A reactive silicon-containing emulsifier and a silane protective material prepared therefrom

Abstract

This invention belongs to the field of high-performance concrete protective materials and discloses a reactive silicone-containing emulsifier. The invention also discloses a preparation method for this reactive silicone-containing emulsifier and its application in silane emulsification and silane protective materials. The preparation method of the reactive silicone-containing emulsifier is as follows: under an inert gas protective atmosphere, a solvent and allyl polyether are added to a reactor, the temperature is raised to 60-110°C, a catalyst is added, followed by the addition of a hydrogen-containing silane, and the reaction is maintained at this temperature for 0.5-3 hours. After the reaction is completed, the solvent is removed to obtain the reactive silicone-containing emulsifier. The silane protective material is made from the following raw materials in weight percentages: 0.1-5% reactive silicone-containing emulsifier, 75-82% alkoxysilane, 0.5-1% thickener, 15-20% deionized water, 0.5-1% preservative, and 0.5-1% bactericide. This invention discloses a preparation method for this silane protective material, and the prepared silane protective material exhibits excellent stability and can provide excellent waterproofing and water-repellent effects for concrete.

Description

Technical Field

[0001] This invention belongs to the field of high-performance concrete protective materials, specifically relating to a reactive silicone-containing emulsifier and the silane protective material prepared therefrom. Background Technology

[0002] Concrete, an indispensable material in modern construction, directly impacts the safety and lifespan of buildings through its durability. However, in practical use, concrete often faces challenges from various corrosive factors, such as moisture, chloride ions, and salts. These factors can lead to cracking, spalling, and steel reinforcement corrosion, severely affecting the durability and safety of concrete structures. Silane protective materials can form a protective layer on the concrete surface. This layer exhibits excellent durability, with a lifespan exceeding 15 years, significantly improving the durability of concrete structures.

[0003] The core technology of silane protective materials lies in the penetration and reaction mechanism of small silane molecules. These small silane molecules can penetrate the surface of concrete, reaching depths of several to tens of millimeters, and react with silicates (such as calcium silicate and calcium carbonate) in the concrete. Under the alkaline catalytic action of the concrete, the silane molecules generate a stable network of organosilicon resin protective layer. This protective layer not only effectively prevents moisture and harmful substances carried by moisture (such as chloride ions) from penetrating into the concrete, but also maintains the concrete's breathability, preventing internal moisture accumulation caused by excessive sealing.

[0004] However, the penetration depth of silanes is directly related to their protective efficacy; the deeper the penetration, the more significant the protective effect. The invention of silane pastes overcomes the problem that liquid silanes cannot remain in vertical or supine positions for long periods, ensuring that silanes have sufficient time to penetrate deep into the concrete to achieve the ideal protective depth, thereby significantly enhancing the durability and protective effect of concrete structures. However, silanes exhibit poor compatibility with traditional emulsifiers, leading to problems such as insufficient stability and easy delamination / demulsification in the prepared silane pastes.

[0005] To address this issue, the amount of emulsifier used in the paste preparation process needs to be increased. However, this introduces new problems because the penetrating power of emulsifiers is far less than that of silanes. Excessive emulsifier tends to remain on the concrete surface, thus weakening the hydrophobic effect of silanes. Although a multifunctional concrete protective paste in existing inventions avoids the use of hydrophilic thickeners, its emulsifier content is still as high as 3-6%, which still affects the hydrophobic effect of silanes. Other inventions have solved the problem of high emulsifier content in silane pastes, but they introduce 5-8% water-based resin into the system, which also affects the hydrophobic properties of silanes, becoming a technical point that requires further balancing and optimization. Summary of the Invention

[0006] In view of the problems and shortcomings of the prior art, the present invention provides a reactive silicone-containing emulsifier and a silane protective material prepared therefrom.

[0007] To achieve the above objectives, the present invention adopts the following technical solution:

[0008] The first aspect of this invention provides a reactive silicone-containing emulsifier, the structural formula of which is as follows:

[0009]

[0010] Where R is any one of -CH3, -C2H5, and -C3H7, 0≤x<10, 1≤y≤10, and x and y are both natural numbers.

[0011] According to the above-mentioned reactive silicone emulsifier, preferably, the average molecular weight of the reactive silicone emulsifier is 250-1200 g / mol; more preferably, the average molecular weight of the reactive silicone emulsifier is 300-1000 g / mol.

[0012] The second aspect of this invention provides a method for preparing the reactive silicone-containing emulsifier described in the first aspect. The method comprises: adding a solvent and allyl polyether to a reactor under an inert gas atmosphere; heating the reactor to 60–110°C; adding a catalyst; and then adding a hydrogen-containing silane to the reaction vessel. The molar ratio of allyl polyether to the hydrogen-containing silane is (0.9–1.1):1. The reaction is maintained at this temperature for 0.5–3 hours. After the reaction is complete, the solvent is removed to obtain the reactive silicone-containing emulsifier. The synthetic route is shown below:

[0013]

[0014] According to the above preparation method, preferably, the average molecular weight of the allyl polyether is 102-1200 g / mol; the catalyst is a platinum molecular complex; the solvent is at least one of isopropanol, toluene, and xylene; the hydrosilane is at least one of trimethoxysilane, triethoxysilane, methyldimethoxysilane, tripropoxysilane, and methyldiethoxysilane; more preferably, the average molecular weight of the allyl polyether is 200-1000 g / mol; the catalyst is Karstedt or Speier; the solvent is toluene; and the hydrosilane is triethoxysilane, trimethoxysilane, methyldimethoxysilane, or methyldiethoxysilane.

[0015] The third aspect of this invention provides the application of the reactive silicone-containing emulsifier described in the first aspect above in silane emulsification and the preparation of silane protective materials.

[0016] The fourth aspect of the present invention provides a silane protective material, which is made from the following raw materials in weight percentage: 0.1-5% reactive silicone emulsifier, 75-82% alkoxysilane, 0.5-1% thickener, 15-20% deionized water, 0.5-1% preservative, and 0.5-1% bactericide.

[0017] According to the above-mentioned silane protective material, preferably, it is made from the following raw materials in weight percentage: 2% reactive silicone emulsifier, 80% alkoxysilane, 0.5% thickener, 16.5% deionized water, 0.5% preservative, and 0.5% bactericide.

[0018] According to the above-mentioned silane protective material, preferably, the silane protective material is a silane paste.

[0019] The fifth aspect of this invention provides a method for preparing the silane protective material described in the fourth aspect above, specifically comprising the following steps:

[0020] (1) The reactive silicone emulsifier described in the first aspect above is added to water and dispersed evenly to obtain a dispersion;

[0021] (2) Add alkoxysilane gradually to the dispersion while stirring. After the alkoxysilane is added, continue stirring until the alkoxysilane and the dispersion are completely emulsified to obtain an emulsion.

[0022] (3) Add a thickener to the emulsion, mix well, then add a preservative and a bactericide, mix well, and the silane protective material is obtained.

[0023] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0024] 1. Compared with traditional emulsifiers, the reactive emulsifier prepared by this invention exhibits superior dispersing power, wetting properties and stability.

[0025] 2. This invention breaks through the limitations of traditional silane paste preparation methods by using a reactive silicone emulsifier for emulsification. This not only reduces the amount of emulsifier used but also effectively avoids the problem of poor surface hydrophobicity caused by the residue of traditional emulsifiers on the concrete surface. Combined with the results of water absorption rate tests, it is confirmed that the reactive silicone emulsifier can undergo hydrolytic cross-linking reaction with silane, effectively avoiding the migration and agglomeration of emulsifiers inside the concrete, thus preventing the formation of water-absorbing nests. This improves the stability of the silane paste and solves the problems of large emulsifier usage, poor stability, and easy delamination and emulsion breaking in traditional silane pastes. Detailed Implementation

[0026] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below through embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.

[0027] Example 1: Preparation of reactive silicone-containing emulsifier

[0028] This embodiment provides different reactive silicone-containing emulsifiers and their preparation methods, namely Examples 1-1 to 1-5, and compares their physicochemical properties with those of traditional emulsifiers.

[0029] Example 1-1

[0030] A reactive silicone emulsifier is prepared as follows: In a 1L four-necked flask equipped with a stirrer, thermometer, and condenser, 500g of allyl polyether with an average molecular weight of 500g / mol and 60g of toluene are added and stirred until homogeneous. After purging the air with nitrogen, the temperature is raised to 70°C, and Speier catalyst (3ppm based on the total mass of polyether and siloxane) is added. Then, 164g of triethoxysilane is slowly added dropwise. After the addition is complete, the reaction is maintained at this temperature for 2 hours. The solvent is removed by vacuum to obtain the reactive silicone emulsifier A-1.

[0031] Examples 1-2

[0032] A reactive silicone emulsifier is prepared as follows: In a 1L four-necked flask equipped with a stirrer, thermometer, and condenser, 525g of allyl polyether with an average molecular weight of 350g / mol and 40g of toluene are added and stirred until homogeneous. After purging the air with nitrogen, the temperature is raised to 60°C, and Karstedt catalyst (2ppm based on the total mass of polyether and siloxane) is added. Then, 183g of trimethoxysilane is slowly added dropwise. After the addition is complete, the reaction is maintained at this temperature for 1 hour. The solvent is removed by vacuum to obtain the reactive silicone emulsifier A-2.

[0033] Examples 1-3

[0034] A reactive silicone emulsifier is prepared as follows: In a 1L four-necked flask equipped with a stirrer, thermometer, and condenser, 700g of allyl polyether with an average molecular weight of 700g / mol and 90g of isopropanol are added and stirred until homogeneous. After purging the air with nitrogen, the temperature is raised to 80℃, and Karstedt catalyst (3ppm based on the total mass of polyether and siloxane) is added. Then, 106g of methyldimethoxysilane is slowly added dropwise. After the addition is complete, the reaction is maintained at this temperature for 3 hours. The solvent is removed by vacuum to obtain the reactive silicone emulsifier A-3.

[0035] Examples 1-4

[0036] A reactive silicone emulsifier is prepared as follows: In a 1L four-necked flask equipped with a stirrer, thermometer, and condenser, 660g of allyl polyether with an average molecular weight of 600g / mol and 30g of isopropanol are added and stirred until homogeneous. After purging the air with nitrogen, the temperature is raised to 90℃, and Speier catalyst (6ppm based on the total mass of polyether and siloxane) is added. Then, 180g of triethoxysilane is slowly added dropwise. After the addition is complete, the reaction is maintained at this temperature for 0.5h. The solvent is removed by vacuum to obtain the reactive silicone emulsifier A-4.

[0037] Examples 1-5

[0038] A reactive silicone emulsifier is prepared as follows: In a 1L four-necked flask equipped with a stirrer, thermometer, and condenser, 660g of allyl polyether with an average molecular weight of 600g / mol and 30g of isopropanol are added and stirred until homogeneous. After purging the air with nitrogen, the temperature is raised to 110℃, and Speier catalyst (6ppm based on the total mass of polyether and siloxane) is added. Then, 180g of triethoxysilane is slowly added dropwise. After the addition is complete, the reaction is maintained at this temperature for 0.5h. The solvent is removed by vacuum to obtain the reactive silicone emulsifier A-5.

[0039] The appearance uniformity and surface tension of the aqueous solutions of the reactive silicone emulsifiers prepared in Examples 1-1 to 1-4 were tested, and compared with those of commercially available SDS and Tween 8. The results are shown in Table 1. The appearance uniformity test involved dissolving the reactive silicone emulsifier in water at a concentration of 0.1% and observing its uniformity. The uniformity criteria were: no oil floating and no insoluble matter. The surface tension test conditions were: dissolving the reactive silicone emulsifier in water at a concentration of 0.1% and measuring the surface tension using a fully automatic surface tension meter, with units of mN / m.

[0040] Table 1 Physicochemical parameters of the prepared reactive silicone-containing emulsifier

[0041]

[0042] As can be seen from Table 1, the reactive silicone emulsifiers prepared in Examples 1-1 to 1-4 of the present invention all exhibit a uniform dispersion in a 0.1% aqueous solution, and have a lower surface tension than commercially available SDS (sodium dodecyl sulfate) and Tween 80. Therefore, the reactive silicone emulsifiers prepared in the present invention have superior dispersing power, wettability and penetration performance.

[0043] Example 2: Preparation of reactive emulsifiers with different structures

[0044] This embodiment investigates the influence of different structures (hydrophilic and hydrophobic segments) on the physicochemical properties of the prepared reactive silicone emulsifier through the synthesis route shown in Formula 1.

[0045] Example 2-1

[0046] A reactive silicone emulsifier is prepared as follows: In a reaction vessel equipped with a stirrer, thermometer, and condenser, 1 mol of allyl polyether with an average molecular weight of 400 g / mol and an appropriate amount of toluene are added and stirred evenly. After purging the air with nitrogen, the temperature is raised to 70°C, and Karstedt catalyst (3 ppm based on the total mass of polyether and siloxane) is added. Then, 1 mol of trimethoxysilane is slowly added dropwise. After the addition is complete, the reaction is kept at the temperature for 2 hours. The solvent is removed by vacuum to obtain the reactive silicone emulsifier B-1.

[0047] Example 2-2

[0048] Example 2-2 is basically the same as Example 2-1, except that trimethoxysilane in Example 2-1 is replaced with triethoxysilane, and reactive silicone emulsifier B-2 is prepared by reaction.

[0049] Example 2-3

[0050] The contents of Examples 2-3 are basically the same as those of Example 2-1, except that the trimethoxysilane in Example 2-1 is replaced with methyldimethoxysilane, and the reactive silicone emulsifier B-3 is prepared by reaction.

[0051] Examples 2-4

[0052] The contents of Examples 2-4 are basically the same as those of Example 2-1, except that the trimethoxysilane in Example 2-1 is replaced with methyldiethoxysilane, and the reactive silicone emulsifier B-4 is prepared by reaction.

[0053] Examples 2-5

[0054] The contents of Examples 2-5 are basically the same as those of Example 2-1, except that the allyl polyether with an average molecular weight of 400 g / mol in Example 2-1 is replaced with an allyl polyether with an average molecular weight of 300 g / mol, and the reactive silicone emulsifier B-5 is prepared by reaction.

[0055] Examples 2-6

[0056] The contents of Examples 2-6 are basically the same as those of Example 2-1, except that the allyl polyether with an average molecular weight of 400 g / mol in Example 2-1 is replaced with an allyl polyether with an average molecular weight of 500 g / mol, and the reactive silicone emulsifier B-6 is prepared by reaction.

[0057] Examples 2-7

[0058] The contents of Examples 2-7 are basically the same as those of Example 2-1, except that the allyl polyether with an average molecular weight of 400 g / mol in Example 2-1 is replaced with an allyl polyether with an average molecular weight of 600 g / mol, and the reactive silicone emulsifier B-7 is prepared by reaction.

[0059] The appearance uniformity and surface tension of the aqueous solutions of the reactive silicone-containing emulsifiers prepared in Examples 2-1 to 2-7 were tested respectively, and the results are shown in Table 1. The appearance uniformity test involved dissolving the reactive silicone-containing emulsifier in water at a concentration of 0.1% and observing its uniformity. The uniformity evaluation criteria were: no oil floating and no insoluble matter. The surface tension test conditions were: dissolving the reactive silicone-containing emulsifier in water at a concentration of 0.1% and measuring the surface tension using a fully automatic surface tension meter, with units of mN / m.

[0060] Table 2 Physicochemical parameters of reactive silicone-containing emulsifiers with different structures

[0061]

[0062] As can be seen from Table 2, the reactive silicone emulsifier of the present invention can flexibly adjust its dispersibility, wettability and permeability by designing different hydrophilic segments (polyethers) and hydrophobic segments (silanes).

[0063] Example 3: Effect of different reactive silicone emulsifiers on the properties of the prepared silane paste

[0064] To investigate the effects of different reactive silicone emulsifiers on the properties of the prepared silane paste, with the raw material ratio and emulsification process fixed, emulsification tests were conducted on silane with different emulsifiers. The stability and application performance of the silane paste prepared by the reactive silicone emulsifiers B-1 to B-7 as shown in Formula 1 in Example 2 were tested.

[0065]

[0066] Example 3-1

[0067] A high-performance silane paste is prepared from the following raw materials by weight percentage: 12% reactive silicone emulsifier B, 80% industrial-grade alkoxysilane, 0.5% thickener, 16.5% deionized water, 0.5% preservative, and 0.5% bactericide.

[0068] The specific steps for preparing the above-mentioned high-performance silane paste are as follows:

[0069] (1) Add reactive silicone emulsifier B-1 to deionized water and stir to disperse at 200 rpm for 5 min;

[0070] (2) Adjust the speed to 1000 rpm and gradually add the alkoxysilane to the emulsifier dispersion at a certain speed for 20 minutes.

[0071] (3) After the addition is complete, adjust the speed to 3000 rpm and perform high-speed emulsification for 60 minutes;

[0072] (4) After emulsification, reduce the speed to 500 rpm, add an appropriate amount of thickener, continue for 20 minutes, then add preservative and bactericide to obtain a high-performance silane paste product.

[0073] Example 3-2

[0074] The content of Example 3-2 is basically the same as that of Example 3-1, except that the reactive silicone emulsifier B-1 described in Example 3-1 is replaced with B-2.

[0075] Example 3-3

[0076] The content of Example 3-3 is basically the same as that of Example 3-1, except that the reactive silicone emulsifier B-1 described in Example 3-1 is replaced with B-3.

[0077] Examples 3-4

[0078] The contents of Examples 3-4 are basically the same as those of Example 3-1, except that the reactive silicone emulsifier B-1 described in Example 3-1 is replaced with B-4.

[0079] Examples 3-5

[0080] The contents of Examples 3-5 are basically the same as those of Example 3-1, except that the reactive silicone emulsifier B-1 described in Example 3-1 is replaced with B-5.

[0081] Examples 3-6

[0082] The contents of Examples 3-6 are basically the same as those of Example 3-1, except that the reactive silicone emulsifier B-1 described in Example 3-1 is replaced with B-6.

[0083] Examples 3-7

[0084] The contents of Examples 3-7 are basically the same as those of Example 3-1, except that the reactive silicone emulsifier B-1 described in Example 3-1 is replaced with B-7.

[0085] Comparative Example 3-1

[0086] The content of Comparative Example 3-1 is basically the same as that of Example 3-1, except that the reactive silicone emulsifier B-1 described in Example 3-1 is replaced with Tween 80.

[0087] Comparative Example 3-2

[0088] The content of Comparative Example 3-2 is basically the same as that of Example 3-1, except that the reactive silicone emulsifier B-1 described in Example 3-1 is replaced with Span 20.

[0089] Comparative Example 3-3

[0090] The content of Comparative Example 3-3 is basically the same as that of Example 3-1, except that the reactive silicone emulsifier B-1 described in Example 3-1 is replaced with SDS.

[0091] The stability and application performance of the silane pastes prepared in Examples 3-1 to 3-7 and Comparative Examples 3-1 to 3-3 were tested respectively. The stability test results are shown in Table 3; the application performance test results for water absorption rate, silane penetration depth, contact angle, and chloride absorption reduction are shown in Table 4. The specific test methods are as follows:

[0092] a. Stability Testing

[0093] (1) Storage stability: The silane paste was sealed and placed at room temperature for 6 months, and the layering, oil floating and precipitation of the silane paste were observed.

[0094] (2) Mechanical stability: Place the silane paste in a centrifuge tube and centrifuge at 8000 r / min for 20 min to observe whether stratification occurs.

[0095] (3) Thermal storage stability: The silane paste was placed in a constant temperature box at 50℃ for 14 days, and its layering, oil floating and precipitation were observed.

[0096] b. Water absorption test

[0097] Concrete specimens with dimensions of 100*100*100mm were prepared according to the requirements of JTS153-2015 Standard for Durability Design of Waterway Engineering Structures. The specimens were dried in a 50℃ oven for 5 hours. After cooling, silane paste was evenly applied to any surface of the concrete specimen, while the remaining surfaces were coated with solvent-free epoxy paint. The coated specimens and blank specimens were cured at 40℃ for 48 hours and then weighed. After immersion in deionized water for a certain period, the water absorption rate and the decrease in water absorption rate were calculated.

[0098] c. Silane penetration depth test

[0099] The silane penetration depth was tested using the dye indicator method according to the JTS153-2015 standard for durability design of waterway engineering structures.

[0100] d. Contact angle test

[0101] The contact angles of concrete specimens and blank specimens after curing with silane paste with water were measured using an optical contact angle meter. Each sample was tested 5 times and the average value was taken.

[0102] e. Effect of reducing chloride absorption

[0103] The tests were conducted in accordance with the requirements of the JTS153-2015 Standard for Durability Design of Waterway Engineering Structures.

[0104] Table 3 Stability test of silane paste

[0105]

[0106] As shown in Table 3, when Tween 80, Span 20, and SDS were used alone as emulsifiers for silanes, the resulting emulsion paste was not ideal, but rather an unstable white emulsion that was prone to separation and demulsification. Conversely, the paste prepared by introducing a silicone-containing emulsifier exhibited superior thermal and mechanical stability. This comparison clearly demonstrates that silicone-containing emulsifiers show a significant advantage over traditional emulsifiers in emulsifying alkoxysilanes. Specifically, the silicone-containing emulsifier exhibits superior compatibility with silanes, a characteristic that effectively reduces the interfacial tension between silanes and water, thereby promoting equilibrium between the two phases. It is based on this mechanism that the silane paste prepared in this invention demonstrates outstanding stability.

[0107] Table 4 Application Performance Data of Silane Paste

[0108]

[0109] As can be seen from Table 4, the silane pastes prepared by the reactive silane emulsifiers used in Examples 3-1 to 3-7 of the present invention maintain an extremely low water absorption rate and a contact angle of over 130° when applied to concrete. They have significant advantages over Comparative Examples 3-1 to 3-3 in terms of various performance indicators.

[0110] Contact angle testing is an important method for measuring the hydrophilicity and hydrophobicity of concrete surfaces. In this invention, by comparing the contact angle tests of Examples 3-1 to 3-7 with those of Comparative Examples 3-1 to 3-3, it was verified that traditional emulsifiers, due to insufficient penetration, easily remain and migrate on the concrete surface, resulting in poor surface hydrophobicity. Furthermore, combined with the results of water absorption rate testing, it was further confirmed that reactive silicone-containing emulsifiers can undergo hydrolytic cross-linking reactions with silanes, effectively avoiding the drawbacks of emulsifier migration and aggregation within the concrete, thus preventing the formation of water-absorbing nests.

[0111] Example 4

[0112] This embodiment provides a high-performance silane paste, which comprises the following raw materials by weight percentage: 1% reactive silicone emulsifier B-1, 80% industrial-grade alkoxysilane, 1% thickener, 17% deionized water, 0.5% preservative, and 0.5% bactericide.

[0113] The preparation method of the above-mentioned high-performance silane paste includes the following steps:

[0114] (1) Add reactive silicone emulsifier B-1 to deionized water and stir to disperse at 200 rpm for 10 min;

[0115] (2) Adjust the speed to 1000 rpm and gradually add the alkoxysilane to the emulsifier dispersion at a certain speed for 20 minutes.

[0116] (3) After the addition is complete, adjust the speed to 3000 rpm and perform high-speed emulsification for 60 minutes;

[0117] (4) After emulsification, reduce the speed to 500 rpm, add an appropriate amount of thickener, continue for 10 minutes, then add preservative and bactericide to obtain a high-performance silane paste product.

[0118] Example 5

[0119] This embodiment provides a high-performance silane paste, which comprises the following raw materials by weight percentage: 1.5% reactive silicone emulsifier B-3, 82% industrial-grade alkoxysilane, 0.5% thickener, 15% deionized water, 0.5% preservative, and 0.5% bactericide.

[0120] The preparation method of the above-mentioned high-performance silane paste is the same as that in Example 4.

[0121] Example 6

[0122] This embodiment provides a high-performance silane paste, which comprises the following raw materials by weight percentage: 0.1% reactive silicone emulsifier B-5, 77% industrial-grade alkoxysilane, 1% thickener, 20% deionized water, 0.9% preservative, and 1% bactericide.

[0123] The preparation method of the above-mentioned high-performance silane paste is the same as that in Example 4.

[0124] Example 7

[0125] This embodiment provides a high-performance silane paste, which comprises the following raw materials by weight percentage: 5% reactive silicone emulsifier B-5, 75% industrial-grade alkoxysilane, 1% thickener, 17% deionized water, 1% preservative, and 1% bactericide.

[0126] The preparation method of the above-mentioned high-performance silane paste is the same as that in Example 4.

[0127] In summary, the silane paste prepared by the reactive silicone emulsifier of this invention can provide excellent waterproofing and water-repellent effects for concrete.

[0128] The above description illustrates the embodiments of the present invention. By describing the disclosed embodiments, those skilled in the art are able to implement or use the present invention, and it is not intended to limit the present invention. The various aspects of the present invention cannot be fully embodied in the above embodiments. Any equivalent changes or modifications made by those skilled in the art without departing from the spirit or scope of the present invention fall within the protection and disclosure scope of the present invention.

Claims

1. A reactive silicone-containing emulsifier, characterized in that, Its structural formula is as follows: ， Wherein, R is any one of -CH3, -C2H5, and -C3H7, 0≤x≤10, 1≤y≤10, and x and y are both natural numbers; the average molecular weight of the reactive silicone emulsifier is 250~1200g / mol.

2. A method for preparing the reactive silicone-containing emulsifier according to claim 1, characterized in that, The preparation method is as follows: Under an inert gas protective atmosphere, solvent and allyl polyether are added to a reactor, the temperature is raised to 60-110°C, a catalyst is added, and then hydrogen-containing silane is added to the reaction vessel. The molar ratio of allyl polyether to hydrogen-containing silane is (0.9-1.1):

1. The reaction is maintained at this temperature for 0.5-3 hours. After the reaction is completed, the solvent is removed to obtain a reactive silicone emulsifier. The structural formula of the allyl polyether is: ; The structural formula of the hydrogen-containing silane is: .

3. The preparation method according to claim 2, characterized in that, The allyl polyether has an average molecular weight of 102–1200 g / mol; the catalyst is a platinum molecular complex.

4. The preparation method according to claim 2, characterized in that, The solvent is at least one of isopropanol, toluene, and xylene; the hydrogen-containing silane is at least one of trimethoxysilane, triethoxysilane, and tripropoxysilane.

5. The preparation method according to claim 3 or 4, characterized in that, The average molecular weight of the allyl polyether is between 200 and 1000 g / mol; the catalyst is Karstedt or Speier; the solvent is toluene; and the hydrogen-containing silane is triethoxysilane or trimethoxysilane.

6. The application of the reactive silicone emulsifier according to claim 1 in silane emulsification and preparation of silane protective materials.

7. A silane protective material, characterized in that, It is made from the following raw materials in weight percentage: 0.1-5% of the reactive silicone emulsifier as described in claim 1, 75-82% of alkoxysilane, 0.5-1% of thickener, 15-20% of deionized water, 0.5-1% of preservative, and 0.5-1% of bactericide.

8. The silane protective material according to claim 7, characterized in that, It is made from the following raw materials by weight percentage: 2% of the reactive silicone emulsifier as described in claim 1, 80% of the alkoxysilane, 0.5% of the thickener, 16.5% of the deionized water, 0.5% of the preservative, and 0.5% of the bactericide.

9. A method for preparing a silane protective material, characterized in that, Specifically, the following steps are included: (1) The reactive silicone emulsifier of claim 1 is added to water and dispersed evenly to obtain a dispersion; (2) Add alkoxysilane gradually to the dispersion while stirring. After the alkoxysilane is added, continue stirring until the alkoxysilane and the dispersion are completely emulsified to obtain an emulsion. (3) Add a thickener to the emulsion, mix well, then add a preservative and a bactericide, mix well, and the silane protective material is obtained.

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