A silicone waterproofing agent for ultra-high performance concrete slabs and a method of preparation

Abstract

The application discloses a kind of organic silicon waterproof agent for ultra-high performance concrete plate and preparation method, including hydroxyl silicone oil 5-20 parts, silane coupling agent 2-10 parts, amino silicone oil 1-5 parts, nano white carbon black 1-10 parts and organic solvent 50-100 parts.The organic silicon waterproof agent of the application can be used on the surface of UHPC plate, cement concrete base material, mortar fast, stone material, etc., can form the effect of super-hydrophobic on the surface of base material, and make the water-repellent performance of base material surface keep long.The method of the application can economically and efficiently produce the waterproof agent by using simple and cheap raw materials, the production process is simple, energy consumption is low, and the waterproof agent can be mass-produced and used.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of waterproof materials, and relates to a silicone waterproof agent, in particular to a silicone waterproof agent for ultra-high performance concrete plate materials, which is stable in properties, resistant to storage, low in raw material cost, low in production equipment requirement, and easy to be produced on a large scale. BACKGROUND

[0002] Ultra-high performance concrete (UHPC) is the most innovative cement-based engineering material in the past three decades, which can realize a leap in the performance of cement-based materials (compression resistance, durability, impact resistance, etc.). Among them, UHPC plate, as a new type of lightweight, environmentally friendly, ultra-high strength and moldable material, is widely used in non-load-bearing exterior wall engineering of various buildings. However, due to the more compact surface structure of UHPC plate and its own waterproof effect, the conventional surface coating waterproof agent is difficult to improve the waterproof performance of UHPC plate.

[0003] The super-hydrophobic surface coating waterproof agent can make the contact angle between the substrate surface and the water droplet greater than 150°, and the rolling angle less than 10°. In order to achieve the super-hydrophobic effect on the surface of UHPC plate, it is necessary to reduce the surface energy of the UHPC plate surface and form a rough microstructure on the surface. In the actual application process, the influence of environmental erosion, friction and wear, ultraviolet aging and other factors also needs to be considered.

[0004] Therefore, it is of great significance and application potential to develop a new type of waterproof agent that can be applied to improve the waterproof effect of UHPC plate. SUMMARY

[0005] In order to solve the above problems, the present application provides a silicone waterproof agent for ultra-high performance concrete plate materials and a preparation method thereof. The present application uses a mixed solution of hydroxyl silicone oil, silane coupling agent and amino silicone oil, which can not only reduce the surface energy of the object, but also combine the silicone oil with the nano white carbon black while the silicone oil and the silane coupling agent are attached to the substrate and react, thereby fixing the nano white carbon black. The nano white carbon black is uniformly fixed on the substrate, the microstructure of the substrate surface is changed, and the super-hydrophobic effect of the substrate surface can be achieved. The waterproof agent of the present application is stable in properties, resistant to storage, low in raw material cost, low in production equipment requirement, and easy to be produced on a large scale.

[0006] In order to achieve the above purpose, the present application adopts the following technical scheme:

[0007] The first aspect of the present application provides a preparation method of a silicone waterproof agent for ultra-high performance concrete plate materials, which comprises the following steps:

[0008] 1) adding hydroxyl silicone oil, silane coupling agent and amino silicone oil, stirring at room temperature, and mixing uniformly to obtain a mixed silicone oil;

[0009] 2) To the mixed silicone oil obtained in step 1), nano white carbon black is added in batches, and stirred to mix uniformly to obtain a paste;

[0010] 3) The paste obtained in step 2) is subjected to temperature curing;

[0011] 4) To the paste obtained in step 3), an organic solvent is added, and stirred to dilute to obtain a silicone waterproof agent;

[0012] In the application, the mixed solution of hydroxyl silicone oil, silane coupling agent and amino silicone oil can not only reduce the surface energy of the object, but also combine with the nano white carbon black while the silicone oil and the silane coupling agent are attached to the substrate and react, thereby fixing the nano white carbon black. The nano white carbon black is uniformly fixed on the substrate, changes the microstructure of the substrate surface, and enables the substrate surface to achieve the effect of super-hydrophobicity.

[0013] In the application, the mixed solution of hydroxyl silicone oil, silane coupling agent and amino silicone oil can not only reduce the surface energy of the object, but also combine with the nano white carbon black while the silicone oil and the silane coupling agent are attached to the substrate and react, thereby fixing the nano white carbon black. The nano white carbon black is uniformly fixed on the substrate, changes the microstructure of the substrate surface, and enables the substrate surface to achieve the effect of super-hydrophobicity.

[0014] In the application, the mixed solution of hydroxyl silicone oil, silane coupling agent and amino silicone oil can not only reduce the surface energy of the object, but also combine with the nano white carbon black while the silicone oil and the silane coupling agent are attached to the substrate and react, thereby fixing the nano white carbon black. The nano white carbon black is uniformly fixed on the substrate, changes the microstructure of the substrate surface, and enables the substrate surface to achieve the effect of super-hydrophobicity.

[0015] In the application, the mixed solution of hydroxyl silicone oil, silane coupling agent and amino silicone oil can not only reduce the surface energy of the object, but also combine with the nano white carbon black while the silicone oil and the silane coupling agent are attached to the substrate and react, thereby fixing the nano white carbon black. The nano white carbon black is uniformly fixed on the substrate, changes the microstructure of the substrate surface, and enables the substrate surface to achieve the effect of super-hydrophobicity.

[0016] As a preferred scheme of the application, in step 1), the viscosity of the hydroxyl silicone oil is 50-1000 cst.

[0017] As a preferred scheme of the application, in step 1), the silane coupling agent includes at least one of vinyltriethoxysilane, vinyltrimethoxysilane, vinyltrichlorosilane, γ-aminopropyltriethoxysilane, γ-(2,3-epoxypropoxy)propyltrimethoxysilane, γ-methacryloyloxypropyltrimethoxysilane, n-octyltriethoxysilane or vinyl-tris(2-methoxyethoxy)silane.

[0018] As a preferred scheme of the application, in step 1), the viscosity of the amino silicone oil is 10-500 cst, and the amino value is 0.1-1.0 mmol / g.

[0019] As a preferred scheme of the present application, in step 2), the nano white carbon black is fumed white carbon black, and the particle size range is 10-200 nm.

[0020] As a preferred scheme of the present application, in step 3), the temperature of the maturation is 50-80℃, and the maturation time is 2-6 h.

[0021] As a preferred scheme of the present application, in step 4), the organic solvent includes at least one of ethanol, isopropanol, n-hexane, cyclohexane, n-heptane, petroleum ether, 120# gasoline, D60, ethyl acetate and butyl acetate.

[0022] As a preferred scheme of the present application, in step 4), the stirring and diluting time is 25-40 min.

[0023] The second aspect of the present application provides the organic silicon waterproof agent for the ultra-high performance concrete plate prepared by the preparation method.

[0024] Compared with the prior art, the present application has the following beneficial effects:

[0025] 1) The organic silicon waterproof agent of the present application can be applied to the surface of the UHPC plate, and after the surface coating of the base material, the surface of the base material has super-hydrophobic effect and obtains long-term water repellency.

[0026] 2) The organic silicon waterproof agent of the present application has wide application range, and can also be surface coated on stone, wood, concrete base material, cement fiber board and other materials.

[0027] 3) The organic silicon waterproof agent of the present application has stable properties, is resistant to storage, has low raw material cost, requires low production equipment, and is easy to mass produce in industry. BRIEF DESCRIPTION OF DRAWINGS

[0028] Figure 1 The property diagram of the organic silicon waterproof agent prepared for the embodiment 1 of the present application.

[0029] Figure 2 The property diagram of the organic silicon waterproof agent prepared for the embodiment 2 of the present application.

[0030] Figure 3 The water droplet effect diagram of the blank UHPC plate.

[0031] Figure 4 The water droplet effect diagram of the organic silicon waterproof agent of the present application on the UHPC plate.

[0032] Figure 5 The water droplet effect diagram of the organic silicon waterproof agent of the present application on the calcium silicate plate.

[0033] Figure 6The water droplet effect diagram of the silicone waterproof agent of the present application on the cement fiber board.

[0034] Figure 7 The effect diagram of the silicone waterproof agent prepared in Example 1 of the present application on the substrate after surface coating, outdoor test for 45 days. DETAILED DESCRIPTION

[0035] In order to make the technical means, creative features, purposes and effects of the present application easy to understand, the present application is further described below in combination with specific examples. However, the following examples are only preferred examples of the present application, not all. Based on the examples in the embodiments, other examples obtained by those skilled in the art without creative labor are within the protection scope of the present application. The experimental methods in the following examples are conventional methods, and the materials, reagents, etc. used in the following examples are commercially available unless otherwise specified.

[0036] The present application provides a preparation method of a silicone waterproof agent for ultra-high performance concrete plate, which comprises the following steps:

[0037] 1) adding hydroxyl silicone oil, silane coupling agent and amino silicone oil, stirring at room temperature, and mixing uniformly to obtain mixed silicone oil;

[0038] 2) adding nano white carbon black into the mixed silicone oil obtained in step 1) in batches, stirring and mixing uniformly to obtain a paste;

[0039] 3) performing temperature curing on the paste obtained in step 2);

[0040] 4) adding an organic solvent into the paste obtained in step 3), stirring and diluting to obtain a silicone waterproof agent;

[0041] Wherein, the raw materials include, by weight fraction, 5-20 parts of hydroxyl silicone oil, 2-8 parts of silane coupling agent, 1-5 parts of amino silicone oil, 1-8 parts of nano white carbon black and 70-100 parts of organic solvent.

[0042] Example 1

[0043] The present embodiment provides a preparation method of a silicone waterproof agent for ultra-high performance concrete plate, which comprises the following steps:

[0044] Take linear silicone oil (PMX-0156) 25g, γ-aminopropyl triethoxysilane 15g, amino silicone oil (RJ-WP58) 10g in a reaction vessel, stir for 20 minutes to mix evenly. Add hydrophobic nano white carbon black 6g in three batches, stir to mix evenly to make a paste. Heat to 80℃, after heating and stirring for 4 hours, add solvent D60 in three batches to dilute, dilute the paste to a 10% weight percentage solution, that is, 10% effective content of silicone waterproof agent (properties as shown in Figure 1

[0045] Example 2

[0046] The present embodiment provides a preparation method of silicone waterproof agent for ultra-high performance concrete plate, comprising the following steps:

[0047] Take linear silicone oil (PMX-0156) 50g, n-octyl triethoxysilane 30g, amino silicone oil (RJ-WP58) 20g in a reaction vessel, stir for 20 minutes to mix evenly. Add hydrophobic nano white carbon black 15g in three batches, stir to mix evenly to make a paste. Heat to 80℃, after heating and stirring for 4 hours, add solvent D60 in three batches to dilute, dilute the paste to a 30% weight percentage solution, that is, 30% effective content of silicone waterproof agent (properties as shown in Figure 2

[0048] Example 3

[0049] The present embodiment provides a preparation method of silicone waterproof agent for ultra-high performance concrete plate, comprising the following steps:

[0050] Take linear silicone oil (PMX-0156) 50g, n-octyl triethoxysilane 30g, amino silicone oil (RJ-WP58) 20g in a reaction vessel, stir for 20 minutes to mix evenly. Add hydrophobic nano white carbon black 15g in three batches, stir to mix evenly to make a paste. Heat to 80℃, after heating and stirring for 4 hours, add solvent D60 in three batches to dilute, dilute the paste to a 30% weight percentage solution, that is, 30% effective content of silicone waterproof agent (properties as shown in

[0051] Experiment 1: super-hydrophobic effect test

[0052] The silicone waterproof agent is evenly coated on the surface of the substrate. In the process of using a microsyringe to push the water droplets to contact, extrude and finally separate from the coating surface, the coating surface does not adhere to the water droplets. And a drop of water is dropped on the coating surface, the water droplet is bounced up without adhering to the coating surface, indicating that the coating has low adhesion to water.

[0053] ​​The 10% effective content of the silicone waterproof agent prepared in Example 1 is uniformly coated on the surface of the UHPC substrate, and after indoor curing for 48 hours, the water drop test is performed, and the water bead effect (as shown in Figures 3-6 The board is slightly inclined, and the water quickly slides away when contacting the coating surface without leaving water stains on the surface, which meets the “lotus effect”.

[0054] Figure 3 The water bead effect diagram of the blank UHPC board is shown in Figure 4 The water bead effect diagram of the silicone waterproof agent prepared in Example 1 on the UHPC board is shown in Figure 5 The water bead effect diagram of the silicone waterproof agent prepared in Example 1 on the calcium silicate board is shown in Figure 6 The water bead effect diagram of the silicone waterproof agent prepared in Example 1 on the cement fiber board is shown, and it can be seen that the silicone waterproof agent of the present application can make the surface of the substrate achieve super-hydrophobic effect, which meets the “lotus effect”.

[0055] Experiment 2: Weathering test

[0056] The weathering test is carried out in an aging oven, the xenon lamp radiation intensity is 1000W / m 2 , the blackboard temperature is 55℃, the humidity is 50%, the test is carried out for 30 days, and the super-hydrophobic performance is maintained.

[0057] Outdoor test: after the board is brushed with the silicone waterproof agent prepared in Example 1, it is placed outdoors for 45 days, and there are multiple rainfall during the period, and the water-repellent effect of the substrate is maintained (as shown in Figure 7 ).

[0058] Experiment 3: Stability test

[0059] The 30% effective content of the silicone waterproof agent prepared in Example 2 is placed in a centrifuge, the rotation speed is set to 3000 revolutions / minute, and the test is carried out for 30 minutes, and the white carbon black is not precipitated, which indicates that the white carbon black is stably dispersed.

[0060] The 10% effective content of the silicone waterproof agent prepared in Example 1 is placed in a freeze-thaw oven, and the cycle freeze-thaw of-20℃ for 8 hours and 25℃ for 8 hours is set, and the cycle is 5 groups, and no white carbon black is precipitated, which indicates that the freeze-thaw stability is good.

[0061] In summary, the silicone waterproof agent of the present application is suitable for various substrates including UHPC board, can realize super-hydrophobic effect on the surface of the substrate, and has certain weather resistance, the waterproof agent of the present application has excellent stability and storage resistance.

[0062] The above merely describes preferred embodiments of the present application, and is not intended to limit the present application in any form or in essence. It should be noted that those skilled in the art can make some improvements and supplements without departing from the method of the present application, and these improvements and supplements should also be considered as the protection scope of the present application. For those skilled in the art, some slight changes, modifications and equivalent changes made by using the disclosed technical content without departing from the spirit and scope of the present application are equivalent embodiments of the present application; meanwhile, any equivalent changes, modifications and evolution made according to the essential technology of the present application to the above embodiments are still within the scope of the technical solutions of the present application.

Claims

1. A method for preparing an organosilicon waterproofing agent for ultra-high performance concrete slabs, characterized in that, The preparation method includes the following steps: 1) Add hydroxyl silicone oil, silane coupling agent and amino silicone oil, stir at room temperature until they are mixed evenly to obtain mixed silicone oil; 2) Add nano-silica to the mixed silicone oil obtained in step 1) in batches, stir and mix evenly to obtain a paste; 3) Heat the paste obtained in step 2) to mature; the maturation temperature is 50-80℃ and the maturation time is 2-6 hours; 4) Add an organic solvent to the paste obtained in step 3), stir and dilute to obtain an organosilicon waterproofing agent; The raw materials, by weight, include: 5-20 parts hydroxyl silicone oil, 2-8 parts silane coupling agent, 1-5 parts amino silicone oil, 1-8 parts nano-silicone black, and 70-100 parts organic solvent; the hydroxyl silicone oil has a viscosity of 50-1000 cst; the silane coupling agent includes at least one of vinyltriethoxysilane, vinyltrimethoxysilane, vinyltrichlorosilane, γ-aminopropyltriethoxysilane, γ-(2,3-epoxypropoxy)propyltrimethoxysilane, γ-methacryloyloxypropyltrimethoxysilane, n-octyltriethoxysilane, or vinyl-tris(2-methoxyethoxy)silane; the amino silicone oil has a viscosity of 10-500 cst and an ammonia value of 0.1-1.0 mmol / g; the nano-silicone black is fumed silica with a particle size range of 10-200 nm.

2. The method for preparing an organosilicon waterproofing agent for ultra-high performance concrete slabs according to claim 1, characterized in that, In step 4), the organic solvent includes at least one of ethanol, isopropanol, n-hexane, cyclohexane, n-heptane, petroleum ether, No. 120 gasoline, D60, ethyl acetate and butyl acetate.

3. The method for preparing an organosilicon waterproofing agent for ultra-high performance concrete slabs according to claim 1, characterized in that, In step 4), the stirring and dilution time is 25-40 minutes.

4. An organosilicon waterproofing agent for ultra-high performance concrete slabs, characterized in that, It is prepared by the preparation method according to any one of claims 1-3.

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