CN113429640A - Rubber composite material containing modified basalt fibers and preparation method thereof - Google Patents
Rubber composite material containing modified basalt fibers and preparation method thereof Download PDFInfo
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- CN113429640A CN113429640A CN202110751730.5A CN202110751730A CN113429640A CN 113429640 A CN113429640 A CN 113429640A CN 202110751730 A CN202110751730 A CN 202110751730A CN 113429640 A CN113429640 A CN 113429640A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2307/00—Characterised by the use of natural rubber
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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Abstract
The invention aims to solve the problems existing in the compounding of the existing basalt fiber and rubber, provides a rubber composite material containing modified basalt fiber and a preparation method thereof, and belongs to the technical field of rubber composite materials. The modified basalt fiber reinforced rubber composite material is composed of the following raw materials in parts by mass: 80-100 parts of natural rubber, 4-6 parts of plasticizer, 8-10 parts of reinforcing agent, 1-2 parts of accelerator, 1-2 parts of sulfur, 0.5-1 part of anti-aging agent and 2-10 parts of modified basalt fiber. According to the invention, the acid etching assistant and the silane coupling agent are adopted to modify the basalt fiber, and the modified basalt fiber is added into the rubber composite material, so that the overall mechanical property of the rubber composite material is improved.
Description
Technical Field
The invention belongs to the technical field of rubber composite materials, and particularly relates to a rubber composite material containing modified basalt fibers and a preparation method thereof.
Background
The basalt fiber is a novel inorganic environment-friendly green high-performance fiber material and is composed of oxides such as silicon dioxide, aluminum oxide, calcium oxide, magnesium oxide, ferric oxide, titanium dioxide and the like. The basalt continuous fiber has high strength, and also has various excellent performances of electrical insulation, corrosion resistance, high temperature resistance and the like. In addition, the production process of the basalt fiber determines that the produced waste is less, the environmental pollution is less, the product can be directly degraded in the environment after being discarded, and no harm is caused, so that the basalt fiber rubber composite material is a genuine green and environment-friendly material, and the basalt fiber rubber composite material comprises products such as automobile tires, conveyor belts, rubber tubes and the like.
The basalt fiber is used for natural rubber, so that the loss factor of the composite material can be effectively reduced, but due to the characteristics of hydrophilicity and lipophobicity of the surface of the basalt fiber, the basalt fiber has weak bonding force with a matrix and is easy to agglomerate in the rubber. In order to improve the mechanical property of the composite material while reducing the loss factor, the basalt fiber needs to be modified to enhance the lipophilicity. In addition, because the surface of the basalt fiber is very smooth, the improvement of the surface roughness of the basalt fiber is also a feasible means; meanwhile, the surface of the film is chemically inert, so that the surface activity of the film is improved by other modification methods, and the adhesion between the film and a substrate is improved.
The commonly used modification methods mainly include: coupling agent modification technology, plasma modification technology, coating modification technology and the like. In the study of surface modification and application of basalt fiber, the most common is coupling agent modification, which can improve filler dispersion in a matrix, prevent aggregation, and enhance interfacial adhesion with the matrix.
CN108585949A discloses a preparation method of modified basalt fiber, which comprises the following steps: mixing a coupling agent and water according to a certain weight ratio to prepare a treatment solution; putting the basalt fibers into the treatment liquid for primary soaking, grinding and stirring; filtering, drying, putting into the treatment liquid again for secondary soaking, filtering and drying to obtain pretreated basalt fibers; sequentially carrying out densification physical modification treatment, preoxidation, low-temperature carbonization and high-temperature carbonization on the pretreated basalt fiber to obtain the modified basalt fiber. The preparation method of the modified basalt fiber is simple and easy to operate, and the prepared modified basalt fiber has good tensile strength and few structural defects of the fiber.
CN111410441A discloses a basalt fiber surface modifier, which comprises the following components: polyethylene, benzyl alcohol, 2-methyl-2-hydroxypropionic acid, glycidyl methacrylate, polypropylene and a silane coupling agent. The basalt fiber prepared by the invention is used for enhancing the AC asphalt mixture, and the anti-rutting performance and the anti-fatigue performance of the asphalt mixture are improved. The anti-rutting high-temperature stability of the asphalt mixture reaches over 12000 times/mm, and compared with a matrix asphalt mixture without fibers, the anti-fatigue performance is improved by over 20 percent, and the anti-rutting performance and the anti-fatigue performance are achieved.
At present, the research of applying the modified basalt fiber to the field of rubber materials is not common.
Disclosure of Invention
The invention aims to solve the problems existing in the compounding of the existing basalt fiber and rubber, and provides a rubber composite material containing modified basalt fiber and a preparation method thereof. According to the invention, the acid etching assistant and the silane coupling agent are adopted to modify the basalt fiber, and the modified basalt fiber is added into the rubber composite material, so that the overall mechanical property and the wear resistance of the rubber composite material are improved.
One of the technical schemes of the invention is that the rubber composite material containing modified basalt fibers comprises the following raw materials in parts by mass:
80-100 parts of natural rubber, 4-6 parts of plasticizer, 8-10 parts of reinforcing agent, 1-2 parts of accelerator, 1-2 parts of sulfur, 0.5-1 part of anti-aging agent and 2-10 parts of modified basalt fiber.
Further, in the modified basalt fiber reinforced rubber composite material, the plasticizer is dioctyl phthalate, diisooctyl phthalate or tricresyl phosphate;
the reinforcing agent is carbon black, zinc oxide or white carbon black;
the accelerator is an accelerator M, and the chemical name is as follows: 2-mercaptobenzothiazole; or the promoter is TMTD, the chemical name is: tetramethylthiuram disulfide, molecular formula: c6H12N2S4；
The anti-aging agent is anti-aging agent 4020, and has the chemical name: n- (1, 3-dimethyl) butyl-N' -phenyl-p-phenylenediamine; or the anti-aging agent is anti-aging agent AW, chemical name: 6-ethoxy-1, 2-dihydro-2, 2, 4-trimethylquinoline.
Further, the modified basalt fiber reinforced rubber composite material has the tensile strength of 22-30 MPa, the tear strength of 35-55 KN/m, the Shore A hardness of 74-80 degrees and the wear resistance (mass loss rate%) of 4-8%.
Further, the preparation method of the modified basalt fiber reinforced rubber composite material comprises the following steps:
1) putting basalt fibers into an acetone aqueous solution with the mass concentration of 30-40%, washing off surface impurities, and then putting the basalt fibers into an oven with the temperature of 60-70 ℃ for drying for 36-48 hours;
2) soaking the cleaned basalt fiber in glacial acetic acid with the concentration of 0.8-1.5 mol/L for 30-60 min, then cleaning in deionized water, and drying in an oven at the temperature of 60-70 ℃ for 36-48 h to prepare the pretreated basalt fiber;
3) immersing the pretreated basalt fiber into a silane coupling agent aqueous solution with the mass concentration of 1.5-2.5%, soaking for 5-10 min, and then cleaning and drying to obtain the modified basalt fiber.
Further, in the modified basalt fiber reinforced rubber composite material, in the step 3), the silane coupling agent is KH 550.
The second technical scheme of the invention is that the preparation method of the modified basalt fiber reinforced rubber composite material comprises the following steps:
1) weighing natural rubber, plasticating, sequentially adding modified basalt fiber, a plasticizer, a reinforcing agent, an accelerator, sulfur and an anti-aging agent according to a proportion, mixing and standing to obtain a rubber compound;
2) and vulcanizing the prepared rubber compound to obtain the modified basalt fiber reinforced rubber composite material.
Further, in the preparation method, in the step 1), the plastication time is 4-5 min; the mixing temperature is 55-65 ℃, the mixing time is 1-20 min, and the standing time is 6-7 h.
Further, in the preparation method, in the step 2), the vulcanization condition is 130-140 ℃, 7-8 MPa and 8-10 min.
Compared with the prior art, the invention has the advantages that:
1. the active groups are introduced to the surface of the basalt fiber, so that the compatibility of the basalt fiber with natural rubber is improved.
2. The Shore A hardness and the wear resistance of the rubber composite material are improved by adding the modified basalt fiber.
Drawings
FIG. 1 is a scanning electron microscope picture of basalt fiber;
wherein, (a) unmodified basalt fiber, and (b) the modified basalt fiber prepared in the examples.
Detailed Description
The natural rubber in the following examples was purchased from Hainan Natural rubber group.
The preparation method of the modified basalt fiber comprises the following steps:
1) putting basalt fibers into an acetone aqueous solution with the mass concentration of 30-40%, washing off surface impurities, and then putting the basalt fibers into an oven with the temperature of 60-70 ℃ for drying for 36-48 hours;
2) soaking the cleaned basalt fiber in glacial acetic acid with the concentration of 0.8-1.5 mol/L for 30-60 min, then cleaning in deionized water, and drying in an oven at the temperature of 60-70 ℃ for 36-48 h to prepare the pretreated basalt fiber;
3) immersing the pretreated basalt fiber into a silane coupling agent aqueous solution with the mass concentration of 1.5-2.5%, soaking for 5-10 min, and then cleaning and drying to obtain the modified basalt fiber.
The preparation method of the modified basalt fiber reinforced rubber composite material comprises the following steps:
1) weighing natural rubber, plasticating for 4-5 min, sequentially adding modified basalt fiber, a plasticizer, a reinforcing agent, an accelerator, sulfur and an anti-aging agent according to a proportion after plasticating, mixing and standing, wherein the mixing temperature is 55-65 ℃, the mixing time is 1-20 min, and the standing time is 6-7 h to obtain a rubber compound;
2) and vulcanizing the prepared rubber compound under the conditions of 130-140 ℃, 7-8 MPa and 8-10 min to obtain the modified basalt fiber reinforced rubber composite material.
Examples
The preparation methods of the rubber composite materials of the examples 1 to 9 and the comparative examples 1 to 3 are as follows:
1) weighing natural rubber, plasticating by adopting an open rubber mixing mill, sequentially adding basalt fiber, the natural rubber, a plasticizer, a reinforcing agent, an accelerator, sulfur and an anti-aging agent, and mixing and standing to obtain rubber compound; the mixing temperature is 60 ℃, the mixing time is 20min, the standing time is 7h, and the plastication time is 5 min;
2) and vulcanizing the prepared rubber compound by adopting a flat vulcanizing machine to obtain the modified basalt fiber natural rubber composite material, wherein the vulcanizing conditions are 140 ℃, 8MPa and 10 min.
The basalt fiber adopted in the embodiments 1 to 9 is a modified basalt fiber, and the preparation method thereof comprises the following steps:
1) putting the basalt fiber into an acetone solution with the mass concentration of 40%, ultrasonically cleaning for 5min, washing off surface impurities, and then putting into an oven (the temperature is 60 ℃) to bake for 48h after suction filtration;
2) putting the cleaned basalt fiber into a large beaker, slowly pouring glacial acetic acid with the concentration of 1mol/L for soaking for 1h, then ultrasonically cleaning in deionized water for 20min, taking the basalt fiber out of the beaker, and drying in an oven (the temperature is 60 ℃) for 48h to prepare the pretreated basalt fiber.
3) Immersing the pretreated basalt fiber into a silane coupling agent KH550 aqueous solution with the mass concentration of 2%, soaking for 10min, fully stirring, filtering, and drying to obtain the modified basalt fiber.
The basalt fiber used in comparative example 1 was an unmodified basalt fiber.
The preparation method of the modified basalt fiber adopted in the comparative example 2 includes the following steps:
1) putting the basalt fiber into an acetone solution with the mass concentration of 40%, ultrasonically cleaning for 5min, washing off surface impurities, and then putting into an oven (the temperature is 60 ℃) to bake for 48h after suction filtration;
2) putting the cleaned basalt fiber into a large beaker, slowly pouring glacial acetic acid with the concentration of 1mol/L for soaking for 1h, then ultrasonically cleaning in deionized water for 20min, taking out the basalt fiber from the beaker, and drying in an oven (the temperature is 60 ℃) for 48h to obtain the basalt fiber.
The preparation method of the modified basalt fiber adopted in the comparative example 3 includes the following steps:
1) putting the basalt fiber into an acetone solution with the mass concentration of 40%, ultrasonically cleaning for 5min, washing off surface impurities, and then putting into an oven (the temperature is 60 ℃) to bake for 48h after suction filtration;
2) immersing the pretreated basalt fiber into a silane coupling agent KH550 aqueous solution with the mass concentration of 2%, soaking for 10min, fully stirring, filtering, and drying to obtain the basalt fiber.
The rubber composite materials of examples 1 to 9 and comparative examples 1 to 3 had the following composition parts and mechanical properties:
the plasticizer is dioctyl phthalate, diisooctyl phthalate or tricresyl phosphate;
the reinforcing agent is carbon black, zinc oxide or white carbon black;
the promotionThe agent is an accelerant M, chemical name: 2-mercaptobenzothiazole; or the promoter is TMTD, the chemical name is: tetramethylthiuram disulfide, molecular formula: c6H12N2S4；
The anti-aging agent is anti-aging agent 4020, and has the chemical name: n- (1, 3-dimethyl) butyl N' -phenyl-p-phenylenediamine; or the anti-aging agent is anti-aging agent AW, chemical name: 6-ethoxy-1, 2-dihydro-2, 2, 4-trimethylquinoline.
TABLE 1 composition parts and mechanical properties of the raw materials in the rubber composite
The method for testing the wear resistance of the modified basalt fiber rubber composite material comprises the following steps: taking the rubber composite materials in the examples and the comparative examples, preparing the modified basalt fiber rubber composite material into a cuboid block with the length of 10cm, the width of 10cm and the height of 3cm as a test sample, measuring the initial mass m of each test sample, then polishing the test sample by using a grinding disc, respectively measuring the polished mass n of each test sample, and calculating the mass loss rate of each test sample according to the formula w being 100% (m-n)/m, namely the mass loss rate, so as to consider the wear resistance of the rubber composite material.
And (3) testing mechanical properties: tensile strength was tested according to GB/T528-2009 test for tensile stress strain Properties of vulcanizates or thermoplastic rubbers. The tear strength was tested in accordance with GB/T529-2008 "determination of tear Strength of vulcanized rubber or thermoplastic rubber (trouser, Right Angle and crescent test specimens"). Shore A hardness was measured according to GB/T531-1999 determination of hardness of vulcanizates or thermoplastic rubbers. From the above table, it can be seen that: the acid etching assisted silane coupling agent surface modification greatly improves the surface activity of the basalt fiber, as shown in SEM images before and after the basalt fiber is modified in figure 1, the surface of the basalt fiber which is not subjected to modification treatment in figure 1(a) is smooth, a layer of the surface of the basalt fiber which is subjected to modification in figure 1(b) is corroded and changed into fine particles, and the specific surface area and the surface roughness of the material are effectively increased. The modified basalt fiber is used as a reinforcement, a layer of the surface of the basalt fiber after acid treatment is corroded to become fine particles, and the fine particles are attached to the surface of the fiber to form a layer of film, so that the surface of the fiber becomes rough and concave, the interface bonding condition between the basalt fiber and an organic polymer is favorably improved, and meanwhile, the tensile property is not damaged.
Compared with comparative examples 1 to 9, the Shore A hardness of examples 1 to 9 of the present invention is improved. However, the fibers in the natural rubber composite material with the amount of 2 parts of the modified basalt fibers are too sparse, the fiber distribution in the natural rubber composite material with the amount of 6 parts of the modified basalt fibers is most ideal, and the fibers in the natural rubber composite material with the amount of 10 parts of the modified basalt fibers are accumulated in the matrix.
Example 10
A rubber composite made from natural rubber: 80g, diisooctyl phthalate: 6g, zinc oxide: 9g, promoter TMTD: 1.5g, sulfur: 1.5g, antioxidant AW: 0.75g, modified basalt fiber: 6 g.
Example 11
A rubber composite made from natural rubber: 100g, tricresyl phosphate: 4g, white carbon black: 8g, accelerator TMTD: 1.0g, sulfur: 1.0g, antioxidant AW: 0.5g, modified basalt fiber: 6 g.
Claims (8)
1. The rubber composite material containing the modified basalt fibers is characterized by comprising the following raw materials in parts by mass:
80-100 parts of natural rubber, 4-6 parts of plasticizer, 8-10 parts of reinforcing agent, 1-2 parts of accelerator, 1-2 parts of sulfur, 0.5-1 part of anti-aging agent and 2-10 parts of modified basalt fiber.
2. The modified basalt fiber-reinforced rubber composite of claim 1, wherein the plasticizer is dioctyl phthalate, diisooctyl phthalate, or tricresyl phosphate;
the reinforcing agent is carbon black, zinc oxide or white carbon black;
the accelerator is an accelerator M or an accelerator TMTD;
the anti-aging agent is anti-aging agent 4020 or anti-aging agent AW.
3. The modified basalt fiber-reinforced rubber composite material according to claim 1, wherein the rubber composite material has a tensile strength of 22 to 30MPa, a tear strength of 35 to 55KN/m, a Shore A hardness of 74 to 80 degrees, and a mass loss rate of 4 to 8%.
4. The modified basalt fiber-reinforced rubber composite material according to claim 1, wherein the preparation method of the modified basalt fiber comprises the following steps:
1) putting basalt fibers into an acetone aqueous solution with the mass concentration of 30-40%, washing off surface impurities, and drying at 60-70 ℃;
2) soaking the cleaned basalt fiber in glacial acetic acid with the concentration of 0.8-1.5 mol/L for 30-60 min, then cleaning in deionized water, and drying at 60-70 ℃ to prepare the pretreated basalt fiber;
3) immersing the pretreated basalt fiber into a silane coupling agent aqueous solution with the mass concentration of 1.5-2.5%, soaking for 5-10 min, and then cleaning and drying to obtain the modified basalt fiber.
5. The modified basalt fiber-reinforced rubber composite according to claim 4, wherein in the step 3), the silane coupling agent is KH 550.
6. The method of preparing a modified basalt fiber-reinforced rubber composite material according to claim 1, comprising the steps of:
1) weighing natural rubber, plasticating, sequentially adding modified basalt fiber, a plasticizer, a reinforcing agent, an accelerator, sulfur and an anti-aging agent according to a proportion, mixing and standing to obtain a rubber compound;
2) and vulcanizing the prepared rubber compound to obtain the modified basalt fiber reinforced rubber composite material.
7. The preparation method of the modified basalt fiber-reinforced rubber composite material according to claim 6, wherein in the step 1), the plastication time is 4-5 min; the mixing temperature is 55-65 ℃, the mixing time is 1-20 min, and the standing time is 6-7 h.
8. The preparation method of the modified basalt fiber-reinforced rubber composite material according to claim 6, wherein in the step 2), the vulcanization conditions are 130 to 140 ℃, 7 to 8MPa, and 8 to 10 min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115107330A (en) * | 2022-07-14 | 2022-09-27 | 中国兵器装备集团西南技术工程研究所 | Composite inner heat insulation layer of aluminum alloy engine combustion chamber and preparation method thereof |
| CN115384144A (en) * | 2022-09-24 | 2022-11-25 | 广东天跃新材料股份有限公司 | Special silicon rubber synthetic leather fabric for automotive interior and manufacturing process thereof |
| CN115745502A (en) * | 2022-11-23 | 2023-03-07 | 安徽理工大学 | Preparation method of basalt fiber rubber cement soil |
| CN115806777A (en) * | 2022-12-22 | 2023-03-17 | 西南石油大学 | Basalt fiber reinforced ethylene propylene diene monomer waterproof coiled material and preparation method thereof |
| CN116177927A (en) * | 2023-03-22 | 2023-05-30 | 宁波奉化交投浩阳新材料有限公司 | Asphalt mixture and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115107330A (en) * | 2022-07-14 | 2022-09-27 | 中国兵器装备集团西南技术工程研究所 | Composite inner heat insulation layer of aluminum alloy engine combustion chamber and preparation method thereof |
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| CN115384144A (en) * | 2022-09-24 | 2022-11-25 | 广东天跃新材料股份有限公司 | Special silicon rubber synthetic leather fabric for automotive interior and manufacturing process thereof |
| CN115745502A (en) * | 2022-11-23 | 2023-03-07 | 安徽理工大学 | Preparation method of basalt fiber rubber cement soil |
| CN115806777A (en) * | 2022-12-22 | 2023-03-17 | 西南石油大学 | Basalt fiber reinforced ethylene propylene diene monomer waterproof coiled material and preparation method thereof |
| CN116177927A (en) * | 2023-03-22 | 2023-05-30 | 宁波奉化交投浩阳新材料有限公司 | Asphalt mixture and preparation method thereof |
| CN116177927B (en) * | 2023-03-22 | 2023-10-13 | 宁波奉化交投浩阳新材料有限公司 | Asphalt mixture and preparation method thereof |
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