CN109761576B - Functional sealing curing agent and preparation method thereof - Google Patents
Functional sealing curing agent and preparation method thereof Download PDFInfo
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- CN109761576B CN109761576B CN201910213153.7A CN201910213153A CN109761576B CN 109761576 B CN109761576 B CN 109761576B CN 201910213153 A CN201910213153 A CN 201910213153A CN 109761576 B CN109761576 B CN 109761576B
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Abstract
The invention provides a functional sealing curing agent and a preparation method thereof, wherein the improved functional sealing curing agent comprises the following components in percentage by weight: 3-30 wt% of silicate, 0.1-10 wt% of double-shell core-shell structure nano particles, 0.05-0.5 wt% of an auxiliary agent and the balance of water; the invention also provides a preparation method comprising the specific steps. The preparation process is simple, the product stability is good, and the product is colorless, nontoxic and environment-friendly; after the coating is applied to the surface of concrete, the coating has excellent durability on the relevant performances of wear resistance, self-cleaning, antibiosis and the like; the strength, hardness, compactness and the like of the concrete surface can be greatly improved.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to a functional sealing curing agent and a preparation method thereof.
Background
At present, concrete terraces are widely applied to the field of buildings, although the concrete terraces are compact, the concrete terraces also have inherent defects of concrete structures, the concrete terraces are ground which is constructed and treated on the original ground and has certain strength and rigidity, and the strength of the concrete terraces mainly comes from calcium silicate compounds generated by silicon and calcium in cement components in the concrete under the action of hydration. The slow hydration reaction is still carried out in the concrete terrace after the initial setting, the reaction can not be completely carried out under the natural condition, and a large amount of free calcium ions can not react to generate calcium silicate compounds, so the concrete hardness has great potential, and the concrete terrace is easy to dust and has poor durability.
Aiming at the problems of the concrete terrace, the concrete sealing and curing agent is generally adopted to treat the concrete structure in the prior art. At present, the combination of the single-component sealing curing agent for the concrete surface and the cement terrace polishing technology can enable the ground to achieve beautiful glossiness and practical effect, and becomes the mainstream of the development of the concrete terrace market. However, people have higher and higher requirements on the aspect of ground functionality, the concept of the multifunctional terrace is advanced, and special concrete ground materials with high wear resistance, self-cleaning function, antibacterial function and the like have wide application prospects. Although some companies at home and abroad report some sealing curing agent materials with special functions, most of the sealing curing agent materials have the defects of poor stability, poor efficacy durability and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a functional sealing curing agent and a preparation method thereof.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
the invention provides a functional sealing curing agent, which comprises the following components in percentage by weight: 3-30 wt% of silicate, 0.1-10 wt% of double-shell core-shell structure nano particles, 0.05-0.5 wt% of an auxiliary agent and the balance of water.
Wherein the silicate is one or more of lithium silicate, sodium silicate and potassium silicate. If the silicate content is too high, the stability of the sealing curing agent is poor, and the sealing curing agent is not beneficial to storage and transportation, and if the silicate content is too low, the curing agent is dried too slowly after application, the construction efficiency is low, and meanwhile, the transportation cost of the curing agent is too high.
The double-shell core-shell structure nano particle is a composite nano particle taking one of nano aluminum oxide, nano zirconium oxide, nano silicon oxide, nano titanium dioxide, doped nano titanium dioxide, nano zinc oxide or nano silver as a core layer, silicon dioxide as an inner shell layer and a silane coating layer as an outer shell layer, and the particle size of the nano particle is 1-100 nm. The nano material is widely used as a functional additive of a plurality of materials due to the specific surface effect and size effect. If the content of the double-shell core-shell structure nano particles in the sealing curing agent is too low, the functional effect is not obvious, and if the content of the double-shell core-shell structure nano particles in the sealing curing agent is too high, the dispersion of the nano particles in the sealing curing agent can be influenced, and the integral bonding force of the sealing curing agent and a concrete matrix can also be reduced. The particle size of the nano particles cannot be too large, and the nano particles are prevented from permeating into the concrete due to the too large size.
The nano particles have a double-shell type core-shell structure, the inner shell layer is a silicon dioxide layer, by means of the layer, chemical bond connection between the whole nano particles and a sealing curing agent and between the whole nano particles and a concrete base material can be realized by using active silicon on the surface of the silicon dioxide layer, the durability of the effect can be greatly improved, and the outer shell layer is a silane coating layer. Due to the double-shell structure of the nano particles, on one hand, the dispersion stability of the nano particles in a curing agent product can be greatly improved, and on the other hand, the abrasion, falling off and the like of the functional nano particles caused by external physical and chemical actions after the curing agent is applied to a concrete base material can be effectively prevented, so that the durability of the efficacy of the nano particles in the service period can be greatly improved.
Preferably, the auxiliary agent is one or a mixture of more than one of a cationic surfactant, an anionic surfactant and a nonionic surfactant.
Further preferably, the cationic surfactant is one or more of long-chain alkyl primary amine salt, secondary amine salt and tertiary amine salt, the anionic surfactant is one or more of stearic acid, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate, and the nonionic surfactant is one or more of tween 60, tween 80, span 60 and span 80.
Preferably, the doped nano titanium dioxide is one or a mixture of more than one of nitrogen-doped titanium dioxide, iron-doped titanium dioxide, vanadium-doped titanium dioxide and chromium-doped titanium dioxide.
Meanwhile, the invention also provides a preparation method of the sealing curing agent, which comprises the following steps:
s1, preparing the double-shell core-shell structure nano particles: adding nano aluminum oxide, nano zirconium oxide, nano silicon oxide, nano titanium dioxide, doped nano titanium dioxide, nano zinc oxide or nano silver into a solvent, adding tetraethoxysilane, a catalyst and water, carrying out ultrasonic stirring reaction for 6-18 hours at 40-120 ℃, adding a silane coupling agent, continuing the reaction for 2-10 hours, removing the solvent, and washing to obtain the double-shell core-shell structure nano particle, wherein the concentration of the nano aluminum oxide, the nano zirconium oxide, the nano silicon oxide, the nano titanium dioxide, the doped nano titanium dioxide, the nano zinc oxide or the nano silver is 1-10 wt%, the concentration of the tetraethoxysilane is 0.5-15 wt%, the concentration of the catalyst is 0.001-0.1 wt%, the concentration of the water is 0.5-5 wt%, and the concentration of the silane coupling agent is 0.1-2.5 wt%;
s2, compounding of each component: adding the double-shell core-shell structure nanoparticles into water according to a proportion, performing ultrasonic dispersion for 2-4 hours, adding silicate for dispersion, adding an auxiliary agent, and uniformly stirring to obtain the functional sealing curing agent.
Preferably, the solvent is one or more of methanol, ethanol, propanol, isopropanol, butanol, hexanol, tetrahydrofuran, ethyl acetate, butyl acetate, MIBK, propylene glycol methyl ether and propylene glycol methyl ether acetate.
Preferably, the catalyst is one of ammonia water, sodium hydroxide, potassium hydroxide, tetramethylammonium hydroxide, tetrabutylammonium hydroxide, nitric acid, sulfuric acid, hydrochloric acid and acetic acid.
Preferably, the silane coupling agent is one or more of kh131, kh132, kh330, kh580, kh222, kh1631, kh560, kh561, kh902, kh554, kh602, kh792, kh550 and kh 540.
Compared with the prior art, the invention has the beneficial effects that:
(1) after the sealing curing agent is applied to the surface of concrete, the sealing curing agent has excellent durability on the relevant performances of wear resistance, self-cleaning, antibiosis and the like;
(2) the preparation process of the sealing curing agent is simple, and the obtained sealing curing agent has good stability;
(3) the invention is a colorless, nontoxic and environment-friendly product, and can greatly improve the strength, hardness, compactness and the like of the concrete surface after being applied to the concrete surface.
Detailed Description
The invention is explained below with reference to specific embodiments, which are intended to illustrate the invention and are not to be construed as limiting the invention.
Example 1
The functional sealing curing agent provided by the invention comprises the following substances in parts by weight: 20 wt% of sodium silicate, 3 wt% of double-shell type core-shell structure nano titanium dioxide, 0.5wt% of sodium dodecyl sulfate and the balance of water. The preparation method comprises the following steps:
(1) preparing core-shell structure nanoparticles: adding nano titanium dioxide into a mixed solvent of ethanol and butyl acetate, adding ethyl orthosilicate, catalyst ammonia water and water, carrying out ultrasonic stirring reaction for 8 hours at 90 ℃, adding kh131 and kh550, continuing the reaction for 5 hours, removing the solvent, and washing to obtain the double-shell core-shell structure nano particles, wherein the concentration of the nano particles is 5wt%, the concentration of the ethyl orthosilicate is 0.5wt%, the concentration of the catalyst is 0.1wt%, the concentration of the water is 5wt%, and the concentration of the silane coupling agent is 0.5 wt%.
(2) Compounding the components: adding the double-shell core-shell structure nano particles into water according to a proportion, performing ultrasonic dispersion for 2 hours, adding silicate for dispersion, adding sodium dodecyl sulfate, and uniformly stirring to obtain the functional sealing curing agent.
And applying the functional sealing curing agent on the surface of the concrete base material, curing and testing related performances.
Example 2
The functional sealing curing agent provided by the invention comprises the following substances in parts by weight: 10wt% of sodium silicate, 5wt% of potassium silicate, 2 wt% of lithium silicate, 10wt% of double-shell type core-shell structure nano alumina, 0.05 wt% of tween 80 and the balance of water.
(1) Preparing core-shell structure nanoparticles: adding nano aluminum oxide into a mixed solvent of butyl acetate and propylene glycol monomethyl ether, adding ethyl orthosilicate, a catalyst nitric acid and water, carrying out ultrasonic stirring reaction for 6 hours at 110 ℃, adding kh330 and kh792, continuing the reaction for 2 hours, removing the solvent, and washing to obtain the double-shell core-shell structure nano particles, wherein the concentration of the nano particles is 1.5 wt%, the concentration of the ethyl orthosilicate is 1wt%, the concentration of the catalyst is 0.05 wt%, the concentration of the water is 1.5 wt%, and the concentration of the silane coupling agent is 0.2 wt%.
(2) Compounding the components: adding the double-shell core-shell structure nano particles into water according to a proportion, performing ultrasonic dispersion for 2 hours, adding silicate for dispersion, adding tween 80, and uniformly stirring to obtain the functional sealing curing agent.
And applying the functional sealing curing agent on the surface of the concrete base material, curing and testing related performances.
Example 3
The functional sealing curing agent provided by the invention comprises the following substances in parts by weight: 20 wt% of sodium silicate, 2 wt% of double-shell type core-shell structure nano zinc oxide, 0.1wt% of long-chain alkyl primary amine salt and the balance of water.
(1) Preparing core-shell structure nanoparticles: adding nano zinc oxide into a mixed solvent of tetrahydrofuran and isopropanol, adding ethyl orthosilicate, a catalyst sodium hydroxide and water, carrying out ultrasonic stirring reaction for 18 hours at 40 ℃, adding kh602, continuing the reaction for 10 hours, removing the solvent, and washing to obtain the double-shell core-shell structure nano particles, wherein the concentration of the nano particles is 5wt%, the concentration of the ethyl orthosilicate is 9 wt%, the concentration of the catalyst is 0.002 wt%, the concentration of the water is 5wt%, and the concentration of the silane coupling agent is 2 wt%.
(2) Compounding the components: adding the double-shell core-shell structure nano particles into water according to a proportion, performing ultrasonic dispersion for 2 hours, adding silicate for dispersion, adding long-chain alkyl primary amine salt, and uniformly stirring to obtain the functional sealing curing agent.
And applying the functional sealing curing agent on the surface of the concrete base material, curing and testing related performances.
Comparative example 1
The sealing curing agent consists of the following substances in parts by weight: 25 wt% sodium silicate, and the balance water.
The sealing curing agent is applied to the surface of a concrete base material and cured, and then relevant performances are tested.
Comparative example 2
The sealing curing agent consists of the following substances in parts by weight: 25 wt% of sodium silicate, 2 wt% of nano zinc oxide and the balance of water. After the sealing curing agent is applied to the surface of the concrete base material and cured, the relevant performance is tested, and the result is shown in table 1.
TABLE 1 comparative table of sample test data of each example
| Blank sample | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | |
| Mohs hardness | 5 | 7 | 8 | 7 | 7 | 6 |
| Abrasion resistance ratio | 100％ | 200％ | 290％ | 230％ | 230％ | 160％ |
| Antibacterial property for 30 days | Is free of | Is free of | Is free of | Is provided with | Is free of | Is provided with |
| Self-cleaning property for 30 days | Is free of | Is provided with | Is free of | Is free of | Is free of | Is free of |
| Antibacterial property for 720 days | Is free of | Is free of | Is free of | Is provided with | Is free of | Is free of |
| Self-cleaning property in 720 days | Is free of | Is provided with | Is free of | Is free of | Is free of | Is free of |
As can be seen from Table 1, the concrete surface hardness-improving agent has a remarkable effect of improving the hardness of the concrete surface, has an excellent wear resistance ratio, is obviously superior to a comparative example in self-cleaning and antibacterial properties, and has excellent durability.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. A functional sealing curing agent is characterized by comprising the following components in percentage by weight: 3-30 wt% of silicate, 2-10 wt% of double-shell core-shell structure nanoparticles, 0.05-0.5 wt% of an auxiliary agent and the balance of water, wherein the silicate is one or more of lithium silicate, sodium silicate and potassium silicate; the double-shell core-shell structure nano particle is a composite nano particle taking one of nano aluminum oxide, nano zirconium oxide, nano silicon oxide, nano titanium dioxide, doped nano titanium dioxide, nano zinc oxide or nano silver as a core layer, silicon dioxide as an inner shell layer and a silane coating layer as an outer shell layer, and the particle size of the nano particle is 1-100 nm;
the auxiliary agent is one or a mixture of more than one of a cationic surfactant, an anionic surfactant and a nonionic surfactant;
the cationic surfactant is one or more of long-chain alkyl primary amine salt, secondary amine salt and tertiary amine salt, the anionic surfactant is one or more of stearic acid, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate, and the nonionic surfactant is one or more of tween 60, tween 80, span 60 and span 80.
2. The functional sealing curing agent according to claim 1, wherein the doped nano titanium dioxide is one or more of nitrogen-doped titanium dioxide, iron-doped titanium dioxide, vanadium-doped titanium dioxide and chromium-doped titanium dioxide.
3. A method for preparing the functional sealing curing agent according to any one of claims 1-2, comprising the steps of:
s1, preparing the double-shell core-shell structure nano particles: adding nano aluminum oxide, nano zirconium oxide, nano silicon oxide, nano titanium dioxide, doped nano titanium dioxide, nano zinc oxide or nano silver into a solvent, adding tetraethoxysilane, a catalyst and water, carrying out ultrasonic stirring reaction for 6-18 hours at 40-120 ℃, adding a silane coupling agent, continuing the reaction for 2-10 hours, removing the solvent, and washing to obtain the double-shell core-shell structure nano particle, wherein the concentration of the nano aluminum oxide, the nano zirconium oxide, the nano silicon oxide, the nano titanium dioxide, the doped nano titanium dioxide, the nano zinc oxide or the nano silver is 1-10 wt%, the concentration of the tetraethoxysilane is 0.5-15 wt%, the concentration of the catalyst is 0.001-0.1 wt%, the concentration of the water is 0.5-5 wt%, and the concentration of the silane coupling agent is 0.1-2.5 wt%;
s2, compounding of each component: adding the double-shell core-shell structure nanoparticles into water according to a proportion, performing ultrasonic dispersion for 2-4 hours, adding silicate for dispersion, adding an auxiliary agent, and uniformly stirring to obtain the functional sealing curing agent.
4. The method of claim 3, wherein the solvent is one or more selected from methanol, ethanol, propanol, isopropanol, butanol, hexanol, tetrahydrofuran, ethyl acetate, butyl acetate, MIBK, propylene glycol methyl ether, and propylene glycol methyl ether acetate.
5. The method of claim 4, wherein the catalyst is one of ammonia, sodium hydroxide, potassium hydroxide, tetramethylammonium hydroxide, tetrabutylammonium hydroxide, nitric acid, sulfuric acid, hydrochloric acid, and acetic acid.
6. The method of claim 4, wherein the silane coupling agent is one or more selected from the group consisting of KH131, KH132, KH330, KH580, KH1631, KH560, KH561, KH902, KH554, KH602, KH792, KH550, and KH 540.
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| CN110304942A (en) * | 2019-08-08 | 2019-10-08 | 北京凯博达地坪科技有限公司 | A kind of construct seals solid agent material and its application method in the nano-silicon on mattess |
| CN112723914B (en) * | 2020-12-11 | 2022-03-04 | 四川砼道科技有限公司 | Concrete surface reinforcing agent and preparation method thereof |
| CN112961520A (en) * | 2021-04-06 | 2021-06-15 | 广州大学 | Water-resistant long-acting inorganic zinc oxide super-hydrophilic coating and preparation method and application thereof |
| CN114634327B (en) * | 2021-12-27 | 2023-03-21 | 德爱威（中国）有限公司 | Pure lithium-based sealing curing agent and preparation method thereof |
| CN114956733A (en) * | 2022-06-10 | 2022-08-30 | 日照海工研新材料有限公司 | High-strength anti-erosion marine concrete and preparation method thereof |
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| WO2009050639A1 (en) * | 2007-10-16 | 2009-04-23 | Nxp B.V. | Particle comprising core and shell and applications thereof |
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