CN113292882A - Slow-release silane powder and preparation method and application thereof - Google Patents

Slow-release silane powder and preparation method and application thereof Download PDF

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CN113292882A
CN113292882A CN202110559706.1A CN202110559706A CN113292882A CN 113292882 A CN113292882 A CN 113292882A CN 202110559706 A CN202110559706 A CN 202110559706A CN 113292882 A CN113292882 A CN 113292882A
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powder
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CN113292882B (en
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黄正强
梁国涛
张茂亮
杨长聚
杜祥建
石嘉
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CCCC Seventh Engineering Co Ltd
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Henan Juyan Material Technology Co ltd
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    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • C09D7/61—Additives non-macromolecular inorganic
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    • 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
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Abstract

The invention relates to the technical field of waterproof materials, and particularly discloses slow-release silane powder and a preparation method and application thereof. The slow-release silane powder is prepared from the following raw materials in parts by weight: 20-40 parts of fluorosilane, 5-10 parts of silicate ester, 5-10 parts of titanate coupling agent, OP-101-2 parts, 801-2 parts of span, 20-30 parts of micro silicon powder, 5-10 parts of calcium carbonate whisker, 2-10 parts of PVA and 15-25 parts of water. The slow-release silane powder prepared by the invention is of a solid-in-oil structure, the main component of the shell of the slow-release silane powder is water-soluble PVA, and the main component of the core of the slow-release silane powder is liquid fluorosilane. The slow-release silane powder with the oil-in-solid structure solves the problems of low cement hydration degree, more gel pores, low waterproof coating strength, high water absorption rate and the like caused by serious influence on cement hydration caused by directly adding silane or silane emulsion into cement paste.

Description

Slow-release silane powder and preparation method and application thereof
The application is a divisional application of an invention patent with the application number of CN 201910676455.8 and the application date of 2019-7-25, and the name of the invention patent is 'slow-release type silane powder, super-hydrophobic cement-based flexible waterproof coating and a preparation method thereof'.
Technical Field
The invention relates to the technical field of waterproof materials, in particular to a super-hydrophobic cement-based flexible waterproof coating and a preparation method thereof.
Background
The waterproof material is developed for four generations, the first generation waterproof material is asphalt coiled material, the asphalt coiled material has low requirements on base materials for construction and high construction speed due to low price, still occupies a large share in the field of roof waterproofing, but has great pollution to human bodies and environment due to tar-containing components, has poor outdoor durability and is not easy to clean in maintenance; the second generation waterproof material is polyurethane, and the waterproof material contains volatile and toxic solvents, so the waterproof material is forbidden to use and is eliminated by the market; the third-generation waterproof material is acrylic acid which is a film-coating type waterproof material, has no seam and no toxicity, is convenient to construct, and still occupies a certain share in the waterproof market; the fourth generation waterproof is polymer cement, and the waterproof material film type waterproof material has no seam, is convenient to construct, and has a hydrophobic function and a permeable crystallization function. The fourth generation waterproof material has an active waterproof function and excellent performance, so that the polymer cement-based waterproof material becomes the mainstream waterproof material in the current market.
Although the polymer cement-based waterproof material is the mainstream waterproof material at present, the polymer cement-based waterproof material with hydrophobic and permeable crystallization functions is more and more researched because the self water absorption is higher and the water resistance can not meet the long-term water immersion environment. Patent documents CN108689648A, CN108530010A, and CN108034287 have studied the modification of polymer cement-based waterproof paint, and mainly include modification of polymer cement waterproof paint with alkoxysilane, aminosilane, silane coupling agent, sodium methyl silicate, sodium silicate, and the like. However, most cement-based waterproof coatings add silane or silane emulsion directly to the cement paste, and this method is not effective in improving the water absorption properties of the coating. Because the cement slurry is in an alkaline environment after the cement is hydrated, the silane functional group is hydrolyzed to generate ≡ Si-OH which is subjected to dehydration condensation reaction with hydroxyl on the surface of cement particles to form hydrated siloxane groups ≡ Si-O-Si ≡ and the functional group is preferentially adsorbed on the surface of negatively charged silicate minerals to form a super-hydrophobic group, which hinders the transportation of a medium, the hydration of the cement can be seriously influenced by directly adding the silane or the silane emulsion into the cement slurry, so that the hydration degree of the cement is low, the gel pores are increased, and the water absorption of the silane or the silane emulsion cannot be obviously reduced. Therefore, the durability of the existing waterproof coating still cannot meet the waterproof requirement of the cement-based material in a long-term water immersion environment.
Disclosure of Invention
Aiming at the problems and the defects in the prior art, the invention aims to provide a super-hydrophobic cement-based flexible waterproof coating and a preparation method thereof.
In order to realize the purpose of the invention, the technical scheme adopted by the invention is as follows:
the slow-release silane powder is prepared from the following raw materials in parts by weight: 20-40 parts of fluorosilane, 5-10 parts of silicate ester, 5-10 parts of titanate coupling agent, OP-101-2 parts, 801-2 parts of span, 20-30 parts of micro silicon powder, 5-10 parts of calcium carbonate whisker, 2-10 parts of PVA and 15-25 parts of water.
According to the above slow-release silane powder, preferably, the fluorosilane is at least one of perfluorooctyltriethoxysilane and perfluorodecyltrimethoxysilane.
According to the above sustained-release silane powder, the silicate is preferably at least one of methyl orthosilicate and ethyl orthosilicate.
According to the above-mentioned slow-release type silane powder, preferably, the titanate coupling agent is a chelate type titanate coupling agent. More preferably, the titanate coupling agents are bis (octyl pyrophosphate) glycolate and bis (dioctyl phosphonate) ethylene glycol titanate.
According to the slow-release silane powder, preferably, the polymerization degree of the PVA is 1600-4000; the mesh number of the micro silicon powder is 1200-1500 meshes; the length of the calcium carbonate whisker is 20-80 mu m, and the diameter of the calcium carbonate whisker is 0.5-1.2 mu m.
The preparation method of the slow-release silane powder comprises the following steps:
(1) uniformly stirring OP-10, span 80, fluorosilane, silicate ester and titanate coupling agent to obtain uniform emulsion, adding PVA, silica micropowder, calcium carbonate whisker and water into the emulsion, and uniformly stirring to obtain slurry;
(2) and (2) drying the slurry prepared in the step (1) to prepare powder with the particle size of 0.1-0.4 mm, thus obtaining the slow-release silane powder.
According to the above production method, preferably, the drying temperature in the step (2) is 60 to 70 ℃.
According to the above production method, preferably, the apparatus used for the drying in the step (2) is a fluidized bed drying apparatus.
The slow-release silane powder can be used for preparing waterproof paint.
A super-hydrophobic cement-based flexible waterproof coating comprises a liquid material and a powder material; the liquid material comprises the following raw materials in parts by weight: 60-80 parts of vinyl versatate, 5-20 parts of carboxylic styrene-butadiene latex, 0.2-0.6 part of defoaming agent, 0.2-1 part of film-forming assistant, 0.1-0.5 part of bactericide and 5-20 parts of water; the powder material comprises the following raw materials in parts by weight: 30-45 parts of portland cement, 5-10 parts of aluminate cement, 5-10 parts of gypsum, 0.4-2 parts of slow-release silane powder, 20-40 parts of quartz sand, 5-20 parts of triple superphosphate, 0.1-0.5 part of thixotropic agent and 0.2-0.5 part of water reducing agent.
According to the above super-hydrophobic cement-based flexible waterproof coating, preferably, the slow-release silane powder is prepared from the following raw materials in parts by weight: 20-40 parts of fluorosilane, 5-10 parts of silicate ester, 5-10 parts of titanate coupling agent, OP-101-2 parts, 801-2 parts of span, 20-30 parts of micro silicon powder, 5-10 parts of calcium carbonate whisker, 2-10 parts of PVA and 15-25 parts of water.
According to the above super-hydrophobic cement-based flexible waterproof coating material, preferably, the fluorosilane is at least one of perfluorooctyltriethoxysilane and perfluorodecyltrimethoxysilane.
According to the above super-hydrophobic cement-based flexible waterproof coating material, preferably, the silicate is at least one of methyl orthosilicate and ethyl orthosilicate.
According to the above-mentioned super-hydrophobic cement-based flexible waterproof coating material, preferably, the titanate coupling agent is a chelate titanate coupling agent. More preferably, the titanate coupling agents are bis (octyl pyrophosphate) glycolate and bis (dioctyl phosphonate) ethylene glycol titanate.
According to the super-hydrophobic cement-based flexible waterproof coating, preferably, the polymerization degree of the PVA is 1600-4000; the mesh number of the micro silicon powder is 1200-1500 meshes; the length of the calcium carbonate whisker is 20-80 mu m, and the diameter of the calcium carbonate whisker is 0.5-1.2 mu m.
According to the super-hydrophobic cement-based flexible waterproof coating, the mass ratio of the liquid material to the powder material is preferably 1 (1-3).
According to the super-hydrophobic cement-based flexible waterproof coating, preferably, the film-forming aid is an alcohol ester dodecafilm-forming aid; the water reducing agent is at least one of a polycarboxylic acid water reducing agent and a naphthalene water reducing agent; the thixotropic agent is high-molecular xanthan powder; the defoaming agent is a mineral oil defoaming agent.
The preparation method of the super-hydrophobic cement-based flexible waterproof coating comprises the following steps:
(a) preparing a liquid material: stirring and uniformly mixing vinyl versatate and carboxylic styrene-butadiene latex, then adding a film-forming assistant, a defoaming agent, a bactericide and water while stirring, and uniformly mixing to obtain a liquid material;
(b) preparing powder: uniformly stirring and mixing portland cement, aluminate cement, gypsum, slow-release silane powder, a thixotropic agent, coarse whiting, quartz sand and a water reducing agent to obtain powder;
(c) adding powder into the liquid material according to the mass ratio of the liquid material to the powder material of 1 (1-3), and uniformly mixing to obtain the super-hydrophobic cement-based flexible waterproof coating.
The reaction mechanism of the super-hydrophobic cement-based flexible waterproof coating is as follows:
(1) the slow-release silane powder is of a solid-in-oil structure, the main component of the shell of the slow-release silane powder is PVA, and the main component of the core of the slow-release silane powder is fluorosilane; after the powder and the liquid of the super-hydrophobic cement-based flexible waterproof coating are mixed, calcium silicate cement and calcium aluminate cement in the powder immediately start to hydrate, a PVA shell of slow-release silane powder in the powder also starts to slowly dissolve under the action of water, internal fluorosilane can be released after the PVA shell is completely dissolved, the rate of cement hydration is far higher than that of PVA dissolution, and cement hydration is mainly used in the stage; after cement hydration is basically finished, silane molecules coated by PVA begin to be released and freely migrate in the coating, silane is quickly hydrolyzed in an alkaline environment after cement hydration, and the hydrolyzed silane structure can be R-Si- (OH)3Is represented by, wherein- (OH)3The hydrophobic layer has reactivity, can be in chemical bond connection with hydroxyl on the surface of a cement hydration product through dehydration condensation, and the fluoroalkyl is arranged on the surface of the cement hydration product to form a permanent hydrophobic layer, so that the hydrophobic layer prevents liquid water from being introduced, and the water resistance of the waterproof coating is improved.
The binding of silane to cement hydrate is illustrated below:
Figure BDA0003078577960000041
(2) when the liquid material and the powder material in the super-hydrophobic cement-based flexible waterproof coating are contacted, cement in the powder material immediately begins to hydrate, part of water is consumed by cement hydration, and with the reduction of water in a system, polymers suspended in the coating are gradually accumulated on the surface of a cement hydration product in the form of compact polymer particles, and the polymer particles can effectively fill capillary pores of cement hydrates, so that the structure of the waterproof coating is more compact, the water absorption rate of the waterproof coating is reduced, and the waterproof and water-resistant performances of the waterproof coating are improved; and as the water content in the system is further reduced, the vinyl versatate in the liquid material begins to be accumulated on the surface of the cement hydration product, and a compact macromolecular polymer film is formed on the surface of the cement hydration product.
(3) The existing polymer cement waterproof coating improves the compactness of the waterproof coating by means of the accumulation of a polymer on the surface of a cement hydration product, thereby reducing the water absorption of the waterproof coating and achieving the effect of improving the waterproof and water-resistant performances of the waterproof coating. According to the invention, hydrophobic groups of fluorosilane are introduced into a coating system, so that a cement hydration product carries the hydrophobic groups and has strong hydrophobic performance; the polymer is accumulated on the surface of the cement hydration product with hydrophobic property, so that the structural compactness of the waterproof coating can be improved, the water absorption of the waterproof coating can be reduced, and the waterproof and waterproof functions of the waterproof coating can be further realized; therefore, the waterproof coating prepared by the invention realizes the waterproof function from two aspects: namely, the self hydrophobicity of the waterproof coating and the self compact structure of the waterproof coating; the hydrophobic property of the waterproof coating enables water molecules to be difficult to enrich on the surface of the waterproof coating for a long time, and the compact structure of the waterproof coating ensures that the water molecules are difficult to penetrate through the waterproof layer. Therefore, the waterproof coating is ensured to have both waterproofness and long-term waterproofness by the hydrophobicity and the compact structure of the waterproof coating itself.
Compared with the prior art, the invention has the following positive beneficial effects:
(1) when the slow-release silane powder is prepared, OP-10, span 80, silicate ester, fluorosilane and titanate coupling agent are added into a high-speed stirrer and dispersed at high speed to form uniform white emulsion, lipophilic groups of the OP-10, span 80, silicate ester and coupling agent are combined with fluorosilane to form an oil phase in the stirring process, and hydrophilic groups of the oil phase are spread outwards to form oil-in-water droplets; then adding PVA, silica powder, calcium carbonate whiskers and water, and continuing stirring, wherein the PVA, calcium carbonate whiskers and silica powder are accumulated on the surface of the oil-in-water droplets in the stirring process to form a uniform water-soluble polymer film, so as to obtain water-based slurry with uniform appearance; and drying the slurry in fluidized bed drying equipment to prepare powder with the particle size of 0.1-0.4 mm, thus obtaining the slow-release silane powder. Therefore, the slow-release silane powder prepared by the invention is of a solid-in-oil structure, the main component of the shell of the slow-release silane powder is water-soluble PVA, and the main component of the core of the slow-release silane powder is liquid fluorosilane.
After the powder and the liquid of the super-hydrophobic cement-based flexible waterproof coating are mixed, cement in the powder begins to hydrate, a PVA shell of slow-release silane powder with an oil-in-solid structure also begins to slowly dissolve under the action of water, and the PVA shell can release fluorosilane inside the slow-release silane powder after being completely dissolved, so that when the fluorosilane inside the slow-release silane powder is released, the early hydration of the cement in the powder is basically completed, the influence of the fluorosilane on the hydration degree of the cement is small, and silicon hydroxyl generated by the hydrolysis of the fluorosilane can be in dehydration condensation with hydroxyl on the surface of a cement hydration product to form chemical bond connection, so that the fluoroalkyl is arranged on the surface of the cement hydration product to form a permanent hydrophobic layer which blocks the intervention of liquid water, and the water resistance of the waterproof coating is improved. Therefore, the slow-release silane powder with the oil-in-solid structure solves the problems of low cement hydration degree, more gel pores, low waterproof coating strength, high water absorption rate and the like caused by the serious influence on cement hydration caused by directly adding silane or silane emulsion into cement paste.
(2) The PVA in the slow-release silane powder composition is PVA with polymerization degree of 1600-4000, the molecular weight of the PVA with the polymerization degree is moderate, the wrapping effect is good, the shell formation is easy, and the PVA with the polymerization degree is moderate in water solubility and is beneficial to the slow release of fluorosilane inside; if the molecular weight of PVA is too small, the wrapping property is poor, and the shell is not easy to form; if the molecular weight of PVA is too large, it has poor water solubility and is not favorable for the release of fluorosilane.
(3) When the slow-release silane powder is prepared, the selected drying temperature is 60-70 ℃, the drying is carried out within the temperature range, the fluorosilane inside the slow-release silane powder is not volatilized, the drying effect is good, the drying time is short, and if the drying temperature exceeds 70 ℃, the fluorosilane inside the slow-release silane powder is volatilized, so that the hydrophobicity of the fluorosilane powder is influenced.
(4) The micro silicon powder contained in the slow-release silane powder has high activity, can fill pores and can participate in the hydration reaction of common Portland cement; in addition, the slow-release silane powder also contains calcium carbonate whiskers, and the calcium carbonate whiskers can react with high-alumina cement to form single-carbon hydrated calcium aluminate and aluminum hydroxide, so that the compactness of the whole waterproof coating is improved.
(5) The invention adopts the tertiary ethylene carbonate emulsion and the carboxylic styrene-butadiene latex as the main components of the waterproof coating liquid material, the tertiary ethylene carbonate is saturated fatty acid ethylene ester with highly branched alpha-carbon, the highly branched chain has large steric hindrance effect and hydrophobic effect, so that the waterproof coating liquid material has excellent hydrophobicity and long-term water resistance, but the adhesive force between the tertiary ethylene carbonate emulsion and the base surfaces of concrete, steel and the like is weaker due to the lack of active groups; the carboxylic styrene-butadiene latex has strong polarity and good adhesion, so the main purpose of introducing the carboxylic styrene-butadiene latex is to improve the adhesion of the coating to substrates such as cement, steel and the like; through mixing the vinyl versatate emulsion and the carboxylic styrene-butadiene latex and adjusting the proportion of the vinyl versatate emulsion and the carboxylic styrene-butadiene latex, the prepared waterproof coating liquid material has excellent hydrophobicity and long-term water resistance, also has good adhesion, can be stably adhered to the surface of a base material, and greatly improves the adhesion strength of the waterproof coating and the base material (concrete, steel and the like).
(6) The Portland cement-aluminate cement-gypsum composite gel system has the characteristics of high early strength and quick setting time, and the aluminate cement and the gypsum provide a large amount of Al (OH)4 -And Ca2+、SO4 2-Provides support for AFt forming time and amount, satisfies early strengthThe need for condensation.
(7) The waterproof coating prepared by the invention has extremely low water absorption rate, excellent hydrophobic, waterproof and anti-permeability performances, high bonding strength with mortar or concrete base surfaces, capability of meeting the use requirement of a long-term water immersion environment, and wide application field.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the scope of the invention.
The first embodiment is as follows: preparation of Slow-Release silane powder
Example 1-1:
the slow-release silane powder is prepared from the following raw materials in parts by weight: 25 parts of fluorosilane, 5 parts of silicate ester, 5 parts of titanate coupling agent, OP-101 parts, 802 parts of span, 30 parts of micro silicon powder, 10 parts of calcium carbonate whisker, 2 parts of PVA and 20 parts of deionized water.
The fluorosilane is perfluorooctyl triethoxysilane; the silicate is methyl orthosilicate; the titanate coupling agent is di (octyl pyrophosphate) hydroxyacetic acid titanate; the polymerization degree of the PVA is 2000; the mesh number of the micro silicon powder is 1200-1500 meshes; the length of the calcium carbonate whisker is 20-80 mu m, and the diameter of the calcium carbonate whisker is 0.5-1.2 mu m.
The preparation method of the slow-release silane powder comprises the following steps:
(1) adding OP-10, span 80, fluorosilane, silicate ester and titanate coupling agent into a high-speed stirrer according to the proportion, and dispersing at high speed for 40-60min to obtain uniform white emulsion; then adding PVA, silicon micropowder, calcium carbonate whiskers and water, and stirring for 30-40min to obtain slurry;
(2) and (2) drying the slurry prepared in the step (1) in fluidized bed drying equipment at the temperature of 60-70 ℃ to prepare powder with the particle size of 0.1-0.4 mm, thus obtaining the slow-release silane powder.
Examples 1 to 2:
the slow-release silane powder is prepared from the following raw materials in parts by weight: 40 parts of fluorosilane, 5 parts of silicate ester, 5 parts of titanate coupling agent, OP-102 parts, 801 parts of span, 20 parts of micro silicon powder, 10 parts of calcium carbonate whisker, 2 parts of PVA and 15 parts of deionized water.
The fluorosilane is perfluorooctyl triethoxysilane; the silicate is methyl orthosilicate; the titanate coupling agent is di (octyl pyrophosphate) hydroxyacetic acid titanate; the polymerization degree of the PVA is 2000; the mesh number of the micro silicon powder is 1200-1500 meshes; the length of the calcium carbonate whisker is 20-80 mu m, and the diameter of the calcium carbonate whisker is 0.5-1.2 mu m.
The preparation method of the slow release type silane powder is the same as that of the example 1.
Examples 1 to 3:
the slow-release silane powder is prepared from the following raw materials in parts by weight: 20 parts of fluorosilane, 5 parts of silicate ester, 10 parts of titanate coupling agent, OP-101.5 parts, 801.5 parts of span, 30 parts of micro silicon powder, 5 parts of calcium carbonate whisker, 7 parts of PVA and 20 parts of deionized water.
The fluorosilane is perfluorooctyl triethoxysilane; the silicate is methyl orthosilicate; the titanate coupling agent is di (octyl pyrophosphate) hydroxyacetic acid titanate; the polymerization degree of the PVA is 2000; the mesh number of the micro silicon powder is 1200-1500 meshes; the length of the calcium carbonate whisker is 20-80 mu m, and the diameter of the calcium carbonate whisker is 0.5-1.2 mu m.
The preparation method of the slow release type silane powder is the same as that of the example 1.
Examples 1 to 4:
the slow-release silane powder is prepared from the following raw materials in parts by weight: 20 parts of fluorosilane, 10 parts of silicate ester, 5 parts of titanate coupling agent, OP-102 parts, 801 parts of span, 25 parts of micro silicon powder, 10 parts of calcium carbonate whisker, 7 parts of PVA and 20 parts of deionized water.
The fluorosilane is perfluorooctyl triethoxysilane; the silicate is methyl orthosilicate; the titanate coupling agent is di (octyl pyrophosphate) hydroxyacetic acid titanate; the polymerization degree of the PVA is 2000; the mesh number of the micro silicon powder is 1200-1500 meshes; the length of the calcium carbonate whisker is 20-80 mu m, and the diameter of the calcium carbonate whisker is 0.5-1.2 mu m.
The preparation method of the slow release type silane powder is the same as that of the example 1.
Examples 1 to 5:
the slow-release silane powder is prepared from the following raw materials in parts by weight: 35 parts of fluorosilane, 6 parts of silicate ester, 6 parts of titanate coupling agent, OP-102 parts, 801 parts of span, 20 parts of micro silicon powder, 5 parts of calcium carbonate whisker, 10 parts of PVA and 15 parts of deionized water.
The fluorosilane is perfluorooctyl triethoxysilane; the silicate is methyl orthosilicate; the titanate coupling agent is di (octyl pyrophosphate) hydroxyacetic acid titanate; the polymerization degree of the PVA is 2000; the mesh number of the micro silicon powder is 1200-1500 meshes; the length of the calcium carbonate whisker is 20-80 mu m, and the diameter of the calcium carbonate whisker is 0.5-1.2 mu m.
The preparation method of the slow release type silane powder is the same as that of the example 1.
Examples 1 to 6:
examples 1 to 6 are substantially the same as examples 1 to 1 except that: the fluorosilane is perfluorodecyl trimethoxy silane; the silicate is ethyl orthosilicate; the titanate coupling agent is bis (dioctyl phosphino) ethylene glycol titanate; the polymerization degree of the PVA is 1600.
Examples 1 to 7:
examples 1 to 7 are substantially the same as examples 1 to 1 except that: the fluorosilane is perfluorodecyl trimethoxy silane; the silicate is ethyl orthosilicate; the titanate coupling agent is bis (dioctyl phosphino) ethylene glycol titanate; the polymerization degree of the PVA is 4000.
Example two: preparation of super-hydrophobic cement-based flexible waterproof coating
1. The super-hydrophobic cement-based flexible waterproof coating comprises the following components in percentage by mass:
in order to investigate the influence of the mass ratio of the liquid material to the powder material on the performance of the prepared super-hydrophobic cement-based flexible waterproof coating material, the inventors performed the following experiments, i.e., example 2-1 to example 2-5.
Example 2-1:
a super-hydrophobic cement-based flexible waterproof coating is composed of a liquid material and a powder material, wherein the mass ratio of the liquid material to the powder material is 1: 3. The liquid material comprises the following raw materials in parts by weight: 75 parts of tertiary ethylene carbonate emulsion, 10 parts of carboxylic styrene-butadiene latex, 0.3 part of defoaming agent, 0.5 part of film-forming assistant, 0.2 part of bactericide and 14 parts of water; the powder material comprises the following raw materials in parts by weight: 45 parts of Portland cement, 5 parts of aluminate cement, 5 parts of gypsum, 1.2 parts of slow-release silane powder, 23 parts of quartz sand, 20 parts of coarse whiting, 0.5 part of thixotropic agent and 0.3 part of water reducing agent. Wherein the slow release type silane powder is the slow release type silane powder prepared in example 1; the film-forming additive is an alcohol ester dodecafilm-forming additive; the water reducing agent is a polycarboxylic acid water reducing agent; the thixotropic agent is high-molecular xanthan powder; the defoaming agent is a mineral oil defoaming agent.
The preparation method of the super-hydrophobic cement-based flexible waterproof coating comprises the following steps:
(a) preparing a liquid material: stirring and uniformly mixing the vinyl versatate emulsion and the carboxylic styrene-butadiene latex, then adding the film-forming assistant, the defoaming agent, the bactericide and water while stirring, and uniformly mixing to obtain a liquid material;
(b) preparing powder: uniformly stirring and mixing portland cement, aluminate cement, gypsum, slow-release silane powder, a thixotropic agent, coarse whiting, quartz sand and a water reducing agent to obtain powder;
(c) and adding the powder into the liquid material according to the mass ratio of the liquid material to the powder material, and uniformly mixing to obtain the super-hydrophobic cement-based flexible waterproof coating.
Example 2-2 to example 2-5:
examples 2-2 to 2-5 were substantially the same as example 2-1 except that the mass ratio of the liquid material to the powdery material was different, and the mass ratio of the liquid material to the powdery material was specifically shown in Table 1.
Tensile strength, elongation at break and adhesive strength properties of the waterproof coatings prepared in examples 2-1 to 2-5 were measured according to the test standard "polymer cement waterproof coating" GB/T23445-2009, and water absorption of the coating films of the waterproof coatings prepared in examples 2-1 to 2-5 were measured according to the test standard JC/T1017-2006 "polymer emulsion for architectural waterproof coatings", and the corresponding test results are shown in table 1. In order to detect the long-term water resistance of the waterproof coating, the performance of the waterproof material after no treatment and 1000h water invasion treatment are respectively carried out in the test. The non-treatment means that liquid materials and powder materials of the waterproof coating are mixed and stirred according to a certain mass ratio, the mixture is kept stand for 3min, the mixture is poured into a mold for coating, the coating is carried out for two times or three times, the maintenance is carried out for 96h under the standard condition, then the demolding is carried out, the reverse side of a demolded sample is upwards treated in an oven at the temperature of 40 +/-2 ℃ for 48h, the sample is taken out and cooled to the room temperature, a slicer is used for punching and cutting the sample into a test piece with the size of 20mm multiplied by 15mm, and then the performance of the test piece is tested. The soaking in water for 1000 hours is to mix and stir liquid materials and powder materials of the waterproof coating according to a certain mass ratio, stand for 3min, pour the mixture into a mold for coating, coat the mixture in two or three times, carry out curing for 96 hours under standard conditions, then carry out demolding, treat the reverse side of a demolded sample in an oven at 40 +/-2 ℃ for 48 hours, take out the sample and cool the sample to room temperature, prepare the sample into a test piece with the size of 20mm multiplied by 15mm, soak the test piece in water at 23 +/-2 ℃ for 1000 hours, and then test the performance of the test piece.
The method for testing the water absorption of the untreated coating film comprises the following steps: weighing the mass m of a test piece0Soaking for 168 +/-1 h, taking out, sucking the attached water on the surface of the test piece by using filter paper, and weighing the mass m again1Then coating the film according to the formula (m) to obtain the film with water absorption rate1-m0)/m0And calculating the water absorption of the coating film of the test piece.
A method for testing the water absorption of a coating film after 1000h of soaking in water comprises the following steps: weighing the mass m of a test piece0Soaking for 1000 +/-1 h, taking out, sucking the attached water on the surface of the test piece by using filter paper, and weighing the mass m again1Then coating the film according to the formula (m) to obtain the film with water absorption rate1-m0)/m0And calculating the water absorption of the coating film of the test piece.
TABLE 1 test results of the performance of the waterproof coatings prepared by different mass ratios of liquid material to powder material
Figure BDA0003078577960000101
As can be seen from Table 1, the tensile strength of the waterproof coating is gradually reduced with the improvement of the mass ratio of the liquid material to the powder material, and when the mass ratio of the liquid material to the powder material is 1:0.5, the tensile strength of the waterproof coating detected under the non-treatment condition is only 2.01MPa, and the tensile strength is lower; the breaking elongation of the waterproof coating gradually increases with the increase of the mass ratio of the liquid material to the powder material, the adhesive strength of the waterproof coating and the water absorption of a coating film tend to increase firstly and then decrease with the increase of the mass ratio of the liquid material to the powder material, and when the mass ratio of the liquid material to the powder material is 1:4 or 1:0.5, the adhesive strength of the waterproof coating is lower. Therefore, the mass ratio of the liquid material to the powder material is preferably 1 (1-3), and more preferably 1:2, in consideration of the tensile strength, elongation at break, adhesive strength and water absorption of the waterproof coating material.
2. Investigation experiment of the amount of carboxylic styrene-butadiene latex:
in order to investigate the influence of the amount of the carboxylated styrene-butadiene latex in the liquid material on the performance of the prepared super-hydrophobic cement-based flexible waterproof coating, the inventors carried out the following experiments, namely, example 3-1 to example 3-8.
Example 3-1:
a super-hydrophobic cement-based flexible waterproof coating is composed of a liquid material and a powder material, wherein the mass ratio of the liquid material to the powder material is 1: 2. The liquid material comprises the following raw materials in parts by weight: 80 parts of vinyl versatate, 0 part of carboxylic styrene-butadiene latex, 0.3 part of defoaming agent, 0.5 part of film-forming assistant, 0.2 part of bactericide and 14 parts of water; the powder material comprises the following raw materials in parts by weight: 45 parts of common 42.5 Portland cement, 5 parts of aluminate cement, 5 parts of gypsum, 1.2 parts of slow-release silane powder, 23 parts of quartz sand, 20 parts of triple superphosphate, 0.5 part of thixotropic agent and 0.3 part of polycarboxylic acid water reducing agent. Wherein the slow release type silane powder is the slow release type silane powder prepared in example 1. The film-forming additive is an alcohol ester dodecafilm-forming additive; the water reducing agent is a polycarboxylic acid water reducing agent; the thixotropic agent is high-molecular xanthan powder; the defoaming agent is a mineral oil defoaming agent.
The preparation method of the super-hydrophobic cement-based flexible waterproof coating comprises the following steps:
(a) preparing a liquid material: stirring and uniformly mixing vinyl versatate and carboxylic styrene-butadiene latex, then adding a film-forming assistant, a defoaming agent, a bactericide and water while stirring, and uniformly mixing to obtain a liquid material;
(b) preparing powder: adding portland cement, aluminate cement, gypsum, slow-release fluorosilane powder, a thixotropic agent, coarse whiting, quartz sand and a water reducing agent into stirring equipment, and uniformly stirring to obtain powder;
(c) when in use, the powder is added into the liquid material according to the mass ratio of the liquid material to the powder, and the mixture is stirred and mixed uniformly to obtain the super-hydrophobic cement-based flexible waterproof coating.
Example 3-2 to example 3-8:
examples 3-2 to 3-8 are substantially the same as example 3-1 except that: the amount of the carboxylated styrene-butadiene latex in the liquid material is different, and the specific amount of the carboxylated styrene-butadiene latex is shown in table 2.
Tensile strength, elongation at break and adhesive strength properties of the waterproof coatings prepared in examples 3-1 to 3-8 were measured according to the test standard "polymer cement waterproof coating" GB/T23445-2009, and water absorption rates of coating films of the waterproof coatings prepared in examples 3-1 to 3-8 were measured according to the test standard JC/T1017-2006 "polymer emulsion for architectural waterproof coatings", and the corresponding test results are shown in table 2.
TABLE 2 influence of amount of carboxylated styrene-butadiene latex on the performance of the water-proof coating
Figure BDA0003078577960000121
As can be seen from table 2, the bonding strength of the waterproof coating gradually increases with the increase of the amount of the carboxylated styrene-butadiene latex, and thus it can be seen that the addition of the carboxylated styrene-butadiene latex can improve the bonding performance of the waterproof coating; in addition, with the increase of the amount of the carboxylated styrene-butadiene latex, the tensile strength and the elongation at break of the waterproof coating do not change obviously, and the water absorption of the coating film has a slight increase trend, so that the content of the carboxylated styrene-butadiene emulsion is preferably 5 to 20 parts, and more preferably 10 to 15 parts, by comprehensively considering the bonding strength and the water absorption of the waterproof coating.
3. Discussion experiment of the amount of slow-release silane powder:
in order to investigate the influence of the amount of the slow-release silane powder in the powder on the performance of the prepared super-hydrophobic cement-based flexible waterproof coating, the inventors carried out the following experiments, namely, example 4-1 to example 4-8.
Example 4-1:
a super-hydrophobic cement-based flexible waterproof coating is composed of a liquid material and a powder material, wherein the mass ratio of the liquid material to the powder material is 1: 2. The liquid material comprises the following raw materials in parts by weight: 75 parts of vinyl versatate, 10 parts of carboxylic styrene-butadiene latex, 0.3 part of defoaming agent, 0.5 part of film-forming assistant, 0.2 part of bactericide and 14 parts of water; the powder material comprises the following raw materials in parts by weight: 45 parts of common 42.5 Portland cement, 5 parts of aluminate cement, 5 parts of gypsum, 0 part of slow-release silane powder, 23 parts of quartz sand, 20 parts of triple superphosphate, 0.5 part of thixotropic agent and 0.3 part of polycarboxylic acid water reducing agent. Wherein the slow release type silane powder is the slow release type silane powder prepared in example 1; the film-forming additive is an alcohol ester dodecafilm-forming additive; the water reducing agent is a polycarboxylic acid water reducing agent; the thixotropic agent is high-molecular xanthan powder; the defoaming agent is a mineral oil defoaming agent.
The preparation method of the super-hydrophobic cement-based flexible waterproof coating comprises the following steps:
(a) preparing a liquid material: stirring and uniformly mixing vinyl versatate and carboxylic styrene-butadiene latex, then adding a film-forming assistant, a defoaming agent, a bactericide and water while stirring, and uniformly mixing to obtain a liquid material;
(b) preparing powder: adding portland cement, aluminate cement, gypsum, slow-release fluorosilane powder, a thixotropic agent, coarse whiting, quartz sand and a water reducing agent into stirring equipment, and uniformly stirring to obtain powder;
(c) when in use, the powder is added into the liquid material according to the mass ratio of the liquid material to the powder, and the mixture is stirred and mixed uniformly to obtain the super-hydrophobic cement-based flexible waterproof coating.
Example 4-2 to example 4-9:
examples 4-2 to 4-9 are substantially the same as example 4-1 except that: the dosage of the slow release type silane powder in the powder material, and the specific dosage of the slow release type silane powder are shown in table 3.
Tensile strength, elongation at break and adhesive strength properties of the waterproof coatings prepared in examples 4-1 to 4-9 were measured according to the test standard "polymer cement waterproof coating" GB/T23445-2009, and water absorption rates of coating films of the waterproof coatings prepared in examples 4-1 to 4-9 were measured according to the test standard JC/T1017-2006 "polymer emulsion for architectural waterproof coatings", and the corresponding test results are shown in table 3.
TABLE 3 discussion of the amount of slow-release silane powder used
Figure BDA0003078577960000131
As can be seen from table 3, when the slow-release silane powder is not added, the water absorption of the prepared waterproof coating is very high, 10.91%, and the water absorption of the waterproof coating is obviously reduced with the increase of the use amount of the slow-release silane powder; when the using amount of the slow-release silane powder is 2.0 parts, the water absorption rate is only 1.26%, and compared with the waterproof coating without the slow-release silane powder, the water absorption rate of the waterproof coating is reduced by 88.5%, so that the water absorption rate of the waterproof coating can be reduced and the waterproof and water-resistant performances of the waterproof coating can be improved by adding the slow-release silane powder. In addition, when the using amount of the slow-release silane powder is within the range of 0.4-2.0 parts, the tensile strength, the elongation at break and the bonding strength of the waterproof coating are not obviously changed along with the increase of the using amount of the slow-release silane powder, and when the using amount of the slow-release silane powder exceeds 2.0 parts, the tensile strength of the waterproof coating has an obvious reduction trend, and the water absorption of a coating film is increased. Therefore, the amount of the silane powder to be used is preferably 0.4 to 2.0 parts, more preferably 1.2 to 2.0 parts.
4. Preparation of super-hydrophobic cement-based flexible waterproof coating
A super-hydrophobic cement-based flexible waterproof coating comprises a liquid material and a powder material, wherein the mass ratio of the liquid material to the powder material is 1: 2; the liquid material comprises the following raw materials in parts by weight: 60-80 parts of vinyl versatate emulsion, 5-20 parts of carboxylic styrene-butadiene latex, 0.2-0.6 part of defoaming agent, 0.2-1 part of film-forming assistant, 0.1-0.5 part of bactericide and 5-20 parts of water; the powder material comprises the following raw materials in parts by weight: 30-45 parts of Portland cement, 5-10 parts of aluminate cement, 5-10 parts of gypsum, 0.5-2 parts of slow-release silane powder, 20-40 parts of quartz sand, 5-20 parts of triple superphosphate, 0.1-0.5 part of thixotropic agent and 0.2-0.5 part of water reducing agent; wherein the film-forming additive is an alcohol ester dodecafilm-forming additive; the water reducing agent is a polycarboxylic acid water reducing agent; the thixotropic agent is high-molecular xanthan powder; the defoaming agent is a mineral oil defoaming agent.
The preparation method of the super-hydrophobic cement-based flexible waterproof coating comprises the following steps:
(a) preparing a liquid material: stirring and uniformly mixing the vinyl versatate emulsion and the carboxylic styrene-butadiene latex, then adding the film-forming assistant, the defoaming agent, the bactericide and water while stirring, and uniformly mixing to obtain a liquid material;
(b) preparing powder: uniformly stirring and mixing portland cement, aluminate cement, gypsum, slow-release silane powder, a thixotropic agent, coarse whiting, quartz sand and a water reducing agent to obtain powder;
(c) and adding the powder into the liquid material according to the mass ratio of the liquid material to the powder material, and uniformly mixing to obtain the super-hydrophobic cement-based flexible waterproof coating.
Table 4 specific examples of preparing super-hydrophobic cement-based flexible waterproof coating
Figure BDA0003078577960000151
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 present invention, but rather as the following description is intended to cover all modifications, equivalents and improvements falling within the spirit and scope of the present invention.

Claims (6)

1. The slow-release silane powder is characterized by being prepared from the following raw materials in parts by weight: 20-40 parts of fluorosilane, 5-10 parts of silicate ester, 5-10 parts of titanate coupling agent, OP-101-2 parts, 801-2 parts of span, 20-30 parts of micro silicon powder, 5-10 parts of calcium carbonate whisker, 2-10 parts of PVA and 15-25 parts of water.
2. The slow-release silane powder according to claim 1, wherein the fluorosilane is at least one of perfluorooctyltriethoxysilane and perfluorodecyltrimethoxysilane; the silicate is at least one of methyl orthosilicate and ethyl orthosilicate; the titanate coupling agent is a chelating titanate coupling agent.
3. The slow-release silane powder according to claim 2, wherein the degree of polymerization of the PVA is 1600 to 4000; the mesh number of the micro silicon powder is 1200-1500 meshes; the length of the calcium carbonate whisker is 20-80 mu m, and the diameter of the calcium carbonate whisker is 0.5-1.2 mu m.
4. A method for preparing the slow-release silane powder according to any one of claims 1 to 3, comprising the steps of:
(1) uniformly stirring OP-10, span 80, fluorosilane, silicate ester and titanate coupling agent to obtain uniform emulsion, adding PVA, silica micropowder, calcium carbonate whisker and water into the emulsion, and uniformly stirring to obtain slurry;
(2) and (2) drying the slurry prepared in the step (1) to prepare powder with the particle size of 0.1-0.4 mm, thus obtaining the slow-release silane powder.
5. The method according to claim 4, wherein the drying temperature in the step (2) is 60 to 70 ℃.
6. Use of the slow-release silane powder of any one of claims 1 to 3 in the preparation of a waterproof coating.
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