阅读说明：本技术 一种混凝土用纳米硅烷基防水乳液及其制备方法 (Nano-silyl waterproof emulsion for concrete and preparation method thereof ) 是由 胡强 吴春春 王基成 李群业 周馨 于 2021-08-11 设计创作，主要内容包括：本发明公开了一种混凝土用纳米硅烷基防水乳液及其制备方法,制备得到的一种混凝土用纳米硅烷基防水乳液,通过提高混凝土表面粗糙度来提高涂层接触角,从而提高混凝土涂层表面疏水性,防止水分渗透进混凝土内部腐蚀钢筋,提高混凝土的耐久性,该纳米硅烷基防水及抗碳化乳液对混凝土有良好的防护效果。(The invention discloses a nano silyl waterproof emulsion for concrete and a preparation method thereof, the prepared nano silyl waterproof emulsion for concrete improves the contact angle of a coating by improving the surface roughness of the concrete, thereby improving the surface hydrophobicity of the concrete coating, preventing water from permeating into the concrete to corrode a steel bar, and improving the durability of the concrete, and the nano silyl waterproof and anti-carbonization emulsion has good protection effect on the concrete.)

1. A preparation method of nano silane-based waterproof emulsion for concrete is characterized by comprising the following steps: the method comprises the following steps:

1) adding an emulsifier into deionized water, and stirring at a high speed of 1000r/min to uniformly distribute the emulsifier in the deionized water;

2) adding industrial-grade beeswax into butyl acetate, heating in a water bath until the mixture is completely transparent, adding isobutyl triethoxysilane, uniformly shaking, pouring the mixture into the material obtained in the step 1) while the mixture is hot, and stirring at a high speed of 1800r/min for 25-35min to obtain white emulsion;

3) ultrasonically dispersing the white emulsion obtained in the step 2) in an ice water bath for 15-25 min;

4) adding a dispersing agent into the material obtained in the step 3), and stirring at 800r/min for 15-25min to obtain nano silane-based waterproof and anti-carbonization emulsion for concrete;

the materials in each step are prepared according to the mass ratio of 1-3 parts of emulsifier, 70-100 parts of deionized water, 1-3 parts of industrial-grade beeswax, 40-60 parts of butyl acetate, 0.5-1.5 parts of isobutyl triethoxysilane and 1-3 parts of dispersant;

the emulsifier in the step 1) is selected from any one of span-20, span-40, span-60, span-80, tween-60 and tween-80;

the dispersing agent in the step 4) is one selected from NS-500LQ, J-601, gelatin and polyvinyl alcohol.

2. The nano silane-based waterproof emulsion for concrete according to claim 1, wherein: the butyl acetate in the step 2) is produced by Aladdin industries, and the purity is 99 percent; the isobutyl triethoxy silane is produced by Aladdin industries, and the purity is 99%.

3. The nano silane-based waterproof emulsion for concrete according to claim 1, wherein: the high-speed stirring in the step 2) is 1800r/min for 30 min.

4. The nano silane-based waterproof emulsion for concrete according to claim 1, wherein: and 3) carrying out ultrasonic dispersion for 20 min.

5. The nano silane-based waterproof emulsion for concrete according to claim 1, wherein: the stirring in the step 4) is carried out at 800r/min for 20 min.

6. The nano silane-based waterproof emulsion for concrete according to claim 1, wherein: the materials in each step are prepared according to the mass ratio of 2.0 parts of emulsifier, 85 parts of deionized water, 2.0 parts of industrial-grade beeswax, 50 parts of butyl acetate, 1.0 part of isobutyl triethoxysilane and 2.0 parts of dispersant.

7. A nano silane-based waterproof emulsion for concrete is characterized in that: the nano silane-based waterproof emulsion for concrete is prepared by the preparation method of the nano silane-based waterproof emulsion for concrete as claimed in any one of claims 1 to 6.

[ technical field ] A method for producing a semiconductor device

The invention relates to the technical field of preparation and application of concrete admixtures, in particular to nano silyl waterproof emulsion for concrete and a preparation method thereof.

[ background of the invention ]

Concrete is the most widely used building material in civil engineering and construction, with the wide application of concrete material, people's performance requirement to concrete also gradually promotes, the problem that concrete is corroded is increasingly outstanding, a large number of concrete buildings are damaged to different degrees because of rain wash, acid rain corrosion and the like every year, so that a lot of concrete (concrete material) fails in advance due to various reasons, some are caused by improper structural design, but most of the concrete (concrete material) fails due to insufficient structural durability and corrosion, water plays an important role in the corrosion process, especially the concrete material in coastal areas is corroded due to the moisture in ocean and air, and in addition, chloride rich in seawater invades into the interior of the concrete structure, so that salt failure is caused by corrosion. Therefore, the demand for concrete waterproof materials is increasing.

At present, the traditional concrete surface protective agent or the traditional concrete surface protective coating, such as asphalt, polyurethane, acrylic resin and the like, belongs to a molding coating, and the pore of the concrete is blocked by covering the surface of the concrete, so that a compact film structure is formed on the surface of the concrete, water cannot permeate into the interior through the surface of the concrete, and the purpose of preventing external moisture from invading is achieved, but the greatest defect of the molding coating is that the surface coating is damaged when internal moisture is discharged, so that the coating fails, the air permeability of the concrete material can not be ensured, the film coating also prevents the exchange of the internal moisture and gas of the concrete with the outside, so that the surface coating is damaged, and the service life of the concrete protective agent is greatly shortened.

Silane is a high-permeability waterproof material, and is a 4 th-generation organic silicon waterproof material. The silane is sprayed on the surface of the concrete in the form of solution, emulsion or paste, so that the waterproof, antifouling, dustproof, anticorrosion, weathering resistance and durability of the concrete can be improved. The silane has very low surface tension, so that the silane has very strong expansibility, when the silane is coated on the surface of a porous concrete base material, the silane can penetrate into the walls of micropores to form a film, hydrophobic groups are leaked on the surface of the material to achieve the aim of water resistance, and the silane has a reticular cross-linked structure, so that the air permeability of the surface of the concrete is not damaged after the silane is soaked, and internal water vapor can be diffused outwards. The silane is coated on the surface of concrete, and is easily infiltrated into capillary pores under the capillary absorption action of concrete micropores. The silane permeated into the capillary gaps is hydrolyzed into silanol under the action of moisture and water, and the silanol and hydroxyl in silicate are subjected to condensation reaction, so that a uniform and compact hydrophobic network siloxane hydrophobic film layer is formed in the capillary holes on the surface of the concrete, the entrance of external moisture and harmful substances is prevented, and the hydrophobic effect is achieved. However, the existing liquid silane and emulsion silane have the problem of poor adhesion.

In the existing research, for example, chinese patent CN201510586193 discloses a preparation method of a water-soluble concrete silane emulsion protective agent, in the preparation process, a polymer base material is prepared by using raw materials such as a compound emulsifier, amino silicone oil, triethylamine, n-octyltriethoxysilane, and the like, then the pH value is adjusted, and a stabilizer is added to disperse to obtain a silane emulsion. Although the method solves the problem of stability of the silane emulsion, the preparation process is complicated, the reaction condition needs high-temperature reflux, and the operation is not easy in the actual production process of a factory. For another example, Chinese patent CN200710053141 discloses a high-stability aqueous alkanyl silane emulsion and its preparation method, wherein the hydrolyzable alkoxy silane oil phase is composed of alkanyl trialkoxy silane R¹Si(OR²)₃And trialkoxysilane R³Si(OR²)₃Or dialkoxysilanes R⁴R⁵Si(OR²)₂And their corresponding hydrolytic polycondensation oligomers, which, although they can achieve highly stable silane emulsions, require temperature control between 30 and 50 ℃ during the preparation process, and require long production times, which undoubtedly increase the production costs.

Isobutyl triethoxy silane, also called triethoxy isobutyl silane, is an important intermediate in the production process of various silane coupling agents, can also be used as concrete anticorrosion silane impregnant, and in the aspects of long-term protection of concrete and prevention of corrosion of chloride ions, isobutyl triethoxy silane treatment is one of the most economic means, and the reasonable service life is longer than 30 years. However, silane groups cannot be directly used in actual engineering, and silane groups are usually prepared into nano-silane-based emulsion, for example, in chinese patent application CN201310014082 liquid water-based waterproofing agent and the preparation method thereof, inorganic silicon compounds, expanding agents, inorganic aluminum salts and other substances are simply added to exert the effect of dense filling, and the application range of the products is limited, the waterproofing and anti-permeability performance is poor, the durability of the waterproofing layer is poor, and the waterproofing layer is easy to crack.

Therefore, it is urgent to research a silane-based waterproofing agent for concrete.

[ summary of the invention ]

The invention provides a nano silyl waterproof emulsion for concrete and a preparation method thereof, aiming at the defects of poor waterproof and anti-permeability performance, poor durability of a waterproof layer and easiness in cracking of a silyl waterproof agent in the prior art.

The purpose of the invention is realized by the following technical scheme:

a preparation method of nano silane-based waterproof emulsion for concrete comprises the following steps:

1) adding an emulsifier into deionized water, and stirring at a high speed of 1000r/min to uniformly distribute the emulsifier in the deionized water;

2) adding industrial-grade beeswax into butyl acetate, heating in a water bath until the mixture is completely transparent, adding isobutyl triethoxysilane, uniformly shaking, pouring the mixture into the material obtained in the step 1) while the mixture is hot, and stirring at a high speed of 1800r/min for 25-35min to obtain white emulsion;

3) ultrasonically dispersing the white emulsion obtained in the step 2) in an ice water bath for 15-25 min;

4) adding a dispersing agent into the material obtained in the step 3), and stirring at 800r/min for 15-25min to obtain nano silane-based waterproof and anti-carbonization emulsion for concrete;

the materials in each step are prepared according to the mass ratio of 1-3 parts of emulsifier(s), 70-100 parts of deionized water, 1-3 parts of industrial-grade beeswax(s), 40-60 parts of butyl acetate, 0.5-1.5 parts of isobutyl triethoxysilane and 1-3 parts of dispersant(s).

The emulsifier in the step 1) is any one selected from span-20, span-40, span-60, span-80, tween-60 and tween-80.

The dispersing agent in the step 4) is one selected from NS-500LQ, J-601, gelatin and polyvinyl alcohol.

In the invention:

the butyl acetate in the step 2) is produced by Aladdin industries, and the purity is 99 percent; the isobutyl triethoxy silane is produced by Aladdin industries, and the purity is 99%.

The high-speed stirring in the step 2) is 1800r/min for 30 min.

And 3) carrying out ultrasonic dispersion for 20 min.

The stirring in the step 4) is carried out at 800r/min for 20 min.

The materials in each step are prepared according to the mass ratio of 2.0 parts of emulsifier, 85 parts of deionized water, 2.0 parts of industrial-grade beeswax, 50 parts of butyl acetate, 1.0 part of isobutyl triethoxysilane and 2.0 parts of dispersant.

The invention also relates to a nano silyl waterproof emulsion for concrete, which is prepared by the preparation method of the nano silyl waterproof and anti-carbonization emulsion for concrete.

Compared with the prior art, the invention has the following advantages:

1. according to the nano silyl waterproof emulsion for concrete, the added isobutyl triethoxysilane can be firmly combined on the surface and in the cavity of the concrete, so that harmful ions are prevented from permeating into the concrete, and a good waterproof effect is achieved.

2. According to the nano silyl waterproof emulsion for concrete, beeswax and isobutyl triethoxysilane act synergistically, so that the prepared nano silyl emulsion is good in overall stability, and the anti-permeability performance of concrete can be effectively improved.

3. The preparation method of the nano silyl waterproof emulsion for concrete has the advantages of simple method, small equipment investment and no generation of three wastes in the production process.

[ description of the drawings ]

FIG. 1 is a perspective electron microscope image of a nano silane-based waterproof emulsion for concrete obtained in example 1 of the present invention.

FIG. 2 is a graph showing the contact angle between the nano silane-based waterproof emulsion for concrete sprayed on the concrete surface and the non-sprayed emulsion obtained in example 1 of the present invention (blank left, emulsion right).

[ detailed description ] embodiments

The following examples are provided to further illustrate the embodiments of the present invention.

Example 1:

a preparation method of nano silane-based waterproof emulsion for concrete comprises the following steps:

1) adding an emulsifier into deionized water, and stirring at a high speed of 1000r/min to uniformly distribute the emulsifier in the deionized water;

2) adding industrial-grade beeswax into butyl acetate, heating in a water bath until the mixture is completely transparent, adding isobutyl triethoxysilane, uniformly shaking, pouring the mixture into the material obtained in the step 1) while the mixture is hot, and stirring at a high speed of 1800r/min for 30min to obtain a white emulsion;

3) ultrasonically dispersing the white emulsion obtained in the step 2) in an ice-water bath for 20 min;

4) adding a dispersing agent into the material obtained in the step 3), and stirring at 800r/min for 20min to obtain nano silane waterproof and anti-carbonization emulsion for concrete;

the materials in each step are prepared according to the mass ratio of 2.0g of emulsifier (span-20), 85g of deionized water, 2.0g of industrial-grade beeswax (the purity is 99 percent, produced by Aladdin industries Co., Ltd.), 50g of butyl acetate, 1.0g of isobutyl triethoxysilane (the purity is 99 percent, produced by Aladdin industries Co., Ltd.), and 2.0g of dispersant (NS-500 LQ).

Example 2:

a preparation method of nano silane-based waterproof emulsion for concrete comprises the following steps:

1) adding an emulsifier into deionized water, and stirring at a high speed of 1000r/min to uniformly distribute the emulsifier in the deionized water;

2) adding industrial-grade beeswax into butyl acetate, heating in a water bath until the mixture is completely transparent, adding isobutyl triethoxysilane, uniformly shaking, pouring the mixture into the material obtained in the step 1) while the mixture is hot, and stirring at a high speed of 1800r/min for 25min to obtain a white emulsion;

3) ultrasonically dispersing the white emulsion obtained in the step 2) in an ice-water bath for 15 min;

4) adding a dispersing agent into the material obtained in the step 3), and stirring at 800r/min for 15min to obtain nano silane waterproof and anti-carbonization emulsion for concrete;

the materials in each step are prepared according to the mass ratio of 1.0g of emulsifier (span-40), 70g of deionized water, 3.0g of industrial-grade beeswax (the purity is 99 percent, produced by Aladdin industries Co., Ltd.), 60g of butyl acetate, 0.5g of isobutyl triethoxysilane (the purity is 99 percent, produced by Aladdin industries Co., Ltd.), and 3.0g of dispersant (J-601).

Example 3:

a preparation method of nano silane-based waterproof emulsion for concrete comprises the following steps:

1) adding an emulsifier into deionized water, and stirring at a high speed of 1000r/min to uniformly distribute the emulsifier in the deionized water;

2) adding industrial-grade beeswax into butyl acetate, heating in a water bath until the mixture is completely transparent, adding isobutyl triethoxysilane, uniformly shaking, pouring the mixture into the material obtained in the step 1) while the mixture is hot, and stirring at a high speed of 1800r/min for 35min to obtain a white emulsion;

3) ultrasonically dispersing the white emulsion obtained in the step 2) in an ice water bath for 15-25 min;

4) adding a dispersing agent into the material obtained in the step 3), and stirring at 800r/min for 25min to obtain nano silane waterproof and anti-carbonization emulsion for concrete;

the materials in each step are prepared according to the mass ratio of 3.0g of emulsifier (span-80), 100g of deionized water, 1.0g of industrial-grade beeswax (the purity is 99 percent, produced by Aladdin industries Co., Ltd.), 40g of butyl acetate, 1.5g of isobutyl triethoxysilane (the purity is 99 percent, produced by Aladdin industries Co., Ltd.), and 1.0g of dispersant (gelatin).

Example 4:

a preparation method of nano silane-based waterproof emulsion for concrete comprises the following steps:

1) adding an emulsifier into deionized water, and stirring at a high speed of 1000r/min to uniformly distribute the emulsifier in the deionized water;

2) adding industrial-grade beeswax into butyl acetate, heating in a water bath until the mixture is completely transparent, adding isobutyl triethoxysilane, uniformly shaking, pouring the mixture into the material obtained in the step 1) while the mixture is hot, and stirring at a high speed of 1800r/min for 30min to obtain a white emulsion;

3) ultrasonically dispersing the white emulsion obtained in the step 2) in an ice water bath for 15-25 min;

4) adding a dispersing agent into the material obtained in the step 3), and stirring at 800r/min for 20min to obtain nano silane waterproof and anti-carbonization emulsion for concrete;

the materials in each step are prepared according to the mass ratio of 2.5g of emulsifier (Tween-60), 75g of deionized water, 1.8g of industrial-grade beeswax (the purity is 99 percent, produced by Aladdin industries Co., Ltd.), 45g of butyl acetate, 1.2g of isobutyl triethoxysilane (the purity is 99 percent, produced by Aladdin industries Co., Ltd.), and 2.4g of dispersant (polyvinyl alcohol).

Comparative example:

a silane-based waterproof emulsion for concrete was prepared in the same manner as in example 1, except that no emulsifier was added as compared with example 1.

As a result:

1. FIG. 1 is a perspective electron microscope image of a nano silyl-based waterproof emulsion for concrete obtained in example 1 of the present invention, and it can be seen from the image that the nanoparticles are spherical and have a particle size of about 100-150 nm.

2. FIG. 2 is a photograph showing the contact angle of a nano silane-based waterproof emulsion for concrete obtained in example 1 of the present invention, in which the water drop sprayed with the emulsion on the surface of the concrete is more round than the water drop not sprayed with the emulsion, indicating that the emulsion increases the contact angle of the surface of the concrete and improves the anti-permeability of the surface of the concrete.

3. The silane emulsions prepared in examples 1 to 4 and comparative example 1 were mixed at a ratio of 500g/m²The amount of the water-based paint is uniformly sprayed on the surface of concrete, dried for 3 days at room temperature (20 ℃) and tested for the contact angle of the surface of the concrete. The contact angle was measured by a contact angle measuring instrument JC2000C1, manufactured by Shanghai Meconsisting of Japan.

The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the inventive concept of the present invention, which falls into the protection scope of the present invention.