CN109626881B - Micro-nano fiber reinforced concrete and preparation method thereof - Google Patents
Micro-nano fiber reinforced concrete and preparation method thereof Download PDFInfo
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- CN109626881B CN109626881B CN201811557424.2A CN201811557424A CN109626881B CN 109626881 B CN109626881 B CN 109626881B CN 201811557424 A CN201811557424 A CN 201811557424A CN 109626881 B CN109626881 B CN 109626881B
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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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
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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
- C04B16/00—Use of organic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of organic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B16/04—Macromolecular compounds
- C04B16/10—Treatment for enhancing the mixability with the mortar
Abstract
The invention discloses micro-nano fiber reinforced concrete which comprises micro fibers with first hydrophilic groups on the surfaces and nano fibers with second hydrophilic groups on the surfaces, wherein the content of the micro fibers in the concrete is set to be 2-5%, and the content of the nano fibers in the concrete is set to be 5-10%. The nano-fiber refines large pores by filling the pore structure between cement hydration products, improves the pore structure inside concrete, makes the microstructure of the concrete more compact, and effectively limits the formation of harmful pores. The reinforced concrete obtained by blending the micro-fibers, the nano-fibers and the cement overcomes the characteristic of multi-scale fracture, the nano-fibers and the micro-fibers with hydrophilic groups and high elastic modulus on the surfaces greatly improve the mechanical property of the concrete, and the addition of the additive further enhances the mechanical property and durability of the concrete, so that the micro-nano fiber reinforced concrete with high bending resistance, high strength and high toughness is obtained.
Description
Technical Field
The application belongs to the technical field of building materials, and particularly relates to micro-nano fiber reinforced concrete and a preparation method thereof.
Background
Concrete is widely applied to the engineering field as the most widely used geotechnical material in the world, but the traditional concrete has the defects of poor crack resistance, low toughness, obvious brittleness and the like, influences the appearance and the service life of a building to a certain extent, and most importantly seriously threatens the life and property safety of people. In order to reduce the accident problem caused by the defects of the concrete material, the quality of the concrete needs to be improved comprehensively.
The strength and toughness of concrete are usually improved by adding mineral, fiber and polymer materials, but no concrete with high bending resistance exists at present. Although the fiber is an ideal concrete reinforcing material, the fiber is easy to agglomerate in the doping process, so that the binding force between the fiber and the base material is greatly influenced, and the mechanical property of the concrete is influenced.
Disclosure of Invention
At least aiming at one of the problems, the invention discloses micro-nano fiber reinforced concrete, which comprises the following components in part by weight:
a microfiber having a surface with a first hydrophilic group;
a nanofiber having a second hydrophilic group on a surface thereof;
wherein the content of the micro-fibers in the concrete is set to be 2-5%, and the content of the nano-fibers in the concrete is set to be 5-10%.
Further, the first hydrophilic group includes an amino group, a carboxyl group, an amide group, or a hydroxyl group, and the second hydrophilic group includes an amino group, a carboxyl group, an amide group, or a hydroxyl group. Further, the nanofibers comprise at least one of thermoplastic polyurethane fibers, polystyrene fibers, fluorinated thermoplastic polyurethane fibers, polydimethylsiloxane, or carbon fibers.
Furthermore, the diameter of the nanofiber is 50-500 nm, and the porosity is 70-80%.
Further, the micro fibers comprise at least one of polyethylene fibers, ultra-high molecular weight polyethylene fibers, polypropylene fibers, polyethylene-propylene blend fibers, or basalt fibers.
Furthermore, the diameter of the micron fiber is 5-20 μm.
Further, the concrete also comprises an additive, wherein the additive comprises at least one of nano silicon dioxide, nano titanium dioxide or nano calcium carbonate, and the content of the additive is set to be 1-2%.
On the other hand, the invention also discloses a preparation method of the micro-nano fiber reinforced concrete, which comprises the following steps:
1) preparing nano fibers by electrostatic spinning;
2) modifying the surface of the microfiber to enable the surface of the microfiber to have a first hydrophilic group;
3) carrying out hydrophilic modification on the surface of the nanofiber to enable the surface of the nanofiber to have a second hydrophilic group;
4) mixing the nano-fibers, the micro-fibers, water and the additive, treating by using ultrasonic waves, and standing;
5) mixing with common concrete, and stirring.
Further, in the preparation method, the preparation of the nanofiber by electrostatic spinning specifically comprises:
adding a solvent into the high molecular polymer, and magnetically stirring to obtain an electrostatic spinning solution;
adding the electrostatic spinning solution into a spray head, and performing electrostatic spinning to obtain nano fibers;
the concentration of the electrostatic spinning solution is set to be 10-30%, the time of magnetic stirring is set to be not less than 6 hours, the voltage of electrostatic spinning is set to be 10-30 kV, the advancing speed of the spinning solution is set to be 0.3-5 mL/h, the receiving distance from a spinning nozzle to a roller is set to be 15-30 cm, the temperature of a spinning environment is set to be 20-45 ℃, and the relative humidity of the surrounding environment is set to be 30-80%.
Furthermore, the preparation method carries out hydrophilic modification on the surface of the nanofiber by using a modifying agent containing amino, carboxyl, amido and hydroxyl, and carries out hydrophilic modification on the surface of the microfiber by using a modifying agent containing amino, carboxyl, amido and hydroxyl.
According to the embodiment of the invention, the provided micro-nano fiber reinforced concrete has the advantages that the nano fiber thins coarse pores by filling the pore structures among cement hydration products, so that the pore structure in the concrete is improved, the microstructure of the concrete is more compact, and the formation of harmful pores is effectively limited. The reinforced concrete obtained by blending the micro-fibers, the nano-fibers and the cement overcomes the characteristic of multi-scale fracture, the nano-fibers and the micro-fibers with hydrophilic groups and high elastic modulus on the surfaces greatly improve the mechanical property of the concrete, and the addition of the additive further enhances the mechanical property and durability of the concrete, so that the micro-nano fiber reinforced concrete with high bending resistance, high strength and high toughness is obtained.
Drawings
FIG. 1 shows a process flow of a preparation method of example 1 of the present invention,
figure 2 example 1 thermoplastic polyurethane nanofiber micro-topography,
figure 3 example 1 thermoplastic polyurethane nanofiber stress-strain curve,
fig. 4 comparison of water contact angle test before and after nanofiber modification of example 1, wherein fig. 4.1 is water contact angle test of thermoplastic polyurethane nanofiber before modification, and fig. 4.2 is water contact angle test of thermoplastic polyurethane nanofiber after modification.
Detailed Description
The word "embodiment" as used herein, is not necessarily to be construed as preferred or advantageous over other embodiments, including any embodiment illustrated as "exemplary". The performance index measurements in the examples of this method, unless otherwise indicated, were carried out using test methods conventional in the art. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure.
Unless defined otherwise, technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs; other raw materials, reagents, test methods and technical means not specifically mentioned as the present invention refer to those generally used by those of ordinary skill in the art, and those generally used; references herein to amounts generally refer to mass amounts, e.g., the amount of nanofibers in concrete, as a percentage of the mass of nanofibers in concrete to the mass of concrete. The first hydrophilic group and the second hydrophilic group mentioned herein are only the hydrophilic groups distinguished and respectively represent the surfaces of the micro fibers and the nano fibers, and do not represent other specific meanings.
The terms "substantially" and "about" are used throughout this disclosure to describe small fluctuations. For example, they may mean less than or equal to ± 5%, such as less than or equal to ± 2%, such as less than or equal to ± 1%, such as less than or equal to ± 0.5%, such as less than or equal to ± 0.2%, such as less than or equal to ± 0.1%, such as less than or equal to ± 0.05%. Concentrations, amounts, and other numerical data may be expressed or presented herein in a range format. Such range format is used merely for convenience and brevity and thus should be interpreted flexibly to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited. For example, a numerical range of "1% to 5%" should be interpreted to include not only the explicitly recited values of 1% to 5%, but also include individual values and sub-ranges within the indicated range. Thus, included in this numerical range are individual values, such as 2%, 3.5%, and 4%, and sub-ranges, such as 1% to 3%, 2% to 4%, and 3% to 5%, etc. This principle applies equally to ranges reciting only one numerical value. Moreover, such an interpretation applies regardless of the breadth of the range or the characteristics being described.
In this disclosure, including the claims, all conjunctions such as "comprising," including, "" carrying, "" having, "" containing, "" involving, "" containing, "and the like are to be understood as being open-ended, i.e., to mean" including but not limited to. Only the conjunction "consisting of" and "consisting of" are closing conjunction.
In the following detailed description, specific details are set forth in order to provide a better understanding of the present disclosure. It will be understood by those skilled in the art that the present invention may be practiced without some of these specific details. In the examples, some methods, means, apparatuses, devices, raw material compositions, molecular structures, etc. known to those skilled in the art are not described in detail in order to highlight the gist of the present invention.
The embodiment of the invention discloses a micro-nano fiber reinforced concrete, which generally refers to that nano fibers and micro fibers are used as common fiber reinforcing components to reinforce and modify the concrete, the obtained reinforced concrete comprises the micro fibers with first hydrophilic groups on the surface and the nano fibers with second hydrophilic groups on the surface, and conventional concrete is subjected to blending composite modification through the hydrophilic nano fibers and the hydrophilic micro fibers, so that the nano fibers and the micro fibers with the hydrophilic groups have further enhanced bonding force with a concrete matrix.
Generally, the content of the micro fibers used for reinforcing concrete has an influence on the performance of the concrete, for example, the content of the micro fibers in the concrete is set to be 2-5% to effectively reinforce the mechanical performance of the concrete, and the content of the nano fibers also has a great influence on the mechanical performance of the reinforced concrete, for example, the content of the nano fibers in the concrete is set to be 5-10% to further reinforce the mechanical performance of the concrete. As a method for improving the mechanical property of concrete, the nanofibers and the microfibers have different diameter ranges, which together have a mutual reinforcing effect as a reinforcing fiber, and further, the reinforcing effect is more facilitated by controlling the relative proportion of the nanofibers and the microfibers, for example, the mass ratio of the nanofibers to the microfibers is set to 1: 1-5: 1.
As a fiber component for enhancing the performance of concrete, the performance of the nanofiber can influence the enhancement effect, for example, the diameter of the nanofiber is 50-500 nm, which is beneficial to the optimization of the enhancement effect, further, the porosity of the nanofiber is 70-80%, the specific surface area of the nanofiber is large, the porosity is high, the tensile strength is high, and the improvement of the enhancement effect is facilitated.
As the fiber component for enhancing the concrete performance, the category and physical and chemical properties of the nanofibers may also have an influence on the enhancing effect, and for example, thermoplastic polyurethane fiber, polystyrene fiber, fluorinated thermoplastic polyurethane fiber, polydimethylsiloxane, or carbon fiber all have a good effect of enhancing the concrete performance. As the method of using the nanofibers, a single kind of fibers may be used, or different kinds of fibers, such as polystyrene fibers and carbon fibers, may be used as the nanofiber component in concrete.
As a fiber component for enhancing the performance of concrete, the performance of the microfiber may affect the enhancing effect, for example, the microfiber such as polyethylene fiber, ultra-high molecular weight polyethylene fiber, polypropylene fiber, polyethylene-propylene blend fiber or basalt fiber may be used as an optional fiber of the concrete enhancing fiber; as the method for using the micron fibers, a single kind of micron fibers can be adopted, and different kinds of fibers can be adopted as the micron fiber component in the concrete. Other properties of the micro-fiber generally affect the properties of the reinforced concrete, for example, the diameter of the micro-fiber is set to be 5-20 μm, which is beneficial to enhancing the reinforcing effect. The diameter of the micron fiber is uniformly distributed, and the micron fiber has the characteristics of high temperature resistance, acid and alkali resistance, wear resistance, fatigue resistance and the like, and is favorable for reinforcing the reinforcing effect on concrete.
The fiber used for reinforcing concrete comprises nano fiber and micron fiber, the surface property of the fiber has influence on the property of concrete, and especially, if the fiber surface has hydrophilicity, the fiber can generate better combination effect with the concrete, and the mechanical property and durability are enhanced. As an alternative to hydrophilicity, fibers having hydrophilic groups on the fiber surface may be selected, for example, hydrophilic groups such as amino groups, carboxyl groups, amide groups, or hydroxyl groups are advantageous in improving the hydrophilicity of the fibers and the interaction with concrete. As the hydrophilic fiber for reinforcing concrete, the surface of the microfiber generally contains a first hydrophilic group, and the surface of the nanofiber generally contains a second hydrophilic group, and as a common use mode of the hydrophilic nanofiber and the hydrophilic microfiber, the nanofiber and the microfiber having the same hydrophilic group can be selected, namely, the first hydrophilic group and the second hydrophilic group have the same molecular structure; the surface hydrophilic groups on the surface of the nanofibers can be selected to be different from the hydrophilic groups on the surface of the microfibers to meet different requirements for reinforcing concrete, i.e., the first hydrophilic groups and the second hydrophilic groups have different molecular structures. Further alternatively, the surface groups of the nanofibers can be selected from a plurality of groups, for example, nanofibers containing different hydrophilic groups are doped and mixed with each other to be used as the nanofiber component for reinforcing concrete. In a similar manner, the surface groups of the microfibers can be selected to be multiple, for example, by intermingling microfibers having different hydrophilic groups, and by acting as the microfiber component of the reinforced concrete.
The hydrophilic group on the surface of the fiber can be achieved by various methods, for example, by surface-treating the fiber with a molecule containing a hydrophilic group to attach the hydrophilic group to the surface of the fiber, by surface-treating methods, such as plasma surface treatment, surface oxidation, graft modification, coupling agent surface modification, and the like. As a hydrophilic treatment method of the fiber surface, the same treatment method can be applied to the nanofibers and the microfibers, for example, if the nanofiber surface and the microfiber surface have the same hydrophilic group, the same hydrophilic treatment method can be applied; for embodiments where the nanofiber surface and the microfiber surface have different hydrophilic groups, different hydrophilic treatment regimes can be selected to accommodate the different hydrophilic group acquisition pathways.
As a hydrophilic surface treatment method, a plasma surface treatment method can be selected. For example, the surface of the electrostatic nano fiber or micro fiber obtained by the electrostatic spinning method is treated by low-temperature plasma to initiate acrylic acid to graft and polymerize on the surface of the fiber, so that the effect of improving the hydrophilicity of the fiber is achieved, and meanwhile, the breaking elongation and breaking strength of the fiber can be enhanced; optionally, the plasma treatment conditions may be set to vacuum degree of 60Pa, gas flow rate of 4L/min, discharge power of 75-150W, and discharge time of 30-60 s.
As a further method for reinforcing concrete, in the method for reinforcing concrete by using nano fiber and micron fiber, the reinforcing effect can be optionally reinforced, for example, an additive can be added into concrete to promote the bonding force between fiber and concrete and improve the microstructure of concrete, and the additive comprises inorganic nano additive, such as nano silicon dioxide, nano titanium dioxide or nano calcium carbonate, which can effectively realize the reinforcing effect; as the admixture, the content thereof generally affects the reinforcing effect and the overall cost, and for example, it is preferable to set the content to 1 to 2%. As the admixture, a single kind of admixture may be used, and also admixtures having mutually reinforcing or complementary actions may be used.
The preparation method of the concrete reinforced by the micro-nano fibers comprises the process of preparing the nano fibers by electrostatic spinning; specifically, the electrospinning process comprises: adding a solvent into the high molecular polymer, and magnetically stirring to obtain an electrostatic spinning solution; adding the electrostatic spinning solution into a spray head, and performing electrostatic spinning to obtain nano fibers; as an optional embodiment, the concentration of the electrostatic spinning solution is set to be 10-30%, and the time of magnetic stirring is set to be not less than 6 hours; the voltage of electrostatic spinning is set to be 10-30 kV, the advancing speed of the spinning solution is set to be 0.3-5 mL/h, the receiving distance from a spinning nozzle to a roller is set to be 15-30 cm, the temperature of the spinning environment is set to be 20-45 ℃, and the relative humidity of the surrounding environment is set to be 30-80%.
The preparation method of the concrete reinforced by the micro-nano fibers comprises the process of modifying the surfaces of the nano fibers and the micro fibers to ensure that the surfaces of the nano fibers and the micro fibers have hydrophilic groups; specifically, modifying agent containing amino, carboxyl, amido and hydroxyl is used for carrying out hydrophilic modification on the surfaces of the nano-fiber and the micro-fiber; for example, acrylic acid surface graft polymerization is initiated on the surfaces of the electrostatic nanofibers and the microfibers by adopting low-temperature plasmas, the polymerization is carried out under the conditions that the vacuum degree is 60Pa, the gas flow is 4L/min, the discharge power is 75-150W, and the discharge time is 30-60 s. The water contact angle test is an important means for testing the hydrophilicity of materials commonly used, and the hydrophilicity of the fibers before and after modification can be compared through the water contact angle test means.
The preparation method of the concrete reinforced by the micro-nano fibers comprises the steps of mixing the hydrophilic modified nano fibers, the hydrophilic modified micro fibers, water and an additive, treating by using ultrasonic waves, and standing; and then mixing with common concrete, and uniformly stirring to obtain the micro-nano fiber reinforced concrete.
Example 1
In this embodiment 1, the micro-nanofiber reinforced concrete includes thermoplastic polyurethane nanofibers, polyethylene-polypropylene blended microfibers, nano-silica, coarse aggregate, fine aggregate, water, and cement, and the preparation process is:
the preparation of the thermoplastic polyurethane nanofiber by the electrostatic spinning technology specifically comprises the following steps: adding a high molecular polymer into a solvent, and performing magnetic stirring to obtain an electrostatic spinning solution; adding the prepared electrostatic spinning solution into a spray head, and performing electrostatic spinning to obtain a nanofiber membrane; and drying the nanofiber membrane to fully volatilize the solvent.
Carrying out hydrophilic modification on the prepared thermoplastic polyurethane nanofiber and the polyethylene-polypropylene blended microfiber by a plasma surface treatment method; the method specifically comprises the following steps: initiating acrylic acid surface grafting polymerization on the surfaces of the electrostatic nanofibers and the microfibers by using low-temperature plasmas; wherein, the modification conditions are as follows: the vacuum degree is 60Pa, the gas flow is 4L/min, the discharge power is 75-150W, and the discharge time is 30-60 s. The water contact angle of the hydrophilic modified nanofibers and microfibers of this example was tested to examine their hydrophilic properties.
Weighing a certain amount of hydrophilic modified thermoplastic polyurethane nano-fiber, polyethylene-polypropylene blended micro-fiber, water and silicon dioxide additive, uniformly stirring, treating by using ultrasonic waves, and standing;
putting the mixture into common concrete containing coarse aggregate, fine aggregate and cement, and uniformly stirring.
Fig. 1 is a process flow of preparing micro-nanofiber reinforced concrete in this example 1, and fig. 2 is a morphology diagram of the thermoplastic polyurethane nanofiber prepared in this example 1, and it can be seen from the figure that the thermoplastic polyurethane nanofiber prepared by the electrostatic spinning method has uniform diameter distribution and smooth and regular fiber surface; FIG. 3 is a stress-strain curve of the thermoplastic polyurethane nanofiber in this example 1, where the strain of the thermoplastic polyurethane nanofiber can be 400%, and the stress can reach over 90 MPa; fig. 4 is a comparison graph of water contact angle tests before and after hydrophilic modification of the thermoplastic polyurethane nanofiber in example 1, fig. 4.1 shows that the contact angle of water on the surface of the nanofiber before modification is 98.26 degrees, fig. 4.2 shows that the contact angle of water on the surface of the nanofiber after modification is only 12.35 degrees, and the hydrophilicity of the surface is obviously improved.
According to the embodiment of the invention, the provided micro-nano fiber reinforced concrete has the advantages that the nano fiber thins coarse pores by filling the pore structures among cement hydration products, so that the pore structure in the concrete is improved, the microstructure of the concrete is more compact, and the formation of harmful pores is effectively limited. The reinforced concrete obtained by blending the micro-fibers, the nano-fibers and the cement overcomes the characteristic of multi-scale fracture, the nano-fibers and the micro-fibers with hydrophilic groups and high elastic modulus on the surfaces greatly improve the mechanical property of the concrete, and the mechanical property and durability of the concrete are further enhanced by adding the additive.
The technical solutions and the technical details disclosed in the embodiments of the present invention are only examples to illustrate the concept of the present invention, and do not constitute a limitation of the present invention, and all the combinations and uses of the technical solutions disclosed in the present invention, which have no inventive equivalent or change, have the same inventive concept as the present invention, and are within the scope of the claims of the present invention.
Claims (5)
1. A micro-nano fiber reinforced concrete is characterized by comprising:
a microfiber having a surface with a first hydrophilic group;
a nanofiber having a second hydrophilic group on a surface thereof;
wherein the mass content of the micro-fibers in the concrete is set to be 2-5%, and the mass content of the nano-fibers in the concrete is set to be 5-10%;
the first hydrophilic group comprises an amino group, a carboxyl group, an amide group or a hydroxyl group, and the second hydrophilic group comprises an amino group, a carboxyl group, an amide group or a hydroxyl group;
the diameter of the nanofiber is 50-500 nm, and the porosity is 70-80%;
the diameter of the micron fiber is 5-20 μm;
the concrete further comprises an additive, wherein the additive comprises at least one of nano silicon dioxide, nano titanium dioxide or nano calcium carbonate, and the mass content of the additive is set to be 1-2%.
2. The micro-nanofiber reinforced concrete according to claim 1, wherein the nanofibers comprise at least one of thermoplastic polyurethane fibers, polystyrene fibers, fluorinated thermoplastic polyurethane fibers, or carbon fibers.
3. The micro-nanofiber reinforced concrete according to claim 1, wherein the micro-nanofibers comprise at least one of polyethylene fibers, polypropylene fibers, polyethylene-propylene blend fibers, or basalt fibers.
4. A method for preparing micro-nano fiber reinforced concrete according to any one of claims 1 to 3, wherein the preparation method comprises the following steps:
1) preparing nano fibers by electrostatic spinning;
2) carrying out hydrophilic modification on the surface of the microfiber to enable the surface of the microfiber to have a first hydrophilic group;
3) carrying out hydrophilic modification on the surface of the nanofiber to enable the surface of the nanofiber to have a second hydrophilic group;
4) mixing the nano-fibers, the micro-fibers, water and the additive, treating by using ultrasonic waves, and standing;
5) mixing with common concrete, and stirring.
5. The preparation method of the micro-nano fiber reinforced concrete according to claim 4, wherein the surface of the micro-nano fiber is subjected to hydrophilic modification by using a modifier containing amino, carboxyl, amido and hydroxyl; and carrying out hydrophilic modification on the surface of the nanofiber by using a modifying agent containing amino, carboxyl, amido and hydroxyl.
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| CN115991589A (en) * | 2021-10-20 | 2023-04-21 | 山东建筑大学 | High-strength high-ductility cement-based composite material, preparation method thereof and application of nanocellulose in cement-based composite material |
| CN114315279A (en) * | 2022-01-12 | 2022-04-12 | 新疆生产建设兵团建筑工程科学技术研究院有限责任公司 | Anti-crack concrete and preparation method thereof |
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