Rubber composition, product thereof, preparation method and application of rubber composition in packer rubber sleeve

Abstract

The invention discloses a rubber composition, a product thereof, a preparation method and application of the rubber composition in a packer rubber sleeve. The rubber composition comprises the following components in parts by weight: 100 parts of hydrogenated butadiene-acrylonitrile rubber, 50-55 parts of carbon black, 1.5-2 parts of an anti-aging agent, 0.5 part of a plasticizer and 6.5-7 parts of a vulcanizing agent, and the anti-aging agent is a 2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer, or a mixture of the 2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer and styrenated phenol, or a mixture of the 2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer and the styrenated phenol. The rubber composition provided by the invention has the beneficial effects that the hydrogenated butadiene-acrylonitrile rubber, the carbon black, the plasticizer, the vulcanizing agent and the anti-aging agent with limited composition are adopted as raw materials and are proportioned according to a proper weight ratio, so that the rubber composition with high mechanical strength, high wear resistance and low cost can be prepared. And the rubber product has excellent chemical resistance, oil resistance, high-temperature aging resistance and compression set resistance, and completely meets the use requirements of the existing packer rubber sleeve.

Description

Technical Field

[0001] The invention belongs to the technical field of elastomeric materials, and in particular relates to a rubber composition, a product thereof, a preparation method thereof and an application in a packer rubber cylinder. Background Art

[0002] The packer is an elastic sealing element located between the casing and the tubing. Its main functions include: (1) isolating the production layer or target layer to prevent the fluid and pressure between the layers from interfering with each other; (2) ensuring the pressure of the sealing layer and improving the production efficiency of the oil well; (3) cooperating with the casing inspection, leak detection, acid fracturing, water injection, well washing and other operations. The packer is of great significance to the production of oil and gas.

[0003] The packer itself is composed of steel parts and rubber cylinders. The rubber cylinder is the key component of the packer. Its development has gone through metal, asbestos, and the current elastomer materials, covering rubber products and plastics. At present, the rubber cylinders with a high market share are mainly based on ethylene propylene diene monomer rubber (EPDM), nitrile rubber (NBR), hydrogenated nitrile rubber (HNBR), fluororubber (FKM), etc. In the process of use, it is found that the packer rubber cylinders based on EPDM and NBR are very easy to expand in the crude oil environment. In addition, the high temperature, high pressure and corrosive environment downhole, the rubber cylinder gradually relaxes and ages, which is manifested as increased hardness, decreased elasticity, reduced strength, and reduced service life. HNBR and FKM, relatively speaking, have better oleophobicity and can better slow down the penetration of corrosive gases and liquids, so they are used in the preparation of packer rubber cylinders. Among them, FKM has a deviation in processability and a higher price. Therefore, for harsh downhole working conditions, HNBR rubber cylinders are generally used.

[0004] At present, II-70 type (II represents the mixed rubber with hydrogenated nitrile as the main body, and 70 represents the Shore hardness of the rubber cylinder) packer rubber cylinder has a large market usage, but the performance varies greatly. Currently, there is still a lack of products with outstanding comprehensive physical properties including mechanical strength, chemical tolerance, high temperature aging resistance, compression deformation resistance, and oil resistance. Summary of the invention

[0005] In view of the shortcomings of the prior art, the present invention provides a rubber composition, its product, preparation method and application in a packer rubber sleeve. The present invention can obtain a rubber composition with excellent comprehensive physical properties and apply it to a packer rubber sleeve by optimizing the raw material ratio.

[0006] One aspect of the present invention provides a rubber composition, which includes the following components in parts by weight: 100 parts of hydrogenated nitrile rubber, 50-55 parts of carbon black, 1.5-2 parts of antioxidant, 0.5 part of plasticizer, and 6.5-7 parts of vulcanizer; the antioxidant is 2,2,4-trimethyl-1,2-dihydroquinoline polymer, or a mixture of 2,2,4-trimethyl-1,2-dihydroquinoline polymer and styrenated phenol.

[0007] As a specific embodiment of the present invention, the antioxidant is a mixture of 2,2,4-trimethyl-1,2-dihydroquinoline polymer and styrenated phenol, in which the mass ratio of 2,2,4-trimethyl-1,2-dihydroquinoline polymer to styrenated phenol is 1-2:1-2, preferably 1:2.

[0008] As a specific embodiment of the present invention, the carbon black is selected from any one of N110 to N220 carbon black, preferably N110 carbon black or N220 carbon black.

[0009] As a specific embodiment of the present invention, the plasticizer is selected from any one of dioctyl terephthalate and di(2-ethylhexyl) phthalate.

[0010] As a specific embodiment of the present invention, the vulcanizing agent includes a peroxide vulcanizing agent, preferably di-tert-butyl peroxide isopropylbenzene.

[0011] The second aspect of the present invention provides a method for preparing the aforementioned rubber composition, comprising: mixing hydrogenated nitrile rubber, carbon black, an antioxidant, a plasticizer and a vulcanizing agent, and vulcanizing the mixed rubber; preferably, first vulcanizing at 175°C for 6.41 to 10.41 minutes, and then vulcanizing at 150°C for 4 hours.

[0012] A third aspect of the present invention provides an annular blowout preventer, comprising a shell, a top cover, a packer rubber cylinder and a piston, wherein the packer rubber cylinder is made of the aforementioned rubber composition.

[0013] A fourth aspect of the present invention provides an oilfield wellhead operation device, which includes the aforementioned annular blowout preventer.

[0014] A fifth aspect of the present invention provides use of the aforementioned rubber composition in a packer rubber sleeve.

[0015] The beneficial effects of the present invention are:

[0016] The rubber composition provided by the present invention adopts hydrogenated nitrile rubber, carbon black, a plasticizer, a vulcanizer and an antioxidant of a limited composition as raw materials and performs appropriate weight proportioning, so as to prepare a rubber product with high mechanical strength and excellent resistance to chemicals, oil, high temperature aging and compression permanent deformation, which can fully meet the use requirements of existing packer rubber cylinders. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is the vulcanization curve test result of the rubber compound obtained after plasticating on the open mill in Example 1. DETAILED DESCRIPTION

[0018] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0019] Example 1

[0020] 100 parts of hydrogenated nitrile rubber (HNBR), 55 parts of carbon black (N110), 2 parts of antioxidant (RD (TMQ)), 0.5 parts of plasticizer (DOTP), and 7 parts of peroxide curing agent (BIPB).

[0021] The preparation method is as follows:

[0022] Use a 200mL internal mixer, adjust the starting temperature to 45°C and the speed to 50rpm. Lift the top bolt, add HNBR within 15 seconds, close the top bolt, and mix for 45 seconds. Lift the top bolt, add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Lift the top bolt again, add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Mix for another 60 seconds and discharge the glue.

[0023] Take out the rubber compound from the internal mixer and weigh it. Compare it with the total mass of all raw materials added to the internal mixer. The rubber compound loss should be controlled within 3%. Adjust the roller temperature of the open mixer to 40℃ and the roller distance to 1.0mm. Mix the rubber compound taken out from the internal mixer to make it into sheets, and then adjust the roller distance to 0.10mm. First, turn over three times, add vulcanizing agent, turn over three times, roll six times, and take off the sheet. After standing for 16 hours, perform the vulcanization curve test.

[0024] Through the rotorless vulcanizer test, it was determined that when the vulcanization temperature was 175°C, t 90 =6.41min. Vulcanize in a flat vulcanizer for 9.41min, let stand for 4h, perform a second stage vulcanization at 150℃×4h, take out the rubber material, and let stand at room temperature for 16h. Cut the rubber material into dumbbell-shaped specimens and conduct relevant performance tests. The results are shown in Table 1.

[0025] Table 1 Physical properties test results

[0026]

[0027] Example 2

[0028] 100 parts of hydrogenated nitrile rubber (HNBR), 50 parts of carbon black (N110), 1.5 parts of antioxidant (RD (TMQ)), 0.5 parts of plasticizer (DOTP), and 7 parts of peroxide curing agent (BIPB).

[0029] The preparation method is as follows:

[0030] Use a 200mL internal mixer, adjust the starting temperature to 45°C and the speed to 50rpm. Lift the top bolt, add HNBR within 15 seconds, close the top bolt, and mix for 45 seconds. Lift the top bolt, add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Lift the top bolt again, add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Mix for another 60 seconds and discharge the glue.

[0031] Take out the rubber compound from the internal mixer and weigh it. Compare it with the total mass of all raw materials added to the internal mixer. The rubber compound loss should be controlled within 3%. Adjust the roller temperature of the open mixer to 40℃ and the roller distance to 1.0mm. Mix the rubber compound taken out from the internal mixer to make it into sheets, and then adjust the roller distance to 0.10mm. First, turn over three times, add vulcanizing agent, turn over three times, roll six times, and take off the sheet. After standing for 16 hours, perform the vulcanization curve test.

[0032] Through the rotorless vulcanizer test, it was determined that when the vulcanization temperature was 175°C, t 90 =6.41min. Vulcanize in a flat vulcanizer for 8.41min, let stand for 4h, perform a second stage vulcanization at 150℃×4h, take out the rubber, and let stand at room temperature for 16h. Cut the rubber into dumbbell-shaped specimens and conduct relevant performance tests. The results are shown in Table 2.

[0033] Table 2 Physical properties test results

[0034]

[0035] Example 3

[0036] 100 parts of hydrogenated nitrile rubber (HNBR), 50 parts of carbon black (N220), 2 parts of antioxidant (RD (TMQ)), 0.5 parts of plasticizer (DOTP), and 7 parts of peroxide curing agent (BIPB).

[0037] The preparation method is as follows:

[0038] Use a 200mL internal mixer, adjust the starting temperature to 45°C and the speed to 50rpm. Lift the top bolt, add HNBR within 15 seconds, close the top bolt, and mix for 45 seconds. Lift the top bolt, add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Lift the top bolt again, add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Mix for another 60 seconds and discharge the glue.

[0039] Take out the rubber compound from the internal mixer and weigh it. Compare it with the total mass of all raw materials added to the internal mixer. The rubber compound loss should be controlled within 3%. Adjust the roller temperature of the open mixer to 40℃ and the roller distance to 1.0mm. Mix the rubber compound taken out from the internal mixer to make it into sheets, and then adjust the roller distance to 0.10mm. First, turn over three times, add vulcanizing agent, turn over three times, roll six times, and take off the sheet. After standing for 16 hours, perform the vulcanization curve test.

[0040] Through the rotorless vulcanizer test, it was determined that when the vulcanization temperature was 175°C, t 90 =6.41min. Vulcanize in a flat vulcanizer for 8.41min, let stand for 4h, perform a second stage vulcanization at 150℃×4h, take out the rubber, and let stand at room temperature for 16h. Cut the rubber into dumbbell-shaped specimens and conduct relevant performance tests. The results are shown in Table 3.

[0041] Table 3 Physical properties test results

[0042]

[0043]

[0044] Example 4

[0045] 100 parts of hydrogenated nitrile rubber (HNBR), 50 parts of carbon black (N110), 2 parts of antioxidant (RD (TMQ)), 0.5 parts of plasticizer (DOTP), and 6.5 parts of peroxide curing agent (BIPB).

[0046] The preparation method is as follows:

[0047] Use a 200mL internal mixer, adjust the starting temperature to 45°C and the speed to 50rpm. Lift the top bolt, add HNBR within 15 seconds, close the top bolt, and mix for 45 seconds. Lift the top bolt, add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Lift the top bolt again, add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Mix for another 60 seconds and discharge the glue.

[0048] Take out the rubber compound from the internal mixer and weigh it. Compare it with the total mass of all raw materials added to the internal mixer. The rubber compound loss should be controlled within 3%. Adjust the roller temperature of the open mixer to 40℃ and the roller distance to 1.0mm. Mix the rubber compound taken out from the internal mixer to make it into sheets, and then adjust the roller distance to 0.10mm. First, turn over three times, add vulcanizing agent, turn over three times, roll six times, and take off the sheet. After standing for 16 hours, perform the vulcanization curve test.

[0049] Through the rotorless vulcanizer test, it was determined that when the vulcanization temperature was 175°C, t 90 =6.41min. Vulcanize in a flat vulcanizer for 9.41min, let stand for 4h, perform a second stage vulcanization at 150℃×4h, take out the rubber material, and let stand at room temperature for 16h. Cut the rubber material into dumbbell-shaped specimens and conduct relevant performance tests. The results are shown in Table 4.

[0050] Table 4 Physical properties test results

[0051]

[0052]

[0053] Example 5

[0054] 100 parts of hydrogenated nitrile rubber (HNBR), 50 parts of carbon black (N110), 2 parts of antioxidant (RD (TMQ)), 0.5 parts of plasticizer (DOTP), and 7 parts of peroxide curing agent (BIPB).

[0055] The preparation method is as follows:

[0056] Use a 200mL internal mixer, adjust the starting temperature to 45°C and the speed to 50rpm. Lift the top bolt, add HNBR within 15 seconds, close the top bolt, and mix for 45 seconds. Lift the top bolt, add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Lift the top bolt again, add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Mix for another 60 seconds and discharge the glue.

[0057] Take out the rubber compound from the internal mixer and weigh it. Compare it with the total mass of all raw materials added to the internal mixer. The rubber compound loss should be controlled within 3%. Adjust the roller temperature of the open mixer to 40℃ and the roller distance to 1.0mm. Mix the rubber compound taken out from the internal mixer to make it into sheets, and then adjust the roller distance to 0.10mm. First, turn over three times, add vulcanizing agent, turn over three times, roll six times, and take off the sheet. After standing for 16 hours, perform the vulcanization curve test.

[0058] Through the rotorless vulcanizer test, it was determined that when the vulcanization temperature was 175°C, t 90=6.41min. Vulcanize in a flat vulcanizer for 9.41min, let stand for 4h, perform a second stage vulcanization at 150℃×4h, take out the rubber, and let stand at room temperature for 16h. Cut the rubber into dumbbell-shaped specimens and conduct relevant performance tests. The results are shown in Table 5.

[0059] Table 5 Physical properties test results

[0060]

[0061]

[0062] Example 6

[0063] 100 parts of hydrogenated nitrile rubber (HNBR), 50 parts of carbon black (N110), 2 parts of antioxidant (RD (TMQ) / SP = 1:1), 0.5 parts of plasticizer (DOTP), and 7 parts of peroxide curing agent (BIPB).

[0064] The preparation method is as follows:

[0065] Use a 200mL internal mixer, adjust the starting temperature to 45°C and the speed to 50rpm. Lift the top bolt, add HNBR within 15 seconds, close the top bolt, and mix for 45 seconds. Lift the top bolt, add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Lift the top bolt again, add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Mix for another 60 seconds and discharge the glue.

[0066] Take out the rubber compound from the internal mixer and weigh it. Compare it with the total mass of all raw materials added to the internal mixer. The rubber compound loss should be controlled within 3%. Adjust the roller temperature of the open mixer to 40℃ and the roller distance to 1.0mm. Mix the rubber compound taken out from the internal mixer to make it into sheets, and then adjust the roller distance to 0.10mm. First, turn over three times, add vulcanizing agent, turn over three times, roll six times, and take off the sheet. After standing for 16 hours, perform the vulcanization curve test.

[0067] Through the rotorless vulcanizer test, it was determined that when the vulcanization temperature was 175°C, t 90 =6.41min. Vulcanize in a flat vulcanizer for 8.41min, let stand for 4h, perform a second stage vulcanization at 150℃×4h, take out the rubber material, and let stand at room temperature for 16h. Cut the rubber material into dumbbell-shaped specimens and conduct relevant performance tests. The results are shown in Table 6.

[0068] Table 6 Physical properties test results

[0069]

[0070] Example 7

[0071] 100 parts of hydrogenated nitrile rubber (HNBR), 50 parts of carbon black (N110), 2 parts of antioxidant (RD (TMQ) / SP = 1:2), 0.5 parts of plasticizer (DOTP), and 7 parts of peroxide curing agent (BIPB).

[0072] The preparation method is as follows:

[0073] Use a 200mL internal mixer, adjust the starting temperature to 45°C and the speed to 50rpm. Lift the top bolt, add HNBR within 15 seconds, close the top bolt, and mix for 45 seconds. Lift the top bolt, add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Lift the top bolt again, add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Mix for another 60 seconds and discharge the glue.

[0074] Take out the rubber compound from the internal mixer and weigh it. Compare it with the total mass of all raw materials added to the internal mixer. The rubber compound loss should be controlled within 3%. Adjust the roller temperature of the open mixer to 40℃ and the roller distance to 1.0mm. Mix the rubber compound taken out from the internal mixer to make it into sheets, and then adjust the roller distance to 0.10mm. First, turn over three times, add vulcanizing agent, turn over three times, roll six times, and take off the sheet. After standing for 16 hours, perform the vulcanization curve test.

[0075] Through the rotorless vulcanizer test, it was determined that when the vulcanization temperature was 175°C, t 90 =6.41min. Vulcanize in a flat vulcanizer for 8.41min, let stand for 4h, perform a second stage vulcanization at 150℃×4h, take out the rubber material, and let stand at room temperature for 16h. Cut the rubber material into dumbbell-shaped specimens and conduct relevant performance tests. The results are shown in Table 7.

[0076] Table 7 Physical properties test results

[0077]

[0078] Example 8

[0079] 100 parts of hydrogenated nitrile rubber (HNBR), 50 parts of carbon black (N110), 2 parts of antioxidant (RD (TMQ) / SP = 2:1), 0.5 parts of plasticizer (DOTP), and 7 parts of peroxide curing agent (BIPB).

[0080] The preparation method is as follows:

[0081] Use a 200mL internal mixer, adjust the starting temperature to 45°C and the speed to 50rpm. Lift the top bolt, add HNBR within 15 seconds, close the top bolt, and mix for 45 seconds. Lift the top bolt, add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Lift the top bolt again, add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Mix for another 60 seconds and discharge the glue.

[0082] Take out the rubber compound from the internal mixer and weigh it. Compare it with the total mass of all raw materials added to the internal mixer. The rubber compound loss should be controlled within 3%. Adjust the roller temperature of the open mixer to 40℃ and the roller distance to 1.0mm. Mix the rubber compound taken out from the internal mixer to make it into sheets, and then adjust the roller distance to 0.10mm. First, turn over three times, add vulcanizing agent, turn over three times, roll six times, and take off the sheet. After standing for 16 hours, perform the vulcanization curve test.

[0083] Through the rotorless vulcanizer test, it was determined that when the vulcanization temperature was 175°C, t 90 =6.41min. Vulcanize in a flat vulcanizer for 8.41min, let stand for 4h, perform a second stage vulcanization at 150℃×4h, take out the rubber material, and let stand at room temperature for 16h. Cut the rubber material into dumbbell-shaped specimens and conduct relevant performance tests. The results are shown in Table 8.

[0084] Table 8 Physical properties test results

[0085]

[0086] Example 9

[0087] 100 parts of hydrogenated nitrile rubber (HNBR), 50 parts of carbon black (N110), 2 parts of antioxidant (RD (TMQ)), 0.5 parts of plasticizer DOP (di(2-ethylhexyl) phthalate), and 7 parts of peroxide vulcanizing agent (BIPB).

[0088] The preparation method is as follows:

[0089] Use a 200mL internal mixer, adjust the starting temperature to 45°C and the speed to 50rpm. Lift the top bolt, add HNBR within 15 seconds, close the top bolt, and mix for 45 seconds. Lift the top bolt, add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Lift the top bolt again, add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Mix for another 60 seconds and discharge the glue.

[0090] Take out the rubber compound from the internal mixer and weigh it. Compare it with the total mass of all raw materials added to the internal mixer. The rubber compound loss should be controlled within 3%. Adjust the roller temperature of the open mixer to 40℃ and the roller distance to 1.0mm. Mix the rubber compound taken out from the internal mixer to make it into sheets, and then adjust the roller distance to 0.10mm. First, turn over three times, add vulcanizing agent, turn over three times, roll six times, and take off the sheet. After standing for 16 hours, perform the vulcanization curve test.

[0091] Through the rotorless vulcanizer test, it was determined that when the vulcanization temperature was 175°C, t 90 =6.41min. Vulcanize in a flat vulcanizer for 8.41min, let stand for 4h, perform a second stage vulcanization at 150℃×4h, take out the rubber material, and let stand at room temperature for 16h. Cut the rubber material into dumbbell-shaped specimens and conduct relevant performance tests. The results are shown in Table 9.

[0092] Table 9 Physical properties test results

[0093]

[0094]

[0095] When the plasticizer was replaced by DOP from DOTP in the experiment, some properties of the mixed rubber decreased (including hot air aging, etc.), as shown in Table 12. The main reason for this phenomenon is the difference in polarity, volatility, etc. caused by the different molecular structures of the two plasticizers.

[0096] Comparative Example 1

[0097] 100 parts of hydrogenated nitrile rubber (HNBR), 50 parts of carbon black (N110), 2 parts of antioxidant SP (styrenated phenol), 0.5 parts of plasticizer (DOTP), and 7 parts of peroxide vulcanizing agent (BIPB).

[0098] The preparation method is as follows:

[0099] Use a 200mL internal mixer, adjust the starting temperature to 45°C and the speed to 50rpm. Lift the top bolt, add HNBR within 15 seconds, close the top bolt, and mix for 45 seconds. Lift the top bolt, add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Lift the top bolt again, add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Mix for another 60 seconds and discharge the glue.

[0100] Take out the rubber compound from the internal mixer and weigh it. Compare it with the total mass of all raw materials added to the internal mixer. The rubber compound loss should be controlled within 3%. Adjust the roller temperature of the open mixer to 40℃ and the roller distance to 1.0mm. Mix the rubber compound taken out from the internal mixer to make it into sheets, and then adjust the roller distance to 0.10mm. First, turn over three times, add vulcanizing agent, turn over three times, roll six times, and take off the sheet. After standing for 16 hours, perform the vulcanization curve test.

[0101] Through the rotorless vulcanizer test, it was determined that when the vulcanization temperature was 175°C, t 90 =6.41min. Vulcanize in a flat vulcanizer for 8.41min, let stand for 4h, perform a second stage vulcanization at 150℃×4h, take out the rubber material, and let stand at room temperature for 16h. Cut the rubber material into dumbbell-shaped specimens and conduct relevant performance tests. The results are shown in Table 10.

[0102] Table 10 Physical properties test results

[0103]

[0104]

[0105] Compared with Comparative Example 1, the only difference between Examples 6 to 8 is that Examples 6 to 8 use a mixture of RD (TMQ) and SP as an antioxidant, while Comparative Example 1 uses a single SP as an antioxidant. The results show that when only SP is used as an antioxidant, the physical properties of the mixed rubber decrease, and even some properties (compression permanent deformation) do not meet the standard requirements. When a mixed antioxidant is used, the performance is improved. By optimizing the ratio, it is found that when RD (TMQ) / SP = 1:2, the performance of the mixed rubber is the best. The main reason may be that both antioxidants are "free radical termination type" antioxidants, which have a synergistic anti-aging effect during use, thereby reducing compression permanent deformation.

[0106] Comparative Example 2

[0107] 100 parts of hydrogenated nitrile rubber (HNBR), 50 parts of carbon black (N110), 2 parts of antioxidant (RD (TMQ)), 0.5 parts of plasticizer (DOTP), and 7 parts of peroxide curing agent (BIPB).

[0108] The preparation method is as follows:

[0109] Use a 200mL internal mixer, adjust the starting temperature to 45°C and the speed to 50rpm. Lift the top bolt, add HNBR within 15 seconds, close the top bolt, and mix for 45 seconds. Lift the top bolt, add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Lift the top bolt again, add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer in sequence within 30 seconds, close the top bolt and mix for 30 seconds. Mix for another 60 seconds and discharge the glue.

[0110] Take out the rubber compound from the internal mixer and weigh it. Compare it with the total mass of all raw materials added to the internal mixer. The rubber compound loss should be controlled within 3%. Adjust the roller temperature of the open mixer to 40℃ and the roller distance to 1.0mm. Mix the rubber compound taken out from the internal mixer to make it into sheets, and then adjust the roller distance to 0.10mm. First, turn over three times, add vulcanizing agent, turn over three times, roll six times, and take off the sheet. After standing for 16 hours, perform the vulcanization curve test.

[0111] Through the rotorless vulcanizer test, it was determined that when the vulcanization temperature was 175°C, t 90 =6.41min. Vulcanize in a flat vulcanizer for 9.41min and let stand at room temperature for 16h. Cut the rubber into dumbbell-shaped specimens and conduct relevant performance tests. The results are shown in Table 11.

[0112] Table 11 Physical properties test results

[0113]

[0114] The only difference between Example 5 and Comparative Example 2 is that Example 5 adds two-stage vulcanization, while Comparative Example 2 does not use two-stage vulcanization. The results show that the physical properties of the sample of Comparative Example 2 and the sample of Example 5 are very different, and even the compression permanent deformation performance of the sample of Comparative Example 2 does not meet the standard requirements. This shows the necessity of two-stage vulcanization in the sample preparation process, which is beneficial to improving the comprehensive physical properties of the mixed rubber.

[0115] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

Claims

1. A rubber composition, characterized in that: By weight, it includes the following components: 100 parts of hydrogenated nitrile rubber, 50-55 parts of carbon black, 1.5-2 parts of antioxidant, 0.5 parts of plasticizer, 6.5-7 parts of vulcanizing agent; The antioxidant is a 2,2,4-trimethyl-1,2-dihydroquinoline polymer or a mixture of a 2,2,4-trimethyl-1,2-dihydroquinoline polymer and styrenated phenol.

2. The rubber composition according to claim 1, characterized in that: The antioxidant is a mixture of 2,2,4-trimethyl-1,2-dihydroquinoline polymer and styrenated phenol. In the mixture, the mass ratio of 2,2,4-trimethyl-1,2-dihydroquinoline polymer to styrenated phenol is 1-2:1-2.

3. The rubber composition according to claim 2, characterized in that: In the mixture, the mass ratio of 2,2,4-trimethyl-1,2-dihydroquinoline polymer to styrenated phenol is 1:

2.

4. The rubber composition according to claim 1, characterized in that: The carbon black is selected from any one of N110 to N220 carbon black; preferably, the carbon black is N110 carbon black or N220 carbon black.

5. The rubber composition according to claim 1, characterized in that: The plasticizer is selected from any one of dioctyl terephthalate and di(2-ethylhexyl) phthalate.

6. The rubber composition according to claim 1, characterized in that: The vulcanizing agent includes a peroxide vulcanizing agent; preferably, the peroxide vulcanizing agent includes di-tert-butyl peroxide isopropylbenzene.

7. A method for preparing the rubber composition according to any one of claims 1 to 6, characterized in that: The preparation method comprises: mixing hydrogenated nitrile rubber, carbon black, antioxidant, plasticizer and vulcanizing agent, and vulcanizing the mixed rubber; preferably, the vulcanization is first vulcanizing at 175° C. for 6.41 to 10.41 minutes, and then vulcanizing at 150° C. for 4 hours.

8. An annular blowout preventer, comprising a housing, a top cover, a packer rubber cylinder and a piston, characterized in that: The material of the packer rubber sleeve is the rubber composition as claimed in any one of claims 1 to 6.

9. An oilfield wellhead operation device, characterized in that: It comprises the annular blowout preventer as claimed in claim 8.

10. Use of the rubber composition according to any one of claims 1 to 6 in a packer rubber sleeve.

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