CN113755035B - Epoxy silane modified nano alumina and polymer cement-based waterproof coating - Google Patents
Epoxy silane modified nano alumina and polymer cement-based waterproof coating Download PDFInfo
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- CN113755035B CN113755035B CN202111144529.7A CN202111144529A CN113755035B CN 113755035 B CN113755035 B CN 113755035B CN 202111144529 A CN202111144529 A CN 202111144529A CN 113755035 B CN113755035 B CN 113755035B
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
- C09C1/407—Aluminium oxides or hydroxides
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
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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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
- C09D1/06—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances cement
- C09D1/08—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances cement with organic additives
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/65—Additives macromolecular
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Abstract
The invention provides an epoxy silane modified nano-alumina and polymer cement-based waterproof coating, and particularly relates to the technical field of waterproof coatings. The epoxy silane modified nano-alumina is mainly obtained by modifying nano-alumina with epoxy silane. The mass ratio of the epoxy silane to the nano alumina is 2-12: 100. the polymer cement-based waterproof coating comprises a component A and a component B; the component A comprises nitrile carboxyl modified styrene-butadiene latex, and the component B comprises epoxy silane modified nano-alumina. The polymer cement-based waterproof coating provided by the invention can solve the problems of low coating bonding strength, large strength loss, separation of a waterproof layer from a base layer or self-destruction of the waterproof layer caused by water intolerance and high waterproof film water absorption rate in a water immersion or high humidity environment, and simultaneously meets the EC1plus environmental protection certification of Germany GEV association, and the safety of a waterproof system of a building structure is comprehensively guaranteed.
Description
Technical Field
The invention relates to the technical field of waterproof coatings, in particular to an epoxy silane modified nano-alumina and polymer cement-based waterproof coating.
Background
In actual use, the common polymer cement-based waterproof coating in the market at present has the problems of large smell and high TVOC release amount, and cannot meet the requirement of EC1plus environmental protection certification of Germany GEV Association. And the environmental conditions of the polymer cement-based waterproof coating and the standard test conditions (23 +/-2 ℃, 50 +/-10% humidity) specified by the national standard are greatly different, so that the performance of the polymer cement-based waterproof coating is greatly reduced. Under the long-term soaking or high-humidity environment, the polymer cement-based waterproof coating has the problems of low bonding strength, high strength loss, separation of the waterproof layer from the base layer or damage of the waterproof layer due to the factors of water intolerance, high water absorption of the waterproof film and the like. In the polymer cement-based waterproof coating, the used auxiliary agents mainly comprise silane coupling agents and nano-alumina. The silane coupling agent is added into the liquid components of the polymer cement-based waterproof coating, and loses effect due to gradual hydrolysis and self-polymerization along with the lapse of time; the nano-alumina is in a thermodynamic unstable state and is easy to agglomerate, so that the polymer cement-based waterproof coating is not uniformly dispersed, and a system is easy to separate.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide epoxy silane modified nano-alumina to solve the technical problems that in the prior art, when a silane coupling agent is added into a waterproof coating liquid component, hydrolysis is easy to occur, self-polymerization fails, and nano-alumina is easy to agglomerate, so that a polymer cement-based waterproof coating is not uniformly dispersed, and a system is easy to separate.
The second purpose of the invention is to provide the preparation method of the epoxy silane modified nano-alumina, which has the advantages of simple preparation process and convenient operation, and is suitable for large-scale industrial production.
The third purpose of the invention is to provide the application of the epoxy silane modified nano alumina in the polymer cement-based waterproof coating, and the application provides a powder assistant with excellent performance for the polymer cement-based waterproof coating, and is beneficial to improving the performance of the polymer cement-based waterproof coating.
The fourth purpose of the invention is to provide a polymer cement-based waterproof coating which has the characteristics of low water absorption, high strength and excellent environmental protection.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention provides epoxy silane modified nano alumina, which is mainly obtained by modifying nano alumina by epoxy silane.
Optionally, the mass ratio of the epoxy silane to the nano alumina is 2-12: 100.
preferably, the mass ratio of the epoxy silane to the nano alumina is 4-10: 100.
the second aspect of the present invention provides the preparation method of the epoxy silane modified nano alumina described in the first aspect, wherein the epoxy silane modified nano alumina is obtained by dispersing the nano alumina and then adding the dispersed nano alumina into the epoxy silane solution to react. Optionally, the temperature of the dispersion is 20-40 ℃.
Preferably, the rotation speed of the dispersion is 50-150 r/min.
Preferably, the temperature of the reaction is 70-100 ℃.
Preferably, the reaction time is 1.5-2.5 h.
Preferably, the rotation speed of the reaction is 100-300 r/min.
The third aspect of the invention provides the application of the epoxy silane modified nano-alumina in the first aspect or the epoxy silane modified nano-alumina prepared by the preparation method in the second aspect in polymer cement-based waterproof coatings.
The invention provides a polymer cement-based waterproof coating in a fourth aspect, which comprises a component A and a component B.
Wherein the A component comprises nitrile carboxyl modified styrene-butadiene latex; the component B comprises cement and epoxy silane modified nano-alumina.
The epoxy silane modified nano alumina is prepared by the epoxy silane modified nano alumina in the first aspect or the preparation method in the second aspect.
Optionally, the mass ratio of the component A to the component B is 1: 1-2.
Preferably, the mass ratio of the component A to the component B is 1: 1.2-1.8.
Preferably, the mass ratio of the component A to the component B is 1: 1.5.
Optionally, the component A comprises the following components in percentage by mass: 68-98% of nitrile carboxyl modified butadiene styrene latex, and the balance of water and/or additives;
preferably, the A component comprises 70-95% of nitrile carboxyl modified styrene-butadiene latex by mass percentage;
preferably, the additive comprises at least one of a defoamer, a preservative, a dispersant and a wetting agent.
Optionally, the mass ratio of the defoaming agent in the component A is 0.05-1%, the mass ratio of the preservative is 0.05-0.8%, the mass ratio of the dispersing agent is 0.05-1.5%, and the mass ratio of the wetting agent is 0.05-1.5%.
Preferably, the mass ratio of the defoaming agent in the component A is 0.1-0.8%, the mass ratio of the preservative is 0.1-0.5%, the mass ratio of the dispersing agent is 0.1-0.8%, and the mass ratio of the wetting agent is 0.1-0.8%.
Optionally, the component B comprises the following components in percentage by mass: 30-65% of cement, 1-10% of epoxy silane modified nano alumina and the balance of pigment, filler and/or auxiliary agent.
Optionally, the component B comprises the following components in percentage by mass: 40-60% of cement, 3-8% of epoxy silane modified nano alumina and the balance of pigment, filler and/or auxiliary agent.
Preferably, the pigment and filler comprises at least one of quartz sand, heavy calcium carbonate, metakaolin and silica micropowder.
Preferably, the auxiliary agent comprises at least one of a water reducing agent, cellulose ether and calcium formate.
Optionally, the mass percentage of the cellulose ether in the component B is 0.1-0.5%, the mass percentage of the quartz sand is 10-30%, the mass percentage of the heavy calcium is 10-30%, the mass percentage of the metakaolin is 1-8%, the mass percentage of the silicon micropowder is 1-6%, the mass percentage of the calcium formate is 0.1-0.5% and the mass percentage of the water reducing agent is 0.1-0.5%.
Preferably, the mass ratio of the quartz sand in the component B is 15-25%, the mass ratio of the triple superphosphate is 15-25%, and the mass ratio of the metakaolin is 3-6%.
The invention has at least the following beneficial effects:
according to the epoxy silane modified nano aluminum oxide provided by the invention, after the epoxy silane is modified, the hydroxyl on the surface of the nano aluminum oxide is reduced, no agglomeration occurs, and the dispersion performance of the nano aluminum oxide in the polymer cement-based waterproof coating is improved.
The preparation method of the epoxy silane modified nano-alumina provided by the invention has the advantages of simple preparation process, good controllability, large processing capacity, suitability for mass production and low cost.
The application of the epoxy silane modified nano-alumina in the polymer cement-based waterproof coating provided by the invention provides a powder auxiliary agent with excellent performance for the polymer cement-based waterproof coating, improves the dispersion performance of the nano-alumina in the polymer cement-based waterproof coating, solves the problem that a silane coupling agent is directly added into a liquid component of the polymer cement-based waterproof coating and is very easy to hydrolyze and self-polymerize, so that the problem of failure is solved, and improves the mechanical property, chemical resistance and water resistance of the coating.
The polymer cement-based waterproof coating provided by the invention uses nitrile carboxyl modified styrene-butadiene latex and epoxy silane modified nano-alumina, wherein epoxy groups in the epoxy silane modified nano-alumina can generate ring-opening crosslinking reaction with carboxyl groups in the nitrile carboxyl modified styrene-butadiene latex, and the epoxy silane modified nano-alumina is grafted onto a nitrile carboxyl modified styrene-butadiene latex molecular chain, so that a compact space network structure is formed after curing, and the crosslinking degree of the coating is improved. And the epoxy silane modified nano-alumina has the characteristics of high strength, high hardness and good water resistance, so that the adhesive force, tensile strength and hydrophobicity of the coating are enhanced, and the polymer cement-based waterproof coating can still keep good performance in a water immersion or high humidity environment.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. The components of embodiments of the present invention may be arranged and designed in a wide variety of different configurations.
In the middle of the 60's of the 20 th century, polymer cement-based waterproofing paints gradually started to be applied in the japanese minor renovation projects. By the 70 s, its range of use has gradually expanded to waterproofing underground works, water storage facilities and kitchen and toilet areas. The polymer cement-based waterproof coating is developed from the beginning of the 90 s in the 20 th century in China, and the promotion of green environment-friendly building material products is increased along with the increase of the national promotion force, so that the heat tide for promotion and production is formed quickly. Over 30 years of development, both in scale and technical content, have been at the forefront of the world. The polymer cement-based waterproof paint is a bi-component cement-based polymer cement-based waterproof paint composed of liquid materials and powder materials, and is uniformly stirred according to a certain liquid-powder ratio when in use, and then is coated on the surface of a substrate, and the polymer phase and a cement solid phase mutually penetrate, are crosslinked and cured to form a high-strength and flexible waterproof coating film.
The polymer cement-based waterproof coating on the market at present has the problems of large smell and high TVOC release amount in actual use, and cannot meet the requirement of EC1plus environmental protection certification of Germany GEV society. And the environmental conditions of the polymer cement-based waterproof coating and the standard test conditions (23 +/-2 ℃, 50 +/-10% humidity) specified by the national standard are greatly different, so that the performance of the polymer cement-based waterproof coating is greatly reduced. Under the long-term soaking or high-humidity environment, the polymer cement-based waterproof coating has the problems of low bonding strength, high strength loss, separation of the waterproof layer from the base layer or damage of the waterproof layer due to the factors of water intolerance, high water absorption of the waterproof film and the like.
The polymer emulsion commonly used by domestic manufacturers comprises VAE emulsion, styrene-acrylic emulsion and pure acrylate emulsion. The VAE emulsion is formed by polymerizing vinyl acetate and ethylene monomers through high-pressure emulsion, has relatively large molecular polarity and strong adhesive force with a base layer, can meet the requirements of EC1plus environmental protection certification of Germany GEV society through process design, but has poor long-term water resistance, can be hydrolyzed after long-term immersion, gradually loses flexibility, and cannot be applied in a long-term immersion environment.
The invention provides epoxy silane modified nano alumina, which is mainly obtained by modifying nano alumina with epoxy silane.
The invention aims to provide epoxy silane modified nano-alumina, which solves the technical problems that in the prior art, when a silane coupling agent is added into a liquid material component of a waterproof coating, hydrolysis and self-polymerization are easy to lose efficacy, and nano-alumina is easy to agglomerate, so that a polymer cement-based waterproof coating is not uniformly dispersed, and a system is easy to separate. After the epoxy silane is modified, the surface hydroxyl of the nano aluminum oxide is reduced, the nano aluminum oxide is not agglomerated, and the dispersion performance of the nano aluminum oxide in the polymer cement-based waterproof coating is improved.
Optionally, the mass ratio of the epoxy silane to the nano alumina is 2-12: 100.
when the mass ratio of the epoxy silane to the nano alumina is less than 2:100 hours, incomplete modification can be caused, the reduction of hydroxyl on the surface of the nano alumina is not obvious, and the dispersion performance of the nano alumina cannot be obviously improved; when the mass ratio of the epoxy silane to the nano alumina is more than 12: when the amount is 100, the epoxy silane is excessive, and the preparation cost is increased.
In some embodiments of the invention, the epoxysilane to nano-alumina mass ratio is typically, but not limited to, 2:100, 4:100, 6:100, 8:100, 10:100, or 12: 100.
Preferably, the mass ratio of the epoxy silane to the nano alumina is 4-10: 100.
in some preferred embodiments of the invention, the epoxysilane to nano-alumina mass ratio is typically, but not limited to, 4:100, 6:100, 8:100, or 10: 100.
The second aspect of the present invention provides a method for preparing the epoxysilane modified nano-alumina described in the first aspect, wherein the epoxysilane modified nano-alumina is obtained by dispersing the nano-alumina and then adding the dispersed nano-alumina into the epoxysilane solution to react.
The preparation method of the epoxy silane modified nano-alumina provided by the invention has the advantages of simple preparation process, good controllability, large processing capacity, suitability for mass production and low cost.
Preferably, the epoxysilane includes at least one of an epoxytrimethoxysilane coupling agent, an epoxytriethoxysilane coupling agent, an epoxytripropoxysilane coupling agent, an epoxymethoxyethoxysilane coupling agent, an epoxyacetoxysilane coupling agent, and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane.
Dissolving epoxy silane in a mixed solution of anhydrous ethanol and deionized water to obtain an epoxy silane solution, adjusting the pH of the epoxy silane solution to 3.3-4.5, and standing for 30-60 min.
In some embodiments of the invention, the time of standing is typically, but not limited to, 30min, 35min, 40min, 45min, 50min, 55min, or 60 min.
Preferably, the pH of the epoxysilane solution is 3.3-4.5.
In some embodiments of the invention, the pH of the epoxysilane solution is typically, but not limited to, 3.3, 3.4, 3.5, 3.6, 3.7, 3.8, 3.9, 4.0, 4.1, 4.2, 4.3, 4.4, or 4.5.
Optionally, the temperature of the dispersion is 20-40 ℃.
In some embodiments of the invention, the temperature of dispersion is typically, but not limited to, 20 ℃, 22 ℃, 24 ℃, 26 ℃, 28 ℃, 30 ℃, 32 ℃, 34 ℃, 36 ℃, 38 ℃ or 40 ℃.
Preferably, the rotation speed of the dispersion is 50-150 r/min.
In some embodiments of the invention, the dispersed rotational speed is typically, but not limited to, 50r/min, 60r/min, 70r/min, 80r/min, 90r/min, 100r/min, 120r/min, 130r/min, or 150 r/min.
Preferably, the pH of the reaction is between 3.3 and 4.5.
In some embodiments of the invention, the pH of the reaction is typically, but not limited to, 3.3, 3.4, 3.5, 3.6, 3.7, 3.8, 3.9, 4.0, 4.1, 4.2, 4.3, 4.4, or 4.5.
Preferably, the temperature of the reaction is 70-100 ℃.
In some embodiments of the invention, the temperature of the reaction is typically, but not limited to, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃ or 100 ℃.
Preferably, the reaction time is 1.5-2.5 h.
When the reaction time is less than 1.5h, the reaction time is insufficient, the modification is insufficient, and the grafting effect is poor; when the reaction time is more than 2.5 hours, at which point the modification is substantially completed, excessive stirring time increases the manufacturing cost. In some embodiments of the invention, the reaction time is typically, but not limited to, 1.5h, 1.6h, 1.7h, 1.8h, 2h, 2.1h, 2.2h, 2.3h, 2.4h, or 2.5 h.
Preferably, the rotation speed of the reaction is 100-300 r/min.
In some embodiments of the invention, the reaction is typically, but not limited to, at 100r/min, 120r/min, 140r/min, 160r/min, 180r/min, 200r/min, 220r/min, 240r/min, 260r/min, 280r/min, or 300 r/min.
According to the third aspect of the invention, the epoxy silane modified nano alumina provided by the first aspect or the epoxy silane modified nano alumina prepared by the preparation method provided by the second aspect is applied to polymer cement-based waterproof coatings.
The application of the epoxy silane modified nano-alumina in the polymer cement-based waterproof coating provided by the invention provides a powder auxiliary agent with excellent performance for the polymer cement-based waterproof coating, improves the dispersion performance of the powder auxiliary agent in the polymer cement-based waterproof coating, and improves the mechanical property, chemical resistance and water resistance of the coating.
According to a fourth aspect of the present invention, there is provided a polymer cement-based waterproofing coating comprising an A component and a B component.
Wherein the component A comprises nitrile carboxyl modified styrene-butadiene latex; the component B comprises cement and epoxy silane modified nano-alumina.
The epoxy silane modified nano alumina is prepared by the epoxy silane modified nano alumina in the first aspect or the preparation method in the second aspect.
According to the polymer cement-based waterproof coating provided by the invention, nitrile carboxyl modified styrene-butadiene latex and epoxy silane modified nano-alumina are used, wherein epoxy groups in the epoxy silane modified nano-alumina can generate ring-opening crosslinking reaction with carboxyl groups in the nitrile carboxyl modified styrene-butadiene latex, so that the epoxy silane modified nano-alumina is grafted onto a molecular chain of the nitrile carboxyl modified styrene-butadiene latex, a compact space network structure is formed after curing, and the crosslinking degree of a coating is improved. And the epoxy silane modified nano-alumina has the characteristics of high strength, large hardness, large specific surface area and good water resistance, so that the adhesive force, tensile strength and hydrophobicity of the coating are enhanced, the polymer cement-based waterproof coating still has high bonding strength and strength retention rate under long-term immersion or high-humidity environment, the problems of low bonding strength, large strength loss, separation of the waterproof layer from the base layer or self damage of the waterproof layer caused by water intolerance, high water absorption rate of a waterproof film and other factors of the common polymer cement-based waterproof coating under long-term immersion or high-humidity environment can be solved, simultaneously the EC1plus environmental protection certification of Germany GEV society is met, and the safety of a waterproof system of a building structure is comprehensively ensured.
The nitrile carboxyl modified styrene-butadiene latex is modified by taking a small amount of unsaturated carboxylic acid and acrylonitrile as functional monomers, and carboxyl and nitrile groups which are uniformly distributed are introduced into a polymerization chain segment of a styrene-butadiene polymer, so that the strength of the polymer cement-based waterproof coating and the bonding strength with a base layer are further improved on the premise of not influencing the water resistance. The butadiene and styrene monomers are hydrophobic monomers, so that the polarity is low, and a crosslinking effect can occur in a film forming process, so that the water resistance is good. The water-absorbing polymer emulsion can be used as a polymer emulsion in a polymer cement-based waterproof coating, and can improve the strength retention rate of the polymer cement-based waterproof coating after being soaked in water and reduce the water absorption rate. And the carboxyl can be hydrated with Ca (OH) generated by cement 2 The chemical reaction is carried out to generate a macromolecular network interweaving structure combined by ionic bonds, and the compactness of the structure is improved. Meanwhile, the coating film can be inhibited from efflorescence, and the product appearance is improved. The nitrile carboxyl modified styrene-butadiene latex does not contain ester groups and amino groups, so the nitrile carboxyl modified styrene-butadiene latex is good in environmental protection and excellent in water resistance, and can realize zero VOC and very low TVOC release amount.
The nitrile carboxyl modified styrene-butadiene latex is self-made, and the raw materials used in the method are polymerized by styrene (10% -30%), butadiene (10% -30%), acrylic acid (0.25% -2%), methacrylic acid (0.25% -2%) and acrylonitrile (0.5% -4%). The nitrile carboxyl modified styrene-butadiene latex is modified by taking a small amount of unsaturated carboxylic acid and acrylonitrile as functional monomers, and carboxyl and nitrile groups which are uniformly distributed are introduced into a polymerization chain segment of a styrene-butadiene polymer. A small amount of polar group-carboxyl (0.5% -2%) and nitrile group (0.5% -2%) are introduced, so that the strength of the waterproof coating and the bonding strength with a base layer can be further improved on the premise of not influencing the water resistance.
In some embodiments of the present invention, when the nitrile group content in the nitrile carboxyl modified styrene-butadiene latex is less than 0.5%, the prepared latex has low strength and poor adhesion; when the nitrile group content is more than 2%, the prepared latex has higher polarity and more reduced water resistance.
In some embodiments of the present invention, the nitrile group content of the nitrile carboxyl-modified styrene-butadiene latex is typically, but not limited to, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, or 2%.
In some embodiments of the present invention, when the content of carboxyl in the nitrile carboxyl modified styrene-butadiene latex is less than 0.5%, the prepared latex has low bonding strength, severe film saltpetering and poor powder compatibility; when the carboxyl content is more than 2%, the prepared latex has larger polarity and more reduced water resistance.
In some embodiments of the invention, the carboxyl content of the nitrile carboxyl modified styrene-butadiene latex is typically, but not limited to, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, or 2%.
Optionally, the mass ratio of the A component to the B component is 1:1-2, preferably 1:1.2-1.8, and more preferably 1: 1.5.
In some embodiments of the invention, the mass ratio of the a component to the B component is typically, but not limited to, 1:1, 1:1.2, 1:1.5, 1:1.8, or 1: 2.
Optionally, the component A comprises the following components in percentage by mass: 68-98% of nitrile carboxyl modified styrene-butadiene latex, and the balance of water and/or additives.
In some embodiments of the present invention, the mass percentage of the nitrile carboxyl-modified styrene-butadiene latex is typically, but not limited to, 68%, 70%, 72%, 74%, 76%, 78%, 80%, 82%, 84%, 86%, 88%, 90%, 92%, 94%, 96%, or 98%.
Preferably, the A component comprises 70-95% of nitrile carboxyl modified styrene-butadiene latex by mass percentage;
preferably, the additive includes at least one of a defoaming agent, a preservative, a dispersing agent, and a wetting agent.
Optionally, the mass ratio of the defoaming agent in the component A is 0.05-1%, the mass ratio of the preservative is 0.05-0.8%, the mass ratio of the dispersing agent is 0.05-1.5%, and the mass ratio of the wetting agent is 0.05-1.5%.
In some embodiments of the invention, the mass fraction of the defoamer is typically, but not limited to, 0.05%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, or 1%.
In some embodiments of the invention, the preservative is typically, but not limited to, 0.05%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, or 0.8% by weight.
In some embodiments of the invention, the mass fraction of the dispersant is typically, but not limited to, 0.05%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 1.1%, 1.2%, 1.3%, 1.4%, or 1.5%.
In some embodiments of the invention, the wetting agent is typically, but not by way of limitation, 0.05%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 1.1%, 1.2%, 1.3%, 1.4%, or 1.5% by mass.
Preferably, the mass ratio of the antifoaming agent in the component A is 0.1-0.8%, the mass ratio of the preservative is 0.1-0.5%, the mass ratio of the dispersing agent is 0.1-0.8%, and the mass ratio of the wetting agent is 0.1-0.8%.
The balance of water means that the sum of the mass percent of water and the mass percent of other substances in the component A is 100%.
Optionally, the component B comprises the following components in percentage by mass: 30-65% of cement, 1-10% of epoxy silane modified nano alumina and the balance of pigment, filler and/or auxiliary agent.
In some embodiments of the invention, the mass percentage of cement is typically, but not limited to, 30%, 35%, 40%, 45%, 50%, 55%, 60%, or 65%.
In some embodiments of the invention, the mass percent of the epoxysilane-modified nano-alumina is typically, but not limited to, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, or 10%.
Optionally, the component B comprises the following components in percentage by mass: 40-60% of cement, 3-8% of epoxy silane modified nano alumina and the balance of pigment, filler and/or auxiliary agent.
Preferably, the pigment and filler comprises at least one of quartz sand, heavy calcium carbonate, metakaolin and silica micropowder.
Preferably, the auxiliary agent comprises at least one of a water reducing agent, cellulose ether and calcium formate.
Optionally, the mass ratio of cellulose ether in the component B is 0.1-0.5%, the mass ratio of quartz sand is 10-30%, the mass ratio of heavy calcium is 10-30%, the mass ratio of metakaolin is 1-8%, the mass ratio of silicon micropowder is 1-6%, the mass ratio of calcium formate is 0.1-0.5% and the mass ratio of water reducer is 0.1-0.5%.
Preferably, the mass ratio of the quartz sand in the component B is 15-25%, the mass ratio of the triple superphosphate is 15-25%, and the mass ratio of the metakaolin is 3-6%.
In some embodiments of the invention, the mass percentage of cellulose ether is typically, but not limited to, 0.1%, 0.2%, 0.3%, 0.4%, or 0.5%.
In some embodiments of the invention, the mass percentage of silica sand is typically, but not limited to, 10%, 15%, 20%, 25%, or 30%.
In some embodiments of the invention, the weight percentage of triple superphosphate is typically, but not limited to, 10%, 15%, 20%, 25%, or 30%.
In some embodiments of the invention, the mass percentage of metakaolin is typically, but not limited to, 1%, 2%, 3%, 4%, 5%, 6%, 7%, or 8%.
In some embodiments of the invention, the mass percentage of the fine silica powder is typically, but not limited to, 1%, 2%, 3%, 4%, 5%, or 6%.
In some embodiments of the invention, the mass percentage of calcium formate is typically, but not limited to, 0.1%, 0.2%, 0.3%, 0.4%, or 0.5%.
In some embodiments of the invention, the water reducing agent is typically, but not limited to, 0.1%, 0.2%, 0.3%, 0.4% or 0.5% by mass.
Preferably, the defoamer comprises at least one of a mineral oil and silica mixture, a polyether modified siloxane, a fatty acid ester, a higher alcohol, a modified polyalkoxy ether, tri-n-butyl phosphate, a triglyceride, and a hydrophobically modified polysiloxane emulsion.
Preferably, the preservative comprises at least one of chloromethylisothiazolinone, methylisothiazolinone, benzisothiazolinone, 2-N-octyl-4-isothiazolin-3-one, 4, 5-dichloro-2-N-octyl-4-isothiazolin-3-one, benzoate, o-methyl-p-chlorophenol, 1, 6-dihydroxy-2, 5-dioxocyclohexane, N-3, 4-dichlorophenyl-N, N-dimethylurea and an organo bromine compound.
Preferably, the wetting agent includes at least one of a nonionic fluorocarbon, a polyether silicone, an alkyl naphthalene sulfonate, sodium lauryl sulfate, an alkyl polyoxyethylene ether, a polyethylene glycol type polyol, and a polyhydroxyalkyl ether.
Preferably, the cellulose ether comprises at least one of ethyl hydroxyethyl cellulose, methyl ethyl hydroxyethyl cellulose, hydrophobically modified methyl hydroxyethyl cellulose, methyl hydroxypropyl cellulose, hydroxyethyl cellulose, and carboxymethyl cellulose.
Preferably, the water reducing agent comprises at least one of calcium lignosulfonate, sodium lignosulfonate, polycyclic aromatic salt, water-soluble resin sulfonate, sodium sulfamate, naphthalene-based superplasticizer, aliphatic superplasticizer and polycarboxylate superplasticizer.
The present invention will be described in further detail with reference to examples and comparative examples.
The specifications and types of the raw materials used in the examples and comparative examples of the present invention are shown in table 1 below, and unless otherwise specified,% means mass percentage; those who do not specify the specific conditions are performed according to the conventional conditions or the conditions recommended by the manufacturer.
Table 1 specification and model of raw materials table
| Components | Model/specification | Manufacturer(s) of |
| Epoxysilanes | KH560 | Zhuo-Hui chemical industry |
| Nano alumina | High-purity nano alumina | Hangzhou Wanjing |
Example 1
This example provides an epoxy silane modified nano alumina, which is prepared by adding 30mL of a mixed solution of absolute ethanol and deionized water (ethanol to water mass ratio 9:1) into a 100mL beaker, then adding 0.4g of epoxy silane into the solution, adjusting the pH to 3.8 with dilute hydrochloric acid, and standing at (23 ± 2) ° c for 45 min. 150mL of mixed solution of absolute ethyl alcohol and deionized water (the mass ratio of the ethyl alcohol to the water is 9:1) is added into a 1L three-neck flask, a reflux condenser tube is connected, 20g of nano alumina is slowly added while stirring, the stirring speed is controlled at 120r/min, the temperature is controlled at 25 ℃, and the nano alumina is fully dispersed in the solution. After the dispersion is uniform, the stirring speed is increased to 200r/min, the temperature is increased to 85 ℃, the epoxy silane solution is added, then the pH value is adjusted to 3.8 by dilute hydrochloric acid, and the reaction is carried out for 2 hours. And carrying out vacuum filtration, washing and drying to obtain the epoxy silane modified nano-alumina.
Example 2
The present embodiment provides an epoxy silane modified nano alumina, which is different from embodiment 1 in that the addition amount of epoxy silane is 0.8g, and the remaining methods and steps are the same as embodiment 1 and are not repeated herein.
Example 3
The present embodiment provides an epoxy silane modified nano alumina, which is different from embodiment 1 in that the addition amount of epoxy silane is 1.2g, and the remaining methods and steps are the same as embodiment 1, and are not repeated herein.
Example 4
The present embodiment provides an epoxy silane modified nano alumina, which is different from embodiment 1 in that the addition amount of epoxy silane is 1.6g, and the remaining methods and steps are the same as embodiment 1, and are not repeated herein.
Example 5
The present embodiment provides an epoxy silane modified nano alumina, which is different from embodiment 1 in that the addition amount of epoxy silane is 2.0g, and the remaining methods and steps are the same as embodiment 1 and are not repeated herein.
Example 6
The present embodiment provides an epoxy silane modified nano alumina, which is different from embodiment 1 in that the addition amount of epoxy silane is 2.4g, and the remaining methods and steps are the same as embodiment 1, and are not repeated herein.
Example 7
The embodiment provides a polymer cement-based waterproof coating, wherein the epoxy silane modified nano alumina is provided in embodiment 6, and the specific components and contents are as follows:
the component A comprises:
and B component:
the component A to component B ratio is 1:1.5
Example 8
The embodiment provides a polymer cement-based waterproof coating, wherein the epoxy silane modified nano alumina is provided in embodiment 6, and the specific components and contents are as follows:
and (2) component A:
and the component B comprises:
the component A to component B ratio is 1:1.5
Example 9
The embodiment provides a polymer cement-based waterproof coating, wherein the epoxy silane modified nano alumina is provided in embodiment 6, and the specific components and contents are as follows:
and (2) component A:
and B component:
the component A and the component B have the ratio of 1:1.5
Example 10
This example provides a polymer cement-based waterproof coating, which is different from example 9 in that the component a: B ratio is 1:2, and the rest of the raw materials and steps are the same as those in example 9, and are not described again.
Example 11
This example provides a polymer cement-based waterproof coating, which is different from example 9 in that the component a: B ratio is 1:1, and the rest of the raw materials and steps are the same as those in example 9, and are not repeated herein.
Example 12
The embodiment provides a polymer cement-based waterproof coating, wherein the epoxy silane modified nano alumina is provided in embodiment 6, and the specific components and contents are as follows:
and (2) component A:
and the component B comprises:
the component A and the component B have the ratio of 1: 1.5.
Example 13
The embodiment provides a polymer cement-based waterproof coating, which is different from embodiment 12 in that the emulsion in the component a is styrene-acrylic emulsion, and other raw materials and contents are the same as those in embodiment 12, and are not described again.
Example 14
This example provides a polymer cement-based waterproof coating, which is different from example 12 in that the emulsion in the component a is a pure acrylate emulsion, and the rest raw materials and contents are the same as those in example 12, and are not repeated herein.
Example 15
The embodiment provides a polymer cement-based waterproof coating, which is different from embodiment 9 in that the emulsion in the component a is a nitrile-based 7% carboxyl 7% butylbenzene emulsion, and the rest raw materials and contents are the same as those in embodiment 9, and are not described again here.
Example 16
The embodiment provides a polymer cement-based waterproof coating, which is different from embodiment 9 in that no epoxy silane modified nano alumina is contained, except quartz sand, the other raw materials and contents are the same as those in embodiment 9, the quartz sand is added in a manner of supplementing the rest, and the total amount of the components B is 100%, and the details are not repeated herein.
Example 17
The embodiment provides a polymer cement-based waterproof coating, which is different from embodiment 9 in that epoxy silane modified nano alumina is provided in embodiment 1, and other raw materials and contents are the same as those in embodiment 9, and are not described again.
Example 18
The embodiment provides a polymer cement-based waterproof coating, which is different from embodiment 9 in that epoxy silane modified nano alumina is provided in embodiment 2, and other raw materials and contents are the same as those in embodiment 9, and are not described again.
Example 19
The embodiment provides a polymer cement-based waterproof coating, which is different from embodiment 9 in that epoxy silane modified nano alumina is provided in embodiment 3, and other raw materials and contents are the same as those in embodiment 9, and are not described again.
Example 20
The embodiment provides a polymer cement-based waterproof coating, which is different from embodiment 9 in that epoxy silane modified nano alumina is provided in embodiment 5, and other raw materials and contents are the same as those in embodiment 9, and are not described again.
Test example 1
In this test example, the epoxy silane modified nano alumina provided in examples 1 to 6 was subjected to surface hydroxyl number and activation degree detection by the following specific detection method:
1. degree of activation detection
Weighing 50mL of deionized water and 1.0g of modified nano-alumina, stirring at the speed of 50r/min for 5min, adding the modified nano-alumina into the water while stirring, standing for 2h at 23 ℃ under the humidity of 50%, separating the modified nano-alumina which is sunk into the bottom after the modified nano-alumina is obviously layered, drying to constant weight in a constant temperature oven at (105 +/-5) DEG C, weighing the mass, and calculating the activation degree according to the formula (1):
the activation degree is (total mass of sample-mass of sediment sample)/total mass of sample × 100%
Formula (1)
2. Determination of surface hydroxyl number
The reaction gas chromatography testing principle is based on the reaction of the Grignard reagent and active hydrogen to release methane gas, so that the quantity of the hydroxyl on the surface of the modified nano-alumina can be determined by measuring the quantity of the methane gas. The amount of methane gas generated by the reaction is in direct proportion to the amount of hydroxyl groups on the surface of the modified nano-alumina, and the mass of the methane gas generated by the reaction can be quantified by adopting a gas chromatography according to the area of the methane gas peak, so that the content of the hydroxyl groups is calculated, and the detection result is shown in table 2. The reaction formula is shown as the following reaction formula (1):
X-OH+CH 3 MgI→X-OMgI+CH 4
reaction formula (1)
Wherein X is modified nano-alumina.
The hydroxyl content N on the surface of the modified nano alumina is calculated according to the following formula (2):
wherein N is A Is an Avogadro constant (6.02 × 10) 23 )；
S is the specific surface area (nm) of the sample 2 /g)；
m is the mass (g) of the sample, and the sample is cooled and weighed after being dried in an oven at 105 ℃ for 2 hours;
M CH4 is the methane molar mass (g/mol);
m CH4 is the mass (g) of methane, see the following formula (3):
S 0 the area of a methane peak in a solvent blank spectrogram: a blank experiment is carried out before each batch of samples are tested, 2.0ml of reaction solution (dried toluene dilutes the Grignard reagent by ten times according to the volume ratio) is injected into a closed sample bottle to prepare a blank sample, and the blank sample is treated and tested as the sample to be tested.
Traces of water in the solvent and water vapor in the air will result in some amount of methane gas being produced in the blank sample. Three blank samples were run in parallel, the area of the methane peak was confirmed to be consistent, and the average S of the peak areas was recorded 0 。
S 1 The area of the methane peak in the spectrogram of the sample to be detected is shown as the following formula (4):
S 1 ＝am 1 +b
formula (4)
a is the slope of a straight line;
m 1 mass of methane in sample vial (mg);
b is the intercept of the ordinate;
the values of a and b can be measured by establishing the above linear regression equation from a series of measurements in an experiment.
TABLE 2 data sheet for properties of epoxy silane modified nano alumina
| Number of surface hydroxyl groups/nm 2 | Degree of activation% | |
| Example 1 | 1.53 | 40 |
| Example 2 | 1.25 | 65 |
| Example 3 | 1.05 | 78 |
| Example 4 | 0.92 | 92 |
| Example 5 | 0.90 | 95 |
| Experimental example 6 | 0.87 | 98 |
As can be seen from Table 2, with the increasing of the consumption of the epoxysilane, the activation degree of the modified nano-alumina is increased and the surface hydroxyl number is decreased, and when the consumption of the epoxysilane reaches 8 percent of the consumption of the modified nano-alumina, the changes of the activation degree and the surface hydroxyl number tend to be smooth; when the dosage of the epoxy silane is 12 percent of the dosage of the modified nano-alumina, the activation degree of the modified nano-alumina is close to 100 percent and the surface hydroxyl number is 0.87/nm 2 。
Test example 2
The polymer cement-based waterproof coating materials obtained in examples 7 to 20 were tested for their properties in the following procedures and methods.
The preparation and test method of the test piece comprises the following steps:
(1) the test piece preparation is 6.3 in GB/T19250 and 2013.
(2) The test method of the "No treatment tensile Property" refers to GB/T16777-2008 at 9.2.1 and a tensile speed of 200 mm/min.
(3) The tensile properties after heat treatment refer to the treatment test piece specified in GB/T16777-2008 of 9.2.1, and the tensile speed is 200 mm/min.
(4) The tensile property after alkali treatment refers to that 9.2.3 in GB/T16777-2008, the test piece is treated, the alkali soaking time is 168 +/-1 h, the test piece is taken out and fully cleaned by water, the test piece is placed for 4h under standard conditions after being wiped dry, and the tensile property is tested according to 9.2.1 in GB/T16777-2008, and the tensile speed is 200 mm/min.
(5) "tensile Property after Water treatment" A test piece prepared according to 6.3 of GB/T19250-.
(6) The "wet and non-treated bond strength" was molded as specified in 7.6.2 of GB/T23445-2009, the molded test pieces were cured (168. + -.1) h under standard conditions, and the bond strength was measured as specified in 7.6.3.1 of GB/T23445-2009.
(7) The samples were treated with "water and alkali treatment adhesive strength" as specified in GB/T23445-2009 at 7.6.3, taken out, washed thoroughly with water, wiped dry, left to stand under standard conditions for 4h, and the adhesive strength was measured as specified in GB/T23445-2009 at 7.6.3.1.
(8) The detection method for determining the VOC content refers to the A-type requirement of the Volatile Organic Compound (VOC) content in JC/T1066-2008 table 2.
(9) The detection method for determining the ammonia content refers to the requirement of the ammonia content A in the JC/T1066-2008 table 2.
(10) The detection method for determining the TVOC refers to appendix B in GB 50325-2001, and the index refers to the EC1plus requirement.
(11) The detection method for determining the water absorption is referred to 6.6.4 in JG/T375-2012.
(12) The standard conditions are (23. + -. 2) ℃ and (50%. + -. 10%) humidity.
The results are shown in Table 3.
TABLE 3 Polymer Cement-based Water repellent coating Performance data Table
As can be seen from table 3, the A, B components have larger performance difference in different proportions, the strength is improved and the elongation is gradually reduced with the increase of the content of the B component, and the performance is moderate and most suitable in all aspects when the proportion of the a component to the B component is 1: 1.5. In the same amount of different polymer emulsions, the component A contains 95% of 2% nitrile group and the formula of 2% carboxyl modified styrene-butadiene latex (example 8), and has the best water absorption, mechanical properties and volatile release amount. As the nitrile group and carboxyl group contents (nitrile group and carboxyl group contents each > 2%, for example, example 14) in the modified styrene-butadiene latex increased, the strength of the coating became higher, and the water resistance became worse, the water absorption increased and the strength loss after the water-alkali treatment became large. When the epoxy silane modified nano-alumina is added into the formula, the improvement of the strength and the water absorption is greatly facilitated, the modification degrees are different, and the performance is different. The closer the activation degree of the modified nano-alumina is to 100%, the smaller the number of surface hydroxyl groups is, the greater the performance improvement is helped, especially in the aspects of water absorption, strength and strength retention rate after water-alkali treatment.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and these modifications or substitutions do not depart from the spirit of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. The polymer cement-based waterproof coating is characterized by comprising a component A and a component B;
wherein the A component comprises nitrile carboxyl modified styrene-butadiene latex; the component B comprises cement and epoxy silane modified nano-alumina;
the epoxy silane modified nano alumina is obtained by modifying nano alumina with epoxy silane, and the mass ratio of the epoxy silane to the nano alumina is (2-12): 100;
the mass ratio of the component A to the component B is 1: 1-2;
the component A comprises the following components in percentage by mass: 68-98% of nitrile carboxyl modified butadiene styrene latex, and the balance of water and/or additives;
the additive in the component A comprises at least one of a defoaming agent, a preservative, a dispersing agent and a wetting agent;
the component B comprises the following components in percentage by mass: 30-65% of cement, 1-10% of epoxy silane modified nano alumina and the balance of pigment, filler and/or auxiliary agent;
the pigment and filler in the component B comprises at least one of quartz sand, heavy calcium carbonate, metakaolin and silica micropowder;
the auxiliary agent in the component B comprises at least one of a water reducing agent, cellulose ether and calcium formate.
2. The polymer cement-based waterproof coating material as claimed in claim 1, wherein the mass ratio of the epoxy silane to the nano alumina is from 4 to 10: 100.
3. the polymer cement-based waterproof coating as claimed in claim 1 or 2, wherein the epoxy silane modified nano alumina is obtained by dispersing the nano alumina and then adding the dispersed nano alumina into the solution of the epoxy silane.
4. The polymer cement-based waterproof coating material as claimed in claim 3, wherein the temperature of the dispersion is 20 to 40 ℃;
the dispersed rotating speed is 50-150 r/min;
the reaction temperature is 70-100 ℃;
the reaction time is 1.5-2.5 h;
the rotating speed of the reaction is 100-300 r/min.
5. The polymer cement-based waterproof coating material as claimed in claim 1, wherein the mass ratio of the A component to the B component is 1:1.2 to 1.8.
6. The polymer cement-based waterproof coating material as claimed in claim 5, wherein the mass ratio of the A component to the B component is 1: 1.5.
7. The polymer cement-based waterproof coating material as claimed in claim 1, wherein the component A comprises 70-95% by mass of nitrile carboxyl modified styrene-butadiene latex.
8. The polymer cement-based waterproof coating material as claimed in claim 1, wherein the B component comprises the following components in percentage by mass: 40-60% of cement, 3-8% of epoxy silane modified nano alumina and the balance of pigment, filler and/or auxiliary agent.
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