CN103396591B - A kind of Oilfield ultrahigh-pressure acid-resistant rubber seal material and preparation method - Google Patents
A kind of Oilfield ultrahigh-pressure acid-resistant rubber seal material and preparation method Download PDFInfo
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Abstract
A kind of Oilfield ultrahigh-pressure acid-resistant rubber seal material, its parts by weight are: hydrogenated nitrile-butadiene rubber 85 ~ 65 parts, paracril 15 ~ 35 parts, 5 ~ 7 parts, zinc oxide, stearic acid, 1 ~ 4 part, 1 ~ 2 part, anti-aging agent, nano carbon black 50 ~ 65 parts, white carbon black 15 ~ 25 parts, 5 ~ 10 parts, resol, tenderizer 5 ~ 10 parts, peroxide vulcanizing agent 3 ~ 6 parts, vulcanization aid 6 ~ 8 parts, 1 ~ 3 part, sulphur, promotor 2 ~ 4 parts; Wherein hydrogenated nitrile-butadiene rubber and paracril sum of the two are 100 parts.The sealing-ring adopting rubber packing material of the present invention to prepare meets the sealing of oil field high-pressure acid-resistant liquid (hydrochloric acid or hydrofluoric acid) pipeline, overcomes existing sealing member and occurs leaking and extruding torn edges phenomenon under high hydraulic pressure.
Description
Technical field
The present invention relates to a kind of rubber packing material, especially relate to a kind of Oilfield ultrahigh-pressure acid-resistant rubber seal material.
Background technology
Along with oilfield exploitation is to dark rock stratum and the expansion of territory, deep-sea, for improving original coefficient of mining, needing to inject high pressure acid solution to stratum and carrying out impingement corrosion subterranean strata, improve crude oil dialysis rate and then improve output.High pressure acid solution needs Cemented filling, and the sealing of pipeline junction is very crucial.In pressure piping, liquid pressure is between 30 ~ 140MPa, the sealing member of current use can play sealing function for below 70MPa conduit under fluid pressure, substantially meet service requirements, but easily occur when using under more than 100MPa hydraulic environment leaking, product bursts phenomenon.Along with the increase of oilfield exploitation difficulty, hydraulic environment pressure will be more common at more than 100MPa, and for guaranteeing the security of oilfield exploitation, being badly in need of that exploitation is a kind of can overpressure resistant conduit seals, meets the demand of oil production.
Sealing material under ultra-high voltage environment requires to have higher hardness, more excellent stretching, tear resistance and ageing-resistant performance, lower compression set, guarantee that it does not under high pressure occur extruding destruction and the sealing effectiveness that can ensure the long period, realize the engineer applied object of high pressure seal.
Hydrogenated nitrile-butadiene rubber is that oil field field of sealing technology uses comparatively general rubber.Containing itrile group in hydrogenated nitrile-butadiene rubber molecular chain, there is good resistance to chemical corrosion, the high saturated structures of its molecular chain in addition, it is made to have the tensile strength higher than common paracril, more superior ageing-resistant, fatigue performance and permanent set at high temperature performance, but because hydrogenated nitrile-butadiene rubber generally adopts peroxide cure, its tear resistance is poor, easily occurs extruding destruction under the effect of super high pressure hydraulic.Superhigh pressure sealing material requirements has higher hardness and comparatively low compression set in addition, guarantees that material crimp is under high pressure little, the sealing function time is long.Add fine particle height structure nano carbon black for improving the most common and most effective means of elastomeric material hardness, but when carbon black loading increases to more than 100 parts, hardness can reach design requirements, but the compression set performance of material significantly declines, and the mixed refining process difficulty in process of rubber.
Chinese Patent Application No. is describe elastomeric material prepared by a kind of key part (packing element) that can be used for oil extraction process in the patent of 201010152487.7 " a kind of preparation methods of high temperature and high pressure resistant rubber sealing material ", this material adopts hydrogenated nitrile-butadiene rubber as base material, add the Synergist S-421 95s such as metal oxide, stearic acid, acrylate to prepare, its principal feature can be play sealing function in 30MPa conduit under fluid pressure at 150 DEG C of high temperature, pressure reduction.Chinese Patent Application No. is the elastomeric material describing a kind of high temperature resistant vitriol oil in the patent of 200510040639.3 " concentrated sulfuric acid resistant fluoro-rubber sealing spacers " in addition, this material adopts 4 third viton and 23 type viton and uses, vulcanization system is made with dicumyl peroxide and triallylcyanurate, add other Synergist S-421 95 mixing sulfurations to form, be applied to the preparation of plate-type heat exchanger gasket seal in sulfuric acid industry.
Summary of the invention
The object of the invention is to design a kind of suitable rubber packing material formula, the sealing member adopting this formula and corresponding technique to prepare can realize the sealing of oil field ultra-high voltage (100MPa ~ 140MPa) acid solution (hydrochloric acid or hydrofluoric acid) transport pipe.
The present invention is a kind of oil field ultra-high voltage acid-resisting rubber sealing material, the feature of this material is that sealing load is large, reach more than 100MPa, sealing medium is hydrochloric acid or hydrofluoric acid solution, main body base material adopts hydrogenated nitrile-butadiene rubber and paracril and uses, from the viewpoint of applied environment and material of main part two, being all different from the patent of two described in background technology, is a kind of novel rubber packing material.
In order to realize described goal of the invention, the present invention adopts following technical scheme:
A kind of Oilfield ultrahigh-pressure acid-resistant rubber seal material, its parts by weight are: hydrogenated nitrile-butadiene rubber 85 ~ 65 parts, paracril 15 ~ 35 parts, 5 ~ 7 parts, zinc oxide, stearic acid, 1 ~ 4 part, 1 ~ 2 part, anti-aging agent, nano carbon black 50 ~ 65 parts, white carbon black 15 ~ 25 parts, 5 ~ 10 parts, resol, tenderizer 5 ~ 10 parts, peroxide vulcanizing agent 3 ~ 6 parts, vulcanization aid 6 ~ 8 parts, 1 ~ 3 part, sulphur, promotor 2 ~ 4 parts; Wherein hydrogenated nitrile-butadiene rubber and paracril sum of the two are 100 parts.
In hydrogenated nitrile-butadiene rubber of the present invention, acrylonitrile content is 23 ~ 27%, and mooney viscosity is 70 ~ 80, and iodine absorption value is 11 ~ 16; In described paracril, acrylonitrile content is 35 ~ 41%, and mooney viscosity is 50 ~ 60.
Anti-aging agent of the present invention is antioxidant MB (2-mercaptobenzimidazole); Described promotor is captax (2-thiol benzothiazole is called for short MBT).
Nano carbon black of the present invention comprises high reinforced type medium super abrasion furnace black and high wear-resistant carbon black.
High reinforced type medium super abrasion furnace black of the present invention is N220 or N242 or N285; Described high wear-resistant carbon black is N330 or N339.
White carbon black of the present invention is gas-phase silica, and surface-area is 150 ~ 250g/m
2.
Peroxide vulcanizing agent of the present invention is one in dicumyl peroxide, 1,1-di-t-butyl peroxy-3,3,5-trimethylammonium cyclohexane, 2,5-2，5-dimethyl-2，5-di(t-butyl peroxy)2，5-hexane or its two or more mixture.
Vulcanization aid of the present invention is one in phenyl-bismaleimide between N, N-, cyanacrylate, zinc methacrylate or its two or more mixture.
Tenderizer of the present invention is liquid acrylonitrile butadiene rubber or liquid butadiene rubber.
A kind of preparation method of Oilfield ultrahigh-pressure acid-resistant rubber seal material, first take hydrogenated nitrile-butadiene rubber 85 ~ 65 parts by weight part, paracril 15 ~ 35 parts, sum of the two is 100 parts, put into mill thin-pass respectively 3 times, then mix on a mill until, then by 5 ~ 7 parts, zinc oxide, stearic acid, 1 ~ 4 part, 1 ~ 2 part, anti-aging agent, nano carbon black 50 ~ 65 parts, white carbon black 15 ~ 25 parts, 5 ~ 10 parts, resol, tenderizer 5 ~ 10 parts, peroxide vulcanizing agent 3 ~ 6 parts, vulcanization aid 6 ~ 8 parts, 1 ~ 3 part, sulphur, promotor 2 ~ 4 parts, add successively in mill and carry out mixingly obtaining rubber unvulcanizate to slice after evenly, rubber unvulcanizate is carried out one step cure on vulcanizing press, controlling curing temperature is 150 DEG C ~ 170 DEG C, curing time is 30 ~ 40 minutes, sulfide stress is 8 ~ 12Mpa, cross-linked rubber is obtained after rubber is carried out 2h post vulcanization from baking oven again under 150 ~ 170 DEG C of conditions after vulcanizing press takes out.
Owing to have employed technique scheme, the present invention has following beneficial effect:
The present invention adopts following method to solve the problem: 1) in hydrogenated nitrile-butadiene rubber, use a small amount of paracril, adopt superoxide and sulphur accelerator system and vulcanization system, obtain by the two covulcanization and synchronic curing all good material with tear resistance that stretches; 2) material hardness is promoted rapidly by interpolation gas-phase silica and resol, by the small-molecule substance adding band activity double key do superoxide cocuring agent, add reactive low molecular weight liquid rubber to reduce material compression set as tenderizer, obtain the higher but material that compression set is lower of hardness.
The nano carbon black that the present invention relates to comprises high reinforced type medium super abrasion furnace black (N220 or N242 or N285), high wear-resistant carbon black (N330 or N339), these two kinds dissimilar fine particle carbon blacks can improve the performance such as tensile strength, tear strength, hardness of cross-linked rubber, to improve the ability of material repels high pressure.
The surface-area of the gas-phase silica that the present invention relates to is 150 ~ 250g/m
2, the white carbon black that specific surface area is large can play the effect promoting rapidly sizing material hardness.
In sum, the sealing-ring adopting rubber packing material of the present invention to prepare meets the sealing of oil field high pressure (about 140MPa) resistance to acid solution (hydrochloric acid or hydrofluoric acid) pipeline, overcomes existing sealing member and occurs leaking and extruding torn edges phenomenon under high hydraulic pressure.
Embodiment
By explanation the present invention that the following examples can be detailed, disclose object of the present invention and be intended to protect all technological improvements in the scope of the invention.
Embodiment 1
The weighing of each component is carried out according to the formula shown in table 1, add successively in mill and carry out mixingly obtaining rubber unvulcanizate to slice after evenly, rubber unvulcanizate is carried out one step cure on vulcanizing press, and controlling curing temperature is 160 DEG C, curing time is 40 minutes, and sulfide stress is 10Mpa; Cross-linked rubber is obtained after rubber is carried out 2h post vulcanization from baking oven again under 170 DEG C of conditions after vulcanizing press takes out.
Table 1 oil field high-pressure acid-resistant sealing material formula (1)
| Sequence number | Starting material title | Consumption (part) |
| 1 | Hydrogenated nitrile-butadiene rubber | 85 |
| 2 | Paracril | 15 |
| 3 | Zinc oxide | 5 |
| 4 | Stearic acid | 1 |
| 5 | Antioxidant MB | 2 |
| 6 | Carbon black N220 | 30 |
| 7 | Carbon black N330 | 25 |
| 8 | Gas-phase silica | 15 |
| 9 | Resol | 8 |
| 10 | Liquid acrylonitrile butadiene rubber | 6 |
| 11 | Dicumyl peroxide | 6 |
| 12 | Zinc methacrylate | 7 |
| 13 | Sulphur | 1.5 |
| Captax | 2 |
Be 24.3MPa according to the tensile strength of the gained cross-linked rubber of filling a prescription table 1 Suo Shi, elongation rate of tensile failure is 230%, breaks and is permanently deformed to 8%, and tear strength is 43.1kN/m, and Shore A hardness is 87; Under 120 DEG C × 72h, rate of compression are 15% condition, compression set is 17.8%; Cross-linked rubber is weight rate in the hydrochloric acid of 20% after soaking at room temperature 72h in mass concentration is 0.63%, and volume change is 0.9%; Be weight rate in 15% hydrofluoric acid after soaking at room temperature 72h in mass concentration be 1.6%, volume change is 2.3%.
Embodiment 2
After carrying out each component weighing according to formula table 2 Suo Shi, add successively in mill and carry out mixingly obtaining rubber unvulcanizate to slice after evenly, rubber unvulcanizate is carried out one step cure on vulcanizing press, and controlling curing temperature is 160 DEG C, curing time is 30 minutes, and sulfide stress is 10Mpa; Cross-linked rubber is obtained after rubber is carried out 2h post vulcanization from baking oven again under 170 DEG C of conditions after vulcanizing press takes out.
Table 2 oil field high-pressure acid-resistant sealing material formula (2)
| Sequence number | Starting material | Consumption (part) |
| 1 | Hydrogenated nitrile-butadiene rubber | 75 |
| 2 | Paracril | 25 |
| 3 | Zinc oxide | 5 |
| 4 | Stearic acid | 2 |
| 5 | Antioxidant MB | 2 |
| 6 | Carbon black N242 | 35 |
| 7 | Carbon black N339 | 30 |
| 8 | Gas-phase silica | 18 |
| 9 | Resol | 6 |
| 10 | Liquid butadiene rubber | 5 |
| 11 | 1,1-di-t-butyl peroxy-3,3,5-trimethylammonium cyclohexane | 5 |
| 12 | Cyanacrylate, zinc methacrylate | 6 |
| 13 | Sulphur | 3 |
| Captax | 2 |
Be 21.7MPa elongation rate of tensile failure be 193% according to the fill a prescription tensile strength of gained cross-linked rubber of table 2, break and be permanently deformed to 8%, tear strength is 49.7kN/m, and Shao A hardness is 86; Under 120 DEG C × 72h, rate of compression are 15% condition, compression set is 16.5%; Cross-linked rubber is weight rate in the hydrochloric acid of 20% after soaking at room temperature 72h in mass concentration is 0.52%, and volume change is 0.76; Be weight rate in 15% hydrofluoric acid after soaking at room temperature 72h in mass concentration be 1.3%, volume change is 1.9%.
Embodiment 3
After carrying out each component weighing according to formula table 3 Suo Shi, add successively in mill and carry out mixingly obtaining rubber unvulcanizate to slice after evenly, rubber unvulcanizate is carried out one step cure on vulcanizing press, and controlling curing temperature is 160 DEG C, curing time is 30 minutes, and sulfide stress is 10Mpa; Cross-linked rubber is obtained after rubber is carried out 2h post vulcanization from baking oven again under 160 DEG C of conditions after vulcanizing press takes out.
Table 3 oil field high-pressure acid-resistant sealing material formula (3)
| Sequence number | Starting material | Consumption (part) |
| 1 | Hydrogenated nitrile-butadiene rubber | 65 |
| 2 | Paracril | 35 |
| 3 | Zinc oxide | 7 |
| 4 | Stearic acid | 4 |
| 5 | Antioxidant MB | 1 |
| 6 | Carbon black N285 | 30 |
| 7 | Carbon black N330 | 25 |
| 8 | Gas-phase silica | 25 |
| 9 | Resol | 10 |
| 10 | Liquid butadiene rubber | 10 |
| 11 | 2,5-2，5-dimethyl-2，5-di(t-butyl peroxy)2，5-hexane | 4 |
| 12 | Phenyl-bismaleimide between N, N- | 8 |
| 13 | Sulphur | 2 |
| Captax | 3 |
Be 20.6MPa according to the tensile strength of table 3 gained cross-linked rubber, elongation rate of tensile failure is 175%, breaks and is permanently deformed to 8%, and tear strength is 43.2kN/m, and Shore A hardness is 88; Under 120 DEG C × 72h, rate of compression are 15% condition, compression set is 19.2%; Cross-linked rubber is weight rate in the hydrochloric acid of 20% after soaking at room temperature 72h in mass concentration is 0.72%, and volume change is 0.96%; Be weight rate in 15% hydrofluoric acid after soaking at room temperature 72h in mass concentration be 1.8%, volume change is 2.5%.
Part not in the detailed description of the invention is prior art.
Claims (7)
1. an Oilfield ultrahigh-pressure acid-resistant rubber seal material, is characterized in that: its parts by weight are: hydrogenated nitrile-butadiene rubber 85 ~ 65 parts, paracril 15 ~ 35 parts, 5 ~ 7 parts, zinc oxide, stearic acid, 1 ~ 4 part, 1 ~ 2 part, anti-aging agent, nano carbon black 50 ~ 65 parts, white carbon black 15 ~ 25 parts, 5 ~ 10 parts, resol, tenderizer 5 ~ 10 parts, peroxide vulcanizing agent 3 ~ 6 parts, vulcanization aid 6 ~ 8 parts, 1 ~ 3 part, sulphur, promotor 2 ~ 4 parts; Wherein hydrogenated nitrile-butadiene rubber and paracril sum of the two are 100 parts; In described hydrogenated nitrile-butadiene rubber, acrylonitrile content is 23 ~ 27%, and mooney viscosity is 70 ~ 80, and iodine absorption value is 11 ~ 16; In described paracril, acrylonitrile content is 35 ~ 41%, and mooney viscosity is 50 ~ 60; Described high reinforced type medium super abrasion furnace black is N220 or N242 or N285; Described high wear-resistant carbon black is N330 or N339; Described peroxide vulcanizing agent is one in dicumyl peroxide, 1,1-di-t-butyl peroxy-3,3,5-trimethylammonium cyclohexane, 2,5-2，5-dimethyl-2，5-di(t-butyl peroxy)2，5-hexane or its two or more mixture; Described vulcanization aid is one in phenyl-bismaleimide between N, N-, cyanacrylate, zinc methacrylate or its two or more mixture.
2. Oilfield ultrahigh-pressure acid-resistant rubber seal material as claimed in claim 1, is characterized in that: described anti-aging agent is antioxidant MB; Described promotor is captax.
3. Oilfield ultrahigh-pressure acid-resistant rubber seal material as claimed in claim 1, is characterized in that: described nano carbon black comprises high reinforced type medium super abrasion furnace black and high wear-resistant carbon black.
4. Oilfield ultrahigh-pressure acid-resistant rubber seal material as claimed in claim 1, it is characterized in that: described white carbon black is gas-phase silica, surface-area is 150 ~ 250g/m
2.
5. Oilfield ultrahigh-pressure acid-resistant rubber seal material as claimed in claim 1, is characterized in that: described vulcanization aid is one in phenyl-bismaleimide between N, N-, cyanacrylate, zinc methacrylate or its two or more mixture.
6. Oilfield ultrahigh-pressure acid-resistant rubber seal material as claimed in claim 1, is characterized in that: described tenderizer is liquid acrylonitrile butadiene rubber or liquid butadiene rubber.
7. the preparation method of an Oilfield ultrahigh-pressure acid-resistant rubber seal material as claimed in claim 1, it is characterized in that: first take hydrogenated nitrile-butadiene rubber 85 ~ 65 parts by weight part, paracril 15 ~ 35 parts, sum of the two is 100 parts, put into mill thin-pass respectively 3 times, then mix on a mill until, then by 5 ~ 7 parts, zinc oxide, stearic acid, 1 ~ 4 part, 1 ~ 2 part, anti-aging agent, nano carbon black 50 ~ 65 parts, white carbon black 15 ~ 25 parts, 5 ~ 10 parts, resol, tenderizer 5 ~ 10 parts, peroxide vulcanizing agent 3 ~ 6 parts, vulcanization aid 6 ~ 8 parts, 1 ~ 3 part, sulphur, promotor 2 ~ 4 parts, add successively in mill and carry out mixingly obtaining rubber unvulcanizate to slice after evenly, rubber unvulcanizate is carried out one step cure on vulcanizing press, controlling curing temperature is 150 DEG C ~ 170 DEG C, curing time is 30 ~ 40 minutes, sulfide stress is 8 ~ 12Mpa, cross-linked rubber is obtained after rubber is carried out 2h post vulcanization from baking oven again under 150 ~ 170 DEG C of conditions after vulcanizing press takes out.
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| CN101967238A (en) * | 2010-09-28 | 2011-02-09 | 浙江沪天胶带有限公司 | Base belt of sub-hydrogenated nitrile butadiene rubber synchronous belt |
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| CN103396591A (en) | 2013-11-20 |
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