CN109401139A - A kind of high temperature resistant, high pressure resistant rubber material and its preparation method and application - Google Patents

A kind of high temperature resistant, high pressure resistant rubber material and its preparation method and application Download PDF

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Publication number
CN109401139A
CN109401139A CN201811272544.8A CN201811272544A CN109401139A CN 109401139 A CN109401139 A CN 109401139A CN 201811272544 A CN201811272544 A CN 201811272544A CN 109401139 A CN109401139 A CN 109401139A
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rubber material
rubber
high temperature
high pressure
graphene
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铁忠银
任俊松
李晖
吕占春
郭明扬
陈华龙
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China Petroleum and Chemical Corp
Sinopec Oilfield Service Corp
Sinopec Southwest Petroleum Engineering Co Ltd Downhole Operation Branch
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Sinopec Oilfield Service Corp
Sinopec Southwest Petroleum Engineering Co Ltd Downhole Operation Branch
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Priority to CN201811272544.8A priority Critical patent/CN109401139A/en
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02Organic and inorganic ingredients
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • C08K3/042Graphene or derivatives, e.g. graphene oxides
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/09Carboxylic acids; Metal salts thereof; Anhydrides thereof
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/14Peroxides
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2217Oxides; Hydroxides of metals of magnesium
    • C08K2003/222Magnesia, i.e. magnesium oxide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2312/00Crosslinking

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Abstract

The invention discloses a kind of high temperature resistants, high pressure resistant rubber material and its preparation method and application.The rubber material is formed with the raw material of following mass percent: tetrapropanate fluorine rubber 60~70%, carbon black 15~25%, stearic acid 0.5~1%, graphene 5~10%, magnesia 0.5~1%, cumyl peroxide 1.5~2%, Triallyl isocyanurate 3~4%, triethoxysilane 1~2%.Each component of the invention mutually cooperates with, compatibility, made rubber material is able to bear at the same time 205 DEG C of height and 105MPa High Pressure Difference, and high temperature resistance and high voltage performance are excellent, and its high hydrogen sulfide environment for having resistance to 20%H2S, remarkable in economical benefits, application prospect are good.

Description

A kind of high temperature resistant, high pressure resistant rubber material and its preparation method and application
Technical field
The present invention relates to rubber material, the system of specifically a kind of high temperature resistant, high pressure resistant rubber material and the rubber material Preparation Method and purposes.
Background technique
Rubber material as having the characteristics that elasticity, insulating properties, waterproof, airtight high-molecular compound material, It is widely applied in industry or life, this just includes the application on the downhole tool packer of oil-gas mining.
In oil-gas mining, it is empty that packer is used as the annular between packing center tubing string and wellbore and between tubing string Between, the control of production (note) liquid is realized to completely cut off payzone.Packer underground set mainly by rubber material it is molding What packing element was realized, and stability and reliability of the packing element under underground working directly affect packer and set effect in underground The development of fruit and subsequent oil-gas mining construction operation.Since the drilling of oil/gas well is needed as deep as several hundred rice in underground, even thousands of Rice, underground are in the work condition environment of high temperature (nearly 200 DEG C), high pressure (nearly 100MPa), this just needs to apply on packer, use The rubber material for preparing packing element has high temperature resistant, high voltage performance, otherwise, high temperature, high pressure underground working environment under, rubber Packing element stability and reliability made of glue material will be deteriorated, and directly affect packer in underground and set effect and subsequent oil The development of gas exploitation construction operation.
Typically, the heatproof of a variety of materials, pressure-resistant performance all have its limit, it is existing be used as prepare packing element Conventional rubber materials heat resistance within 200 DEG C, pressure-resistant performance is within 100MPa.However, opening with oil/gas well It adopts and constantly develops to deep-well, ultradeep well, underground working condition becomes increasingly complex, and downhole temperature has broken through 200 DEG C, pressure dashed forward Broken 100MPa, this is able to satisfy the existing heat resistance as the conventional rubber materials for preparing packing element and resistance to pressure not The production technique requirement of deep-well, ultradeep well.
Currently, the exploitation for deep-well, ultradeep well, it is used and packing element provided for external associated companies, it is resistance to Temperature is up to 205 DEG C, pressure resistance up to 105MPa.However, they are only mentioned to the country with fancy price based on external technology blockage For finished-product material or part, and underground corresponding technical measures, needless to say corresponding technical measures are provided, this to fit Answer domestic deep-well, ultradeep well exploitation packer it is with high costs, increase domestic deep-well, ultradeep well production technique difficulty and at This.
Development in view of China's oil gas well mining to deep-well, ultradeep well, and improve the independence of oil-gas mining, reduce Cost of winning, it would be highly desirable to develop it is being suitable for the downhole packer of oil-gas mining, there is more high-temperature resistant and pressure-resistant effect Rubber material.
Summary of the invention
Technical purpose of the invention is: in view of the above-mentioned state of the art and insufficient, a kind of heatproof of independent research can Up to 205 DEG C, high temperature resistant, the preparation method and purposes of high pressure resistant rubber material and the rubber material of the reachable 105MPa of pressure resistance.
The present invention realizes its technical purpose the technical scheme adopted is that a kind of high temperature resistant, high pressure resistant rubber material, described Rubber material is formed with the raw material of following mass percent:
One of preferably, the rubber material is formed with the raw material of following mass percent:
One of preferably, the tetrapropanate fluorine rubber is 4 third fluorine raw rubbers, the dynamic shearing of the 4 third fluorine raw rubber Storage modulus is 340KPa, and Mooney viscosity value of 4 third fluorine raw rubber under the conditions of 100 DEG C of temperature is 160.
One of preferably, the graphene is graphene oxide, piece diameter >=3 μm of the graphene.
One of preferably, the triethoxysilane is methyltriethoxysilane and vinyl triethoxyl silicon The mixture of alkane.
A kind of above-mentioned high temperature resistant, the preparation method of high pressure resistant rubber material, the preparation method is, by the rubber material Feed components put into open mill, the drum temperature of the open mill remains 45~70 DEG C, the rolling of the open mill Cylinder revolving speed remains 30~40rpm, and the open mill is kneaded 1~1.5 hour to the raw material of the rubber material, during milling Interior, successively thin logical processing 4~6 times is beaten triangle bag and is handled 3~5 times, last uniform slice, acquisition high temperature resistant, high voltage bearing rubber Material.
One of preferably, release sequence of the feed components of the rubber material in open mill is 4 third Fluorubber, carbon black, stearic acid, graphene, magnesia, cumyl peroxide, Triallyl isocyanurate, triethoxysilicane The successively dispensing of alkane.
One of preferably, the two roller spacing of the open mill during milling remain 2~4mm, described Two roller spacing of the open mill in thin logical processing remain 1mm.
A kind of above-mentioned high temperature resistant, the purposes of high pressure resistant rubber material, the rubber material are used as the glue prepared on packer Cylinder.
One of preferably, the packer is 5 1/2 " small size RTTS-112 packers.
The method have the benefit that:
1. each component of the invention mutually cooperates with, compatibility, wherein tetrapropanate fluorine rubber is main raw material(s), is used as main real Existing rubber function;Carbon black is as reinforcing filler, the physical mechanical property as raising rubber, while can improve the operation of rubber Performance;Cumyl peroxide realizes the performance of rubber as promoting rubber molecular chain to crosslink as vulcanizing agent;Triolefin Propyl isocyanuric acid ester is as assistant crosslinking agent, as the vulcanization for accelerating fluorubber;Stearic acid can improve rubber as operation agent Process operation;Graphene can improve the resistance to H2S performance of rubber, improve tolerance of the rubber in H2S as special filler Degree;Magnesia is used as absorption rubber and the substances such as hydrogen fluoride is precipitated in sulfidation, reduce low point in rubber as acid absorbent Sub- object improves the comprehensive performance of rubber;Triethoxysilane is as coupling agent, as the further chemical crosslinking for promoting rubber, and The aging speed for slowing down rubber improves the service life of rubber;It after tested, can be simultaneously with rubber material of the present invention made from this 205 DEG C of high temperature and 105MPa High Pressure Difference are born, high temperature resistance and high voltage performance are excellent, and its height for having resistance to 20%H2S Hydrogen-sulfide environmental, remarkable in economical benefits, application prospect are good;
2. rubber material of the invention is used as the packing element for preparing packer, particularly small size packer, it is based on its resistance to height Warm, high voltage bearing excellent properties can be effectively adapted to the underground working environment of deep-well, ultradeep well, after tested, with the present invention The packer of the made packing element of rubber material is under the working condition of 205 DEG C of underground high temperature, 105MPa High Pressure Difference and 20%H2S content It can be continuous work 168 hours;It can be seen that the packer with the made packing element of rubber material of the present invention effectively meets depth Well, ultradeep well exploitation to the technical requirements of packing element, be conducive to improve China's deep-well, ultradeep well oil gas well mining it is autonomous Property, also advantageously reduce China's deep-well, the technical difficulty and cost that ultradeep well is especially exploited, application prospect is good.
Specific embodiment
The present invention relates to rubber material, the preparation method of specifically a kind of high temperature resistant, high pressure resistant rubber and the rubber and Purposes is below described in detail technology contents of the invention with multiple embodiments.
Embodiment 1
The present invention is formed with the raw material of following mass percent: tetrapropanate fluorine rubber 62%, carbon black 22.9%, stearic acid 0.8%, graphene 7%, magnesia 0.8%, cumyl peroxide 1.5%, Triallyl isocyanurate 4%, three ethoxies Base silane 1%.
In above-mentioned formula, tetrapropanate fluorine rubber is 4 third fluorine raw rubbers, and the dynamic storage shear modulus of the 4 third fluorine raw rubber is 340KPa, Mooney viscosity value under the conditions of 100 DEG C of temperature are 160.
In above-mentioned formula, graphene is graphene oxide, and the piece diameter of graphene is 3 μm.
In above-mentioned formula, triethoxysilane is the mixing of methyltriethoxysilane and vinyltriethoxysilane Object, mixed proportion 1:1.
The preparation method is that:
By each component in formula material according to tetrapropanate fluorine rubber, carbon black, stearic acid, graphene, magnesia, peroxidating two Isopropylbenzene, Triallyl isocyanurate, triethoxysilane sequencing successively launch in open mill;
The drum temperature of open mill remains 66 DEG C, and the drum rotation speed of open mill remains 35rpm;Open mill is with this technique Condition is kneaded the raw material components launched into 1.3 hours, and the spacing between two rollers during mixing remains 2.5mm; During milling, triangle bag processing 5 times is played in successively thin logical processing 5 times to open mill, between two rollers when thin logical processing between Away from remaining 1mm;
Last uniform slice, obtains high temperature resistant, high voltage bearing rubber material.
High temperature resistant that the present invention obtains, high pressure resistant rubber material are used as preparation 5 1/2 " on small size RTTS-112 packer Packing element.
Embodiment 2
The present invention is formed with the raw material of following mass percent: tetrapropanate fluorine rubber 67.8%, carbon black 18%, stearic acid 0.7%, graphene 6%, magnesia 0.5%, cumyl peroxide 2%, Triallyl isocyanurate 3%, triethoxy Silane 2%.
In above-mentioned formula, tetrapropanate fluorine rubber is 4 third fluorine raw rubbers, and the dynamic storage shear modulus of the 4 third fluorine raw rubber is 340KPa, Mooney viscosity value under the conditions of 100 DEG C of temperature are 160.
In above-mentioned formula, graphene is graphene oxide, and the piece diameter of graphene is 4 μm.
In above-mentioned formula, triethoxysilane is the mixing of methyltriethoxysilane and vinyltriethoxysilane Object, mixed proportion 1:1.
The preparation method is that:
By each component in formula material according to tetrapropanate fluorine rubber, carbon black, stearic acid, graphene, magnesia, peroxidating two Isopropylbenzene, Triallyl isocyanurate, triethoxysilane sequencing successively launch in open mill;
The drum temperature of open mill remains 70 DEG C, and the drum rotation speed of open mill remains 40rpm;Open mill is with this condition The raw material components launched into are kneaded 1 hour, the spacing between two rollers during mixing remains 2mm;Open mill exists During mixing, triangle bag processing 3 times is played in successively thin logical processing 4 times, and the spacing between two rollers when thin logical processing remains 1mm;
Last uniform slice, obtains high temperature resistant, high voltage bearing rubber material.
High temperature resistant that the present invention obtains, high pressure resistant rubber material are used as preparation 5 1/2 " on small size RTTS-112 packer Packing element.
Embodiment 3
The present invention is formed with the raw material of following mass percent: tetrapropanate fluorine rubber 65%, carbon black 19.5%, stearic acid 0.7%, graphene 7.5%, magnesia 0.7%, cumyl peroxide 1.7%, Triallyl isocyanurate 3.4%, three Ethoxysilane 1.5%.
In above-mentioned formula, tetrapropanate fluorine rubber is 4 third fluorine raw rubbers, and the dynamic storage shear modulus of the 4 third fluorine raw rubber is 340KPa, Mooney viscosity value under the conditions of 100 DEG C of temperature are 160.
In above-mentioned formula, graphene is graphene oxide, and the piece diameter of graphene is 5 μm.
In above-mentioned formula, triethoxysilane is the mixing of methyltriethoxysilane and vinyltriethoxysilane Object, mixed proportion 1:1.
The preparation method is that:
By each component in formula material according to tetrapropanate fluorine rubber, carbon black, stearic acid, graphene, magnesia, peroxidating two Isopropylbenzene, Triallyl isocyanurate, triethoxysilane sequencing successively launch in open mill;
The drum temperature of open mill remains 63 DEG C, and the drum rotation speed of open mill remains 34rpm;Open mill is with this technique Condition is kneaded the raw material components launched into 1.4 hours, and the spacing between two rollers during mixing remains 3mm;It opens During milling, triangle bag processing 5 times, the spacing between two rollers when thin logical processing are beaten in successively thin logical processing 4 times to mill Remain 1mm;
Last uniform slice, obtains high temperature resistant, high voltage bearing rubber material.
High temperature resistant that the present invention obtains, high pressure resistant rubber material are used as preparation 5 1/2 " on small size RTTS-112 packer Packing element.
Rubber material made from the present embodiment has carried out following performance test.
Rubber material made from the present embodiment is divided into A and two parts of B.
Wherein, after A parts of rubber materials are placed for 24 hours, one step cure is carried out on vulcanizer, conditions of vulcanization is 150 DEG C of * 40min, 8~10MPa of sulfide stress;Post vulcanization is carried out in oven heat, conditions of vulcanization is 230 DEG C of * 4h, and standard rubbers are made Test piece.By the standard rubbers test piece made, according to GB/T2941-2006, " rubber physical test method sample prepares and adjusts logical With program " it provides to park test piece;According to GB/T531.1-2008 " vulcanized rubber or thermoplastic elastomer penetration hardness test method A part: Shore durometer method (Shao Er hardness) " test sample hardness;According to GB/T528-2009 " vulcanized rubber or thermoplastic The measurement of property rubber-tensile stress-strain performance " test sample tensile strength, elongation at break;According to GB/T3512-2001 The thermal aging property of " vulcanized rubber or the accelerated ageing of thermoplastic elastomer hot-air and heat resistant test " test sample and Medium-resistance in 20%H2S.The results are shown in Table 1 for the test performance obtained by aforementioned test technology.
The test performance result of 1 standard rubbers test piece of table
Detection project Test result
Hardness, shore A degree 82~86
Tensile strength, MPa 20~22
Elongation at break, % 190~220
Hot air aging 205℃×168h
Firmness change, shore A degree 0~+2
Tensile strength change rate, % - 0.5~-3
Elongation at break change rate, % - 11~-15
Packing element is made by following methods in B parts of rubber materials:
Firstly, being aged to rigid rubber material obtained;Specifically, rubber material is wrapped, after clot, is placed in drum In wind baking oven, 2~4h is aged under the conditions of 60~90 DEG C of temperature of temperature to get ageing rubber;
Then it is fabricated to the packing element of needs with sulfidization molding technique by being molded using obtained ageing rubber;Specifically It is to preheat the mold for being used for packing element injection molding and sulfidization molding under conditions of 100~120 DEG C of temperature, 5~6MPa of pressure 60min, then by ageing rubber in the type chamber that the pressure of 20MPa is pushed down into mold, molding, after mold is warming up to 150~160 DEG C Vulcanize 110~150min;After the completion of vulcanizing, mold is placed into 20~30min, opening mold, after taking out vulcanization at room temperature Product is to get packing element.
Packing element set obtained above is used in 5 1/2 and " has carried out down-hole simulation test, mould on small size RTTS-112 packer Quasi- experimental condition is 205 DEG C of high temperature, 105MPa High Pressure Difference and 20%H2S content;Test result shows using the resistance to height of the present invention Small size packing element prepared by warm, high pressure resistant rubber material can actually 205 DEG C of high temperature, 105MPa High Pressure Difference and Under conditions of 20%H2S content, continuous work 168 hours.
Embodiment 4
The present invention is formed with the raw material of following mass percent: tetrapropanate fluorine rubber 63%, carbon black 21%, stearic acid 1%, Graphene 8%, magnesia 0.9%, cumyl peroxide 1.8%, Triallyl isocyanurate 3.2%, triethoxysilicane Alkane 1.1%.
In above-mentioned formula, tetrapropanate fluorine rubber is 4 third fluorine raw rubbers, and the dynamic storage shear modulus of the 4 third fluorine raw rubber is 340KPa, Mooney viscosity value under the conditions of 100 DEG C of temperature are 160.
In above-mentioned formula, graphene is graphene oxide, and the piece diameter of graphene is 5 μm.
In above-mentioned formula, triethoxysilane is the mixing of methyltriethoxysilane and vinyltriethoxysilane Object, mixed proportion 1:1.
The preparation method is that:
By each component in formula material according to tetrapropanate fluorine rubber, carbon black, stearic acid, graphene, magnesia, peroxidating two Isopropylbenzene, Triallyl isocyanurate, triethoxysilane sequencing successively launch in open mill;
The drum temperature of open mill remains 58 DEG C, and the drum rotation speed of open mill remains 37rpm;Open mill is with this technique Condition is kneaded the raw material components launched into 1.5 hours, and the spacing between two rollers during mixing remains 2mm;It opens During milling, triangle bag processing 5 times, the spacing between two rollers when thin logical processing are beaten in successively thin logical processing 4 times to mill Remain 1mm;
Last uniform slice, obtains high temperature resistant, high voltage bearing rubber material.
High temperature resistant that the present invention obtains, high pressure resistant rubber material are used as preparation 5 1/2 " on small size RTTS-112 packer Packing element.
Embodiment 5
The present invention is formed with the raw material of following mass percent: tetrapropanate fluorine rubber 60%, carbon black 23%, stearic acid 0.5%, graphene 9%, magnesia 1%, cumyl peroxide 1.5%, Triallyl isocyanurate 3%, triethoxy Silane 2%.
In above-mentioned formula, tetrapropanate fluorine rubber is 4 third fluorine raw rubbers, and the dynamic storage shear modulus of the 4 third fluorine raw rubber is 340KPa, Mooney viscosity value under the conditions of 100 DEG C of temperature are 160.
In above-mentioned formula, graphene is graphene oxide, and the piece diameter of graphene is 6 μm.
In above-mentioned formula, triethoxysilane is the mixing of methyltriethoxysilane and vinyltriethoxysilane Object, mixed proportion 1:1.
The preparation method is that:
By each component in formula material according to tetrapropanate fluorine rubber, carbon black, stearic acid, graphene, magnesia, peroxidating two Isopropylbenzene, Triallyl isocyanurate, triethoxysilane sequencing successively launch in open mill;
The drum temperature of open mill remains 53 DEG C, and the drum rotation speed of open mill remains 39rpm;Open mill is with this technique Condition is kneaded the raw material components launched into 1.4 hours, and the spacing between two rollers during mixing remains 4mm;It opens During milling, triangle bag processing 3 times, the spacing between two rollers when thin logical processing are beaten in successively thin logical processing 6 times to mill Remain 1mm;
Last uniform slice, obtains high temperature resistant, high voltage bearing rubber material.
High temperature resistant that the present invention obtains, high pressure resistant rubber material are used as preparation 5 1/2 " on small size RTTS-112 packer Packing element.
Embodiment 6
The present invention is formed with the raw material of following mass percent: tetrapropanate fluorine rubber 66%, carbon black 17%, stearic acid 0.6%, graphene 10%, magnesia 0.6%, cumyl peroxide 1.6%, Triallyl isocyanurate 3%, three ethoxies Base silane 1.2%.
In above-mentioned formula, tetrapropanate fluorine rubber is 4 third fluorine raw rubbers, and the dynamic storage shear modulus of the 4 third fluorine raw rubber is 340KPa, Mooney viscosity value under the conditions of 100 DEG C of temperature are 160.
In above-mentioned formula, graphene is graphene oxide, and the piece diameter of graphene is 5 μm.
In above-mentioned formula, triethoxysilane is the mixing of methyltriethoxysilane and vinyltriethoxysilane Object, mixed proportion 1:1.
The preparation method is that:
By each component in formula material according to tetrapropanate fluorine rubber, carbon black, stearic acid, graphene, magnesia, peroxidating two Isopropylbenzene, Triallyl isocyanurate, triethoxysilane sequencing successively launch in open mill;
The drum temperature of open mill remains 45 DEG C, and the drum rotation speed of open mill remains 38rpm;Open mill is with this technique Condition is kneaded the raw material components launched into 1.1 hours, and the spacing between two rollers during mixing remains 3.5mm; During milling, triangle bag processing 5 times is played in successively thin logical processing 5 times to open mill, between two rollers when thin logical processing between Away from remaining 1mm;
Last uniform slice, obtains high temperature resistant, high voltage bearing rubber material.
High temperature resistant that the present invention obtains, high pressure resistant rubber material are used as preparation 5 1/2 " on small size RTTS-112 packer Packing element.
Embodiment 7
The present invention is formed with the raw material of following mass percent: tetrapropanate fluorine rubber 63.3%, carbon black 24%, stearic acid 0.8%, graphene 5%, magnesia 0.8%, cumyl peroxide 1.6%, Triallyl isocyanurate 3.5%, three second Oxysilane 1%.
In above-mentioned formula, tetrapropanate fluorine rubber is 4 third fluorine raw rubbers, and the dynamic storage shear modulus of the 4 third fluorine raw rubber is 340KPa, Mooney viscosity value under the conditions of 100 DEG C of temperature are 160.
In above-mentioned formula, graphene is graphene oxide, and the piece diameter of graphene is 10 μm.
In above-mentioned formula, triethoxysilane is the mixing of methyltriethoxysilane and vinyltriethoxysilane Object, mixed proportion 1:1.
The preparation method is that:
By each component in formula material according to tetrapropanate fluorine rubber, carbon black, stearic acid, graphene, magnesia, peroxidating two Isopropylbenzene, Triallyl isocyanurate, triethoxysilane sequencing successively launch in open mill;
The drum temperature of open mill remains 52 DEG C, and the drum rotation speed of open mill remains 40rpm;Open mill is with this technique Condition is kneaded the raw material components launched into 1.3 hours, and the spacing between two rollers during mixing remains 3mm;It opens During milling, triangle bag processing 4 times, the spacing between two rollers when thin logical processing are beaten in successively thin logical processing 6 times to mill Remain 1mm;
Last uniform slice, obtains high temperature resistant, high voltage bearing rubber material.
High temperature resistant that the present invention obtains, high pressure resistant rubber material are used as preparation 5 1/2 " on small size RTTS-112 packer Packing element.
Embodiment 8
The present invention is formed with the raw material of following mass percent: tetrapropanate fluorine rubber 61%, carbon black 20%, stearic acid 0.6%, graphene 10%, magnesia 0.7%, cumyl peroxide 1.9%, Triallyl isocyanurate 4%, three ethoxies Base silane 1.8%.
In above-mentioned formula, tetrapropanate fluorine rubber is 4 third fluorine raw rubbers, and the dynamic storage shear modulus of the 4 third fluorine raw rubber is 340KPa, Mooney viscosity value under the conditions of 100 DEG C of temperature are 160.
In above-mentioned formula, graphene is graphene oxide, and the piece diameter of graphene is 7 μm.
In above-mentioned formula, triethoxysilane is the mixing of methyltriethoxysilane and vinyltriethoxysilane Object, mixed proportion 1:1.
The preparation method is that:
By each component in formula material according to tetrapropanate fluorine rubber, carbon black, stearic acid, graphene, magnesia, peroxidating two Isopropylbenzene, Triallyl isocyanurate, triethoxysilane sequencing successively launch in open mill;
The drum temperature of open mill remains 56 DEG C, and the drum rotation speed of open mill remains 34rpm;Open mill is with this technique Condition is kneaded the raw material components launched into 1.4 hours, and the spacing between two rollers during mixing remains 2.5mm; During milling, triangle bag processing 4 times is played in successively thin logical processing 4 times to open mill, between two rollers when thin logical processing between Away from remaining 1mm;
Last uniform slice, obtains high temperature resistant, high voltage bearing rubber material.
High temperature resistant that the present invention obtains, high pressure resistant rubber material are used as preparation 5 1/2 " on small size RTTS-112 packer Packing element.
Embodiment 9
The present invention is formed with the raw material of following mass percent: tetrapropanate fluorine rubber 70%, carbon black 16%, stearic acid 0.7%, graphene 6.3%, magnesia 0.6%, cumyl peroxide 1.5%, Triallyl isocyanurate 3.3%, three Ethoxysilane 1.6%.
In above-mentioned formula, tetrapropanate fluorine rubber is 4 third fluorine raw rubbers, and the dynamic storage shear modulus of the 4 third fluorine raw rubber is 340KPa, Mooney viscosity value under the conditions of 100 DEG C of temperature are 160.
In above-mentioned formula, graphene is graphene oxide, and the piece diameter of graphene is 4 μm.
In above-mentioned formula, triethoxysilane is the mixing of methyltriethoxysilane and vinyltriethoxysilane Object, mixed proportion 1:1.
The preparation method is that:
By each component in formula material according to tetrapropanate fluorine rubber, carbon black, stearic acid, graphene, magnesia, peroxidating two Isopropylbenzene, Triallyl isocyanurate, triethoxysilane sequencing successively launch in open mill;
The drum temperature of open mill remains 67 DEG C, and the drum rotation speed of open mill remains 32rpm;Open mill is with this technique Condition is kneaded the raw material components launched into 1 hour, and the spacing between two rollers during mixing remains 4mm;Mill Machine during milling, beat triangle bag and handle 3 times, the spacing guarantor between two rollers when thin logical processing by successively thin logical processing 4 times It holds as 1mm;
Last uniform slice, obtains high temperature resistant, high voltage bearing rubber material.
High temperature resistant that the present invention obtains, high pressure resistant rubber material are used as preparation 5 1/2 " on small size RTTS-112 packer Packing element.
Embodiment 10
The present invention is formed with the raw material of following mass percent: tetrapropanate fluorine rubber 68%, carbon black 19%, stearic acid 0.9%, graphene 5%, magnesia 0.8%, cumyl peroxide 1.7%, Triallyl isocyanurate 3.2%, three second Oxysilane 1.4%.
In above-mentioned formula, tetrapropanate fluorine rubber is 4 third fluorine raw rubbers, and the dynamic storage shear modulus of the 4 third fluorine raw rubber is 340KPa, Mooney viscosity value under the conditions of 100 DEG C of temperature are 160.
In above-mentioned formula, graphene is graphene oxide, and the piece diameter of graphene is 6 μm.
In above-mentioned formula, triethoxysilane is the mixing of methyltriethoxysilane and vinyltriethoxysilane Object, mixed proportion 1:1.
The preparation method is that:
By each component in formula material according to tetrapropanate fluorine rubber, carbon black, stearic acid, graphene, magnesia, peroxidating two Isopropylbenzene, Triallyl isocyanurate, triethoxysilane sequencing successively launch in open mill;
The drum temperature of open mill remains 48 DEG C, and the drum rotation speed of open mill remains 30rpm;Open mill is with this technique Condition is kneaded the raw material components launched into 1.5 hours, and the spacing between two rollers during mixing remains 2mm;It opens During milling, triangle bag processing 5 times, the spacing between two rollers when thin logical processing are beaten in successively thin logical processing 5 times to mill Remain 1mm;
Last uniform slice, obtains high temperature resistant, high voltage bearing rubber material.
High temperature resistant that the present invention obtains, high pressure resistant rubber material are used as preparation 5 1/2 " on small size RTTS-112 packer Packing element.
Embodiment 11
The present invention is formed with the raw material of following mass percent: tetrapropanate fluorine rubber 65%, carbon black 15%, stearic acid 1%, Graphene 10%, magnesia 1%, cumyl peroxide 2%, Triallyl isocyanurate 4%, triethoxysilane 2%.
In above-mentioned formula, tetrapropanate fluorine rubber is 4 third fluorine raw rubbers, and the dynamic storage shear modulus of the 4 third fluorine raw rubber is 340KPa, Mooney viscosity value under the conditions of 100 DEG C of temperature are 160.
In above-mentioned formula, graphene is graphene oxide, and the piece diameter of graphene is 7 μm.
In above-mentioned formula, triethoxysilane is the mixing of methyltriethoxysilane and vinyltriethoxysilane Object, mixed proportion 1:1.
The preparation method is that:
By each component in formula material according to tetrapropanate fluorine rubber, carbon black, stearic acid, graphene, magnesia, peroxidating two Isopropylbenzene, Triallyl isocyanurate, triethoxysilane sequencing successively launch in open mill;
The drum temperature of open mill remains 65 DEG C, and the drum rotation speed of open mill remains 33rpm;Open mill is with this technique Condition is kneaded the raw material components launched into 1.3 hours, and the spacing between two rollers during mixing remains 2mm;It opens During milling, triangle bag processing 5 times, the spacing between two rollers when thin logical processing are beaten in successively thin logical processing 6 times to mill Remain 1mm;
Last uniform slice, obtains high temperature resistant, high voltage bearing rubber material.
High temperature resistant that the present invention obtains, high pressure resistant rubber material are used as the 7 " packing elements on size packer of preparation.
Embodiment 12
The present invention is formed with the raw material of following mass percent: tetrapropanate fluorine rubber 60%, carbon black 25%, stearic acid 0.7%, graphene 7.4%, magnesia 0.7%, cumyl peroxide 1.6%, Triallyl isocyanurate 3.4%, three Ethoxysilane 1.2%.
In above-mentioned formula, tetrapropanate fluorine rubber is 4 third fluorine raw rubbers, and the dynamic storage shear modulus of the 4 third fluorine raw rubber is 340KPa, Mooney viscosity value under the conditions of 100 DEG C of temperature are 160.
In above-mentioned formula, graphene is graphene oxide, and the piece diameter of graphene is 7 μm.
In above-mentioned formula, triethoxysilane is the mixing of methyltriethoxysilane and vinyltriethoxysilane Object, mixed proportion 1:1.
The preparation method is that:
By each component in formula material according to tetrapropanate fluorine rubber, carbon black, stearic acid, graphene, magnesia, peroxidating two Isopropylbenzene, Triallyl isocyanurate, triethoxysilane sequencing successively launch in open mill;
The drum temperature of open mill remains 60 DEG C, and the drum rotation speed of open mill remains 36rpm;Open mill is with this technique Condition is kneaded the raw material components launched into 1.2 hours, and the spacing between two rollers during mixing remains 3mm;It opens During milling, triangle bag processing 4 times, the spacing between two rollers when thin logical processing are beaten in successively thin logical processing 5 times to mill Remain 1mm;
Last uniform slice, obtains high temperature resistant, high voltage bearing rubber material.
High temperature resistant that the present invention obtains, high pressure resistant rubber material are used as preparation 5 1/2 " on small size RTTS-112 packer Packing element.
The above various embodiments is only to illustrate the present invention, rather than its limitations.Although referring to the various embodiments described above to this hair It is bright to be described in detail, those skilled in the art should understand that: the present invention still can be to the various embodiments described above In specific technical solution modify perhaps equivalent replacement of some of the technical features and these modifications or replace It changes, the spirit and scope of the present invention that it does not separate the essence of the corresponding technical solution.

Claims (10)

1. a kind of high temperature resistant, high pressure resistant rubber material, which is characterized in that the rubber material is with following mass percent Raw material composition:
Tetrapropanate fluorine rubber 60~70%,
Carbon black 15~25%,
Stearic acid 0.5~1%,
Graphene 5~10%,
Magnesia 0.5~1%,
Cumyl peroxide 1.5~2%,
Triallyl isocyanurate 3~4%,
Triethoxysilane 1~2%.
2. high temperature resistant, high pressure resistant rubber material according to claim 1, which is characterized in that the rubber material is with following The raw material of mass percent forms:
Tetrapropanate fluorine rubber 65%,
Carbon black 19.5%,
Stearic acid 0.7%,
Graphene 7.5%,
Magnesia 0.7%,
Cumyl peroxide 1.7%,
Triallyl isocyanurate 3.4%,
Triethoxysilane 1.5%.
3. high temperature resistant according to claim 1 or claim 2, high pressure resistant rubber material, which is characterized in that the tetrapropanate fluorine rubber is four The dynamic storage shear modulus of third fluorine raw rubber, the 4 third fluorine raw rubber is 340KPa, and the 4 third fluorine raw rubber is in 100 DEG C of temperature strips Mooney viscosity value under part is 160.
4. high temperature resistant according to claim 1 or claim 2, high pressure resistant rubber material, which is characterized in that the graphene is oxidation stone Black alkene, piece diameter >=3 μm of the graphene.
5. high temperature resistant according to claim 1 or claim 2, high pressure resistant rubber material, which is characterized in that the triethoxysilane is The mixture of methyltriethoxysilane and vinyltriethoxysilane.
6. a kind of high temperature resistant as claimed in claim 1 or 2, the preparation method of high pressure resistant rubber material, which is characterized in that the preparation Method is to put into the feed components of the rubber material in open mill, and the drum temperature of the open mill remains 45 ~70 DEG C, the drum rotation speed of the open mill remains 30~40rpm, and the open mill is kneaded the raw material of the rubber material 1~1.5 hour, during milling in, it is successively thin it is logical processing 4~6 times, beat triangle bag handle 3~5 times, finally uniform slice, obtain Obtain high temperature resistant, high voltage bearing rubber material.
7. high temperature resistant, the preparation method of high pressure resistant rubber material according to claim 6, which is characterized in that the rubber material Release sequence of the feed components of material in open mill is tetrapropanate fluorine rubber, carbon black, stearic acid, graphene, magnesia, mistake Aoxidize the successively dispensing of diisopropylbenzene (DIPB), Triallyl isocyanurate, triethoxysilane.
8. high temperature resistant, the preparation method of high pressure resistant rubber material according to claim 6, which is characterized in that the open mill Two roller spacing during milling remain 2~4mm, and two roller spacing of the open mill in thin logical processing are kept For 1mm.
9. a kind of high temperature resistant as claimed in claim 1 or 2, the purposes of high pressure resistant rubber material, which is characterized in that the rubber material As the packing element prepared on packer.
10. high temperature resistant, the purposes of high pressure resistant rubber material according to claim 9, which is characterized in that the packer is 5 " small size RTTS-112 packer.
CN201811272544.8A 2018-10-29 2018-10-29 A kind of high temperature resistant, high pressure resistant rubber material and its preparation method and application Pending CN109401139A (en)

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CN110157124A (en) * 2019-05-10 2019-08-23 上海杜实新材料科技有限公司 A kind of tetrapropanate fluorine rubber composition of hydrogen sulfide corrosion-resistant and its application
CN110218405A (en) * 2019-05-10 2019-09-10 上海杜实新材料科技有限公司 A kind of fluoro-rubber composite of hydrogen sulfide corrosion-resistant and its application
CN110551350A (en) * 2019-09-30 2019-12-10 中国石油集团川庆钻探工程有限公司 High-temperature and high-pressure resistant packer
CN115521562A (en) * 2022-11-28 2022-12-27 中石化西南石油工程有限公司 High-temperature-resistant packer sealing rubber cylinder and preparation method thereof

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN110157124A (en) * 2019-05-10 2019-08-23 上海杜实新材料科技有限公司 A kind of tetrapropanate fluorine rubber composition of hydrogen sulfide corrosion-resistant and its application
CN110218405A (en) * 2019-05-10 2019-09-10 上海杜实新材料科技有限公司 A kind of fluoro-rubber composite of hydrogen sulfide corrosion-resistant and its application
CN110551350A (en) * 2019-09-30 2019-12-10 中国石油集团川庆钻探工程有限公司 High-temperature and high-pressure resistant packer
CN115521562A (en) * 2022-11-28 2022-12-27 中石化西南石油工程有限公司 High-temperature-resistant packer sealing rubber cylinder and preparation method thereof
CN115521562B (en) * 2022-11-28 2023-01-31 中石化西南石油工程有限公司 High-temperature-resistant packer sealing rubber cylinder and preparation method thereof

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