A rubber material, a method of making the same, and packer boots based thereon

Abstract

The application provides a rubber material, a preparation method thereof and a packer rubber sleeve based on the rubber material, and the rubber material comprises, in terms of mass fraction, 100 parts of hydrogenated nitrile rubber, 60-70 parts of carbon black, 2 parts of an antioxidant, 0.5 parts of a plasticizer and 6.5-7.0 parts of a peroxide vulcanizing agent; the antioxidant is RD (TMQ) or a mixture of RD (TMQ) and styrenated phenol. The rubber material of the application is added with the antioxidant RD (TMQ) or the mixture of RD (TMQ) and styrenated phenol, and can achieve a good anti-aging effect; when RD (TMQ) and SP are used together, the aging performance of the rubber material can be further improved, which indicates that RD (TMQ) and SP can achieve a certain synergistic effect; and the overall performance of the rubber material of the application meets the requirements of relevant standards. The rubber material of the application is used to prepare a packer rubber sleeve, and a high-performance and low-cost packer rubber sleeve product can be achieved.

Description

Technical Field

[0001] This invention belongs to the field of elastomer materials, and relates to a rubber material, its preparation method, and a packer cartridge based thereon. Background Technology

[0002] Packers are elastic sealing elements located between casing and tubing, and are of great importance for oil and gas extraction. The main functions of packers include: (1) sealing the producing or target layer to prevent fluids and pressures from interfering with each other; (2) ensuring the pressure of the sealing layer and improving the production efficiency of the oil well; and (3) assisting in operations such as casing inspection, leak detection, acid fracturing, water injection, and well washing.

[0003] The packer itself consists of steel components and a rubber sleeve. The rubber sleeve is a key component of the packer, and its development has progressed from metal to asbestos, and now to elastomer materials, encompassing rubber products and plastics. Currently, the most common rubber sleeves on the market are made primarily of ethylene propylene diene monomer (EPDM), nitrile butadiene rubber (NBR), hydrogenated nitrile butadiene rubber (HNBR), and fluororubber (FKM). During use, it has been found that EPDM and NBR-based packer sleeves are prone to expansion in crude oil environments. Combined with the high temperature, high pressure, and corrosive environment downhole, the sleeves gradually experience stress relaxation and aging, resulting in increased hardness, decreased elasticity, and reduced strength, thus shortening their service life. HNBR and FKM, relatively speaking, have better oleophobic properties and can better mitigate the penetration of corrosive gases and liquids, therefore they are used in the manufacture of packer sleeves. However, FKM has processing deviations and a higher price. Therefore, for harsh downhole conditions, HNBR material sleeves are generally used.

[0004] Currently, the II-80 type (II represents the compound rubber mainly composed of hydrogenated nitrile butadiene rubber, and 80 represents the Shore hardness of the rubber cartridge) packer cartridges have a large market share, but their performance varies greatly and needs further improvement. Summary of the Invention

[0005] To address the problems of the prior art, this invention provides a rubber material, a method for preparing the same, and a packer cartridge based thereon. The rubber material of this invention enables the commercialization of high-performance, cost-effective, and highly durable cartridges.

[0006] This invention is achieved through the following technical solution:

[0007] A rubber material, by weight parts, comprises: 100 parts hydrogenated nitrile rubber, 60-70 parts carbon black, 2 parts antioxidant, 0.5 parts plasticizer, and 6.5-7.0 parts peroxide vulcanizing agent; wherein the antioxidant is RD(TMQ), or a mixture of RD(TMQ) and styrene-modified phenol.

[0008] Preferably, when the antioxidant is a mixture of RD(TMQ) and SP, the ratio of RD(TMQ) to SP is 1:2.

[0009] Preferably, the carbon black is carbon black N220.

[0010] Preferably, the plasticizer is dioctyl terephthalate.

[0011] Preferably, the peroxide sulfiding agent is bis-tert-butylperoxide isopropylbenzene.

[0012] The method for preparing the rubber material includes:

[0013] Hydrogenated nitrile butadiene rubber is mixed; some carbon black, some antioxidant and some plasticizer are added and mixed; the remaining carbon black, antioxidant and plasticizer are added and mixed, and the rubber compound is discharged to obtain the rubber compound;

[0014] The rubber compound is plasticized; a portion of the peroxide vulcanizing agent is added and plasticized again; then the remaining vulcanizing agent is added and plasticized again.

[0015] The plasticized rubber compound undergoes a first-stage vulcanization and a second-stage vulcanization.

[0016] Preferably, the vulcanization time is 8.77 to 10.77 minutes.

[0017] Preferably, the plasticizing temperature is 45–50°C.

[0018] Preferably, the plasticized rubber compound is subjected to vulcanization curve testing, and the plasticized rubber compound is subjected to a first-stage vulcanization based on the test results.

[0019] A packer sleeve, the material of which is the aforementioned rubber material.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] This invention relates to a rubber material based on hydrogenated nitrile butadiene rubber, incorporating an anti-aging agent RD(TMQ) or a mixture of RD(TMQ) and SP (styrene-modified phenol). This combination provides excellent anti-aging effects, particularly when RD(TMQ) and SP are used in combination, further improving the aging performance of the rubber material, indicating a synergistic effect between the two. The addition of carbon black increases the hardness of the rubber material, while the addition of a plasticizer increases its elongation at break. The overall performance of the rubber material of this invention meets relevant standards.

[0022] Furthermore, when RD(TMQ) / SP = 1:2, the rubber material exhibits the best performance, significantly outperforming the performance of RD(TMQ) and SP alone as antioxidants.

[0023] The method for preparing the rubber material of the present invention involves two-stage vulcanization of the compound. Experimental results show that the material properties obtained by two-stage vulcanization are superior to those obtained by single-stage vulcanization, indicating that two-stage vulcanization is crucial to the preparation of the rubber material of the present invention.

[0024] Using the rubber material of this invention to prepare packer cartridges can achieve the commercialization of high-performance, cost-effective, and highly durable cartridges. Attached Figure Description

[0025] Figure 1 The vulcanization curve of the rubber compound obtained after plasticizing on the open mill in Example 1 is shown. Detailed Implementation

[0026] To further understand the present invention, the present invention will be described below with reference to embodiments. These descriptions are only for further explaining the features and advantages of the present invention and are not intended to limit the claims of the present invention.

[0027] The rubber material of the present invention comprises, by weight parts: 100 parts hydrogenated nitrile rubber, 60-70 parts carbon black, 2 parts antioxidant, 0.5 parts plasticizer, and 6.5-7.0 parts peroxide vulcanizing agent; wherein the antioxidant is RD(TMQ), or a mixture of RD(TMQ) and SP.

[0028] The carbon black is preferably carbon black N220, the plasticizer is preferably dioctyl terephthalate, and the peroxide vulcanizing agent is preferably bis-tert-butylperoxide isopropylbenzene. When the antioxidant is a mixture of RD(TMQ) and SP, the ratio of RD(TMQ) to SP is preferably 1:2.

[0029] The method for preparing the rubber material of the present invention includes:

[0030] Hydrogenated nitrile rubber was added and mixed using an internal mixer; some carbon black, antioxidant, and plasticizer were added and mixed; the remaining carbon black, antioxidant, and plasticizer were added and mixed; the rubber compound was discharged to obtain the final product.

[0031] Adjust the roller temperature of the open mill to 45-50℃ and the roller gap to 1.0mm. Plasticize the rubber compound taken from the internal mixer until it forms sheets. Then adjust the roller gap to 0.1-0.15mm. Repeat the rolling several times, add 1 / 2 equivalent vulcanizing agent, repeat the rolling several times, add the remaining vulcanizing agent, and repeat the rolling several times. Roll the sheets several times and then sheet them. After standing, perform vulcanization curve testing.

[0032] Vulcanize in a flat vulcanizer for 8.77–10.77 min, let stand, perform a second stage of vulcanization, remove the rubber compound, and let it stand at room temperature.

[0033] The rubber material can be used to prepare the rubber sleeve of the packer.

[0034] The following examples illustrate this.

[0035] Example 1

[0036] 100 parts hydrogenated nitrile rubber, 70 parts carbon black N220, 2 parts antioxidant RD (TMQ), 0.5 parts plasticizer dioctyl terephthalate (DOTP), and 6.5 parts peroxide vulcanizing agent bis-tert-butyl peroxide isopropylbenzene (BIPB).

[0037] Sample preparation:

[0038] Using a 200mL internal mixer, adjust the initial temperature to 50℃ and the rotation speed to 40rpm. Lift the top plug and add the hydrogenated nitrile rubber within 15 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Mix for another 60 seconds, discharge the rubber compound, and obtain the final rubber compound.

[0039] Weigh the internally mixed rubber compound and compare it with the total mass of all raw materials added to the internal mixer. The loss of rubber compound should be controlled within 3%. Adjust the roller temperature of the open mill to 45℃ and the roller gap to 1.0mm. Plasticize the rubber compound taken from the internal mixer until it forms sheets, then adjust the roller gap to 0.12mm. First, recycle three times, adding 1 / 2 equivalent vulcanizing agent and recycling three more times. Then add the remaining vulcanizing agent and recycle three more times. Roll the mixture six times and sheet it. After standing for 16 hours, perform vulcanization curve testing.

[0040] Using a rotorless vulcanizing apparatus, it was determined that at a vulcanizing temperature of 175℃, t 10 =0.58min,t 90 =6.77min, Figure 1 This is the vulcanization curve of the rubber compound obtained after plasticizing on an open mill. The compound was vulcanized in a flat vulcanizing apparatus for 8.77 min, allowed to stand for 4 h, and then subjected to a second-stage vulcanization at 150℃ for 4 h. The compound was then removed and allowed to stand at room temperature for 16 h. The compound was cut into dumbbell-shaped samples, and relevant performance tests were performed according to "HG / T2701-2016 Compression Packer Cylinder". The test results are shown in Table 1.

[0041] Table 1. Results of physical property testing of the compound in Example 1

[0042]

[0043]

[0044] Table 1 shows the test results of the physical properties of the compound in Example 1. All test results meet the relevant standard requirements.

[0045] Example 2

[0046] 100 parts hydrogenated nitrile rubber, 70 parts carbon black N220, 2 parts antioxidant RD (TMQ), 0.5 parts plasticizer DOTP, and 7.0 parts peroxide vulcanizing agent BIPB.

[0047] Sample preparation:

[0048] Using a 200mL internal mixer, adjust the initial temperature to 50℃ and the rotation speed to 40rpm. Lift the top plug and add the hydrogenated nitrile rubber within 15 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Mix for another 60 seconds, discharge the rubber compound, and obtain the final rubber compound.

[0049] Weigh the internally mixed rubber compound and compare it with the total mass of all raw materials added to the internal mixer. The loss of rubber compound should be controlled within 3%. Adjust the roller temperature of the open mill to 45℃ and the roller gap to 1.0mm. Plasticize the rubber compound taken from the internal mixer until it forms sheets, then adjust the roller gap to 0.12mm. First, recycle three times, adding 1 / 2 equivalent vulcanizing agent and recycling three more times. Then add the remaining vulcanizing agent and recycle three more times. Roll the mixture six times and sheet it. After standing for 16 hours, perform vulcanization curve testing.

[0050] Using a rotorless vulcanizing apparatus, it was determined that at a vulcanizing temperature of 175℃, t 90 = 6.77 min. The compound was vulcanized in a flat vulcanizing apparatus for 8.77 min, allowed to stand for 4 h, and then subjected to a second-stage vulcanization at 150℃ for 4 h. The compound was then removed and allowed to stand at room temperature for 16 h. The compound was cut into dumbbell-shaped samples, and relevant performance tests were conducted according to "HG / T 2701-2016 Compression Packer Cylinder". The test results are shown in Table 2.

[0051] Table 2. Results of Physical Property Tests for Compounds in Example 2

[0052]

[0053] As shown in Table 2, Example 2, compared to Example 1, increased the amount of BIPB by 0.5 parts, resulting in a significantly larger change in the elongation at break under hot air aging. This indicates that the amount of plasticizer used has a significant impact on the performance of the compound.

[0054] Example 3

[0055] 100 parts hydrogenated nitrile rubber, 60 parts carbon black N220, 2 parts antioxidant RD (TMQ), 0.5 parts plasticizer DOTP, and 7.0 parts peroxide vulcanizing agent BIPB.

[0056] Sample preparation:

[0057] Using a 200mL internal mixer, adjust the initial temperature to 50℃ and the rotation speed to 40rpm. Lift the top plug and add the hydrogenated nitrile rubber within 15 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Mix for another 60 seconds, discharge the rubber compound, and obtain the final rubber compound.

[0058] Weigh the internally mixed rubber compound and compare it with the total mass of all raw materials added to the internal mixer. The loss of rubber compound should be controlled within 3%. Adjust the roller temperature of the open mill to 45℃ and the roller gap to 1.0mm. Plasticize the rubber compound taken from the internal mixer until it forms sheets, then adjust the roller gap to 0.12mm. First, recycle three times, adding 1 / 2 equivalent vulcanizing agent and recycling three more times. Then add the remaining vulcanizing agent and recycle three more times. Roll the mixture six times and sheet it. After standing for 16 hours, perform vulcanization curve testing.

[0059] Using a rotorless vulcanizing apparatus, it was determined that at a vulcanizing temperature of 175℃, t 90 = 6.77 min. The compound was vulcanized in a flat vulcanizing apparatus for 8.77 min, allowed to stand for 4 h, and then subjected to a second-stage vulcanization at 150℃ for 4 h. The compound was then removed and allowed to stand at room temperature for 16 h. The compound was cut into dumbbell-shaped samples, and relevant performance tests were conducted according to "HG / T 2701-2016 Compression Packer Cylinder". The test results are shown in Table 3.

[0060] Table 3. Results of physical property testing of the compound in Example 3

[0061]

[0062] Compared to Example 1, Example 3 reduced the amount of carbon black N220 used (by 10 parts). As shown in Table 3, the hardness of the compound decreased slightly, while the tensile strength and elongation at break increased significantly.

[0063] Example 4

[0064] 100 parts hydrogenated nitrile rubber, 60 parts carbon black N220, 2 parts antioxidant RD (TMQ), 0.5 parts plasticizer DOTP, and 6.5 parts peroxide vulcanizing agent BIPB.

[0065] Sample preparation:

[0066] Using a 200mL internal mixer, adjust the initial temperature to 50℃ and the rotation speed to 40rpm. Lift the top plug and add the hydrogenated nitrile rubber within 15 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Mix for another 60 seconds, discharge the rubber compound, and obtain the final rubber compound.

[0067] Weigh the internally mixed rubber compound and compare it with the total mass of all raw materials added to the internal mixer. The loss of rubber compound should be controlled within 3%. Adjust the roller temperature of the open mill to 45℃ and the roller gap to 1.0mm. Plasticize the rubber compound taken from the internal mixer until it forms sheets, then adjust the roller gap to 0.12mm. First, recycle three times, adding 1 / 2 equivalent vulcanizing agent and recycling three more times. Then add the remaining vulcanizing agent and recycle three more times. Roll the mixture six times and sheet it. After standing for 16 hours, perform vulcanization curve testing.

[0068] Using a rotorless vulcanizing apparatus, it was determined that at a vulcanizing temperature of 175℃, t 90 = 6.77 min. The compound was vulcanized in a flat vulcanizing apparatus for 8.77 min, allowed to stand for 4 h, and then subjected to a second-stage vulcanization at 150℃ for 4 h. The compound was then removed and allowed to stand at room temperature for 16 h. The compound was cut into dumbbell-shaped samples, and relevant performance tests were conducted according to "HG / T 2701-2016 Compression Packer Cylinder". The test results are shown in Table 4.

[0069] Table 4. Results of Physical Property Tests for Compounds in Example 4

[0070]

[0071]

[0072] Compared to Example 1, Example 4 has a certain reduction in the amount of carbon black and BIPBN used, which leads to a significant change in the elongation at break of the compound. At the same time, the changes in elongation at break and compression set during hot air aging tend to worsen.

[0073] Example 5

[0074] 100 parts hydrogenated nitrile rubber, 65 parts carbon black N220, 2 parts antioxidant RD (TMQ), 0.5 parts plasticizer DOTP, and 7.0 parts peroxide vulcanizing agent BIPB.

[0075] Sample preparation:

[0076] Using a 200mL internal mixer, adjust the initial temperature to 50℃ and the rotation speed to 40rpm. Lift the top plug and add the hydrogenated nitrile rubber within 15 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Mix for another 60 seconds, discharge the rubber compound, and obtain the final rubber compound.

[0077] Weigh the internally mixed rubber compound and compare it with the total mass of all raw materials added to the internal mixer. The loss of rubber compound should be controlled within 3%. Adjust the roller temperature of the open mill to 48℃ and the roller gap to 1.0mm. Plasticize the rubber compound taken from the internal mixer until it forms sheets, then adjust the roller gap to 0.15mm. First, recycle three times, adding 1 / 2 equivalent vulcanizing agent and recycling three more times. Then add the remaining vulcanizing agent and recycle three more times. Roll the mixture six times and sheet it. After standing for 16 hours, perform vulcanization curve testing.

[0078] Using a rotorless vulcanizing apparatus, it was determined that at a vulcanizing temperature of 175℃, t 90 = 6.97 min. The compound was vulcanized in a flat vulcanizing apparatus for 8.97 min, allowed to stand for 4 h, and then subjected to a second-stage vulcanization at 150℃ for 4 h. The compound was then removed and allowed to stand at room temperature for 16 h. The compound was cut into dumbbell-shaped samples, and relevant performance tests were conducted according to "HG / T 2701-2016 Compression Packer Cylinder". The test results are shown in Table 5.

[0079] Table 5. Results of physical property testing of the compound in Example 5

[0080]

[0081] As shown in the table above, the roller gap has a certain impact on the vulcanization time. Compared with Example 1 and Example 2, the amount of carbon black affects the elongation at break and compression set.

[0082] Example 6

[0083] 160 parts hydrogenated nitrile rubber, 112 parts carbon black N220, 3.2 parts antioxidant RD (TMQ), 0.8 parts plasticizer DOTP, and 11.2 parts peroxide vulcanizing agent BIPB.

[0084] Sample preparation:

[0085] Using a 500mL internal mixer, adjust the initial temperature to 50℃ and the rotation speed to 40rpm. Lift the top plug and add the hydrogenated nitrile rubber within 15 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add half an equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add the remaining half equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Mix for another 60 seconds, discharge the rubber compound, and obtain the final rubber compound.

[0086] Weigh the internally mixed rubber compound and compare it with the total mass of all raw materials added to the internal mixer. The loss of rubber compound should be controlled within 3%. Adjust the roller temperature of the open mill to 50℃ and the roller gap to 1.0mm. Plasticize the rubber compound taken from the internal mixer until it forms sheets, then adjust the roller gap to 0.12mm. First, recycle three times, adding 1 / 2 equivalent vulcanizing agent and recycling three more times. Then add the remaining vulcanizing agent and recycle three more times. Roll the mixture six times and sheet it. After standing for 16 hours, perform vulcanization curve testing.

[0087] Using a rotorless vulcanizing apparatus, it was determined that at a vulcanizing temperature of 175℃, t 90 = 6.72 min. Vulcanize in a flat vulcanizing apparatus for 9.72 min, let stand for 4 h, then perform a second-stage vulcanization at 150℃ for 4 h. Remove the rubber compound and let it stand at room temperature for 16 h. Cut the rubber compound into dumbbell-shaped samples and perform relevant performance tests according to "HG / T 2701-2016 Compression Packer Cylinder". The test results are shown in Table 6.

[0088] Table 6. Results of Physical Property Tests for Compounds in Example 6

[0089]

[0090] Compared to Example 1, Example 6 increased the amount of compound to 1.6 times. Table 6 shows that the increased amount of compound did not affect the relevant properties of the compound.

[0091] Example 7

[0092] 200 parts hydrogenated nitrile rubber, 140 parts carbon black N220, 4 parts antioxidant RD (TMQ), 1.0 part plasticizer DOTP, and 13 parts peroxide vulcanizing agent BIPB.

[0093] Sample preparation

[0094] Using a 500mL internal mixer, adjust the initial temperature to 50℃ and the rotation speed to 40rpm. Lift the top plug and add the hydrogenated nitrile rubber within 15 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add 1 / 3 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add 1 / 3 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add the remaining 1 / 3 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Mix for another 60 seconds, discharge the rubber compound, and obtain the final rubber compound.

[0095] Weigh the internally mixed rubber compound and compare it with the total mass of all raw materials added to the internal mixer. The loss of rubber compound should be controlled within 3%. Adjust the roller temperature of the open mill to 50℃ and the roller gap to 1.0mm. Plasticize the rubber compound taken from the internal mixer until it forms sheets, then adjust the roller gap to 0.12mm. First, recycle three times, adding 1 / 2 equivalent vulcanizing agent and recycling three more times. Then add the remaining vulcanizing agent and recycle three more times. Roll the mixture six times and sheet it. After standing for 16 hours, perform vulcanization curve testing.

[0096] Using a rotorless vulcanizing apparatus, it was determined that at a vulcanizing temperature of 175℃, t 90 = 6.72 min. Vulcanize in a flat vulcanizing apparatus for 10.72 min, let stand for 4 h, then perform a second-stage vulcanization at 150℃ for 4 h. Remove the rubber compound and let it stand at room temperature for 16 h. Cut the rubber compound into dumbbell-shaped samples and perform relevant performance tests according to "HG / T 2701-2016 Compression Packer Cylinder". The test results are shown in Table 7.

[0097] Table 7 Results of Physical Property Tests for Compound in Example 7

[0098]

[0099] Compared to Example 2, Example 6 increased the amount of compound to 2.0 times. Table 7 shows that as the amount of compound is increased, some properties of the compound (such as elongation at break) will change to some extent.

[0100] Comparative Example 1

[0101] 100 parts hydrogenated nitrile rubber, 70 parts carbon black N220, 2 parts antioxidant SP (styrene-modified phenol), 0.5 parts plasticizer dioctyl terephthalate (DOTP), and 6.5 parts peroxide vulcanizing agent bis-tert-butyl peroxide isopropylbenzene (BIPB).

[0102] Sample preparation:

[0103] Using a 200mL internal mixer, adjust the initial temperature to 50℃ and the rotation speed to 40rpm. Lift the top plug and add the hydrogenated nitrile rubber within 15 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Mix for another 60 seconds, discharge the rubber compound, and obtain the final rubber compound.

[0104] Weigh the internally mixed rubber compound and compare it with the total mass of all raw materials added to the internal mixer. The loss of rubber compound should be controlled within 3%. Adjust the roller temperature of the open mill to 45℃ and the roller gap to 1.0mm. Plasticize the rubber compound taken from the internal mixer until it forms sheets, then adjust the roller gap to 0.12mm. First, recycle three times, adding 1 / 2 equivalent vulcanizing agent and recycling three more times. Then add the remaining vulcanizing agent and recycle three more times. Roll the mixture six times and sheet it. After standing for 16 hours, perform vulcanization curve testing.

[0105] Using a rotorless vulcanizing apparatus, it was determined that at a vulcanizing temperature of 175℃, t 10 =0.58min,t 90 =6.36min, Figure 1 This is the vulcanization curve of the rubber compound obtained after plasticizing on an open mill. The compound was vulcanized in a flat vulcanizing apparatus for 8.36 min, allowed to stand for 4 h, and then subjected to a second-stage vulcanization at 150℃ for 4 h. The compound was then removed and allowed to stand at room temperature for 16 h. The compound was cut into dumbbell-shaped samples, and relevant performance tests were performed according to "HG / T2701-2016 Compression Packer Cylinder". The test results are shown in Table 8.

[0106] Table 8. Test results of physical properties of the compound from Comparative Example 1

[0107]

[0108]

[0109] Table 8 shows the test results of the physical properties of the compound in Comparative Example 1. Compared with Example 1, after the antioxidant was replaced with SP, some properties of the compound failed to meet the requirements (compression set).

[0110] Example 8

[0111] 100 parts hydrogenated nitrile rubber, 70 parts carbon black N220, 2 parts antioxidant (RD(TMQ) / SP=1 / 1), 0.5 parts plasticizer dioctyl terephthalate (DOTP), and 6.5 parts peroxide vulcanizing agent bis-tert-butyl peroxide isopropylbenzene (BIPB).

[0112] Sample preparation:

[0113] Using a 200mL internal mixer, adjust the initial temperature to 50℃ and the rotation speed to 40rpm. Lift the top plug and add the hydrogenated nitrile rubber within 15 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Mix for another 60 seconds, discharge the rubber compound, and obtain the final rubber compound.

[0114] Weigh the internally mixed rubber compound and compare it with the total mass of all raw materials added to the internal mixer. The loss of rubber compound should be controlled within 3%. Adjust the roller temperature of the open mill to 45℃ and the roller gap to 1.0mm. Plasticize the rubber compound taken from the internal mixer until it forms sheets, then adjust the roller gap to 0.12mm. First, recycle three times, adding 1 / 2 equivalent vulcanizing agent and recycling three more times. Then add the remaining vulcanizing agent and recycle three more times. Roll the mixture six times and sheet it. After standing for 16 hours, perform vulcanization curve testing.

[0115] Using a rotorless vulcanizing apparatus, it was determined that at a vulcanizing temperature of 175℃, t 10 =0.58min,t 90 =6.47min, Figure 1 This is the vulcanization curve of the rubber compound obtained after plasticizing on an open mill. The compound was vulcanized in a flat vulcanizing apparatus for 8.47 min, allowed to stand for 4 h, and then subjected to a second-stage vulcanization at 150℃ for 4 h. The compound was then removed and allowed to stand at room temperature for 16 h. The compound was cut into dumbbell-shaped samples, and relevant performance tests were performed according to "HG / T2701-2016 Compression Packer Cylinder". The test results are shown in Table 9.

[0116] Table 9. Results of Physical Property Tests for Compound in Example 8

[0117]

[0118] Table 9 shows the test results of the physical properties of the compound in Example 8. Compared with Comparative Example 1, after the antioxidant was replaced with RD(TMQ) / SP=1 / 1, the compression set of the compound was improved, and all performance indicators met the requirements.

[0119] Example 9

[0120] 100 parts hydrogenated nitrile rubber, 70 parts carbon black N220, 2 parts antioxidant (RD(TMQ) / SP=1 / 2), 0.5 parts plasticizer dioctyl terephthalate (DOTP), and 6.5 parts peroxide vulcanizing agent bis-tert-butyl peroxide isopropylbenzene (BIPB).

[0121] Sample preparation:

[0122] Using a 200mL internal mixer, adjust the initial temperature to 50℃ and the rotation speed to 40rpm. Lift the top plug and add the hydrogenated nitrile rubber within 15 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Mix for another 60 seconds, discharge the rubber compound, and obtain the final rubber compound.

[0123] Weigh the internally mixed rubber compound and compare it with the total mass of all raw materials added to the internal mixer. The loss of rubber compound should be controlled within 3%. Adjust the roller temperature of the open mill to 45℃ and the roller gap to 1.0mm. Plasticize the rubber compound taken from the internal mixer until it forms sheets, then adjust the roller gap to 0.12mm. First, recycle three times, adding 1 / 2 equivalent vulcanizing agent and recycling three more times. Then add the remaining vulcanizing agent and recycle three more times. Roll the mixture six times and sheet it. After standing for 16 hours, perform vulcanization curve testing.

[0124] Using a rotorless vulcanizing apparatus, it was determined that at a vulcanizing temperature of 175℃, t 10 =0.58min,t 90 =6.57min, Figure 1 This is the vulcanization curve of the rubber compound obtained after plasticizing on an open mill. The compound was vulcanized in a flat vulcanizing apparatus for 8.57 min, allowed to stand for 4 h, and then subjected to a second-stage vulcanization at 150℃ for 4 h. The compound was then removed and allowed to stand at room temperature for 16 h. The compound was cut into dumbbell-shaped samples, and relevant performance tests were performed according to "HG / T2701-2016 Compression Packer Cylinder". The test results are shown in Table 10.

[0125] Table 10 Results of Physical Property Tests for Compound in Example 9

[0126]

[0127] Table 10 shows the test results of the physical properties of the compound in Example 9. Compared with Example 1, after the antioxidant was replaced with RD(TMQ) / SP=1 / 2, the compression set properties of the compound were further optimized, and all performance indicators met the requirements.

[0128] Example 10

[0129] 100 parts hydrogenated nitrile rubber, 70 parts carbon black N220, 2 parts antioxidant (RD(TMQ) / SP=1 / 3), 0.5 parts plasticizer dioctyl terephthalate (DOTP), and 6.5 parts peroxide vulcanizing agent bis-tert-butyl peroxide isopropylbenzene (BIPB).

[0130] Sample preparation:

[0131] Using a 200mL internal mixer, adjust the initial temperature to 50℃ and the rotation speed to 40rpm. Lift the top plug and add the hydrogenated nitrile rubber within 15 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Mix for another 60 seconds, discharge the rubber compound, and obtain the final rubber compound.

[0132] Weigh the internally mixed rubber compound and compare it with the total mass of all raw materials added to the internal mixer. The loss of rubber compound should be controlled within 3%. Adjust the roller temperature of the open mill to 45℃ and the roller gap to 1.0mm. Plasticize the rubber compound taken from the internal mixer until it forms sheets, then adjust the roller gap to 0.12mm. First, recycle three times, adding 1 / 2 equivalent vulcanizing agent and recycling three more times. Then add the remaining vulcanizing agent and recycle three more times. Roll the mixture six times and sheet it. After standing for 16 hours, perform vulcanization curve testing.

[0133] Using a rotorless vulcanizing apparatus, it was determined that at a vulcanizing temperature of 175℃, t 10 =0.58min,t 90 =6.60min, Figure 1 This is the vulcanization curve of the rubber compound obtained after plasticizing on an open mill. The compound was vulcanized in a flat vulcanizing apparatus for 8.60 min, allowed to stand for 4 h, and then subjected to a second-stage vulcanization at 150℃ for 4 h. The compound was then removed and allowed to stand at room temperature for 16 h. The compound was cut into dumbbell-shaped samples, and relevant performance tests were performed according to "HG / T2701-2016 Compression Packer Cylinder". The test results are shown in Table 11.

[0134] Table 11 Results of Physical Property Tests for Compound in Example 10

[0135]

[0136]

[0137] Table 11 shows the test results of the physical properties of the rubber compound in Example 11. All performance indicators meet the requirements.

[0138] As shown in Examples 1, 1 Comparative Example, and 9-10, when only SP is used as an antioxidant, the physical properties of the compound decrease, and some properties (compression set) even fail to meet the standard requirements. When only RD(TMQ) is used as an antioxidant, all test results meet the relevant standard requirements. When using a mixed antioxidant, the compression set performance is not as good as when RD(TMQ) is used alone as an antioxidant when RD(TMQ) / SP = 1:1. However, when RD(TMQ) / SP = 1:2, the compression set performance is significantly improved compared to RD(TMQ) and SP used alone. That is, although SP as an antioxidant has relatively poor performance, it can effectively improve product performance when used in combination with RD(TMQ) in a specific ratio. An improper ratio cannot improve performance. By optimizing the ratio, it was found that the compound has the best performance when RD(TMQ) / SP = 1:2. The main reason may be that both antioxidants are "free radical terminating" antioxidants, which have a synergistic anti-aging effect during use, thereby reducing compression set.

[0139] Comparative Example 2

[0140] 100 parts hydrogenated nitrile rubber, 70 parts carbon black N220, 2 parts antioxidant RD (TMQ), 0.5 parts plasticizer dioctyl terephthalate (DOTP), and 6.5 parts peroxide vulcanizing agent bis-tert-butyl peroxide isopropylbenzene (BIPB).

[0141] Sample preparation:

[0142] Using a 200mL internal mixer, adjust the initial temperature to 50℃ and the rotation speed to 40rpm. Lift the top plug and add the hydrogenated nitrile rubber within 15 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Lift the top plug again and add the remaining 1 / 2 equivalent of carbon black, antioxidant, and plasticizer sequentially within 30 seconds, then close the top plug and mix for 60 seconds. Mix for another 60 seconds, discharge the rubber compound, and obtain the final rubber compound.

[0143] Weigh the internally mixed rubber compound and compare it with the total mass of all raw materials added to the internal mixer. The loss of rubber compound should be controlled within 3%. Adjust the roller temperature of the open mill to 45℃ and the roller gap to 1.0mm. Plasticize the rubber compound taken from the internal mixer until it forms sheets, then adjust the roller gap to 0.12mm. First, recycle three times, adding 1 / 2 equivalent vulcanizing agent and recycling three more times. Then add the remaining vulcanizing agent and recycle three more times. Roll the mixture six times and sheet it. After standing for 16 hours, perform vulcanization curve testing.

[0144] Using a rotorless vulcanizing apparatus, it was determined that at a vulcanizing temperature of 175℃, t 10 =0.58min,t 90=6.77min, Figure 1 This is the vulcanization curve of the rubber compound obtained after plasticizing on an open mill. The compound was vulcanized in a flat vulcanizer for 8.77 min (without secondary vulcanization), then removed and allowed to stand at room temperature for 16 h. The compound was cut into dumbbell-shaped samples, and relevant performance tests were performed according to "HG / T 2701-2016 Compression Packer Cylinder". The test results are shown in Table 12.

[0145] Table 12 Results of Physical Property Tests for Comparative Example 2 Rubber Compound

[0146]

[0147] Table 12 shows the test results of the physical properties of the compound in Comparative Example 2. Since two-stage vulcanization was not carried out, the test results were compared with those in Example 1. Some properties (change rate of elongation at break under hot air aging and compression set) could not meet the standards, indicating that two-stage vulcanization is crucial to the experimental process.

Claims

1. A rubber material, characterized in that, The product comprises, by weight parts: 100 parts hydrogenated nitrile rubber, 60-70 parts carbon black, 2 parts antioxidant, 0.5 parts plasticizer, and 6.5-7.0 parts peroxide vulcanizing agent; the antioxidant is a mixture of RD(TMQ) and styrene-modified phenol, with the ratio of RD(TMQ) to SP being 1:2; the plasticizer is dioctyl terephthalate, and the peroxide vulcanizing agent is di-tert-butyl peroxide isopropylbenzene.

2. The rubber material according to claim 1, characterized in that, The carbon black is carbon black N220.

3. The method for preparing the rubber material according to any one of claims 1 to 2, characterized in that, include: Hydrogenated nitrile rubber is mixed; some carbon black, some antioxidant and some plasticizer are added and mixed. Add the remaining carbon black, antioxidant and plasticizer, mix, remove the glue, and obtain the rubber compound; The rubber compound is plasticized; a portion of the peroxide vulcanizing agent is added and plasticized again; then the remaining vulcanizing agent is added and plasticized again. The plasticized rubber compound undergoes a first-stage vulcanization and a second-stage vulcanization.

4. The method for preparing the rubber material according to claim 3, characterized in that, The vulcanization time is 8.77~10.77 min.

5. The method for preparing the rubber material according to claim 3, characterized in that, The plasticizing temperature is 45~50℃.

6. The method for preparing the rubber material according to claim 3, characterized in that, The plasticized rubber compound was subjected to vulcanization curve testing, and the plasticized rubber compound was subjected to a first-stage vulcanization based on the test results.

7. A packer cartridge, characterized in that, Its material is the rubber material described in any one of claims 1 to 2.

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