An epoxy resin plugging agent, a preparation method and application thereof

Abstract

The application provides an epoxy resin leak stopper, a preparation method and application thereof, and relates to the field of epoxy resin preparation. The epoxy resin leak stopper is prepared by taking hexanediamine, acrylic acid, epoxy resin, an emulsifier and hydrophobic powder as main raw materials. The application utilizes the reaction of acrylic acid and hexanediamine, maintains the dispersion stability of the epoxy resin and the hydrophobic powder, and reduces the reaction activity of the hexanediamine epoxy curing agent, so as to ensure that the leak stopper occurs curing reaction after reaching the crack. Meanwhile, the addition of the hydrophobic powder increases the gravity of the leak stopper, so that the leak stopper cannot be decomposed by water pressure before reaching the crack in the underwater environment. At the same time of weighting, the hydrophobic powder forms a bridging block at the crack position, positions the epoxy resin curing point, enables the epoxy resin to adapt to the crack shape, and enhances the consolidation performance. The epoxy resin leak stopper prepared by the application is stable in the underwater environment, has good filling and consolidation performance, has high compressive strength, and has no deformation.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of epoxy resin preparation, in particular to an epoxy resin plugging agent and a preparation method and application thereof. BACKGROUND

[0002] With the rapid development of rail transit in China, more and more plugging and reinforcing materials are used in subway and tunnel engineering, such as acrylic salt, polyurethane, epoxy resin and other chemical grouting materials. Among these grouting materials, epoxy resin grouting material has excellent mechanical properties, can effectively cure in water medium, has high solidification body strength, good adhesion to concrete and metal, low shrinkage, and at the same time, epoxy material has plugging and reinforcing functions, and has broad application prospect in plugging.

[0003] Water leakage of hydraulic structures is the most common and difficult problem. How to more effectively seal the underwater leakage position, improve the sealing strength, reduce the operation risk and ensure the operation safety is an important direction of the development of underwater sealing agent. However, epoxy resin needs to be combined with a curing agent to form a three-dimensional network structure with good mechanical properties, and to achieve underwater plugging, the following problems exist: the epoxy resin and the curing agent cannot be cured before reaching the crack.

[0004] Therefore, it is particularly important to provide an epoxy resin plugging agent with stable properties in underwater environment to ensure that it occurs curing reaction after reaching the crack. SUMMARY

[0005] In view of the above problems existing in the prior art, the first technical problem to be solved by the present application is to provide a preparation method of an epoxy resin plugging agent; the second technical problem to be solved by the present application is to provide an epoxy resin plugging agent prepared by the method; and the third technical problem to be solved by the present application is to provide an application of the epoxy resin plugging agent.

[0006] To solve the above problems, the present application provides the following technical solutions:

[0007] In a first aspect, a preparation method of an epoxy resin plugging agent comprises the following steps:

[0008] S1, mixing acrylic acid and hexanediamine according to a molar ratio, and heating to react to obtain component A;

[0009] S2, mixing epoxy resin and emulsifier according to a use amount ratio to obtain component B;

[0010] S3, mixing and stirring component A, component B and hydrophobic powder according to a use amount ratio to obtain the epoxy resin plugging agent.

[0011] As a preferred embodiment of the present application, the reaction of hexanediamine and acrylic acid is as follows:

[0012]

[0013] The curing mechanism is as follows:

[0014]

[0015] As a preferred embodiment of the present application, the molar ratio of acrylic acid to hexamethylene diamine in step S1 is 1:1 to 1.3.

[0016] As a preferred embodiment of the present application, the temperature of the heating reaction in step S1 is 60 to 70°C, and the time of the heating reaction is 1 to 2 hours.

[0017] As a preferred embodiment of the present application, the product after the reaction of acrylic acid and hexamethylene diamine can dilute the epoxy resin, and maintain the dispersion stability of the epoxy resin and the hydrophobic powder.

[0018] As a preferred embodiment of the present application, the reactivity of the hexamethylene diamine epoxy curing agent is reduced by using acrylic acid.

[0019] As a preferred embodiment of the present application, the epoxy resin in step S2 is selected from at least one of XT101 epoxy resin, E51 epoxy resin, E44 epoxy resin, and R140 epoxy resin.

[0020] As a preferred embodiment of the present application, the mass ratio of the epoxy resin in step S2 to the A component prepared in step S1 is 8:1 to 1.5.

[0021] In the present example, the material of the emulsifier can be any material capable of emulsifying in the prior art, and is not particularly limited, and can be specifically selected according to actual needs, for example, can be Span80.

[0022] As a preferred embodiment of the present application, the addition amount of the emulsifier in step S2 is 0.1 to 0.2% of the mass of the epoxy resin.

[0023] In the present example, the hydrophobic powder can be any particle capable of achieving hydrophobic performance in the prior art, and is not particularly limited, and can be specifically selected according to actual needs, for example, can be silica powder or lycopodium powder.

[0024] As a preferred embodiment of the present application, the hydrophobic powder is directly used as a commercially available product.

[0025] As a preferred embodiment of the present application, the particle size of the hydrophobic powder in step S3 is 25 to 75 μm.

[0026] As a preferred embodiment of the present application, the addition amount of the hydrophobic powder in step S3 is 3 to 7% of the total mass of the A component and the B component.

[0027] As a preferred embodiment of the present application, the hydrophobic powder increases the gravity of the epoxy resin plugging agent and forms a bridging block at the crack position, positioning the epoxy resin curing point.

[0028] In a second aspect, the epoxy resin plugging agent prepared by the above method is also within the protection scope of the present application.

[0029] As a preferred embodiment of the present application, the main raw materials of the epoxy resin plugging agent are hexamethylene diamine, acrylic acid, epoxy resin, emulsifier and hydrophobic powder.

[0030] As a preferred embodiment of the present application, the epoxy resin plugging agent is a viscous liquid prepared by using hexamethylene diamine, acrylic acid, epoxy resin, emulsifier and hydrophobic powder.

[0031] In a third aspect, the epoxy resin plugging agent is applied in plugging of hydraulic structures.

[0032] Compared with the prior art, the present application has the following beneficial effects:

[0033] 1) The present application utilizes the reaction of acrylic acid and hexamethylene diamine to reduce the reaction activity of the hexamethylene diamine epoxy curing agent, ensuring that the plugging agent does not cure before reaching the crack, and then curing after reaching the crack. At the same time, the product after the reaction of acrylic acid and hexamethylene diamine can dilute the epoxy resin, which is conducive to the dispersion stability of the epoxy resin and the hydrophobic powder.

[0034] 2) The present application increases the gravity of the plugging agent by adding hydrophobic powder, ensuring that the plugging agent will not be decomposed by water pressure before reaching the crack in the underwater environment. At the same time, the hydrophobic powder forms a bridging block at the crack position, increasing the wetting ability and penetration ability of the epoxy resin at the crack position, positioning the epoxy resin curing point, enabling the epoxy resin to adapt to the shape of the crack, and enhancing the consolidation performance.

[0035] 3) The preparation process of the present application is simple and has high operability, which is easy to popularize.

[0036] 4) The epoxy resin plugging agent prepared by the present application is stable in the underwater environment, relies on its own gravity to settle at the underwater leakage site, and after reaching the crack, begins to cure with time, filling and reinforcing the crack, has good consolidation performance, and has high compressive strength without deformation. DETAILED DESCRIPTION

[0037] The technical solutions in the embodiments of the present application will be described below in a clear and complete manner. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the protection scope of the present application.

[0038] To enable those skilled in the art to better understand the features and effects of the present application, the following is a general description and definition of the terms and phrases mentioned in the specification. Unless otherwise specified, all technical and scientific words used herein are in the ordinary meaning understood by those skilled in the art of the present application, and in the event of a conflict, the definition in the specification shall prevail.

[0039] Theories or mechanisms described and disclosed herein, whether correct or not, should not be considered limiting on the scope of the present application, i.e., the present application can be practiced without regard to any particular theory or mechanism.

[0040] Herein, all features defined in the form of numerical ranges or percentage ranges, such as numerical values, amounts, contents and concentrations, are for the sake of brevity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to have encompassed and specifically disclosed all possible sub-ranges and individual numerical values within the range (including integers and fractions).

[0041] Herein, unless otherwise specified, "comprise", "include", "contain", "have" or similar words encompass the meaning of "consist of" and "consist essentially of", e.g., "A comprises a" encompasses the meaning of "A comprises a and other" and "A comprises only a".

[0042] In the following examples, conventional apparatuses in the art were used. In the following examples, unless otherwise specified, the experimental methods were carried out under conventional conditions or under the conditions recommended by the manufacturers. In the following examples, various raw materials were used, and unless otherwise specified, conventional commercially available products were used, which were of conventional specifications in the art. In the specification of the present application and in the following examples, unless otherwise specified, "%" means weight percent, "parts" means weight parts, and the ratio means weight ratio.

[0043] Example 1

[0044] Hexamethylene diamine was melted in a hot water bath, and then 16.2 g of hexamethylene diamine and 10 g of acrylic acid were placed in a four-necked flask equipped with a reflux condenser, a stirrer and a thermometer, and reacted at 60°C for 1 h under nitrogen to obtain Component A. 140 g of XT101 epoxy resin and 0.14 g of Span-80 emulsifier were mixed to obtain Component B. Components A and B were mixed and stirred for 1 h to obtain a stable viscous liquid, i.e., the underwater cementing agent of the epoxy resin.

[0045] Example 2

[0046] Hexamethylene diamine was melted in a hot water bath, then 18.8 g of hexamethylene diamine and 9 g of acrylic acid were put into a four-necked flask equipped with reflux condenser, stirrer and thermometer, and reacted at 70°C for 2 h under nitrogen to obtain component A. Component B was obtained by mixing 222 g of E51 epoxy resin and 0.44 g of Span-80 emulsifier. Component A, component B and 17.5 g of lycopodium powder (the particle size of lycopodium powder was 25-75 μm) were mixed and stirred for 1 h to obtain a stable viscous liquid, which was the epoxy resin underwater plugging agent.

[0047] Example 3

[0048] Hexamethylene diamine was melted in a hot water bath, then 17 g of hexamethylene diamine and 10 g of acrylic acid were put into a four-necked flask equipped with reflux condenser, stirrer and thermometer, and reacted at 60°C for 2 h under nitrogen to obtain component A. Component B was obtained by mixing 180 g of E44 epoxy resin and 0.2 g of Span-80 emulsifier. Component A, component B and 9 g of silicon powder (the particle size of silicon powder was 25-75 μm) were mixed and stirred for 1 h to obtain a stable viscous liquid, which was the epoxy resin underwater plugging agent.

[0049] Example 4

[0050] Hexamethylene diamine was melted in a hot water bath, then 10 g of hexamethylene diamine and 6 g of acrylic acid were put into a four-necked flask equipped with reflux condenser, stirrer and thermometer, and reacted at 70°C for 1 h under nitrogen to obtain component A. Component B was obtained by mixing 100 g of R140 epoxy resin and 0.15 g of Span-80 emulsifier. Component A, component B and 6 g of lycopodium powder (the particle size of lycopodium powder was 25-75 μm) were mixed and stirred for 1 h to obtain a stable viscous liquid, which was the epoxy resin underwater plugging agent.

[0051] Example 5

[0052] Hexamethylene diamine was melted in a hot water bath, then 15 g of hexamethylene diamine and 8 g of acrylic acid were put into a four-necked flask equipped with reflux condenser, stirrer and thermometer, and reacted at 60°C for 2 h under nitrogen to obtain component A. Component B was obtained by mixing 150 g of XT101 epoxy resin and 0.25 g of Span-80 emulsifier. Component A, component B and 7 g of silicon powder (the particle size of silicon powder was 25-75 μm) were mixed and stirred for 1 h to obtain a stable viscous liquid, which was the epoxy resin underwater plugging agent.

[0053] Example 6

[0054] Hexamethylene diamine was melted in a hot water bath, then 17g of hexamethylene diamine and 10g of acrylic acid were put into a four-necked flask equipped with a reflux condenser, a stirrer and a thermometer, and reacted at 60°C for 1 hour under nitrogen to obtain component A. 150g of E44 epoxy resin and 0.2g of Span-80 emulsifier were mixed to obtain component B. Component A, component B and 9g of silicon powder (the particle size of the silicon powder was 25-75 μm) were mixed and stirred for 1 hour to obtain a stable viscous liquid, which was the epoxy resin underwater plugging agent.

[0055] Example 7

[0056] Hexamethylene diamine was melted in a hot water bath, then 16g of hexamethylene diamine and 9g of acrylic acid were put into a four-necked flask equipped with a reflux condenser, a stirrer and a thermometer, and reacted at 60°C for 1 hour under nitrogen to obtain component A. 150g of E51 epoxy resin and 0.25g of Span-80 emulsifier were mixed to obtain component B. Component A, component B and 10g of silicon powder (the particle size of the silicon powder was 25-75 μm) were mixed and stirred for 1 hour to obtain a stable viscous liquid, which was the epoxy resin underwater plugging agent.

[0057] Example 8

[0058] Hexamethylene diamine was melted in a hot water bath, then 16g of hexamethylene diamine and 8g of acrylic acid were put into a four-necked flask equipped with a reflux condenser, a stirrer and a thermometer, and reacted at 60°C for 1 hour under nitrogen to obtain component A. 140g of R140 epoxy resin and 0.2g of Span-80 emulsifier were mixed to obtain component B. Component A, component B and 9g of silicon powder (the particle size of the silicon powder was 25-75 μm) were mixed and stirred for 1 hour to obtain a stable viscous liquid, which was the epoxy resin underwater plugging agent.

[0059] Example 9

[0060] Hexamethylene diamine was melted in a hot water bath, then 20g of hexamethylene diamine and 12g of acrylic acid were put into a four-necked flask equipped with a reflux condenser, a stirrer and a thermometer, and reacted at 60°C for 1 hour under nitrogen to obtain component A. 180g of E44 epoxy resin and 0.2g of Span-80 emulsifier were mixed to obtain component B. Component A, component B and 8g of lycopodium powder (the particle size of the lycopodium powder was 25-75 μm) were mixed and stirred for 1 hour to obtain a stable viscous liquid, which was the epoxy resin underwater plugging agent.

[0061] The basic properties of the epoxy resin underwater plugging agents prepared in Examples 1-9 were tested, and the specific test methods were as follows:

[0062] Underwater initial setting time: under laboratory standard conditions [temperature (23+2)℃, relative humidity (50+10)%], the prepared epoxy resin underwater leak stopper is poured into a glass beaker to spread evenly. The surface of the slurry mixture is contacted once every 5 min with a glass rod until the "stringing" phenomenon appears. The time elapsed at this time is recorded, which is the initial setting time of the epoxy resin leak stopper under water.

[0063] Compressive strength: tested according to the test method in GB / T 2567-2008 "Resin cast performance test".

[0064] Underwater bonding strength, impermeable pressure: tested according to the test method in Q / SDKS 015-2017 "Modified epoxy resin leak stoppage grouting material".

[0065] Table 1 is the basic performance of the epoxy resin underwater leak stopper prepared in Examples 1-9. As can be seen from Table 1, the curing speed of the epoxy resin underwater leak stopper is moderate, and there is enough operation time when single liquid grouting. The leak stopper relies on its own gravity to settle and adsorb to the underwater leakage site, and the comprehensive mechanical properties of the solidified body are better.

[0066] Table 1 Basic performance of epoxy resin underwater leak stopper

[0067]

[0068]

[0069] The above is only to illustrate the technical idea of the present application, and cannot limit the protection scope of the present application. Any modification made according to the technical idea of the present application on the basis of the technical scheme falls within the protection scope of the claims of the present application.

Claims

1. A method for preparing an epoxy resin sealant, characterized in that, Includes the following steps: S1. Acrylic acid and hexamethylenediamine are mixed in a molar ratio and heated to react to obtain component A; S2. Mix epoxy resin and emulsifier according to the specified ratio to obtain component B; S3. Mix and stir components A, B, and hydrophobic powder according to the dosage ratio to obtain epoxy resin sealant; In step S1, the molar ratio of acrylic acid to hexamethylenediamine is 1:1 to 1.

3.

2. The method for preparing the epoxy resin sealant according to claim 1, characterized in that, In step S1, the temperature of the heating reaction is 60-70℃, and the heating reaction time is 1-2 hours.

3. The method for preparing the epoxy resin sealant according to claim 1, characterized in that, In step S2, the epoxy resin is selected from at least one of XT101 epoxy resin, E51 epoxy resin, E44 epoxy resin, and R140 epoxy resin.

4. The method for preparing the epoxy resin sealant according to claim 1, characterized in that, The mass ratio of epoxy resin in step S2 to component A obtained in step S1 is 8:1 to 1.

5.

5. The method for preparing the epoxy resin sealant according to claim 1, characterized in that, In step S2, the amount of emulsifier added is 0.1 to 0.2% of the mass of epoxy resin.

6. The method for preparing the epoxy resin sealant according to claim 1, characterized in that, In step S3, the particle size of the hydrophobic powder is 25–75 μm.

7. The method for preparing the epoxy resin sealant according to claim 1, characterized in that, In step S3, the amount of hydrophobic powder added is 3-7% of the total mass of components A and B.

8. An epoxy resin sealant prepared by the preparation method according to any one of claims 1 to 7.

9. The application of the epoxy resin sealant according to claim 8 in the sealing of leaks in hydraulic structures.

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