A basalt fiber impregnant based on nanocomposite microgel and a preparation method thereof
The preparation of nanocomposite microgels by in-situ free radical polymerization and pulverization-swelling method solves the problems of complex composition and preparation of basalt fiber impregnating agents, and achieves good bonding and efficient reinforcement between basalt fibers and matrix, which is suitable for industrial application.
Patent Information
- Application Number
- CN202310583305.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-05-23
- Publication Date
- 2025-12-30
- Estimated Expiration
- 2043-05-23
AI Technical Summary
Existing basalt fiber impregnating agents have complex compositions or preparation processes, resulting in poor fiber reinforcement effects and difficulty in effectively improving the bonding force and dispersibility between basalt fibers and the matrix.
Nanocomposite hydrogels were prepared by free radical in-situ polymerization, and nanocomposite microgels were prepared by pulverization-swelling method for use as basalt fiber impregnating agents. The nanocomposite microgels are composed of propylene polymers and inorganic nanoparticles, and have good compatibility and binding force.
It significantly improves the bundle properties and mechanical properties of basalt fibers, enhances the interfacial properties of basalt fiber composites, and has a simple preparation method suitable for industrial production.
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Figure CN116655260B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to a basalt fiber impregnating agent based on nanocomposite microgels and its preparation method, belonging to the field of impregnating agent technology. Background Technology
[0002] Basalt fiber is made from natural volcanic basalt through a platinum-rhodium spinneret. It is composed of oxides such as silicon dioxide, aluminum oxide, calcium oxide, magnesium oxide, iron oxide, and titanium dioxide, and is a novel, environmentally friendly silicate fiber. Due to its outstanding mechanical properties, thermal stability, chemical stability, thermal and sound insulation properties, and wave transmission properties, it is currently a research hotspot in the field of high-performance fibers. In recent years, the preparation of basalt fiber and its application in composite materials have made rapid progress. In many fields, the performance of basalt fiber has reached or even surpassed that of aramid fiber, carbon fiber, and steel wire, and it is widely used in road construction, aerospace, military equipment, automobiles, and ships.
[0003] The development of specialized basalt fiber sizing agents is a major challenge in basalt fiber application research. Due to the smooth surface, inertness, high polarity, and high surface energy of basalt fibers, their interfacial bonding ability with the matrix is low. Therefore, surface modification of basalt fibers is necessary to reduce surface energy, improve their dispersibility and stability in the matrix, reduce interfacial tension, and enhance the compatibility and bonding force between basalt fibers and the matrix resin, thereby improving the performance of the composite material. To this end, in basalt fiber production, a sizing agent is typically applied to the fiber surface. This enhances surface lubrication, prevents mutual wear between fibers, and provides a certain degree of fiber bundle formation; furthermore, it improves the surface properties of the fibers.
[0004] Chinese patent application CN109761510A discloses a basalt fiber reinforcing sizing agent and its preparation method. The resulting reinforcing sizing agent is green and environmentally friendly, effectively reinforcing basalt fibers while fully recycling oil resources. Chinese patent application CN111153607A discloses an organic-inorganic hybrid phosphate-based high-temperature resistant basalt fiber sizing agent. When this sizing agent operates at temperatures above 300℃, the organosilicon precursor undergoes a dehydration polymerization reaction, transforming into a highly chemically active silicon oxide inorganic ceramic phase. During this process, the highly chemically active silicon oxide inorganic ceramic phase undergoes complex chemical interactions with the phosphate gel material and the oxides of the basalt fiber itself, further constructing a high-temperature resistant oxide film on the surface of the basalt fiber. However, existing sizing agents suffer from drawbacks such as complex composition or complicated preparation processes, and the reinforcing effect of the fiber still falls far short of the theoretical strength.
[0005] Nanocomposite hydrogels are typically composed of hydrophilic polymers, inorganic nanoparticles, and a large amount of water as a solvent. Due to their good mechanical properties or certain functional characteristics, they are widely used in fields such as drive devices, biomedicine, and intelligent bionics. The effective bonding of hydrogels with various materials such as metals, ceramics, glass, and plastics is fundamental to their application. In recent years, scholars at home and abroad have conducted research on the adhesion properties of hydrogels to various materials, demonstrating the important role of hydrogel adhesion in effectively realizing their functional properties. Professor Xuanhe Zhao of MIT discovered that pre-silanization treatment of the substrate surface helps achieve strong adhesion between hydrogels and various non-porous solid surfaces [H Yuk, T Zhang, XH Zhao, et al., Nat. Mater. 2016, 15, 190.][A Inoue, H Yuk, BY Lu, XH Zhao, et al., Sci. Adv. 2020, 6: eaay5394.]. Professor Zhigang Suo of Harvard University and Professor Tongqing Lu of Xi'an Jiaotong University have developed a series of functional interfacial bridging polymers [J Li, AD Celiz, Z Suo, et al., Science 2017, 357, 378.][JW Yang, RB Bai, ZG Suo, Adv. Mater. 2018, 30, 1800671][Y Gao, JJ Chen, TQLu, et al., Adv. Funct. Mater. [2020, 30, 2003207] These polymer solutions, when spread between the hydrogel and the substrate and subjected to pressure for a period of time, can form a strong adhesion. Currently, there is no information regarding the application of nanocomposite hydrogels in the field of wetting agents. Summary of the Invention
[0006] In view of this, the purpose of this invention is to provide a basalt fiber sizing agent based on nanocomposite microgels and its preparation method. First, a nanocomposite hydrogel is prepared by free radical in-situ polymerization, and then a nanocomposite microgel is prepared by a pulverization-swelling method. The sizing agent can significantly improve the bundle properties of basalt fibers, enhance mechanical properties, and thus improve the interfacial properties of basalt fiber composite materials.
[0007] To achieve the above objectives, the technical solution of the present invention is as follows.
[0008] A basalt fiber impregnating agent based on nanocomposite microgel, wherein the mass fraction of nanocomposite microgel is 0.5% to 1.5% based on the total mass of the impregnating agent (100%), and the balance is water with a purity greater than or equal to that of deionized water (such as deionized water, ultrapure water, etc.).
[0009] The nanocomposite microgel has a particle size of 10 nm to 20 nm and is obtained by crushing and swelling nanocomposite hydrogel.
[0010] The nanocomposite hydrogel is composed of propylene polymers and inorganic nanoparticles.
[0011] Preferably, the mass fraction of the nanocomposite microgel is 0.8% to 1.2%.
[0012] Preferably, the nanocomposite hydrogel is obtained by free radical in-situ polymerization of propylene-based polymer monomers, initiators, physical crosslinking agents, redox catalysts, and water with a purity of deionized water or higher; the physical crosslinking agent is inorganic nanoparticles.
[0013] Preferably, the propylene monomer is one or more of acrylic acid, N,N-dimethylacrylamide, hydroxyethyl 2-acrylate, and acrylamide; the initiator is ammonium persulfate and / or potassium persulfate; the physical crosslinking agent is nano-aluminum hydroxide sol, nano-clay, or alumina nanoparticles; and the redox catalyst is tannic acid / ferric ions.
[0014] A method for preparing a basalt fiber impregnating agent based on nanocomposite microgels according to the present invention, the method comprising the following steps:
[0015] (1) Dissolve the initiator in water with a purity of deionized water or higher, then add propylene polymer monomers and physical crosslinking agents, stir evenly to obtain a prepolymer solution;
[0016] (2) Add a redox catalyst to the prepolymer solution, mix well, pour into a mold, and let stand to obtain a nanocomposite hydrogel;
[0017] (3) The nanocomposite hydrogel is crushed, and water with a purity of deionized water or higher is added to swell it. The crushing and swelling are repeated to obtain a basalt fiber impregnating agent based on nanocomposite microgel.
[0018] Preferably, in step (1), the propylene monomer is acrylic acid, N,N-dimethylacrylamide, hydroxyethyl 2-acrylate or acrylamide; the initiator is ammonium persulfate and / or potassium persulfate; and the physical crosslinking agent is nano aluminum hydroxide sol, nano clay or alumina nanoparticles.
[0019] Preferably, in step (1), the initiator in the prepolymer solution has a mass fraction of 0.05% to 0.2%; the total molar concentration of the prepolymer solution is 2 to 6 mol / L; the molar fraction of propylene monomers is 5% to 25%; and the physical crosslinking agent accounts for 1% to 5% of the mass fraction of water.
[0020] Preferably, in step (1), the stirring time is 15 min to 30 min.
[0021] Preferably, in step (2), the redox catalyst is a mixed aqueous solution of tannic acid and ferric chloride hexahydrate, wherein the mass fraction of ferric chloride hexahydrate in the redox catalyst is 2%~6%, and the mass ratio of tannic acid to ferric chloride hexahydrate is 10~30:1.
[0022] Preferably, in step (2), the mass ratio of the prepolymer liquid to the redox catalyst is 10~100:1.
[0023] Preferably, in step (2), the standing time is 2 min to 15 min.
[0024] Preferably, in step (3), the crushing power is 1200 W~2000 W and the crushing time is 5 min~10 min.
[0025] Preferably, in step (3), the mass of water during swelling is 3 to 5 times the mass of the nanocomposite hydrogel.
[0026] Beneficial effects
[0027] This invention provides a basalt fiber sizing agent based on a nanocomposite microgel. The nanocomposite microgel has the advantages of adjustable chemical composition and physical properties. Its inorganic nanoparticle component can strongly bind to basalt fibers, while its organic polymer component has good compatibility with the resin matrix. Through the synergistic effect of the organic and inorganic components of the microgel, basalt fibers treated with the microgel-type sizing agent can efficiently reinforce the resin matrix, especially exhibiting good compatibility with polyurethane resin. A relatively low content of the effective component in the nanocomposite microgel can achieve a highly efficient wetting effect, resulting in good economic efficiency. When the solid content of the microgel sizing agent exceeds 1.5 wt%, the sizing agent will agglomerate after 24 hours, exhibiting poor stability and making it unsuitable for use as a sizing agent.
[0028] This invention provides a method for preparing a basalt fiber sizing agent based on nanocomposite microgels. A pulverization-swelling cycle method is used to prepare nanocomposite hydrogels into nanocomposite microgels, optimizing the hydrogel preparation method and significantly reducing the hydrogel polymerization time. The resulting nanocomposite microgel sizing agent is stable, has controllable viscosity, and can adhere to various material matrices with high strength. When the nanocomposite microgel sizing agent is used to modify basalt fibers, the strength of the modified basalt fibers is significantly improved. This method is simple to prepare, suitable for industrial production, and easy to scale up. Attached Figure Description
[0029] Figure 1This is a scanning electron microscope (SEM) image of the nanocomposite hydrogel obtained in Example 1.
[0030] Figure 2 The image shows a surface SEM image of basalt fibers coated with the nanocomposite microgel-type wetting agent described in Example 1.
[0031] Figure 3 The graph shows the viscosity of the 1 wt% nanocomposite microgel wetting agent obtained in Example 1 as a function of time.
[0032] Figure 4 The graph shows the particle size test results of the nanocomposite microgel wetting agent microgel in Example 1.
[0033] Figure 5 This is a photograph of the basalt fiber modified with microgel impregnator in Example 1, which was then combined with polyurethane for fiber pull-out experiments.
[0034] Figure 6 The graph shows the effect of the solid content of different nanocomposite microgel impregnators on the reinforcement effect of basalt fibers in Example 1. Detailed Implementation
[0035] The present invention will be further described in detail below with reference to specific embodiments.
[0036] The present invention describes a method for preparing a basalt fiber impregnating agent based on nanocomposite microgels, which is prepared by a two-step process. First, a nanocomposite hydrogel is prepared by in-situ rapid free radical polymerization, and then a nanocomposite microgel is prepared by a pulverization-swelling cycle method.
[0037] Example 1
[0038] (A) Add 0.01 g of ammonium persulfate to 10 g of deionized water and stir for 30 min to prepare an ammonium persulfate solution with a mass fraction of 0.1 wt%. According to the total molar mass fraction of the solution being 3 mol / L, acrylic acid accounting for 10% of the total molar mass, and aluminum hydroxide nanoparticles accounting for 1 wt% of the deionized water solvent, take 0.22 g of acrylic acid, 2.68 g of N,N-dimethylacrylamide, and 0.33 g of aluminum hydroxide sol, respectively, and stir for 30 min under nitrogen bubbling conditions to obtain a prepolymer solution;
[0039] (B) According to the mass ratio of tannic acid to ferric chloride hexahydrate of 1:10, add 0.03 g of tannic acid and 0.3 g of ferric chloride hexahydrate to 10 g of deionized water and stir for 30 min to obtain a redox catalyst;
[0040] (C) Take 2 g of the prepolymer liquid obtained in step (A), add 0.1 g of the redox catalyst obtained in step (B) according to the redox catalyst: prepolymer liquid mass ratio of 1:20, stir quickly and evenly, pour into a mold of a certain shape, the prepolymer liquid gels in 20 s, wait for 10 min and take it out to obtain AD-Al nanocomposite hydrogel.
[0041] (D) The nanocomposite hydrogel obtained in step (C) is pulverized at a speed of 1500 W for 5 min, and then 50 g of deionized water is added to swell it.
[0042] (E) After the gel obtained in step (D) has swollen, it is further crushed and then 100 g of deionized water is added to swell. This process is repeated once, and then 140 g of deionized water is added to obtain a basalt fiber impregnating agent with a solid content of 1.0 wt% based on nanocomposite microgel.
[0043] Figure 1 This is a SEM image of the AD-Al nanocomposite hydrogel obtained in this embodiment. Figure 1 It can be observed that the nanocomposite hydrogel has a large number of micron-sized porous structures. Figure 2 This is a SEM image of the surface of basalt fibers coated with the nanocomposite microgel-type wetting agent described in this embodiment.
[0044] Figure 3 This is a graph showing the viscosity of the 1 wt% nanocomposite microgel wetting agent obtained in this embodiment as a function of time. Figure 3 It can be observed that the viscosity of the nanocomposite microgel-type wetting agent remained almost unchanged at around 20.40 mPa / s after being placed at room temperature for seven days. This indicates that the prepared microgel-type wetting agent can be stored stably for a long time, and the microgels do not aggregate, thus exhibiting high economic efficiency.
[0045] Figure 4 The figure shows the particle size test results of the nanocomposite microgel wetting agent in this embodiment. The microgel particles are relatively uniformly distributed in the wetting agent. The particle size with the highest proportion is used as the average particle size, and the average particle size of the microgel particles is 18.17 nm.
[0046] After the sizing agent of this embodiment is coated onto the basalt fiber and dried, the tensile strength of the basalt fiber bundle at room temperature increases from 0.115 N / tex to 0.191 N / tex.
[0047] Figure 5This image shows a physical picture of the basalt fiber modified with microgel impregnator and the polyurethane composite in this embodiment, and the fiber pull-out test results show that when the basalt fiber and polyurethane composite material is pulled out, the fracture mode of the composite material is the fracture on one side of the fiber, while no cracks occur at the interface of the composite material, indicating that the modified basalt fiber and polyurethane have good bonding.
[0048] Figure 6 The effect of varying solid content of different nanocomposite microgel impregnating agents on the reinforcement effect of basalt fibers is shown in the figure. Figure 6 It can be observed that the basalt fiber exhibits an extreme strength after coating when the solid content is 1.0 wt%. Changes in the solid content of the sizing agent lead to changes in viscosity and the proportion of sizing agent by mass. As the solid content increases, both the viscosity and the proportion of sizing agent by mass also increase. When the solid content exceeds 1.0 wt%, the high viscosity of the sizing agent results in high energy consumption, affecting the coating effect and hindering the wetting enhancement of the basalt fiber.
[0049] Example 2
[0050] (A) Add 0.01 g of ammonium persulfate to 10 g of deionized water and stir for 30 min to prepare a 0.1 wt% ammonium persulfate solution. According to the total molar mass fraction of the solution being 3 mol / L, acrylic acid accounting for 10% of the total molar mass, and aluminum hydroxide nanoparticles accounting for 3 wt% of the deionized water solvent, take 0.22 g of acrylic acid, 2.68 g of N,N-dimethylacrylamide, and 0.99 g of aluminum hydroxide sol, respectively, and stir for 30 min under nitrogen bubbling conditions to obtain a prepolymer solution;
[0051] (B) According to the mass ratio of tannic acid to ferric chloride hexahydrate of 1:10, add 0.03 g of tannic acid and 0.3 g of ferric chloride hexahydrate to 10 g of deionized water and stir for 30 min to obtain a redox catalyst;
[0052] (C) Take 2 g of the prepolymer liquid obtained in step (A), add 0.1 g of the redox catalyst obtained in step (B) according to the redox catalyst: prepolymer liquid mass ratio of 1:20, stir quickly and evenly, pour into a mold of a certain shape, the prepolymer liquid gels after 20 s, wait 10 min and take it out to obtain nanocomposite hydrogel;
[0053] (D) The nanocomposite hydrogel obtained in step (C) is pulverized at a speed of 1500 W for 5 min, and then 50 g of deionized water is added to swell it.
[0054] (E) After the gel obtained in step (D) has been swollen, it is further crushed and then 100 g of deionized water is added to swell. This process is repeated once, and deionized water is added to obtain a basalt fiber impregnating agent with a solid content of 1.0 wt% based on nanocomposite microgel.
[0055] After the sizing agent of this embodiment is coated onto the basalt fiber and dried, the tensile strength of the basalt fiber bundle at room temperature increases from 0.115 N / tex to 0.219 N / tex.
[0056] Example 3
[0057] (A) Add 0.01 g of ammonium persulfate to 10 g of deionized water and stir for 30 min to prepare a 0.1 wt% ammonium persulfate solution. According to the total molar mass fraction of the solution being 3 mol / L, acrylic acid accounting for 20% of the total molar mass, and aluminum hydroxide nanoparticles accounting for 3 wt% of the solvent water, take 0.43 g of acrylic acid, 2.38 g of N,N-dimethylacrylamide, and 0.99 g of aluminum hydroxide sol, respectively, and stir for 30 min under nitrogen bubbling conditions to obtain a prepolymer solution;
[0058] (B) According to the mass ratio of tannic acid to ferric chloride hexahydrate of 1:10, add 0.03 g of tannic acid and 0.3 g of ferric chloride hexahydrate to 10 g of deionized water and stir for 30 min to obtain a redox catalyst;
[0059] (C) Take 2 g of the prepolymer liquid obtained in step (A), add 0.1 g of the redox catalyst obtained in step (B) according to the redox catalyst: prepolymer liquid mass ratio of 1:20, stir quickly and evenly, pour into a mold of a certain shape, the prepolymer liquid gels after 20 s, wait 10 min and take it out to obtain nanocomposite hydrogel;
[0060] (D) The nanocomposite hydrogel obtained in step (C) is pulverized at a speed of 1500 W for 5 min, and then 50 g of deionized water is added to swell it.
[0061] (E) After the gel obtained in step (D) has been swollen, it is further crushed and then 100 g of deionized water is added to swell. This process is repeated once, and deionized water is added to obtain a basalt fiber impregnating agent with a solid content of 1.0 wt% based on nanocomposite microgel.
[0062] After the sizing agent of this embodiment is coated onto the basalt fiber and dried, the tensile strength of the basalt fiber bundle at room temperature increases from 0.115 N / tex to 0.204 N / tex.
[0063] Example 4
[0064] (A) Add 0.01 g of ammonium persulfate to 10 g of deionized water and stir for 30 min to prepare a 0.1 wt% ammonium persulfate solution. According to the total molar mass fraction of the solution being 3 mol / L, acrylic acid accounting for 10% of the total molar mass, and aluminum hydroxide nanoparticles accounting for 3 wt% of the deionized water solvent, take 0.22 g of acrylic acid, 2.68 g of N,N-dimethylacrylamide, and 0.99 g of aluminum hydroxide sol, respectively, and stir for 30 min under nitrogen bubbling conditions to obtain a prepolymer solution;
[0065] (B) According to the mass ratio of tannic acid to ferric chloride hexahydrate of 1:10, add 0.03 g of tannic acid and 0.3 g of ferric chloride hexahydrate to 10 g of deionized water and stir for 30 min to obtain a redox catalyst;
[0066] (C) Take 2 g of the prepolymer liquid obtained in step (A), add 0.1 g of the redox catalyst obtained in step (B) according to the redox catalyst: prepolymer liquid mass ratio of 1:20, stir quickly and evenly, pour into a mold of a certain shape, the prepolymer liquid gels in 20 s, wait 10 min and take it out to obtain nanocomposite hydrogel;
[0067] (D) The nanocomposite hydrogel obtained in step (C) is pulverized at a speed of 1500 W for 5 min, and then 50 g of deionized water is added to swell it.
[0068] (E) After the gel obtained in step (D) has been swollen, it is further crushed and then 100 g of deionized water is added to swell. This process is repeated once, and deionized water is added to obtain a basalt fiber impregnating agent with a solid content of 0.8 wt% based on nanocomposite microgel.
[0069] After the sizing agent of this embodiment is coated onto the basalt fiber and dried, the tensile strength of the basalt fiber bundle at room temperature increases from 0.115 N / tex to 0.166 N / tex.
[0070] Example 5
[0071] (A) Add 0.01 g of ammonium persulfate to 10 g of deionized water and stir for 30 min to prepare a 0.1 wt% ammonium persulfate solution. According to the total molar mass fraction of the solution being 3 mol / L, acrylic acid accounting for 10% of the total molar mass, and aluminum hydroxide nanoparticles accounting for 3 wt% of the deionized water solvent, take 0.22 g of acrylic acid, 2.68 g of N,N-dimethylacrylamide, and 0.99 g of aluminum hydroxide sol, respectively, and stir for 30 min under nitrogen bubbling conditions to obtain a prepolymer solution;
[0072] (B) According to the mass ratio of tannic acid to ferric chloride hexahydrate of 1:10, add 0.03 g of tannic acid and 0.3 g of ferric chloride hexahydrate to 10 g of deionized water and stir for 30 min to obtain a redox catalyst;
[0073] (C) Take 2 g of the prepolymer liquid obtained in step (A), add 0.1 g of the redox catalyst obtained in step (B) according to the redox catalyst: prepolymer liquid mass ratio of 1:20, stir quickly and evenly, pour into a mold of a certain shape, the prepolymer liquid gels in 20 s, wait 10 min and take it out to obtain nanocomposite hydrogel;
[0074] (D) The nanocomposite hydrogel obtained in step (C) is pulverized at a speed of 1500 W for 5 min, and then 50 g of deionized water is added to swell it.
[0075] (E) After the gel obtained in step (D) has been swollen, it is further crushed and then 100 g of deionized water is added to swell. This process is repeated once, and deionized water is added to obtain a basalt fiber impregnating agent with a solid content of 1.2 wt% based on nanocomposite microgel.
[0076] After the sizing agent of this embodiment is coated onto the basalt fiber and dried, the tensile strength of the basalt fiber bundle at room temperature increases from 0.115 N / tex to 0.192 N / tex.
[0077] Example 6
[0078] (A) Add 0.01 g of ammonium persulfate to 10 g of deionized water and stir for 30 min to prepare a 0.1% ammonium persulfate solution. According to the total molar mass fraction of the solution being 3 mol / L, acrylic acid accounting for 10% of the total molar mass, and aluminum hydroxide nanoparticles accounting for 3% of the mass fraction of the solvent deionized water, take 0.22 g of acrylic acid, 3.14 g of hydroxyethyl 2-acrylate, and 0.99 g of aluminum hydroxide sol, respectively, and stir for 30 min under nitrogen bubbling conditions to obtain a prepolymer solution;
[0079] (B) According to the mass ratio of tannic acid to ferric chloride hexahydrate of 1:10, add 0.03 g of tannic acid and 0.3 g of ferric chloride hexahydrate to 10 g of deionized water and stir for 30 min to obtain a redox catalyst;
[0080] (C) Take 2 g of the prepolymer liquid obtained in step (A), add 0.1 g of the redox catalyst obtained in step (B) according to the redox catalyst: prepolymer liquid mass ratio of 1:20, stir quickly and evenly, pour into a mold of a certain shape, the prepolymer liquid gels in 20 s, wait 10 min and take it out to obtain nanocomposite hydrogel;
[0081] (D) The nanocomposite hydrogel obtained in step (C) is pulverized at a speed of 1500 W for 5 min, and then 50 g of deionized water is added to swell it.
[0082] (E) After the gel obtained in step (D) has been swollen, it is further crushed and then 100 g of deionized water is added to swell. This process is repeated once, and deionized water is added to obtain a basalt fiber impregnating agent with a solid content of 1.0 wt% based on nanocomposite microgel.
[0083] After the sizing agent of this embodiment is coated onto the basalt fiber and dried, the tensile strength of the basalt fiber bundle at room temperature increases from 0.115 N / tex to 0.172 N / tex.
[0084] In summary, the invention includes, but is not limited to, the above embodiments. Any equivalent substitutions or partial improvements made under the spirit and principles of this invention shall be considered to be within the protection scope of this invention.
Claims
1. A basalt fiber saturant based on nanocomposite microgels, characterized in that: The mass fraction of the nanocomposite microgel is 0.5% to 1.5% based on the total mass of the infiltrant being 100%, and the balance is water with a deionized water purity; The nanocomposite microgel has a particle size of 10 nm to 20 nm and is obtained by crushing and swelling the nanocomposite hydrogel; The nanocomposite hydrogel is obtained by free radical in-situ polymerization of acrylic polymer monomers, an initiator, a physical crosslinking agent, a redox catalyst, and water with a deionized water purity; The acrylic polymer monomers are one or more of acrylic acid, N,N-dimethyl acrylamide, 2-hydroxyethyl acrylate, and acrylamide; the initiator is ammonium persulfate and / or potassium persulfate; and the physical crosslinking agent is nano-aluminum hydroxide sol, nano-clay, or aluminum oxide nanoparticles.
2. A basalt fiber saturant based on nanocomposite microgels according to claim 1, characterized in that: The mass fraction of the nanocomposite microgel is 0.8% to 1.2%.
3. A method of preparing a basalt fiber saturant based on nanocomposite microgels according to claim 1 or 2, characterized by: The method comprises the following steps: (1) Dissolve the initiator in water with a deionized water purity, then add the acrylic polymer monomers and the physical crosslinking agent, and stir until uniform to obtain a pre-polymer solution; (2) Add the redox catalyst to the pre-polymer solution, mix well, then pour into a mold, and in-situ polymerize and stand to obtain a nanocomposite hydrogel; (3) Crush the nanocomposite hydrogel, swell with water with a deionized water purity, and repeat the crushing and swelling to obtain a basalt fiber infiltrant based on the nanocomposite microgel.
4. A method of preparing a basalt fiber saturant based on nanocomposite microgels according to claim 3, characterized in that: In step (1), the acrylic polymer monomers are acrylic acid, N,N-dimethyl acrylamide, 2-hydroxyethyl acrylate, or acrylamide; the initiator is ammonium persulfate and / or potassium persulfate; and the physical crosslinking agent is nano-aluminum hydroxide sol, nano-clay, or aluminum oxide nanoparticles.
5. A method of preparing a basalt fiber saturant based on nanocomposite microgels according to claim 4, characterized in that: In step (1), the mass fraction of the initiator in the pre-polymer solution is 0.05% to 0.2%; the total molar concentration of the pre-polymer solution is 2 to 6 mol / L, and the molar fraction of the acrylic polymer monomers is 5% to 25%; and the mass fraction of the physical crosslinking agent in water is 1% to 5%.
6. A method of preparing a basalt fiber saturant based on nanocomposite microgels according to claim 3, characterized in that: In step (2), the redox catalyst is a mixed aqueous solution of tannic acid and ferric chloride hexahydrate, the mass fraction of ferric chloride hexahydrate in the redox catalyst is 2% to 6%, the mass ratio of tannic acid to ferric chloride hexahydrate is 10 to 30:1, and the mass ratio of the pre-polymer solution to the redox catalyst is 10 to 100:
1.
7. A method of preparing a basalt fiber saturant based on nanocomposite microgels according to claim 3, characterized in that: In step (1), the stirring time is 15 min to 30 min; in step (2), the in-situ polymerization time is 20 s to 30 s, and the standing time is 2 min to 10 min.
8. A method of preparing a basalt fiber saturant based on nanocomposite microgels according to claim 3, characterized in that: In step (3), the crushing power is 1200 W to 2000 W, and the crushing time is 5 min to 10 min; when swelling, the mass of the added water is 3 times to 5 times the mass of the nanocomposite hydrogel.
Citation Information
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Basalt fiber reinforced impregnating agent and preparation method thereof
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