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CN-122010425-A - Preparation method of modified basalt fiber, modified basalt fiber and application

CN122010425ACN 122010425 ACN122010425 ACN 122010425ACN-122010425-A

Abstract

The invention belongs to the technical field of fiber reinforced composite materials, and relates to a preparation method of modified basalt fiber, modified basalt fiber and application, wherein the preparation method comprises the following steps that S1, basalt fiber is placed in a reactor, silicon tetrafluoride gas is introduced for etching treatment, and etched basalt fiber is obtained; and S2, performing radio frequency magnetron sputtering treatment by taking the etched basalt fiber as a substrate and taking titanium dioxide or zirconium dioxide as a target material, and then performing annealing treatment to obtain surface-coated basalt fiber, and S3, immersing the surface-coated basalt fiber into a sizing agent, taking out, and drying and curing to obtain the modified basalt fiber. The method ensures that the modified basalt fiber can obviously improve the key performance index of asphalt concrete after being applied to the asphalt concrete.

Inventors

  • ZHENG YI
  • ZHENG BIAO

Assignees

  • 北京玄泽新材料科技有限公司

Dates

Publication Date
20260512
Application Date
20260214

Claims (10)

  1. 1. The preparation method of the modified basalt fiber is characterized by comprising the following steps of: s1, surface etching treatment, namely placing basalt fibers in a reactor, and introducing silicon tetrafluoride gas to carry out etching treatment to obtain etched basalt fibers; s2, performing surface sputtering coating treatment, namely performing radio frequency magnetron sputtering treatment by taking the etched basalt fiber as a substrate and titanium dioxide or zirconium dioxide as a target material, and then performing annealing treatment to obtain the surface coating basalt fiber; and S3, soaking the basalt fiber with the surface coating into a sizing agent, taking out, and drying and curing to obtain the modified basalt fiber.
  2. 2. The method according to claim 1, wherein in the step S1, the etching treatment is performed at 130-140 ℃ for 40-60 min and/or, The flow rate of the silicon tetrafluoride gas is 100-150 mL/min, and/or, And step S1, washing the etched basalt fiber for 2-3 times by using deionized water.
  3. 3. The method of claim 1, wherein in step S2, the power of the RF magnetron sputtering is 150-200W, the sputtering time is 30-60min, and/or, The annealing treatment temperature is 500-600 ℃, the annealing time is 1-2 h, and/or, After the radio frequency magnetron sputtering and annealing treatment, the thickness of the titanium dioxide or zirconium dioxide nano coating formed on the surface of the etched basalt fiber is 200-300 nm, preferably 220-250 nm, and/or, In the step S3, the immersion time of the immersion treatment is 12-15 h, and/or, The temperature of the drying and curing is 100-150 ℃ and the time is 10-15 h, and/or, The mass ratio of basalt fiber raw materials to the sizing agent is 1 (5-10).
  4. 4. The preparation method according to claim 1, wherein in the step S3, the impregnating compound comprises, by weight, 3% -6% of film forming agent 1, 2% -5% of film forming agent 2, 5% -8% of polyvinyl acetate, 0.1% -1% of surfactant, 0.2% -1.2% of silane coupling agent, 1% -2% of pH regulator, 0.2% -0.4% of antistatic agent, 0.2% -0.5% of lubricant and the balance deionized water, preferably, the solid content of the film forming agent 1 is 40-50wt%, the solid content of the film forming agent 2 is 25-35wt%, and the mass concentration of the pH regulator is 25-30%.
  5. 5. The process according to claim 4, wherein the film-forming agent 1 is an epoxy resin emulsion, and/or, The film forming agent 2 is acrylate emulsion, and/or, The silane coupling agent is an amino silane coupling agent or an epoxy silane coupling agent, preferably one or more of gamma-aminopropyl triethoxy silane, gamma-glycidol ether oxypropyl trimethoxy silane and gamma-methacryloxy propyl trimethoxy silane, and/or, The pH regulator is organic amine or ammonia water, and/or, The antistatic agent is polyquaternium or ammonium chloride, and/or, The surfactant is a mixture of fatty alcohol polyoxyethylene ether and sodium stearyl sulfate or a polyoxypropylene-polyoxyethylene block copolymer, and/or, The lubricant is an organosilicon lubricant; preferably, the polyquaternium is selected from dodecyl dimethyl benzyl ammonium chloride, octadecyl trimethyl ammonium chloride or hexadecyl trimethyl ammonium bromide.
  6. 6. The preparation method of the sizing agent according to claim 4 or 5, wherein the preparation method comprises the steps of adding the pH regulator and the silane coupling agent into part of deionized water, uniformly stirring, adding the film forming agent 1, the film forming agent 2 and the polyvinyl acetate, stirring for 15-20 min, adding the antistatic agent, the lubricant, the surfactant and the rest of deionized water, continuously stirring for 15-20 min, and performing ultrasonic vibration for 20-30 min, wherein the pH value of the sizing agent is 7-8.
  7. 7. A modified basalt fiber produced by the production method according to any one of claims 1 to 6.
  8. 8. The modified basalt fiber according to claim 7, wherein the surface of the modified basalt fiber is sequentially provided with a roughened etching layer formed by etching silicon tetrafluoride, a titanium dioxide or zirconium dioxide nano-coating deposited by radio frequency magnetron sputtering and subjected to annealing treatment, and an organic composite film layer formed by curing the impregnating compound from inside to outside.
  9. 9. Use of the modified basalt fiber of claim 7 or 8 in asphalt concrete.
  10. 10. The use according to claim 9, wherein the modified basalt fiber is added to asphalt concrete in a chopped form, the fiber length is 6-12 mm, and the mixing amount in the asphalt concrete is 0.2% -0.5% of the total mass of the asphalt mixture.

Description

Preparation method of modified basalt fiber, modified basalt fiber and application Technical Field The invention belongs to the technical field of fiber reinforced composite materials, and relates to a preparation method of modified basalt fibers, the modified basalt fibers and application thereof. Background In the field of road engineering, asphalt concrete is widely used for its good driving comfort and maintainability. However, the temperature change and the long-term action of the vehicle load are easy to generate temperature cracks, fatigue cracks, ruts and other diseases, and the service life of the road and the driving safety are seriously influenced. In order to improve the performance of asphalt concrete, the fiber is added to become an effective reinforcing and toughening means. The basalt fiber is used as an inorganic fiber prepared by melting and drawing natural basalt ores, has the advantages of high strength, high temperature resistance, corrosion resistance, good compatibility with asphalt and the like, and is regarded as an asphalt concrete reinforcing material with great potential. In theory, the addition of basalt fiber can improve the toughness of asphalt cement and disperse stress through bridging and crack resistance, so that crack initiation and expansion are inhibited, and the high-temperature rutting resistance and low-temperature crack resistance of the mixture are improved. However, in practice it has been found that the interfacial bond between untreated basalt fibers and the asphalt concrete matrix tends to be weak. The main reasons are that the basalt fiber surface is smooth and inert, the wettability and the binding power of the basalt fiber with asphalt are insufficient, and the asphalt concrete is in a weak alkaline environment in the service process, so that slow corrosion can be generated on the fiber surface, and the interface strength is further weakened. In addition, in the high Wen Banhe and construction process of the asphalt mixture, the fibers are easy to agglomerate or break due to friction and static electricity, so that the fibers are unevenly dispersed in a matrix, and the reinforcing effect of the asphalt mixture is difficult to fully develop. In the prior art, the sizing agent is generally adopted to carry out surface treatment on basalt fibers so as to improve the bundling property and the dispersibility of the basalt fibers and the cohesiveness of the basalt fibers with asphalt concrete. However, conventional treating with sizing agents focuses on physical wrapping and static elimination, and has limited changes in physicochemical properties of the fiber surface itself, and the formed interface bonding layer has insufficient long-term stability under complex stress and alkaline environments, and it is difficult to significantly improve performance indexes (durability, low-temperature flexibility and high-temperature stability under freeze-thawing environments) for critical roads. There are also studies on attempts to perform single chemical etching or physical coating treatment on the fibers to increase surface roughness or activity, but these methods often have complicated processes, single modification effects, or difficulty in ensuring the bulk strength of the fibers, so that after the fibers are applied to asphalt concrete, key performance indexes (durability, low-temperature flexibility and high-temperature stability) of the asphalt concrete cannot be significantly improved. Therefore, developing a method for improving the surface characteristics of basalt fibers, so that the modified basalt fibers can obviously improve key performance indexes (durability, low-temperature flexibility and high-temperature stability in a freeze thawing environment) of asphalt concrete after being applied to the asphalt concrete, is a technical problem to be solved in the field. Disclosure of Invention The invention aims to provide a preparation method of modified basalt fiber, the modified basalt fiber and application of the modified basalt fiber in asphalt concrete. According to the method, basalt fibers are sequentially subjected to silicon tetrafluoride etching, titanium dioxide or zirconium dioxide magnetron sputtering and infiltration treatment, and a composite structure of a rough etching layer, an inorganic coating and an organic functional film is constructed on the surfaces of the fibers. After the modified basalt fiber is applied to asphalt concrete, key performance indexes (durability under a freeze thawing environment, asphalt leaching rate in a construction process, low-temperature flexibility and high-temperature stability) of the asphalt concrete can be obviously improved. In order to achieve the above purpose, the present invention adopts the following technical scheme: In a first aspect, the invention provides a method for preparing modified basalt fiber, comprising the following steps: s1, surface etching treatment, namely placing basalt fibers in a reac