CN111171409A - High-temperature-resistant, high-strength and high-expansion-rate rubber and preparation method thereof - Google Patents
High-temperature-resistant, high-strength and high-expansion-rate rubber and preparation method thereof Download PDFInfo
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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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/041—Carbon nanotubes
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- C08K7/24—Expanded, porous or hollow particles inorganic
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Abstract
The invention discloses a high-temperature-resistant, high-strength and high-expansion-rate rubber which comprises the following components in parts by weight: 100 parts of nitrile butadiene rubber, 0.5-2 parts of stearic acid, 10-20 parts of fumed silica, 3-5 parts of carbon nano tubes, 20-30 parts of carbon black N3301, 1-2 parts of silane coupling agent, 3-8 parts of metal oxide, 1-3 parts of anti-aging agent, 0.7-0.9 part of cross-linking agent and 5-10 parts of auxiliary cross-linking agent. According to the rubber disclosed by the invention, the carbon black N330 is added as a filling agent, and the consumption of a cross-linking agent can be reduced to below 1 part by adding the fumed silica and the carbon nano tubes, so that the rubber with higher elongation at break and tensile strength at high temperature can be obtained. The invention also discloses a preparation method of the high-temperature-resistant, high-strength and high-expansion-rate rubber, and the rubber prepared by the preparation method has higher elongation at break and tensile strength.
Description
Technical Field
The invention relates to rubber and a preparation method thereof, in particular to high-temperature-resistant, high-strength and high-expansion-rate rubber and a preparation method thereof.
Background
The expansion bridge plug is a downhole tool used in the field of oil fields, the diameter of the expansion bridge plug is expanded for multiple times to be attached to a sleeve after the expansion bridge plug is placed in a well to a target position, the annular space is sealed, pressure difference is borne, and the function of the expansion bridge plug is achieved. The ambient temperature of the bridge plug is about 120 ℃ when the bridge plug is used, and the bridge plug belongs to a high-temperature environment. The common bridge plug has diameter expansion 1.1-2.5 times that of the original common bridge plug, and the oil pipe expansion bridge plug with higher expansion rate has very high requirement on the high-temperature mechanical property of rubber and very high difficulty. The requirement of the high-temperature high-expansion-rate oil pipe expansion bridge plug can be met only by using the rubber material which still keeps high elongation rate at high temperature, has high-temperature high strength and oil resistance.
The currently disclosed information, fluororubber, nitrile rubber and hydrogenated nitrile rubber commonly used in the field of oil fields, has fast reduction of tensile strength and elongation at break at high temperature, and cannot meet the requirements of high-temperature high-expansion rate (expansion rate is more than 300%) oil pipe expansion bridge plugs.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the rubber with high temperature resistance, high strength and high expansion rate.
In order to achieve the purpose, the invention adopts the technical scheme that: a high-temperature-resistant, high-strength and high-expansion-rate rubber comprises the following components in parts by weight: 100 parts of nitrile butadiene rubber, 0.5-2 parts of stearic acid, 10-20 parts of fumed silica, 3-5 parts of carbon nano tubes, 20-30 parts of carbon black N3301, 1-2 parts of silane coupling agent, 3-8 parts of metal oxide, 1-3 parts of anti-aging agent, 0.7-0.9 part of cross-linking agent and 5-10 parts of auxiliary cross-linking agent.
According to the rubber, the carbon black N330 is added as a filling agent, and the consumption of a cross-linking agent can be reduced to below 1 part by adding the fumed silica and the carbon nano tubes, so that the optimal material performance can be obtained, the elongation at break of the rubber is more than 800% at normal temperature, and the tensile strength is more than 20 MPa; the elongation at break at the high temperature of 120 ℃ is more than 600 percent, and the tensile strength is more than 9 MPa. The nitrile rubber is preferably high-acrylonitrile-content and high-Mooney nitrile rubber. Preferably, the acrylonitrile-butadiene rubber has an acrylonitrile content of 40% or more and a Mooney viscosity of 75 or more.
As a preferable embodiment of the high temperature resistant, high strength and high expansion ratio rubber of the invention, the fumed silica has a specific surface area of 120m or more2(ii) in terms of/g. The fumed silica with the specific surface area is used as a high-temperature-resistant reinforcing agent, so that the elongation at break and the tensile strength of the rubber at high temperature are improved.
As a preferable embodiment of the high temperature resistant, high strength and high expansion ratio rubber of the present invention, the carbon nanotubes are multi-walled carbon nanotubes having an aspect ratio of 200 or more. The multi-walled carbon nano-tube with the length-diameter ratio is used as a high-temperature heat conducting agent, so that the tensile elongation and tensile strength of the rubber at high temperature can be improved.
As a preferred embodiment of the high temperature resistant, high strength and high expansion ratio rubber of the present invention, the metal oxide is at least one of magnesium oxide, zinc oxide and lead oxide, but is not limited to the above-mentioned oxides.
As a preferable embodiment of the high temperature resistant, high strength and high expansion ratio rubber of the present invention, the antioxidant is at least one of antioxidant RD, antioxidant MB and antioxidant 445, but is not limited thereto.
As a preferred embodiment of the high temperature resistant, high strength and high expansion ratio rubber of the present invention, the silane coupling agent is Si-69.
As a preferable embodiment of the high temperature resistant, high strength and high expansion ratio rubber of the present invention, the crosslinking agent is at least one of DCP (dicumyl peroxide), a vulcanizing agent BIPB and a di-penta vulcanizing agent.
As a preferable embodiment of the high temperature resistant, high strength and high expansion ratio rubber of the present invention, the co-crosslinking agent is acrylate. The acrylate is used as the assistant crosslinking agent and the high-temperature reinforcing agent, and the elongation at break and the tensile strength of the rubber at high temperature can be effectively improved without adding larger amount of the assistant crosslinking agent. More preferably, the acrylate is magnesium methacrylate and/or zinc methacrylate.
The invention also aims to provide a preparation method of the high-temperature-resistant, high-strength and high-expansion-rate rubber, which comprises the following steps:
(1) first-stage mixing: heat-treating a part of nitrile rubber, fumed silica and a silane coupling agent at 125-135 ℃ for 8-12 minutes, taking out the nitrile rubber, standing for 10-14 hours, and marking as a sizing material A; dissolving the rest nitrile rubber and the carbon nano tubes in a tetrahydrofuran solution, stirring for 2-6 hours by using an ultrasonic stirrer, and then drying in an oven at 45-55 ℃ for 10-14 hours to obtain a sizing material B;
(2) and (3) second-stage mixing: carrying out heat treatment on the rubber material A and the rubber material B at the temperature of 98-102 ℃ for 12-18 minutes, taking out the rubber material A and the rubber material B, standing for 20-30 hours, and marking as rubber material C;
(3) three-stage mixing: adding stearic acid, metal oxide, carbon black and an anti-aging agent into the rubber material C, mixing at 75-85 ℃, standing for 4-8 hours, and marking as rubber material D;
(4) four-stage mixing: adding an auxiliary crosslinking agent and a crosslinking agent into the rubber material D, mixing at the temperature of below 45-55 ℃, discharging after thin passing, and standing for 10-14 hours;
(5) and (3) vulcanization: and (3) vulcanizing at the first stage of 10-15 MPa, 160-170 ℃ and 10-30 minutes for the first stage of vulcanization to obtain the high-temperature-resistant, high-strength and high-expansion-rate rubber.
According to the invention, the filler (fumed silica, carbon nano tube and the like) with small particle size can be well dispersed by a four-stage mixing method, and finally the rubber material with high strength and high elongation at high temperature of 120 ℃ is obtained, and the rubber material is especially suitable for being used in the environment requiring the rubber to have high strength and high elongation at high temperature, such as an oil pipe expansion bridge plug with high temperature and high expansion rate.
The invention also aims to provide the oil pipe passing expansion bridge plug which is prepared from the high-temperature-resistant, high-strength and high-expansion-rate rubber. The rubber material has higher elongation at break and tensile strength at high temperature of 120 ℃, and can be used for preparing the oil pipe passing expansion bridge plug with high expansion rate (the expansion rate is more than 3) at high temperature.
The invention has the beneficial effects that: the invention provides a high-temperature-resistant, high-strength and high-expansion-rate rubber, wherein carbon black N330 is added into the rubber as a filler, and the use amount of a cross-linking agent can be reduced to below 1 part by adding fumed silica and carbon nanotubes, so that the best material performance can be obtained, the elongation at break of the rubber is more than 800% at normal temperature, and the tensile strength is more than 20 MPa; the elongation at break at the high temperature of 120 ℃ is more than 600 percent, and the tensile strength is more than 9 MPa. The invention also provides a preparation method of the high-temperature-resistant, high-strength and high-expansion-rate rubber, and the rubber prepared by the preparation method has higher elongation at break and tensile strength.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Each of the raw materials in the examples and comparative examples was purchased from the market, wherein the nitrile rubber was purchased from LG corporation, model No. 3280; fumed silica is purchased from cabot corporation, model number TS 610; carbon nanotubes were purchased from tiannai corporation under the model number FT 7011; carbon black N330 was purchased from Cabot corporation under the model number N330; si-69 was purchased from Jinchang, Guangzhou; zinc oxide was purchased from Yanggu Huatai corporation, model ZnO-80; magnesium oxide was purchased from golden Changsheng, Guangzhou; anti-aging agent RD was purchased from Guangzhou Jinchangshang company; stearic acid was purchased from golden Changsheng, Guangzhou; the antioxidant MB is purchased from Yanggu Huatai company, and has the model of MBI-80; the crosslinker BIPB was purchased from Acksonobel under the model Perkadox 14; crosslinker DCP was purchased from Guangzhou Jinchangshan corporation; magnesium methacrylate was purchased from sienna organic chemical company. The formulations of the rubbers described in examples 1 to 5 and comparative examples 1 to 6 are shown in Table 1.
The preparation method of the rubber described in the examples 1 to 5 and the comparative examples 1 to 6 comprises the following steps:
(1) 50 parts of nitrile rubber, white carbon black and Si-69 are subjected to heat treatment at the high temperature of 130 ℃ for 10 minutes, and are taken out and kept stand for 12 hours to be marked as a sizing material A; dissolving the remaining 50 parts of nitrile rubber and carbon nano tubes in tetrahydrofuran solution, stirring for 4 hours by using an ultrasonic stirrer, and then drying in a 50 ℃ oven for 12 hours to obtain a sizing material B;
(2) and (3) second-stage mixing: carrying out heat treatment on the rubber materials A and B at the high temperature of 100 ℃ for 15 minutes, taking out the rubber materials A and B, standing for 24 hours, and marking as rubber material C;
(3) three-stage mixing: adding stearic acid, metal oxide, carbon black and an anti-aging agent into the rubber material C, mixing at about 80 ℃, standing for 6 hours, and marking as rubber material D;
(4) four-stage mixing: adding an auxiliary crosslinking agent and a crosslinking agent into the rubber material D, mixing at the temperature of below 50 ℃, discharging sheets after thin passing, and standing for 12 hours;
(5) and (3) vulcanization: and (3) obtaining the rubber by the first-stage vulcanization pressure of 10MPa, the vulcanization temperature of 170 ℃ and the vulcanization time of 18 minutes.
Comparative example 7
The rubber formulation of comparative example 7 is the same as that of example 1, except for the preparation method, which is: plasticating rubber, adding zinc oxide, stearic acid and an anti-aging agent, mixing for 5 minutes, then adding carbon black, fumed silica and carbon nanotubes, mixing for 10 minutes, adding a cross-linking agent and an auxiliary cross-linking agent, discharging sheets after passing through, and standing for 12 hours; and (3) vulcanization: and (3) vulcanizing at the vulcanization pressure of 10MPa and the vulcanization temperature of 170 ℃ for 5 minutes to obtain the rubber.
TABLE 1
The rubber of examples 1-5 and comparative examples 1-6 was tested for performance by the following test methods: the tensile strength and elongation at break were measured at 23 ℃ or 120 ℃ and the tensile properties were measured according to GB/T528-1998 standards, the test specimens were dumbbell-shaped, type I in the standards, and the tensile rate was 500 m/min.
TABLE 2
As can be seen from Table 1, the rubber materials of examples 1 to 5 of the present invention have high tensile strength and elongation at break at high temperature, the elongation at break of the rubber is greater than 800% at normal temperature, and the tensile strength is greater than 20 MPa; the elongation at break at the high temperature of 120 ℃ is more than 600 percent, the tensile strength is more than 9MPa, the rubber is very suitable for being applied to the high-temperature environment, and the material is required to be manufactured into rubber parts with higher tensile strength and elongation at break, such as expansion bridge plugs of oil pipes with high expansion rates at high temperature.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The rubber with high temperature resistance, high strength and high expansion rate is characterized by comprising the following components in parts by weight: 100 parts of nitrile butadiene rubber, 0.5-2 parts of stearic acid, 10-20 parts of fumed silica, 3-5 parts of carbon nano tubes, 20-30 parts of carbon black N3301, 1-2 parts of silane coupling agent, 3-8 parts of metal oxide, 1-3 parts of anti-aging agent, 0.7-0.9 part of cross-linking agent and 5-10 parts of auxiliary cross-linking agent.
2. The high temperature resistant, high strength and high expansion rubber according to claim 1, wherein the fumed silica has a specific surface area of 120m or more2/g。
3. The high temperature, high strength, and high expansion rubber of claim 1, wherein the carbon nanotubes are multi-walled carbon nanotubes having an aspect ratio of 200 or more.
4. The high temperature, high strength and high expansion rubber of claim 1, wherein said metal oxide is at least one of magnesium oxide, zinc oxide and lead oxide.
5. The high temperature, high strength and high expansion rubber according to claim 1, wherein said antioxidant is at least one of antioxidant RD, antioxidant MB and antioxidant 445.
6. The high temperature, high strength and high expansion rubber of claim 1, wherein said silane coupling agent is Si-69.
7. The high temperature, high strength and high expansion rubber of claim 1 wherein said cross-linking agent is at least one of dicumyl peroxide, the vulcanizing agents BIPB and bis-penta-vulcanizing agents.
8. The high temperature resistant, high strength, high expansion rubber of claim 1 wherein said co-crosslinking agent is an acrylate; preferably, the acrylate is magnesium methacrylate and/or zinc methacrylate.
9. The method for preparing the high temperature resistant, high strength and high expansion rubber according to any one of claims 1 to 8, comprising the steps of:
(1) first-stage mixing: heat-treating a part of nitrile rubber, fumed silica and a silane coupling agent at 125-135 ℃ for 8-12 minutes, taking out the nitrile rubber, standing for 10-14 hours, and marking as a sizing material A; dissolving the rest nitrile rubber and the carbon nano tubes in a tetrahydrofuran solution, stirring for 2-6 hours by using an ultrasonic stirrer, and then drying in an oven at 45-55 ℃ for 10-14 hours to obtain a sizing material B;
(2) and (3) second-stage mixing: carrying out heat treatment on the rubber material A and the rubber material B at the temperature of 98-102 ℃ for 12-18 minutes, taking out the rubber material A and the rubber material B, standing for 20-30 hours, and marking as rubber material C;
(3) three-stage mixing: adding stearic acid, metal oxide, carbon black and an anti-aging agent into the rubber material C, mixing at 75-85 ℃, standing for 4-8 hours, and marking as rubber material D;
(4) four-stage mixing: adding an auxiliary crosslinking agent and a crosslinking agent into the rubber material D, mixing at the temperature of below 45-55 ℃, discharging after thin passing, and standing for 10-14 hours;
(5) and (3) vulcanization: and (3) vulcanizing at the first stage of 10-15 MPa, 160-170 ℃ and 10-30 minutes for the first stage of vulcanization to obtain the high-temperature-resistant, high-strength and high-expansion-rate rubber.
10. An oil pipe expansion bridge plug, which is characterized by being prepared from the high-temperature-resistant, high-strength and high-expansion-rate rubber as claimed in any one of claims 1 to 8.
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Cited By (3)
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| CN112679810A (en) * | 2020-12-15 | 2021-04-20 | 泉州市华实橡塑科技有限公司 | Rubber compound for diamond wire saw, preparation method and diamond wire saw |
| CN113603945A (en) * | 2021-08-12 | 2021-11-05 | 中铁工程装备集团有限公司 | Oil-resistant, heat-resistant and wear-resistant rubber material, preparation method thereof and application thereof in shield machine sealing |
| CN116023723A (en) * | 2021-10-27 | 2023-04-28 | 中国石油化工股份有限公司 | Hydrogenated nitrile rubber composition and application thereof, vulcanized rubber and preparation method and application thereof |
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Cited By (4)
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| CN112679810A (en) * | 2020-12-15 | 2021-04-20 | 泉州市华实橡塑科技有限公司 | Rubber compound for diamond wire saw, preparation method and diamond wire saw |
| CN113603945A (en) * | 2021-08-12 | 2021-11-05 | 中铁工程装备集团有限公司 | Oil-resistant, heat-resistant and wear-resistant rubber material, preparation method thereof and application thereof in shield machine sealing |
| CN113603945B (en) * | 2021-08-12 | 2023-08-04 | 中铁工程装备集团有限公司 | Oil-resistant heat-resistant wear-resistant rubber material, preparation method and application thereof in shield machine sealing |
| CN116023723A (en) * | 2021-10-27 | 2023-04-28 | 中国石油化工股份有限公司 | Hydrogenated nitrile rubber composition and application thereof, vulcanized rubber and preparation method and application thereof |
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