CN114621544A - Self-lubricating sealing injection agent and preparation method thereof - Google Patents
Self-lubricating sealing injection agent and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/18—Homopolymers or copolymers or tetrafluoroethene
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08K2003/3009—Sulfides
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/08—Fiber-containing well treatment fluids
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/34—Lubricant additives
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Abstract
The invention relates to the technical field of oil exploitation equipment sealing, and particularly provides a self-lubricating sealing injection agent and a preparation method thereof, wherein the self-lubricating sealing injection agent comprises the following components: 20-60 parts of tetrapropylene fluoride rubber, 30-70 parts of polytetrafluoroethylene micro powder, 15-40 parts of powder reinforcing and regulating agent, 15-40 parts of fiber reinforcing and regulating agent, 20-60 parts of plasticizer oil, 5-30 parts of surfactant and 5-30 parts of cohesive tackifier. The invention develops an oil-resistant, temperature-resistant, shape-following, self-lubricating and wear-resistant sealing material which is injected, filled and supplemented under the conditions of no shutdown and no disassembly, and achieves the purpose of good online sealing.
Description
Technical Field
The invention relates to the technical field of sealing of oil exploitation equipment, and particularly provides a self-lubricating sealing injection agent and a preparation method thereof.
Background
Among five main reasons for crude oil leakage of a thick oil thermal recovery wellhead, the performance and the geometric shape of the sealing material cannot meet the requirement of complex working conditions on site, and the leakage accounts for one fifth of the total leakage reasons. The existing sealing element with a fixed shape has the problems of good elasticity, no high temperature resistance or no elasticity. And even if the non-plastic solid piece with good elasticity and high temperature resistance is restrained by other four leakage factors (1, well deviation, Christmas tree deviation and packing box deviation, 2, poor surface smoothness of a polished rod caused by mechanical, mineral and environmental reasons, 3, only static centering of the packing box can be adjusted, 4, the viscosity of thick oil is high, the crude oil has high back pressure, and the sealing is failed due to high boosting force), the abrasion of the solid sealing piece is caused, and the oil leakage is inevitable.
After the polished rod with eccentric wear formed by five leakage factors reciprocates for 1-3 ten thousand times (1296-1728 times/day), namely about 48 hours, the coaxiality of the polished rod and the packing box is more than 1mm, and gap oil leakage is formed.
Disclosure of Invention
In order to solve the technical problems, the invention provides a self-lubricating sealing injection agent and a preparation method thereof.
The invention is realized by firstly providing a self-lubricating sealing injection agent which comprises the following components in parts by weight: 20-60 parts of tetrapropylene fluoride rubber, 30-70 parts of polytetrafluoroethylene micro powder, 15-40 parts of powder reinforcing and regulating agent, 15-40 parts of fiber reinforcing and regulating agent, 20-60 parts of plasticizer oil, 5-30 parts of surfactant and 5-30 parts of cohesive tackifier.
Preferably, the powder reinforcing and regulating agent is one or more of precipitated silica, titanium dioxide and molybdenum disulfide, and the fiber reinforcing and regulating agent is one or more of aramid pulp, glass fiber and polytetrafluoroethylene fiber.
Preferably, the plasticizer oil is one or more of acetone, white oil, glycerin, kerosene, silicone oil and vaseline.
Preferably, the surfactant is a room temperature silicon coupling agent.
Preferably, the cohesive and adhesive agent is one or two of liquid polysulfide rubber and liquid silica gel.
The invention also provides a preparation method of the self-lubricating sealing injection agent, which comprises the following steps:
1) plasticating raw rubber: an open mill, wherein the tetrapropylene fluororubber is subjected to low-temperature thin-pass plastication until the Mooney viscosity is 30-40;
2) mixing the tetrapropylene fluoride rubber and a surfactant;
3) mixing the powder reinforcing regulator and the cohesive tackifier, adding the mixture into the rubber material prepared in the step 2), mixing to obtain a colloid, and taking out a rubber sheet to be dissolved into a colloidal-state rubber cement system;
4) the polytetrafluoroethylene micro powder and the fiber reinforcing and regulating agent are soaked in plasticizer oil and soaked and cured into a fiber oil-immersed system;
5) mixing and stirring the mucilage system prepared in the step 3) and the fiber oil immersion system prepared in the step 4) uniformly;
6) mixing the materials processed in the steps 1), 2) and 3) together in an internal mixer, and smashing and refining the materials in an open mill to obtain a semi-finished rubber sheet;
7) extruding the sealant rod.
Preferably, in the step 4), the polytetrafluoroethylene micro powder, the reinforcing regulator and the plasticizer oil are mixed and stirred in a stirring tank for 0.5 hour, and are soaked and cured for 5 hours at the temperature of 60 ℃.
Compared with the prior art, the invention has the advantages that:
the sealing material is oil-resistant, temperature-resistant, shape-following (compensation of alternating vibration load deformation in reciprocating motion), self-lubricating, wear-resistant, injection-filled without shutdown and disassembly and additionally installed, and the purpose of online good sealing is achieved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a self-lubricating sealing injection agent and a preparation method thereof.
The novel sealing injection agent takes ternary polymerization tetrafluoroethylene-propylene rubber (AFLS200) with excellent high and low temperature resistance and oil resistance and polytetrafluoroethylene micro powder with high and low temperature resistance (-70-260 ℃) as main materials; ultra-short aramid pulp with high temperature resistance, wear resistance and tearing resistance, polytetrafluoroethylene fiber, glass fiber, precipitated silica and titanium dioxide are used as filling and reinforcing functional fillers; glycerin (glycerol), white oil (C16-C31 alkane oil) and kerosene (oil mixture, wherein alkane is 28-48%, aromatic hydrocarbon is 20-50%, unsaturated hydrocarbon is 1-6%, cyclic hydrocarbon is 17-44%), silicone oil (poly-diethylsiloxane) and vaseline (C) are adopted, and the glycerin (glycerol), the white oil and the kerosene have good high-low temperature resistance and good compatibility with main materials17H36～C21H44Petroleum lubricating hydrocarbon) and the like, so that the sealing injection agent is easy to mix uniformly when being prepared, has excellent field extrusion filling property and proper hardness, good lubricity and good compactness when being used.
This novel sealed agent technique principle of annotating:
tetrapropylene fluororubber is a copolymer having tetrafluoroethylene (C2F4) and propylene (C3H6) as basic skeletons, and the polytetrafluoroethylene fine powder is a polymer obtained by polymerizing tetrafluoroethylene (C2F4) as a monomer. In the chemical components, the tetrapropylene fluoride rubber and the polytetrafluoroethylene micro powder are basically isomers and have good compatibility. In physical form, tetrapropylene fluoride rubber is a colloidal substance with a low mooney viscosity (e.g. aflas (l)150, with a mooney viscosity ML (1+4)100 of 40). The polytetrafluoroethylene fine powder is in the form of plastic.
The tetrapropylene fluoride rubber has the advantages that: 1) excellent high temperature aging resistance, and continuous service life of 2 years at 200 ℃. 2) Excellent in acid and alkali resistance. 3) Excellent high temperature steam resistance. 4) Excellent compression set resistance at high temperatures. Disadvantages of tetrapropylene fluoride rubber: the cold resistance is poor, and the brittleness temperature of the lower temperature resistant variety Aflas (L)150 is-40 ℃.
The polytetrafluoroethylene micro powder has the advantages that: 1) high temperature resistance, and the working temperature reaches 250 ℃. 2) Low temperature resistance, good mechanical toughness, and 5 percent of elongation rate can be maintained even if the temperature is reduced to-196 ℃. 3) Corrosion resistance, inertness to most chemicals and solvents, resistance to strong acids and bases, water and various organic solvents. 4) Weather resistance, optimum aging life in plastics. 5) High lubrication, the lowest coefficient of friction in solid materials. 6) Non-stick, which is the smallest surface tension in a solid material, does not stick any substance. 7) The electric insulation can resist 1500V high voltage electricity. The disadvantages of polytetrafluoroethylene micropowder: 1) the packing has "plastic flow property", namely plastic deformation (creep) of a material product under the action of long-term continuous load, namely the packing or the gasket can generate "plastic flow" (creep) under continuous external force to be flattened, and the deformation is permanent deformation, so that the elastic recovery sealing property is lost. 2) PTFE has outstanding (self-lubricating) non-tackiness, i.e. very poor self-adhesiveness and mutual adhesiveness. 3) The linear expansion coefficient of PTFE is 10-20 times that of steel, and the linear expansion coefficient of PTFE changes irregularly along with the change of temperature.
The performance of the tetrapropylene fluoride rubber and the performance of the polytetrafluoroethylene are complementary. The polytetrafluoroethylene micro powder has excellent low temperature resistance and good self-lubrication, and makes up the defect of poor low temperature resistance of the tetrapropylene fluorocarbon rubber; the tetrapropylene fluoride rubber has strong cohesive force, excellent adhesiveness and excellent compression set resistance, and compensates the defects of poor self-adhesiveness and plastic deformation (creep) and loss of elastic recovery sealing property due to permanent deformation of the polytetrafluoroethylene micropowder under the action of long-time continuous load. This is important in the dynamic sealing of the drill rod of the wellhead pumping unit.
The linear expansion coefficient of the polytetrafluoroethylene is changed irregularly along with the change of the temperature by the filling stability of reinforcing agents such as aramid pulp, glass fiber, precipitated silica and the like. Blending of the two phases requires conditioning with oils such as common processing oils. After the polytetrafluoroethylene micro powder is mixed with the colloidal tetrapropylene fluoride gum with good affinity and the filler operating agent, a single-phase continuous structure with the tetrapropylene fluoride gum as a continuous phase is formed in a mixed phase, a two-phase continuous area is formed, and a dispersed phase is formed by reinforcing agents such as aramid pulp and the like and tetrafluoroethylene in an amorphous area of the tetrapropylene fluoride and is uniformly distributed.
Examples 1,
The embodiment provides a self-lubricating sealing injection agent, which comprises the following formula:
| serial number | Starting materials | Parts by weight |
| 1 | Tetrapropylene rubber | 40 |
| 2 | Silicon coupling agent | 8 |
| 3 | Liquid polysulfide glue | 10 |
| 4 | Titanium dioxide | 15 |
| 5 | Polytetrafluoroethylene micropowder | 40 |
| 6 | Aramid fiber pulp | 15 |
| 7 | White oil | 25 |
| 8 | Kerosene oil | 10 |
| 9 | Vaseline | 5 |
The preparation method of the self-lubricating sealing injection agent comprises the following steps:
1) plasticating raw rubber: an open mill, wherein the tetrapropylene fluororubber is subjected to low-temperature thin-pass plastication until the Mooney viscosity is 30-40;
2) mixing the tetrafluoroethylene-propylene rubber and a silicon coupling agent;
3) mixing the powder reinforcing regulator titanium dioxide and the internal cohesive tackifier liquid polysulfide glue, adding the mixture into the glue stock prepared in the step 2), mixing to obtain a glue body, and taking out a glue sheet to be dissolved into a glue paste system in a glue viscous state;
4) soaking polytetrafluoroethylene micro powder and fiber reinforcing regulator aramid pulp in plasticizer oils (white oil, kerosene, vaseline) to obtain a fiber oil-immersed system; specifically, the polytetrafluoroethylene micro powder, the fiber reinforcing regulator and the plasticizer oil are mixed and stirred in a stirring tank for 0.5 hour, and then are soaked and cured for 5 hours at the temperature of 60 ℃.
5) Mixing and stirring the mucilage system prepared in the step 3) and the fiber oil immersion system prepared in the step 4) uniformly;
6) mixing the materials processed in the steps 1), 2) and 3) together in an internal mixer, and smashing and refining the materials in an open mill to obtain a semi-finished rubber sheet;
7) extruding the sealant rod.
Examples 2,
The embodiment provides a self-lubricating sealing injection agent, which comprises the following formula:
the preparation method of the self-lubricating sealing injection agent comprises the following steps:
1) plasticating raw rubber: an open mill, wherein the tetrapropylene fluororubber is subjected to low-temperature thin-pass plastication until the Mooney viscosity is 30-40;
2) mixing the tetrafluoroethylene-propylene rubber and a silicon coupling agent;
3) mixing the powder reinforcing regulator precipitated silicon dioxide and the cohesive tackifier liquid silica gel, adding the mixture into the glue stock prepared in the step 2), mixing to obtain a glue body, and taking out a glue sheet to be dissolved into a glue paste system in a glue viscous state;
4) polytetrafluoroethylene micro powder, aramid pulp as fiber reinforcing regulator and oils (white oil and glycerol) of polytetrafluoroethylene fiber soaking plasticizer, soaking and curing to form a fiber oil-immersed system; specifically, the polytetrafluoroethylene micro powder, the fiber reinforcing regulator and the plasticizer oil are mixed and stirred in a stirring tank for 0.5 hour, and then are soaked and cured for 5 hours at the temperature of 60 ℃.
5) Mixing and stirring the mucilage system prepared in the step 3) and the fiber oil immersion system prepared in the step 4) uniformly;
6) mixing the materials processed in the steps 1), 2) and 3) together in an internal mixer, and smashing and refining the materials in an open mill to obtain a semi-finished rubber sheet;
7) extruding the sealant rod.
Examples 3,
The embodiment provides a self-lubricating sealing injection agent, which comprises the following formula:
| serial number | Raw materials | Parts by weight |
| 1 | Tetrapropylene rubber | 50 |
| 2 | Silicon coupling agent | 10 |
| 3 | Polytetrafluoroethylene micropowder | 40 |
| 4 | Precipitated silica | 20 |
| 5 | Molybdenum disulfide | 10 |
| 6 | Liquid polysulfide rubber | 20 |
| 7 | Aramid fiber pulp | 15 |
| 8 | Glass fiber | 15 |
| 9 | Glycerol | 15 |
| 10 | Kerosene oil | 45 |
The preparation method of the self-lubricating sealing injection agent comprises the following steps:
1) plasticating raw rubber: an open mill, wherein the tetrapropylene fluororubber is subjected to low-temperature thin-pass plastication until the Mooney viscosity is 30-40;
2) mixing the tetrafluoroethylene-propylene rubber and a silicon coupling agent;
3) mixing the powder reinforcing regulator precipitated silicon dioxide, molybdenum disulfide and the cohesion tackifier liquid silica gel, adding the mixture into the rubber material prepared in the step 2), mixing to obtain a colloid, and dissolving the obtained sheet into a colloidal system;
4) polytetrafluoroethylene micro powder, aramid pulp as fiber reinforcing and regulating agent and oils (glycerin and kerosene) as plasticizer soaking and curing of glass fiber, and soaking and curing into fiber oil immersion system; specifically, the polytetrafluoroethylene micro powder, the fiber reinforcing regulator and the plasticizer oil are mixed and stirred in a stirring tank for 0.5 hour, and then are soaked and cured for 5 hours at the temperature of 60 ℃.
5) Mixing and stirring the mucilage system prepared in the step 3) and the fiber oil immersion system prepared in the step 4) uniformly;
6) mixing the materials processed in the steps 1), 2) and 3) together in an internal mixer, and smashing and refining the materials in an open mill to obtain a semi-finished rubber sheet;
7) and extruding the sealant injection bar.
The performance of the sealant prepared in example 3 was tested and the results were as follows:
in conclusion, the self-lubricating sealing injection agent provided by the invention has the following advantages:
1. plasticity and persistence: the service life is one year, and the product can be deformed and filled in the service life;
2. lubricity: the extrusion is easy;
3. cohesion force: the bar is compact;
4. high and low temperature environment extrusion test: the high temperature 40 low temperature 40 degree extrusion performance is good.
The present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (7)
1. The self-lubricating sealing injection agent is characterized by comprising the following components in parts by weight: 20-60 parts of tetrapropylene fluoride rubber, 30-70 parts of polytetrafluoroethylene micro powder, 15-40 parts of powder reinforcing and regulating agent, 15-40 parts of fiber reinforcing and regulating agent, 20-60 parts of plasticizer oil, 5-30 parts of surfactant and 5-30 parts of cohesive tackifier.
2. The self-lubricating sealant according to claim 1, wherein the powder reinforcing modifier is one or more of precipitated silica, titanium dioxide and molybdenum disulfide, and the fiber reinforcing modifier is one or more of aramid pulp, glass fiber and polytetrafluoroethylene fiber.
3. The self-lubricating sealant according to claim 1 wherein the plasticizer oil is one or more of acetone, white oil, glycerin, kerosene, silicone oil, petrolatum.
4. The self-lubricating sealant according to claim 1, wherein the surfactant is a room temperature silicon coupling agent.
5. The self-lubricating sealant according to claim 1, wherein the cohesive adhesion agent is one or both of liquid polysulfide rubber, liquid silicone rubber.
6. A method of making a self-lubricating sealant according to claim 1, comprising the steps of:
1) plasticating raw rubber: an open mill, wherein the tetrapropylene fluororubber is subjected to low-temperature thin-pass plastication until the Mooney viscosity is 30-40;
2) mixing the tetrapropylene fluoride rubber and a surfactant;
3) mixing the powder reinforcing regulator and the cohesive tackifier, adding the mixture into the rubber material prepared in the step 2), mixing to obtain a colloid, and taking out a rubber sheet to be dissolved into a colloidal-state rubber cement system;
4) the polytetrafluoroethylene micro powder and the fiber reinforcing and regulating agent are soaked in plasticizer oil and soaked and cured into a fiber oil-immersed system;
5) mixing and stirring the mucilage system prepared in the step 3) and the fiber oil immersion system prepared in the step 4) uniformly;
6) mixing the materials processed in the steps 1), 2) and 3) in an internal mixer, and smashing in an open mill to obtain semi-finished rubber sheets;
7) extruding the sealant rod.
7. The method for preparing a self-lubricating sealant according to claim 6, wherein in the step 4), the polytetrafluoroethylene micro powder, the reinforcing modifier and the plasticizer oil are mixed and stirred in a stirring tank for 0.5 hour, and then are soaked and cured at 60 ℃ for 5 hours.
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