CN108249798B - Modification method of polyvinyl alcohol fiber for high-ductility cement-based composite material - Google Patents
Modification method of polyvinyl alcohol fiber for high-ductility cement-based composite material Download PDFInfo
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- CN108249798B CN108249798B CN201810026429.6A CN201810026429A CN108249798B CN 108249798 B CN108249798 B CN 108249798B CN 201810026429 A CN201810026429 A CN 201810026429A CN 108249798 B CN108249798 B CN 108249798B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/10—Coating or impregnating
- C04B20/12—Multiple coating or impregnating
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Abstract
The invention provides a method for modifying polyvinyl alcohol fibers for a high-ductility cement-based composite material. Because the surface of the polyvinyl alcohol fiber contains a large number of hydroxyl groups, the hydroxyl groups on the surface of the polyvinyl alcohol fiber can react with the cement matrix to form strong chemical bonding force, and the strong chemical bonding force can cause the fiber to be pulled off in the pulling-out process, thereby influencing the exertion of ductility. The method comprises the steps of taking polyvinyl alcohol fiber as a raw material, firstly coating a layer of epoxy resin on the surface of the polyvinyl alcohol fiber, and then coating a layer of fumed silica powder on the surface of the epoxy resin coating; the surface of the modified polyvinyl alcohol fiber is hydrophobic, so that the interface strength of the polyvinyl alcohol fiber and a cement matrix can be effectively weakened, the chemical bonding force is reduced, and the polyvinyl alcohol fiber is pulled out of the cement matrix and cannot be pulled off in the stretching process; the hydrophobic performance and the wear-resistant sliding performance of the product are more stable, the coating is more wear-resistant, and the original physical and mechanical properties of the PVA fiber cannot be influenced.
Description
Technical Field
The invention relates to the technical field of modification of composite materials, in particular to a method for modifying polyvinyl alcohol fibers on the surface of a high-ductility cement-based composite material by using epoxy resin and hydrophobic fumed silica as coatings.
Background
The high-ductility cement-based composite material is a novel fiber reinforced cement-based composite material developed in recent 20 years. The high-ductility cement-based composite material is prepared by considering fiber performance, matrix performance and fiber-matrix interface characteristics based on micro-mechanics, fracture mechanics and statistical basic principles through system design and performance optimization. It has multi-slit crack characteristics and strain hardening properties as well as excellent crack control capability. When the high-ductility cement-based composite material is subjected to bending and tensile loads, the fracture can stably extend due to the bridging effect of fibers at the fracture and stress transmission between the fibers and a matrix, so that the high-ductility cement-based composite material shows obvious multi-fracture cracking characteristics and strain hardening behaviors. Therefore, compared with the traditional fiber reinforced cement-based composite material, the composite material has better mechanical property and durability.
The polyvinyl alcohol fiber is regarded as the most suitable fiber for preparing the high-ductility cement-based composite material due to high strength and high elastic modulus and relatively reduced price, but the polyvinyl alcohol fiber has a large amount of hydroxyl groups on the surface and has strong affinity with cement, and the polyvinyl alcohol fiber is pulled out instead of being pulled out in the pulling process due to strong adhesive force between the polyvinyl alcohol fiber and a cement matrix. Resulting in a high ductility cement-based composite material whose properties will be severely affected.
At present, in order to adjust the interface performance of polyvinyl alcohol fibers and a cement matrix, an oil agent (such as Chinese patent application No. 201210468413.3) is generally coated on the surfaces of the polyvinyl alcohol fibers, on one hand, the oil agent easily enters the cement matrix to influence the performance of the cement matrix, and on the other hand, an oil film coating is easily separated during the molding and stirring process of the oil agent coated on the surfaces of the fibers; for example, in the patent (chinese patent application No. 201610375068.7), a strong oxidant potassium permanganate is used to oxidize the surface of the polyvinyl alcohol fiber to make the surface of the polyvinyl alcohol fiber rough, and then a layer of hydrophobic substance is coated on the surface of the polyvinyl alcohol fiber, which may damage the surface of the polyvinyl alcohol fiber and reduce the performance of the fiber, and meanwhile, the hydrophobic coating only depends on the physical adsorption force between the coating and the surface of the fiber, and the stability cannot be guaranteed to solve the problem.
Disclosure of Invention
Aiming at the existing problems, the invention aims to provide a method for modifying the surface of polyvinyl alcohol fiber by taking epoxy resin and hydrophobic fumed silica as coatings, which can well regulate and control the interface performance of the polyvinyl alcohol fiber and a cement matrix, can ensure the stability of the coatings, and can not damage the fiber per se.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a modification method of polyvinyl alcohol fiber for high-ductility cement-based composite material is provided, wherein the method comprises the steps of taking polyvinyl alcohol fiber as a raw material, firstly coating a layer of epoxy resin on the surface of the polyvinyl alcohol fiber, and then coating a layer of fumed silica powder on the surface of the epoxy resin coating; the modification can effectively weaken the interface strength of the polyvinyl alcohol fiber and the cement matrix, and the polyvinyl alcohol fiber is pulled out of the cement matrix and cannot be pulled off in the stretching process; the surface of the modified polyvinyl alcohol fiber is hydrophobic, so that the chemical bonding force between the fiber and a cement matrix is reduced, and the ductility performance of the high-ductility cement-based composite material is better exerted.
The epoxy resin is coated on the surface of the polyvinyl alcohol fiber in a solvent soaking mode, so that the epoxy resin can be uniformly coated on the surface of the fiber in the solvent soaking mode, and the coating amount of the epoxy resin is easy to control; the coating amount of the epoxy resin is 5-15% of the mass of the polyvinyl alcohol fiber, the epoxy resin is used for increasing the bonding between the nano fumed silica and the polyvinyl alcohol fiber, so that the bonding between the nano fumed silica and the polyvinyl alcohol fiber is more stable and is not easy to fall off, the original physical and mechanical properties of the polyvinyl alcohol fiber can not be influenced, the coating amount of the epoxy resin is too low, the bonding between the nano fumed silica and the polyvinyl alcohol fiber can be insufficient, and the excessive high coating amount of the epoxy resin can cause the excessive high viscosity of the fibers and is not beneficial to the dispersion of the fibers.
The fumed silica powder is coated on the surface of the epoxy resin coating in a mechanical stirring manner, the mechanical stirring manner is simple and easy to operate, the hydrophobic fumed silica can be stably attached to the surface under the condition that the epoxy resin coating is not damaged, and the epoxy resin coating can be damaged if the solution soaking manner is adopted; the coating amount of the fumed silica powder is 10-50% of the mass of the polyvinyl alcohol fiber, and when the coating amount of the epoxy resin is 5-15% of the mass of the polyvinyl alcohol fiber, the coating amount of the corresponding fumed silica powder is 10-50% of the mass of the polyvinyl alcohol fiber; the coating amount of the fumed silica powder depends on the coating amount of the epoxy resin.
The fumed silica powder is hydrophobic nano fumed silica powder, and the particle size of the fumed silica powder is 7-40 nm; the adoption of the fumed silica powder ensures the stability of the coating and does not damage the fiber; meanwhile, the surface hydrophobic property and the wear-resistant sliding property of the polyvinyl alcohol fiber are more stable, the coating is more wear-resistant, and the original physical and mechanical properties of the PVA fiber cannot be influenced.
The invention provides a method for modifying polyvinyl alcohol fibers for a high-ductility cement-based composite material, which is characterized by comprising the following steps of:
1) preparing a pretreatment solution of epoxy resin by using an organic solvent, wherein the mass fraction of the epoxy resin is 2-10%;
2) soaking the raw material polyvinyl alcohol fiber in a pretreatment solution of epoxy resin at the temperature of 50-60 ℃ for 2-3 h;
3) taking out the polyvinyl alcohol fiber treated in the step 2), and vacuumizing and drying the polyvinyl alcohol fiber to constant weight by using a vacuum drying oven, wherein the drying temperature is 50-60 ℃, and the drying time is 12-24 h;
4) and 3) mechanically stirring and mixing the polyvinyl alcohol fiber treated in the step 3) and fumed silica, wherein the stirring speed is 1000-3000 r/min, and the stirring time is 2-3 h.
In the operation process of the step 1), the organic solvent is one or a mixture of more of acetone, toluene, benzene and alcohol; the pretreatment liquid of the epoxy resin prepared by the organic solvent can more uniformly coat the epoxy resin on the surface of the polyvinyl alcohol fiber.
The invention has the advantages that: the surface modification of the polyvinyl alcohol fiber with the epoxy resin-hydrophobic fumed silica coating can effectively weaken the interface strength of the polyvinyl alcohol fiber and the cement matrix, and the polyvinyl alcohol fiber is pulled out of the cement matrix and cannot be pulled off in the stretching process. The surface of the modified polyvinyl alcohol fiber is hydrophobic, so that the chemical bonding force between the fiber and a cement matrix is reduced, the surface hydrophobic property and the wear-resistant sliding property of the polyvinyl alcohol fiber are more stable, the coating is more wear-resistant, and the original physical and mechanical properties of the PVA fiber cannot be influenced. And is more beneficial to the exertion of the ductility performance of the high-ductility cement-based composite material.
The contact angle of the modified polyvinyl alcohol fiber can reach 140-150 degrees, the interfacial property of the polyvinyl alcohol fiber and a cement matrix is effectively regulated and controlled, and the ductility of the polyvinyl alcohol fiber high-ductility cement-based composite material is improved; the modification method has the advantages of simple operation, easy control of coating amount, low cost and continuous and stable industrial production, so the technical method has great application prospect.
Drawings
FIG. 1 is a surface topography of unmodified polyvinyl alcohol fibers;
FIG. 2 shows the surface morphology of modified polyvinyl alcohol fibers;
figure 3 is a contact angle test of polyvinyl alcohol fibers after modification.
Wherein acc.v represents an acceleration voltage; spot represents the beam Spot size; magn stands for magnification; det represents the probe; SE represents a secondary electron; WD represents the working distance; CA Left represents the sitting contact angle; CA Right represents the Right contact angle;
μ m stands for unit micron.
Detailed Description
The invention is described in further detail below with reference to the following description of the drawings and the detailed description.
Example 1: a method for modifying polyvinyl alcohol fiber used for high-ductility cement-based composite material.
1) Preparing an epoxy resin pretreatment solution; preparing diluted epoxy resin pretreatment liquid, wherein alcohol is selected as an epoxy resin diluent, and the mass fraction of the epoxy resin is 5%.
2) Soaking polyvinyl alcohol fiber in epoxy resin pretreatment liquid; soaking untreated polyvinyl alcohol fibers in epoxy resin pretreatment liquid at the temperature of 50 ℃ for 3 hours.
3) Drying the pretreated polyvinyl alcohol fibers; and taking out the polyvinyl alcohol fiber soaked in the epoxy resin pretreatment solution, and vacuumizing and drying the polyvinyl alcohol fiber to constant weight by using a vacuum drying oven at the drying temperature of 50 ℃.
4) Coating hydrophobic fumed silica on the surface of the polyvinyl alcohol fiber; and mechanically stirring and mixing the dried polyvinyl alcohol fibers and the hydrophobic nano fumed silica, wherein the particle size of the polyvinyl alcohol fibers is 7-40nm, stirring and mixing the polyvinyl alcohol fibers and the hydrophobic nano fumed silica by using an electric stirrer, the stirring speed is 2000 rpm, and the mechanical stirring and mixing time is 2 hours.
The product is as follows: the contact angle of the modified polyvinyl alcohol fiber can reach 142 degrees, the coating amount of the epoxy coating is 11 percent, and the coating amount of the hydrophobic nano fumed silica coating reaches 40 percent. The surface of the modified polyvinyl alcohol fiber is uniformly coated with a layer of epoxy resin-nano fumed silica coating, so that the interface performance of the fiber and a cement matrix can be effectively improved.
Example 2: a method for modifying polyvinyl alcohol fiber used for high-ductility cement-based composite material.
1) Preparing an epoxy resin pretreatment solution; preparing a diluted epoxy resin pretreatment solution, wherein acetone is selected as an epoxy resin diluent, and the mass fraction of the epoxy resin is 2%.
2) Soaking polyvinyl alcohol fiber in epoxy resin pretreatment liquid; soaking untreated polyvinyl alcohol fibers in epoxy resin pretreatment liquid at the temperature of 60 ℃ for 2 hours.
3) Drying the pretreated polyvinyl alcohol fibers; and taking out the polyvinyl alcohol fiber soaked in the epoxy resin pretreatment solution, and vacuumizing and drying the polyvinyl alcohol fiber to constant weight by using a vacuum drying oven at the drying temperature of 60 ℃.
4) Coating hydrophobic fumed silica on the surface of the polyvinyl alcohol fiber; and mechanically stirring and mixing the dried polyvinyl alcohol fibers and the hydrophobic nano fumed silica, and stirring and mixing by adopting an electric stirrer, wherein the stirring speed is 1000 revolutions per minute, and the mechanical stirring and mixing time is 3 hours.
The product is as follows: the contact angle of the modified polyvinyl alcohol fiber can reach 140 degrees, the coating amount of the epoxy coating is 5 percent, and the coating amount of the hydrophobic nano fumed silica coating reaches 20 percent. The surface of the modified polyvinyl alcohol fiber is uniformly coated with a layer of epoxy resin-nano fumed silica coating, so that the interface performance of the fiber and a cement matrix can be effectively improved.
Example 3: a method for modifying polyvinyl alcohol fiber used for high-ductility cement-based composite material.
1) Preparing an epoxy resin pretreatment solution; preparing diluted epoxy resin pretreatment liquid, wherein alcohol is selected as an epoxy resin diluent, and the mass fraction of the epoxy resin is 6%.
2) Soaking polyvinyl alcohol fiber in epoxy resin pretreatment liquid; soaking untreated polyvinyl alcohol fibers in epoxy resin pretreatment liquid at the temperature of 60 ℃ for 3 hours.
3) Drying the pretreated polyvinyl alcohol fibers; and taking out the polyvinyl alcohol fiber soaked in the epoxy resin pretreatment solution, and vacuumizing and drying the polyvinyl alcohol fiber to constant weight by using a vacuum drying oven at the drying temperature of 60 ℃.
4) Coating hydrophobic fumed silica on the surface of the polyvinyl alcohol fiber; and mechanically stirring and mixing the dried polyvinyl alcohol fibers and the hydrophobic nano fumed silica, and stirring and mixing by adopting an electric stirrer at a stirring speed of 1500 revolutions per minute for 3 hours.
The product is as follows: the contact angle of the modified polyvinyl alcohol fiber can reach 145 degrees, the coating amount of the epoxy coating is 12 percent, and the coating amount of the hydrophobic nano fumed silica coating reaches 40 percent. The surface of the modified polyvinyl alcohol fiber is uniformly coated with a layer of epoxy resin-nano fumed silica coating, so that the interface performance of the fiber and a cement matrix can be effectively improved.
Example 4: a method for modifying polyvinyl alcohol fiber used for high-ductility cement-based composite material.
1) Preparing an epoxy resin pretreatment solution; preparing a diluted epoxy resin pretreatment solution, wherein toluene is selected as an epoxy resin diluent, and the mass fraction of the epoxy resin is 10%.
2) Soaking polyvinyl alcohol fiber in epoxy resin pretreatment liquid; soaking untreated polyvinyl alcohol fibers in epoxy resin pretreatment liquid at the temperature of 60 ℃ for 2 hours.
3) Drying the pretreated polyvinyl alcohol fibers; and taking out the polyvinyl alcohol fiber soaked in the epoxy resin pretreatment solution, and vacuumizing and drying the polyvinyl alcohol fiber to constant weight by using a vacuum drying oven at the drying temperature of 60 ℃.
4) Coating hydrophobic fumed silica on the surface of the polyvinyl alcohol fiber; and mechanically stirring and mixing the dried polyvinyl alcohol fibers and the hydrophobic nano fumed silica, and stirring and mixing by adopting an electric stirrer, wherein the stirring speed is 3000 r/min, and the mechanical stirring and mixing time is 2 hours.
The product is as follows: the contact angle of the modified polyvinyl alcohol fiber can reach 150 degrees, the coating amount of the epoxy coating is 15 percent, and the coating amount of the hydrophobic nano fumed silica coating reaches 50 percent. The surface of the modified polyvinyl alcohol fiber is uniformly coated with a layer of epoxy resin-nano fumed silica coating, so that the interface performance of the fiber and a cement matrix can be effectively improved.
Example 5: a method for modifying polyvinyl alcohol fiber used for high-ductility cement-based composite material.
1) Preparing an epoxy resin pretreatment solution; preparing diluted epoxy resin pretreatment liquid, wherein alcohol is selected as an epoxy resin diluent, and the mass fraction of the epoxy resin is 2%.
2) Soaking polyvinyl alcohol fiber in epoxy resin pretreatment liquid; soaking untreated polyvinyl alcohol fibers in epoxy resin pretreatment liquid at the temperature of 60 ℃ for 3 hours.
3) Drying the pretreated polyvinyl alcohol fibers; and taking out the polyvinyl alcohol fiber soaked in the epoxy resin pretreatment solution, and vacuumizing and drying the polyvinyl alcohol fiber to constant weight by using a vacuum drying oven at the drying temperature of 60 ℃.
4) Coating hydrophobic fumed silica on the surface of the polyvinyl alcohol fiber; and mechanically stirring and mixing the dried polyvinyl alcohol fibers and the hydrophobic nano fumed silica, and stirring and mixing by adopting an electric stirrer at a stirring speed of 1500 revolutions per minute for 3 hours.
The product is as follows: the contact angle of the modified polyvinyl alcohol fiber can reach 130 degrees, the coating amount of the epoxy coating is 5 percent, and the coating amount of the hydrophobic nano fumed silica coating reaches 35 percent. Although the modified polyvinyl alcohol fiber can have a hydrophobic effect, the hydrophobic nano fumed silica coating has insufficient adhesion with the fiber due to the small amount of the epoxy coating, and the modified fiber coating has insufficient stability and is easy to fall off.
Example 6: a method for modifying polyvinyl alcohol fiber used for high-ductility cement-based composite material.
1) Preparing an epoxy resin pretreatment solution; preparing diluted epoxy resin pretreatment liquid, wherein alcohol is selected as an epoxy resin diluent, and the mass fraction of the epoxy resin is 20%.
2) Soaking polyvinyl alcohol fiber in epoxy resin pretreatment liquid; soaking untreated polyvinyl alcohol fibers in epoxy resin pretreatment liquid at the temperature of 60 ℃ for 3 hours.
3) Drying the pretreated polyvinyl alcohol fibers; and taking out the polyvinyl alcohol fiber soaked in the epoxy resin pretreatment solution, and vacuumizing and drying the polyvinyl alcohol fiber to constant weight by using a vacuum drying oven at the drying temperature of 60 ℃.
4) Coating hydrophobic fumed silica on the surface of the polyvinyl alcohol fiber; and mechanically stirring and mixing the dried polyvinyl alcohol fibers and the hydrophobic nano fumed silica, and stirring and mixing by adopting an electric stirrer at a stirring speed of 1500 revolutions per minute for 3 hours.
The product is as follows: the contact angle of the modified polyvinyl alcohol fiber can reach 145 degrees, the coating amount of the epoxy coating is 20 percent, and the coating amount of the hydrophobic nano fumed silica coating reaches 55 percent. Although the modified polyvinyl alcohol fibers have a hydrophobic effect, the polyvinyl alcohol fibers are too strongly bonded to each other and are difficult to disperse due to an excessive amount of the epoxy coating.
It should be noted that the above-mentioned embodiments are merely preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and any combination or equivalent changes made on the basis of the above-mentioned embodiments are also within the scope of the present invention.
Claims (5)
1. A modification method of polyvinyl alcohol fiber for high-ductility cement-based composite material is characterized in that the polyvinyl alcohol fiber is used as a raw material, firstly a layer of epoxy resin is coated on the surface of the polyvinyl alcohol fiber, and then a layer of hydrophobic fumed silica powder is coated on the surface of the epoxy resin coating; the method comprises the following steps:
1) preparing a pretreatment solution of epoxy resin by using an organic solvent, wherein the mass fraction of the epoxy resin is 2-10%;
2) soaking the raw material polyvinyl alcohol fiber in a pretreatment solution of epoxy resin at the temperature of 50-60 ℃ for 2-3 h;
3) taking out the polyvinyl alcohol fiber treated in the step 2), and vacuumizing and drying the polyvinyl alcohol fiber to constant weight by using a vacuum drying oven, wherein the drying temperature is 50-60 ℃, and the drying time is 12-24 h;
4) and 3) mechanically stirring and mixing the polyvinyl alcohol fiber treated in the step 3) and fumed silica, wherein the stirring speed is 1000-3000 r/min, and the stirring time is 2-3 h.
2. The method of claim 1, wherein the epoxy resin is coated in an amount of 5 to 15% by mass based on the polyvinyl alcohol fiber.
3. The method of claim 1, wherein the fumed silica powder is coated in an amount of 10 to 50% by mass of the polyvinyl alcohol fiber.
4. The method for modifying polyvinyl alcohol fibers for high ductility cement-based composite material as claimed in claim 1, wherein the fumed silica is hydrophobic nano fumed silica, and the particle size is 7-40 nm.
5. The method for modifying polyvinyl alcohol fiber for high ductility cement-based composite material as claimed in claim 1, wherein the organic solvent is selected from one or a mixture of acetone, toluene, benzene, and alcohol during the operation of step 1).
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| CN110700041A (en) * | 2019-08-28 | 2020-01-17 | 维特国际新材料（武汉）有限公司 | Highway construction and maintenance method based on cement-based composite material |
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| CN113816684A (en) * | 2021-09-30 | 2021-12-21 | 上海市建筑科学研究院有限公司 | Ultra-high-ductility cement-based composite material for anti-permeability reinforcement and preparation method thereof |
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