CN107267061B - Nano inorganic powder modified organic silicon waterproof coating - Google Patents
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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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- 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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- 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
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Abstract
The invention discloses a nano inorganic powder modified organic silicon waterproof coating, and belongs to the technical field of building waterproofing. The nano inorganic powder modified organosilicon waterproof coating is prepared from the following raw materials in parts by weight: 200-300 parts of oligomer siloxane base material, 10-30 parts of emulsifier, 20-60 parts of stabilizer, 4-6 parts of curing agent, 180-200 parts of diluent, 3-6 parts of thickener and 100-150 parts of nano inorganic powder; the nano inorganic powder is prepared by mixing the following raw materials in parts by weight: 60-80 parts of nano silicon dioxide, 20-30 parts of nano alumina, 8-10 parts of nano zirconia and 10-15 parts of nano hydroxyapatite. The invention has the beneficial effects that: the nano inorganic powder modified organosilicon waterproof coating has better weather resistance and long service life, and a hydrophobic bionic structure formed by the added inorganic nano particles does not hinder the water vapor in the substrate from permeating.
Description
Technical Field
The invention relates to a nano inorganic powder modified organic silicon waterproof coating, and belongs to the technical field of building waterproofing.
Background
The building waterproof coating has the characteristics of simple and convenient construction and strong adaptability to complex structures, and is used in large amount in building construction. The waterproof coating is mainly used for waterproofing, moistureproof, seepage prevention and the like of some structural parts of buildings which are possibly corroded by water, so that certain requirements on high and low temperature resistance and corrosion resistance of the waterproof coating are met. The existing building waterproof coating mainly comprises a polyurethane waterproof coating, a polymer cement waterproof coating and an organosilicon waterproof coating, wherein the organosilicon waterproof coating is widely applied.
The organosilicon waterproof coating is divided into water-based environment-friendly waterproof coating and solvent-based organosilicon waterproof coating. The water environment-friendly waterproof coating is prepared by taking silicon rubber latex and nano composite latex thereof as main base materials and mixing inorganic filler and various auxiliary agents. The solvent-type organosilicon waterproof coating is prepared by mixing active organosiloxane and active organosilicon resin, uniformly stirring, adding alcohol serving as a solvent under the protection of inert gas, adding a catalyst to form a premix, stirring the premix, aging for reaction for 1 hour, and packaging under the protection of nitrogen. However, in the use process of the existing waterproof coating, the capillary pores of the substrate material are easily closed by the waterproof film formed by curing, so that the moisture in the substrate cannot be dissipated from the wall, and the waterproof film has poor weather resistance and short service life.
Therefore, it is important to develop a waterproof coating material which does not prevent moisture from being released, has good weather resistance of a waterproof film, and has a long service life.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems that in the use process of the traditional waterproof coating, the capillary pores of a substrate material are easily closed by a waterproof film formed by curing, so that the moisture in the substrate cannot be dissipated from a wall body, the weather resistance of the waterproof film is poor, and the service life of the waterproof film is short, the nano inorganic powder modified organic silicon waterproof coating is provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
a nano inorganic powder modified organosilicon waterproof coating is composed of the following raw materials in parts by weight: 200-300 parts of oligomer siloxane base material, 10-30 parts of emulsifier, 20-60 parts of stabilizer, 4-6 parts of curing agent, 180-200 parts of diluent, 3-6 parts of thickener and 100-150 parts of nano inorganic powder;
the nano inorganic powder is prepared by mixing the following raw materials in parts by weight: 60-80 parts of nano silicon dioxide, 20-30 parts of nano alumina, 8-10 parts of nano zirconia and 10-15 parts of nano hydroxyapatite;
the specific configuration method is as follows:
(1) adding a diluent, an emulsifier, a stabilizer, a curing agent, a thickening agent and nano inorganic powder into a reaction kettle according to a formula, uniformly stirring at constant temperature, then adding an oligomer siloxane base material, and continuously stirring at constant temperature for reaction;
(2) after the constant-temperature stirring reaction is finished, transferring the materials in the reaction kettle into a high-pressure homogenizer for emulsification to obtain an emulsion;
(3) removing floating substances on the surface of the emulsion, adjusting the pH value by hydrochloric acid, and filling to obtain the nano inorganic powder modified organosilicon waterproof coating.
The oligomer siloxane base material is two of hydroxyl-terminated polydimethylsiloxane, carboxyl-terminated polydimethylsiloxane or amino-terminated polydimethylsiloxane, and the mass ratio of the two is 1: 1.
The emulsifier is one of sodium stearate, tween-60 or span-80.
The stabilizer is one of sodium dodecyl benzene sulfonate, cetyl trimethyl ammonium bromide or octadecyl polyoxyethylene ether.
The curing agent is one of triethanolamine or polyamide curing agent 651.
The diluent is one of deionized water, softened water or distilled water.
The thickening agent is one of sodium carboxymethylcellulose, hydroxyethyl cellulose, polyvinylpyrrolidone or sodium alginate.
The nano silicon dioxide is modified nano silicon dioxide, and the modification method comprises the following steps: according to the weight parts, 60-80 parts of ethyl orthosilicate, 100-150 parts of absolute ethyl alcohol, 20-30 parts of citric acid solution with the concentration of 0.1mol/L and 10-20 parts of silane coupling agent KH-560 are mixed and then hydrolyzed at the constant temperature of 60-65 ℃ for 3-5 hours, after the hydrolysis is finished, heating and evaporating are carried out to obtain mixed gel, the obtained mixed gel is washed by deionized water until the washing liquid is neutral, and then drying, crushing and sieving are carried out to obtain the modified nano silicon dioxide.
The pH value is 4.8-5.2.
Compared with other methods, the method has the beneficial technical effects that:
(1) the invention firstly modifies the nano-silica generated by hydrolyzing tetraethoxysilane through a silane coupling agent, so that the adsorbed water and silicon hydroxyl on the surface of the nano-silica are partially replaced by organic groups of the silane coupling agent to form the modified nano-silica which can be stably and uniformly dispersed, and is supplemented with nano-alumina, nano-zirconia and nano-hydroxyapatite, in the process of curing and film-forming the product, the nano particles can form a hydrophobic bionic structure similar to lotus leaves on the surface of a substrate, the contact angle can reach more than 150 degrees, the wetting by water is avoided, in addition, the organosilicon component contained in the product can form a compact reticular siloxane film on the surface and inside the substrate material, and is matched with a hydrophobic bionic structure formed on the surface of the substrate, therefore, the waterproof effect is achieved, the corrosion of acid, alkali and salt solutions to the waterproof film can be effectively avoided, and meanwhile, the hydrophobic bionic structure formed by the added inorganic nano particles does not hinder the water vapor in the substrate from permeating out;
(2) the existence of the added inorganic nano-powder such as nano-silica can effectively shield ultraviolet light, thereby protecting the waterproof film, preventing the waterproof film from aging, improving the weather resistance of the waterproof film and prolonging the service life of the waterproof coating;
(3) according to the invention, through the addition of the nano inorganic powder and the modification of the nano silicon dioxide, the combination of the nano material, the polymer and the substrate material at the molecular level is promoted, the strength of the formed waterproof film and the adhesive force of the waterproof film and the substrate are enhanced, and the service life of the product is further prolonged.
Detailed Description
Taking 60-80 parts by weight of ethyl orthosilicate, 100-150 parts by weight of absolute ethyl alcohol, 20-30 parts by weight of 0.1mol/L citric acid solution and 10-20 parts by weight of silane coupling agent KH-560 in sequence, firstly pouring the absolute ethyl alcohol, the citric acid solution and the silane coupling agent KH-560 into a reaction kettle, stirring at a constant temperature of 60-65 ℃ and a rotation speed of 300-500 r/min for 30-60 min, then dropwise adding the ethyl orthosilicate into the reaction kettle, continuously stirring at a constant temperature for hydrolysis for 3-5 h after the dropwise adding is finished, obtaining a hydrolysate, pouring the obtained hydrolysate into an evaporation vessel, heating and evaporating to obtain mixed gel, washing the obtained mixed gel with deionized water until the washing liquid is neutral, transferring the washed mixed gel into an oven, drying at a temperature of 105-110 ℃ to a constant weight to obtain dried gel, then pouring the dried gel into a pulverizer, after crushing, sieving with a sieve of 400-600 meshes to obtain modified nano silicon dioxide; then adding 60-80 parts by weight of modified nano-silica, 20-30 parts by weight of nano-alumina, 8-10 parts by weight of nano-zirconia and 10-15 parts by weight of nano-hydroxyapatite into a mixer, and stirring and mixing for 2-4 hours to obtain nano inorganic powder; then sequentially taking 200-300 parts by weight of oligomer siloxane base material, 10-30 parts by weight of emulsifier, 20-60 parts by weight of stabilizer, 4-6 parts by weight of curing agent, 180-200 parts by weight of diluent, 3-6 parts by weight of thickener and 100-150 parts by weight of nano inorganic powder, firstly adding the diluent, the emulsifier, the stabilizer, the curing agent, the thickener and the nano inorganic powder into a reaction kettle according to a formula, stirring and mixing for 45-60 min at a constant temperature of 60-70 ℃ and a rotation speed of 600-800 r/min, adding the oligomer siloxane base material, continuously stirring and reacting for 4-6 h at a constant temperature, transferring the materials in the reaction kettle into a high-pressure homogenizer, emulsifying under the pressure of 140-180 MPa to obtain an emulsion, standing for 10-20 min, removing floating substances on the surface of the emulsion, adjusting the pH to 4.8-5.2 by using hydrochloric acid with the mass fraction of 8-10%, and filling to obtain the nano inorganic powder modified organic silicon waterproof coating. Wherein the oligomer siloxane base material is two of hydroxyl-terminated polydimethylsiloxane, carboxyl-terminated polydimethylsiloxane or amino-terminated polydimethylsiloxane, and the mass ratio of the two is 1: 1. Wherein the emulsifier is one of sodium stearate, tween-60 or span-80. Wherein the stabilizer is one of sodium dodecyl benzene sulfonate, cetyl trimethyl ammonium bromide or octadecyl polyoxyethylene ether. Wherein the curing agent is one of triethanolamine or polyamide curing agent 651. Wherein the diluent is one of deionized water, softened water or distilled water. Wherein the thickening agent is one of sodium carboxymethylcellulose, hydroxyethyl cellulose, polyvinylpyrrolidone or sodium alginate.
Example 1
Adding 60 parts of nano silicon dioxide, 20 parts of nano alumina, 8 parts of nano zirconia and 10 parts of nano hydroxyapatite into a mixer by weight, and stirring and mixing for 2 hours to obtain nano inorganic powder; then according to the weight portion, taking 100 portions of hydroxyl-terminated polydimethylsiloxane, 100 portions of carboxyl-terminated polydimethylsiloxane, 10 portions of sodium stearate, 20 portions of sodium dodecyl benzene sulfonate, 4 portions of triethanolamine, 180 portions of deionized water, 3 portions of sodium carboxymethyl cellulose and 100 portions of nano inorganic powder in sequence, firstly adding deionized water, sodium stearate, sodium dodecyl benzene sulfonate, triethanolamine, sodium carboxymethyl cellulose and nano inorganic powder into a reaction kettle according to the formula, stirring and mixing for 45min at the constant temperature of 60 ℃ and the rotation speed of 600r/min, then adding the hydroxyl-terminated polydimethylsiloxane and the carboxyl-terminated polydimethylsiloxane, continuing stirring and reacting for 4h at the constant temperature, then transferring the materials in the reaction kettle into a high-pressure homogenizer, emulsifying under the pressure of 140MPa to obtain an emulsion, removing floaters on the surface of the emulsion after 10min, and then hydrochloric acid with the mass fraction of 8% is used for adjusting the pH value to 4.8, and filling is carried out, thus obtaining the nano inorganic powder modified organic silicon waterproof coating.
Example 2
According to the weight portion, 70 portions of ethyl orthosilicate, 130 portions of absolute ethyl alcohol, 25 portions of citric acid solution with the concentration of 0.1mol/L and 15 portions of silane coupling agent KH-560 are taken in turn, firstly, the absolute ethyl alcohol, the citric acid solution and the silane coupling agent KH-560 are poured into a reaction kettle, stirring at constant temperature of 63 deg.C and rotation speed of 400r/min for 45min, adding ethyl orthosilicate dropwise into the reaction kettle, stirring at constant temperature for hydrolyzing for 4 hr to obtain hydrolysate, pouring the hydrolysate into an evaporating dish, heating for evaporating to obtain mixed gel, washing the obtained mixed gel with deionized water until the washing solution is neutral, transferring the washed mixed gel into an oven, drying at 108 ℃ to constant weight to obtain dried gel, then pouring the dried gel into a pulverizer, and sieving with a 500-mesh sieve after pulverizing to obtain modified nano silicon dioxide; adding 70 parts of modified nano-silica, 25 parts of nano-alumina, 9 parts of nano-zirconia and 13 parts of nano-hydroxyapatite into a mixer according to parts by weight, and stirring and mixing for 3 hours to obtain nano inorganic powder; then according to the weight portion, 125 portions of carboxyl-terminated polydimethylsiloxane, 125 portions of amino-terminated polydimethylsiloxane, 20 portions of tween-60, 40 portions of hexadecyl trimethyl ammonium bromide, 5 portions of polyamide curing agent 651, 190 portions of softened water, 5 portions of hydroxyethyl cellulose and 130 portions of nano inorganic powder are taken in sequence, softened water, tween-60, hexadecyl trimethyl ammonium bromide, polyamide curing agent 651, hydroxyethyl cellulose and nano inorganic powder are firstly added into a reaction kettle according to the formula, the mixture is stirred and mixed for 52min at the constant temperature of 65 ℃ and the rotating speed of 700r/min, then carboxyl-terminated polydimethylsiloxane and amino-terminated polydimethylsiloxane are added, the mixture is stirred and reacted for 5h at the constant temperature, then the materials in the reaction kettle are transferred into a high-pressure homogenizer and emulsified under the pressure of 160MPa to obtain an emulsified liquid, the emulsified liquid is stood for 15min, removing floating substances on the surface of the emulsion, adjusting the pH to 5.0 by using 9% hydrochloric acid by mass, and filling to obtain the nano inorganic powder modified organic silicon waterproof coating.
Comparative example: silicone water-proof paint sold in texas corporation.
The nano inorganic powder modified organosilicon waterproof coating obtained in the above embodiment and the organosilicon waterproof coating obtained in the control example are detected, specifically, the detection is as follows:
1. and (3) testing the permeability: preparing concrete blocks of 10cm multiplied by 10cm, curing the concrete blocks in a standard curing box for 28 days, drying in a 60 ℃ drying oven to constant weight, respectively coating the nano inorganic powder modified organosilicon waterproof coating and the organosilicon waterproof coating obtained in the comparative example on the surfaces of the concrete blocks, drying the concrete blocks coated with the waterproof coating at room temperature for 1 day, vertically splitting, wetting with water, and testing the penetration depth of the waterproof coating of each test block;
2. water absorption test: respectively weighing the concrete block coated with the nano inorganic powder modified organosilicon waterproof coating and the concrete block coated with the organosilicon waterproof coating obtained in the control example, putting the concrete blocks on a metal shelf in a container, confirming that the test surface is downward, adding distilled water at a standard test temperature, keeping the liquid level higher than the shelf by 3mm, taking out the concrete block after 24 hours, sucking water by using towel paper, and immediately weighing;
3. scrub resistance test: respectively placing the concrete block coated with the nano inorganic powder modified organosilicon waterproof coating and the concrete block coated with the organosilicon waterproof coating obtained in the control example on a scrub resistance tester to perform a parallel scrubbing test;
4. the coating resists temperature change: the concrete block coated with the nano inorganic powder modified organosilicon waterproof coating and the concrete block coated with the organosilicon waterproof coating obtained in the control example are respectively put into a constant temperature box at 90 +/-2 ℃ for 240 hours, taken out and placed at room temperature for 0.5 hour, then put into a low temperature box at (-20 +/-2) ℃ for 24 hours, and then taken out and placed at room temperature for 0.5 hour.
The detection results are shown in the table I.
Table one:
| detecting items | Penetration depth/mm | Water absorption ratio/%) | Service life/year | Washing and brushing resistance | Coating temperature resistance (5 cycles) | Contact angle |
| Example 1 | 13 | 10 | 13 | Washing 2500 times without exposing the substrate | No abnormality | 155° |
| Example 2 | 15 | 9 | 15 | Washing 2500 times without exposing the substrate | No abnormality | 170° |
| Comparative example | 12 | 12 | 12 | Washing 2500 times to expose the substrate | The coating has the phenomena of chalking and cracking | 150° |
As can be seen from the above table, the nano inorganic powder modified organosilicon waterproof coating has better weather resistance and long service life.
Claims (8)
1. A nanometer inorganic powder modified organosilicon waterproof coating is characterized in that: the composite material is prepared from the following raw materials in parts by weight: 200-300 parts of oligomer siloxane base material, 10-30 parts of emulsifier, 20-60 parts of stabilizer, 4-6 parts of curing agent, 180-200 parts of diluent, 3-6 parts of thickener and 100-150 parts of nano inorganic powder;
the nano inorganic powder is prepared by mixing the following raw materials in parts by weight: 60-80 parts of nano silicon dioxide, 20-30 parts of nano alumina, 8-10 parts of nano zirconia and 10-15 parts of nano hydroxyapatite;
the specific configuration method is as follows:
(1) adding a diluent, an emulsifier, a stabilizer, a curing agent, a thickening agent and nano inorganic powder into a reaction kettle according to a formula, uniformly stirring at constant temperature, then adding an oligomer siloxane base material, and continuously stirring at constant temperature for reaction;
(2) after the constant-temperature stirring reaction is finished, transferring the materials in the reaction kettle into a high-pressure homogenizer for emulsification to obtain an emulsion;
(3) removing floating substances on the surface of the emulsion, adjusting the pH value by hydrochloric acid, and filling to obtain the nano inorganic powder modified organosilicon waterproof coating;
the nano silicon dioxide is modified nano silicon dioxide, and the modification method comprises the following steps: according to the weight parts, 60-80 parts of ethyl orthosilicate, 100-150 parts of absolute ethyl alcohol, 20-30 parts of citric acid solution with the concentration of 0.1mol/L and 10-20 parts of silane coupling agent KH-560 are mixed and then hydrolyzed at the constant temperature of 60-65 ℃ for 3-5 hours, after the hydrolysis is finished, heating and evaporating are carried out to obtain mixed gel, the obtained mixed gel is washed by deionized water until the washing liquid is neutral, and then drying, crushing and sieving are carried out to obtain the modified nano silicon dioxide.
2. The nano inorganic powder modified organosilicon waterproof coating of claim 1, which is characterized in that: the oligomer siloxane base material is two of hydroxyl-terminated polydimethylsiloxane, carboxyl-terminated polydimethylsiloxane or amino-terminated polydimethylsiloxane, and the mass ratio of the two is 1: 1.
3. The nano inorganic powder modified organosilicon waterproof coating of claim 1, which is characterized in that: the emulsifier is one of sodium stearate, tween-60 or span-80.
4. The nano inorganic powder modified organosilicon waterproof coating of claim 1, which is characterized in that: the stabilizer is one of sodium dodecyl benzene sulfonate, cetyl trimethyl ammonium bromide or octadecyl polyoxyethylene ether.
5. The nano inorganic powder modified organosilicon waterproof coating of claim 1, which is characterized in that: the curing agent is one of triethanolamine or polyamide curing agent 651.
6. The nano inorganic powder modified organosilicon waterproof coating of claim 1, which is characterized in that: the diluent is one of deionized water, softened water or distilled water.
7. The nano inorganic powder modified organosilicon waterproof coating of claim 1, which is characterized in that: the thickening agent is one of sodium carboxymethylcellulose, hydroxyethyl cellulose, polyvinylpyrrolidone or sodium alginate.
8. The nano inorganic powder modified organosilicon waterproof coating of claim 1, which is characterized in that: the pH value is 4.8-5.2.
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| CN115926742A (en) * | 2022-12-02 | 2023-04-07 | 江苏中恒电子新材料有限公司 | Organic silicon gel for waterproofing instruments and meters and preparation method thereof |
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| CN103436165B (en) * | 2013-09-13 | 2016-01-13 | 上海交通大学 | Water-proof stain-resistant nano composite dope and preparations and applicatio method thereof |
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