
(2) preparation of an anti-leaching mildew inhibitor:
weighing nano halloysite, filling the nano halloysite into a reaction eggplant-shaped bottle, vacuumizing the reaction eggplant-shaped bottle by using a vacuum pump to ensure that the vacuum degree in the eggplant-shaped bottle reaches 100-200 Pa, keeping the vacuum for 30-40 min, adding the silica gel mould-proof auxiliary agent with the mass 2-5 times of that of the nano halloysite into the eggplant-shaped bottle, stirring and reacting for 24-30 h by using a magnetic stirrer at the rotating speed of 200-300 r/min, and discharging after the stirring and reacting are finished to obtain the anti-leaching mould-proof agent for later use;
(3) preparing a waterproof pre-emulsion:
weighing 10-15 parts of sodium silicate, 5-8 parts of propanedione, 15-16 parts of n-butanol and 1-2 parts of stearic acid in parts by weight, putting the beaker into a thermostat, raising the temperature of the thermostat to 60-70 ℃, and stirring and reacting for 1-2 hours by using a stirrer at constant temperature to prepare a waterproof pre-emulsion;
(4) preparing a waterproof emulsion:
dripping hydrochloric acid with the concentration of 1mol/L into the beaker, adjusting the pH value to 5-6, mixing and stirring for 10-15 min at the rotating speed of 300-350 r/min by using a stirrer, putting the mixture into a sand bath, heating to 150-180 ℃, and continuously stirring for reacting for 30-40 min to prepare a waterproof emulsion;
(5) preparing a self-made swelling agent:
mixing triethylamine hydrogen trifluoride and ammonium hexafluorophosphate according to the mass ratio of 5: 1 to obtain a self-made swelling agent;
(6) preparing bamboo wood waterproof and mildew-proof coating:
adding 13-15 parts by weight of standby anti-loss mildew inhibitor, 70-80 parts by weight of waterproof emulsion, 35-40 parts by weight of isophorone diisocyanate, 15-20 parts by weight of maleic anhydride, 10-15 parts by weight of glycerol and 10-12 parts by weight of self-made swelling agent into a reaction kettle, heating to 85-95 ℃, stirring for reaction for 3-4 hours, and discharging to obtain the bamboo waterproof and mildew-proof coating.
The beneficial technical effects of the invention are as follows:
(1) the invention utilizes the mixed solution of triethylamine trihydrofluoride and ammonium hexafluorophosphate to prepare the bamboo self-made swelling agent, ionized ions in the mixed solution of triethylamine trihydrofluoride and ammonium hexafluorophosphate can penetrate into an amorphous area of bamboo fibers and reach the outer surface of a crystalline area, and swelling in the amorphous area of cellulose occurs by destroying hydrogen bond bonding between water and cellulose, thereby being beneficial to further penetration of the waterproof anticorrosive coating, meanwhile, the invention also utilizes tetraethoxysilane and silver ion to prepare the silica gel silver mildew preventive, after the coating penetrates into the bamboo, the silica gel can firmly fix metal silver ions in the bamboo fibers, thereby improving the anti-losing property of the mildew preventive, and improving the protection property of the bamboo to mildew through good mildew resistance of the metal silver ions, in addition, the invention also uses nano halloysite particles as a carrier, under the negative pressure condition, the silica gel mildew inhibitor is loaded and fixed in the pores of the nano halloysite, so that the loss resistance is further realized, and in addition, the mildew inhibitor fixed in the rich pore structure of the nano halloysite can be slowly released, so that the mildew-proof aging is prolonged;
(2) the invention introduces sodium silicate into the paint directly, produces the ortho silicic acid precipitate through the reaction with hydrochloric acid, in the later heating and temperature rising process, the ortho silicic acid precipitate is heated and decomposed to generate nano silicon dioxide particles, after the nano silicon dioxide particles are immersed into the bamboo fiber, the nano silicon dioxide particles are embedded among molecules in the microstructure of the bamboo fiber, on one hand, the compactness of the bamboo is improved through the filling of the nano silicon dioxide, the infiltration of water is prevented, simultaneously, a large amount of nano silicon dioxide particles are bonded on the bamboo fiber, the roughness of the surface of each molecule of the wood is enhanced, and microscopic rough bulges are formed on the surface and the inside of the bamboo fiber, the existence of the bulge structures is similar to the microscopic synapse function on the surface of lotus leaves, the contact angle between the bamboo and water can be increased, water molecules are difficult to adhere after contacting the bamboo, and further a hydrophobic interface, further improves the corrosion resistance and the water resistance of the bamboo wood, and has wide application prospect.
Detailed Description
(1) Preparation of silica gel mildew-proof auxiliary agent:
mixing ethyl orthosilicate, absolute ethyl alcohol and deionized water according to a mass ratio of 2:7:11, then putting the mixture into a beaker, then transferring the beaker into a water bath kettle, heating to 70-80 ℃, adding hydrochloric acid into the beaker to adjust the pH value to 3-4, and stirring and reacting for 30-40 min;
after the stirring reaction is finished, continuously stirring at 50-60 ℃, slowly adding 1mol/L silver nitrate solution with the mass of 2-3 times of that of the ethyl orthosilicate and 50% of 3-aminopropyltriethoxysilane with the mass of the ethyl orthosilicate into a beaker under the stirring state, and continuously stirring for reaction for 4-6 hours to obtain a silica gel mildew-proof auxiliary agent;
(2) preparation of an anti-leaching mildew inhibitor:
weighing nano halloysite, filling the nano halloysite into a reaction eggplant-shaped bottle, vacuumizing the reaction eggplant-shaped bottle by using a vacuum pump to ensure that the vacuum degree in the eggplant-shaped bottle reaches 100-200 Pa, keeping the vacuum for 30-40 min, adding the silica gel mould-proof auxiliary agent with the mass 2-5 times of that of the nano halloysite into the eggplant-shaped bottle, stirring and reacting for 24-30 h by using a magnetic stirrer at the rotating speed of 200-300 r/min, and discharging after the stirring and reacting are finished to obtain the anti-leaching mould-proof agent for later use;
(3) preparing a waterproof pre-emulsion:
weighing 10-15 parts of sodium silicate, 5-8 parts of propanedione, 15-16 parts of n-butanol and 1-2 parts of stearic acid in parts by weight, putting the beaker into a thermostat, raising the temperature of the thermostat to 60-70 ℃, and stirring and reacting for 1-2 hours by using a stirrer at constant temperature to prepare a waterproof pre-emulsion;
(4) preparing a waterproof emulsion:
dripping hydrochloric acid with the concentration of 1mol/L into the beaker, adjusting the pH value to 5-6, mixing and stirring for 10-15 min at the rotating speed of 300-350 r/min by using a stirrer, putting the mixture into a sand bath, heating to 150-180 ℃, and continuously stirring for reacting for 30-40 min to prepare a waterproof emulsion;
(5) preparing a self-made swelling agent:
mixing triethylamine hydrogen trifluoride and ammonium hexafluorophosphate according to the mass ratio of 5: 1 to obtain a self-made swelling agent;
(6) preparing bamboo wood waterproof and mildew-proof coating:
adding 13-15 parts by weight of standby anti-loss mildew inhibitor, 70-80 parts by weight of waterproof emulsion, 35-40 parts by weight of isophorone diisocyanate, 15-20 parts by weight of maleic anhydride, 10-15 parts by weight of glycerol and 10-12 parts by weight of self-made swelling agent into a reaction kettle, heating to 85-95 ℃, stirring for reaction for 3-4 hours, and discharging to obtain the bamboo waterproof and mildew-proof coating.
Example 1
(1) Preparation of silica gel mildew-proof auxiliary agent:
mixing tetraethoxysilane, absolute ethyl alcohol and deionized water according to the mass ratio of 2:7:11, then putting the mixture into a beaker, then transferring the beaker into a water bath kettle, heating to 70 ℃, adding hydrochloric acid into the beaker to adjust the pH value to 3, and stirring and reacting for 30 min;
after the stirring reaction is finished, continuously stirring at 50 ℃, slowly adding a silver nitrate solution with the concentration of 1mol/L and 2 times of the mass of the tetraethoxysilane and 3-aminopropyl triethoxysilane with the mass of 50% of the tetraethoxysilane into a beaker under the stirring state, and continuously stirring for reacting for 4 hours to obtain the silica gel mildew-proof auxiliary agent;
(2) preparation of an anti-leaching mildew inhibitor:
weighing nano halloysite, filling the nano halloysite into a reaction eggplant-shaped bottle, vacuumizing the reaction eggplant-shaped bottle by using a vacuum pump to ensure that the vacuum degree in the eggplant-shaped bottle reaches 100Pa, keeping the vacuum for 30min, adding the silica gel mould-proof auxiliary agent with the mass 2 times of that of the nano halloysite into the eggplant-shaped bottle, stirring and reacting for 24h by using a magnetic stirrer at the rotating speed of 200-300 r/min, and discharging after the stirring reaction is finished to obtain the anti-leaching mould inhibitor for later use;
(3) preparing a waterproof pre-emulsion:
weighing 10 parts of sodium silicate, 5 parts of propanedione, 15 parts of n-butanol and 1 part of stearic acid according to parts by weight, putting the beaker into a thermostat, raising the temperature of the thermostat to 60 ℃, and stirring and reacting for 1 hour by using a stirrer at constant temperature to prepare waterproof pre-emulsion;
(4) preparing a waterproof emulsion:
dripping hydrochloric acid with the concentration of 1mol/L into the beaker, adjusting the pH value to 5, mixing and stirring for 10min at the rotating speed of 300r/min by using a stirrer, putting the mixture into a sand bath kettle, heating to 150 ℃, and continuously stirring and reacting for 30min to prepare waterproof emulsion;
(5) preparing a self-made swelling agent:
mixing triethylamine hydrogen trifluoride and ammonium hexafluorophosphate according to the mass ratio of 5: 1 to obtain a self-made swelling agent;
(6) preparing bamboo wood waterproof and mildew-proof coating:
adding 13 parts by weight of standby anti-leaching mildew preventive, 70 parts by weight of the waterproof emulsion, 35 parts by weight of isophorone diisocyanate, 15 parts by weight of maleic anhydride, 10 parts by weight of glycerol and 10 parts by weight of self-made swelling agent into a reaction kettle, heating to 85 ℃, stirring for reaction for 3 hours, and discharging to obtain the bamboo waterproof and mildew-proof coating.
Example 2
(1) Preparation of silica gel mildew-proof auxiliary agent:
mixing ethyl orthosilicate, absolute ethyl alcohol and deionized water according to the mass ratio of 2:7:11, then putting the mixture into a beaker, then transferring the beaker into a water bath kettle, heating to 75 ℃, adding hydrochloric acid into the beaker to adjust the pH value to 3, and stirring to react for 35 min;
after the stirring reaction is finished, continuously stirring at 55 ℃, slowly adding a silver nitrate solution with the concentration of 1mol/L and 3-aminopropyltriethoxysilane with the mass of 50% of the ethyl orthosilicate, which are 3 times of the mass of the ethyl orthosilicate, into the beaker under the stirring state, and continuously stirring for reaction for 5 hours to obtain the silica gel mildew-proof auxiliary agent;
(2) preparation of an anti-leaching mildew inhibitor:
weighing nano halloysite, filling the nano halloysite into a reaction eggplant-shaped bottle, vacuumizing the reaction eggplant-shaped bottle by using a vacuum pump to ensure that the vacuum degree in the eggplant-shaped bottle reaches 150Pa, keeping the vacuum for 35min, adding the silica gel mould-proof auxiliary agent with the mass 3 times of that of the nano halloysite into the eggplant-shaped bottle, stirring and reacting for 27h by using a magnetic stirrer at the rotating speed of 250r/min, discharging after the stirring reaction is finished, and obtaining the anti-leaching mould inhibitor for later use;
(3) preparing a waterproof pre-emulsion:
weighing 13 parts of sodium silicate, 7 parts of propanedione, 15 parts of n-butanol and 2 parts of stearic acid in parts by weight, putting the beaker into a thermostat, raising the temperature of the thermostat to 65 ℃, and stirring and reacting for 1 hour by using a stirrer at constant temperature to prepare a waterproof pre-emulsion;
(4) preparing a waterproof emulsion:
dripping hydrochloric acid with the concentration of 1mol/L into the beaker, adjusting the pH value to 5, mixing and stirring for 13min at the rotating speed of 330r/min by using a stirrer, then putting the mixture into a sand bath kettle, heating to 165 ℃, and continuously stirring and reacting for 35min to obtain waterproof emulsion;
(5) preparing a self-made swelling agent:
mixing triethylamine hydrogen trifluoride and ammonium hexafluorophosphate according to the mass ratio of 5: 1 to obtain a self-made swelling agent;
(6) preparing bamboo wood waterproof and mildew-proof coating:
according to the weight parts, 14 parts of standby anti-loss mildew inhibitor, 75 parts of the waterproof emulsion, 38 parts of isophorone diisocyanate, 17 parts of maleic anhydride, 13 parts of glycerol and 11 parts of self-made swelling agent are added into a reaction kettle, the temperature is raised to 90 ℃, the materials are stirred and react for 4 hours, and then the materials are discharged, so that the bamboo waterproof and mildew-proof coating is obtained.
Example 3
(1) Preparation of silica gel mildew-proof auxiliary agent:
mixing tetraethoxysilane, absolute ethyl alcohol and deionized water according to the mass ratio of 2:7:11, then putting the mixture into a beaker, then transferring the beaker into a water bath kettle, heating to 80 ℃, adding hydrochloric acid into the beaker to adjust the pH value to 4, and stirring to react for 40 min;
after the stirring reaction is finished, continuously stirring at 60 ℃, slowly adding a silver nitrate solution with the concentration of 1mol/L and 3-aminopropyltriethoxysilane with the mass of 50% of the ethyl orthosilicate, which are 3 times of the mass of the ethyl orthosilicate, into the beaker under the stirring state, and continuously stirring for reacting for 6 hours to obtain the silica gel mildew-proof auxiliary agent;
(2) preparation of an anti-leaching mildew inhibitor:
weighing nano halloysite, filling the nano halloysite into a reaction eggplant-shaped bottle, vacuumizing the reaction eggplant-shaped bottle by using a vacuum pump to ensure that the vacuum degree in the eggplant-shaped bottle reaches 200Pa, keeping the vacuum for 40min, adding the silica gel mould-proof auxiliary agent with the mass 5 times of that of the nano halloysite into the eggplant-shaped bottle, stirring and reacting for 30h by using a magnetic stirrer at the rotating speed of 300r/min, discharging after the stirring reaction is finished, and obtaining the anti-leaching mould inhibitor for later use;
(3) preparing a waterproof pre-emulsion:
weighing 15 parts of sodium silicate, 8 parts of propanedione, 16 parts of n-butanol and 2 parts of stearic acid in parts by weight, putting the beaker into a thermostat, raising the temperature of the thermostat to 70 ℃, and stirring and reacting for 2 hours by using a stirrer at constant temperature to prepare waterproof pre-emulsion;
(4) preparing a waterproof emulsion:
dripping hydrochloric acid with the concentration of 1mol/L into the beaker, adjusting the pH value to 6, mixing and stirring the mixture for 15min at the rotating speed of 350r/min by using a stirrer, putting the mixture into a sand bath kettle, heating the mixture to 180 ℃, and continuously stirring and reacting the mixture for 40min to prepare waterproof emulsion;
(5) preparing a self-made swelling agent:
mixing triethylamine hydrogen trifluoride and ammonium hexafluorophosphate according to the mass ratio of 5: 1 to obtain a self-made swelling agent;
(6) preparing bamboo wood waterproof and mildew-proof coating:
adding 15 parts by weight of standby anti-loss mildew inhibitor, 80 parts by weight of the waterproof emulsion, 40 parts by weight of isophorone diisocyanate, 20 parts by weight of maleic anhydride, 15 parts by weight of glycerol and 12 parts by weight of self-made swelling agent into a reaction kettle, heating to 95 ℃, stirring for reaction for 4 hours, and discharging to obtain the bamboo waterproof and mildew-proof coating.
Comparative example 1: the preparation method is similar to that of example 1 of the present application, except that the self-made swelling agent of the present invention is not added;
comparative example 2: the preparation method is similar to that of example 1 of the present application, except that the anti-run-off mildewcide of the present invention is not added;
comparative example 3: the preparation method is similar to that of example 1 of the present application, except that the waterproof emulsion of the present invention is not added;
the performance of the bamboo waterproof anticorrosive paint in the embodiment and the comparative example of the application is detected, and the detection results are shown in table 1:
water resistance test method: the waterproof and anticorrosive paint is uniformly coated on the surfaces of bamboo samples with the same size according to the same coating amount, the samples are placed in hot water at 40-50 ℃ after being naturally dried and cured, the samples are taken out after 96 hours, and the water absorption of the samples is detected.
And (3) mildew condition: the paints of examples 1 to 3 and comparative example were applied to the surface of a square, and the area of the applied paint was 1m2And keeping the brushing thickness consistent during brushing, standing for 2 weeks in an environment with the relative humidity of air of 70-80% and the temperature of 30-40 ℃ after brushing is finished, and calculating the average mildew area ratio of the coating surface, wherein the average mildew area ratio is the ratio of the average mildew area in the unit area of the coating to the average mildew area in the unit area of the coating of the comparative example.
TABLE 1 measurement results of Properties
| Test items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Water absorption (96 h) | 6 | 4 | 2 | 16 | 6 | 13 |
| Average area ratio of mildew | 0.25 | 0.22 | 0.17 | 0.49 | 0.47 | 0.26 |
| Escherichia coli inhibitory rate （%） | 95.38 | 96.19 | 99.23 | 89.12 | 80.24 | 94.39 |
| Staphylococcus aureus Bacteriostatic ratio (%) | 95.90 | 97.53 | 99.72 | 90.41 | 80.62 | 94.41 |
As can be seen from the detection data in the above table, the self-made swelling agent of the present invention is not added in the comparative example 1 of the present invention, so the water absorption rate is increased, the mildew area ratio is increased, and the bacteriostatic rate is decreased, and it can be seen that the water resistance and mildew resistance of the coating of the present invention are improved by the addition of the self-made swelling agent of the present invention, the average mildew area ratio is increased and the bacteriostatic rate is decreased by the addition of the loss-resistant mildew preventive of the present invention, and thus it can be seen that the mildew-resistant and antibacterial properties of the coating of the present invention are improved by the addition of the loss-resistant mildew preventive of the present invention, and the water absorption rate is increased, the mildew area ratio is increased and the bacteriostatic rate is decreased by the addition of the waterproof emulsion of the present invention, and it can be seen that the water resistance and mildew resistance of the coating of the present invention are improved, and the application prospect is broad.
Claims (3)
1. A preparation method of bamboo wood waterproof and mildew-proof coating is characterized by comprising the following specific preparation steps:
(1) preparation of silica gel mildew-proof auxiliary agent:
mixing and heating ethyl orthosilicate, absolute ethyl alcohol and deionized water, adjusting the pH value by using hydrochloric acid, adding a silver nitrate solution and 3-aminopropyltriethoxysilane in a stirring state, and reacting to obtain a silica gel mildew-proof auxiliary agent;
(2) preparation of an anti-leaching mildew inhibitor:
stirring and reacting the nano halloysite and the silica gel mildew-proof auxiliary agent under a vacuum condition to obtain the anti-leaching mildew-proof agent;
(3) preparing a waterproof pre-emulsion:
mixing sodium silicate, propanedione, n-butanol and stearic acid, heating and reacting to obtain waterproof pre-emulsion;
(4) preparing a waterproof emulsion:
adding hydrochloric acid into the waterproof pre-emulsion, and stirring at a high temperature to react to obtain a waterproof emulsion;
(5) preparing a self-made swelling agent:
triethylamine hydrogen trifluoride and ammonium hexafluorophosphate are mixed and reacted to prepare a self-made swelling agent;
(6) preparing bamboo wood waterproof and mildew-proof coating:
mixing the anti-leaching mildew preventive, the waterproof emulsion, isophorone diisocyanate, maleic anhydride, glycerol and the self-made swelling agent, and heating to react to obtain the bamboo waterproof and mildew-proof coating.
2. The preparation method of the bamboo wood waterproof and mildewproof coating as claimed in claim 1, which is characterized by comprising the following specific preparation steps:
(1) preparation of silica gel mildew-proof auxiliary agent:
mixing ethyl orthosilicate, absolute ethyl alcohol and deionized water, then putting the mixture into a beaker, moving the beaker into a water bath kettle, heating, adding hydrochloric acid into the beaker to adjust the pH value, and stirring for reaction;
after the stirring reaction is finished, continuously stirring, slowly adding a silver nitrate solution and 3-aminopropyltriethoxysilane into a beaker in a stirring state, and continuously stirring for reaction to obtain a silica gel mildew-proof auxiliary agent;
(2) preparation of an anti-leaching mildew inhibitor:
weighing nano halloysite, filling the nano halloysite into a reaction eggplant-shaped bottle, vacuumizing the reaction eggplant-shaped bottle by using a vacuum pump, keeping the vacuum, adding a silica gel mildew-proof auxiliary agent into the eggplant-shaped bottle, stirring the mixture by using a magnetic stirrer for reaction, and discharging the mixture after the stirring reaction is finished to obtain a loss-resistant mildew-proof agent for later use;
(3) preparing a waterproof pre-emulsion:
weighing sodium silicate, propanedione, n-butanol and stearic acid, putting the beaker into a thermostat, raising the temperature of the thermostat, and stirring and reacting at constant temperature by using a stirrer to prepare waterproof pre-emulsion;
(4) preparing a waterproof emulsion:
dropwise adding hydrochloric acid into the beaker, adjusting the pH, mixing and stirring by using a stirrer, putting into a sand bath, heating, raising the temperature, and continuously stirring for reaction to obtain a waterproof emulsion;
(5) preparing a self-made swelling agent:
mixing triethylamine hydrogen trifluoride and ammonium hexafluorophosphate to obtain a self-made swelling agent;
(6) preparing bamboo wood waterproof and mildew-proof coating:
adding the standby anti-leaching mildew preventive, the waterproof emulsion, isophorone diisocyanate, maleic anhydride, glycerol and the self-made swelling agent into a reaction kettle, heating, stirring for reaction, and discharging to obtain the bamboo waterproof and mildew-proof coating.
3. The preparation method of the bamboo wood waterproof and mildew-proof coating according to claim 1 or 2, which is characterized by comprising the following specific preparation steps:
(1) preparation of silica gel mildew-proof auxiliary agent:
mixing ethyl orthosilicate, absolute ethyl alcohol and deionized water according to a mass ratio of 2:7:11, then putting the mixture into a beaker, then transferring the beaker into a water bath kettle, heating to 70-80 ℃, adding hydrochloric acid into the beaker to adjust the pH value to 3-4, and stirring and reacting for 30-40 min;
after the stirring reaction is finished, continuously stirring at 50-60 ℃, slowly adding 1mol/L silver nitrate solution with the mass of 2-3 times of that of the ethyl orthosilicate and 50% of 3-aminopropyltriethoxysilane with the mass of the ethyl orthosilicate into a beaker under the stirring state, and continuously stirring for reaction for 4-6 hours to obtain a silica gel mildew-proof auxiliary agent;
(2) preparation of an anti-leaching mildew inhibitor:
weighing nano halloysite, filling the nano halloysite into a reaction eggplant-shaped bottle, vacuumizing the reaction eggplant-shaped bottle by using a vacuum pump to ensure that the vacuum degree in the eggplant-shaped bottle reaches 100-200 Pa, keeping the vacuum for 30-40 min, adding the silica gel mould-proof auxiliary agent with the mass 2-5 times of that of the nano halloysite into the eggplant-shaped bottle, stirring and reacting for 24-30 h by using a magnetic stirrer at the rotating speed of 200-300 r/min, and discharging after the stirring and reacting are finished to obtain the anti-leaching mould-proof agent for later use;
(3) preparing a waterproof pre-emulsion:
weighing 10-15 parts of sodium silicate, 5-8 parts of propanedione, 15-16 parts of n-butanol and 1-2 parts of stearic acid in parts by weight, putting the beaker into a thermostat, raising the temperature of the thermostat to 60-70 ℃, and stirring and reacting for 1-2 hours by using a stirrer at constant temperature to prepare a waterproof pre-emulsion;
(4) preparing a waterproof emulsion:
dripping hydrochloric acid with the concentration of 1mol/L into the beaker, adjusting the pH value to 5-6, mixing and stirring for 10-15 min at the rotating speed of 300-350 r/min by using a stirrer, putting the mixture into a sand bath, heating to 150-180 ℃, and continuously stirring for reacting for 30-40 min to prepare a waterproof emulsion;
(5) preparing a self-made swelling agent:
mixing triethylamine hydrogen trifluoride and ammonium hexafluorophosphate according to the mass ratio of 5: 1 to obtain a self-made swelling agent;
(6) preparing bamboo wood waterproof and mildew-proof coating:
adding 13-15 parts by weight of standby anti-loss mildew inhibitor, 70-80 parts by weight of waterproof emulsion, 35-40 parts by weight of isophorone diisocyanate, 15-20 parts by weight of maleic anhydride, 10-15 parts by weight of glycerol and 10-12 parts by weight of self-made swelling agent into a reaction kettle, heating to 85-95 ℃, stirring for reaction for 3-4 hours, and discharging to obtain the bamboo waterproof and mildew-proof coating.
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