CN112552985A - Low-temperature rod-shaped valve rod sealing grease composition and preparation method thereof - Google Patents

Low-temperature rod-shaped valve rod sealing grease composition and preparation method thereof Download PDF

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CN112552985A
CN112552985A CN202011470424.6A CN202011470424A CN112552985A CN 112552985 A CN112552985 A CN 112552985A CN 202011470424 A CN202011470424 A CN 202011470424A CN 112552985 A CN112552985 A CN 112552985A
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parts
low
temperature
shaped valve
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CN112552985B (en
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邵聪
吴超
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Wuhan Boda Special Lubricant Technology Co ltd
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Wuhan Boda Special Lubricant Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04—Mixtures of base-materials and additives
    • C10M169/048—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution, non-macromolecular and macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04—Elements
    • C10M2201/041—Carbon; Graphite; Carbon black
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06—Metal compounds
    • C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10—Compounds containing silicon
    • C10M2201/105—Silica
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/026—Butene
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/14—Synthetic waxes, e.g. polythene waxes
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
    • C10M2209/084—Acrylate; Methacrylate
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/22—Heterocyclic nitrogen compounds
    • C10M2215/223—Five-membered rings containing nitrogen and carbon only
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/10—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring
    • C10M2219/104—Heterocyclic compounds containing sulfur, selenium or tellurium compounds in the ring containing sulfur and carbon with nitrogen or oxygen in the ring
    • C10M2219/106—Thiadiazoles
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/04—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions having a silicon-to-carbon bond, e.g. organo-silanes
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04—Siloxanes with specific structure
    • C10M2229/041—Siloxanes with specific structure containing aliphatic substituents

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Sealing Material Composition (AREA)
  • Lubricants (AREA)

Abstract

The invention discloses a low-temperature rod-shaped valve rod sealant composition which comprises the following components in parts by weight: 18-67.4 parts of methyl silicone oil, 2-8 parts of tackifier, 2-10 parts of fumed silica, 0.5-5 parts of structure improver, 15-25 parts of polyethylene wax, 2-8 parts of asbestos fiber, 10-20 parts of colloidal graphite, 1-5 parts of titanium dioxide and 0.1-1 part of corrosion inhibitor. The invention also discloses a preparation method of the sealing agent composition for the rod-shaped valve rod. The rod-shaped valve rod sealant compound prepared by thickening methyl silicone oil by adopting gas phase method silicon dioxide and matching with tackifier, solid lubricant, forming agent and corrosion inhibitor has excellent low-temperature performance, good thermal stability and chemical stability, strong medium erosion resistance, excellent sealing property, pressure resistance, adhesion and abrasion resistance, and is non-toxic, non-sticky, plastic, non-curing and randomly formed.

Description

Low-temperature rod-shaped valve rod sealing grease composition and preparation method thereof
Technical Field
The invention relates to the technical field of sealing lubricants, in particular to a low-temperature rod-shaped valve rod sealing grease composition and a preparation method thereof.
Background
The valve rod is an important part of the valve and is used for transmitting power, the valve rod is connected with an actuating mechanism or a handle, and the lower part of the valve rod directly drives the valve core or the valve plate to move or rotate so as to realize the opening and closing or adjusting function of the valve. The valve rod is not only a moving part and a stressed part but also a sealing part in the opening and closing process of the valve. At the same time, it is impacted and corroded by the media and also rubs against the filler.
The wellhead device for oil and gas production in oil field is formed by connecting and combining a plurality of valves, wherein the wellhead hydraulic control blowout preventer and the hydraulic control gate valve are safety devices, once oil and gas blowout occurs, the blowout prevention valve is opened rapidly to lead high-pressure oil and gas flow out of a well site so as to ensure the safety of the wellhead device and personnel, so that the rapid and sensitive opening and closing of the blowout prevention valve is particularly important, and a valve rod sealant for lubricating and sealing is required to be provided for the blowout prevention valve.
The oil field oil extraction and gas production well in cold or extremely cold weather area has working environment temperature as low as-50 deg.c and is in the bad conditions of wind, snow and low temperature weather for long period. The common sealing grease can be directly frozen due to poor low-temperature rheological property, and the sealing and lubricating functions of the common sealing grease are lost.
The low-temperature performance of the valve rod sealant directly influences the openness and sensitivity of the well head hydraulic control blowout preventer and the hydraulic control flashboard valve switch in the low-temperature environment. At present, no low-temperature valve rod sealing agent is available on the market, and common sealing grease or lithium-based lubricating grease is used for an anti-spraying valve and a gate valve in a low-temperature environment, so that the following defects exist:
1) the low temperature is poor, and the rapid and sensitive switching of the blowout prevention valve and the gate valve is influenced when the northern area is in winter;
2) the medium erosion resistance is poor, and the oil gas is easy to dissolve and dilute;
3) poor sealing performance and pressure resistance, which causes poor sealing of the valve rod;
4) the high temperature can not meet the requirement and is easy to lose;
no relevant literature report is found about the low-temperature valve stem sealing agent.
Disclosure of Invention
Aiming at the defects of the lubrication and the sealing of the valve rod of the wellhead hydraulic control blowout preventer and the hydraulic control gate valve in the low-temperature environment, the invention provides a low-temperature rod-shaped valve rod sealant composition, which is prepared by thickening methyl silicone oil by adopting gas-phase method silicon dioxide and matching with a tackifier, a solid lubricant, a forming agent and a corrosion inhibitor, has excellent low-temperature performance, good thermal stability and chemical stability, strong medium erosion resistance, excellent sealing property, pressure resistance, adhesiveness and abrasion resistance, is nontoxic, non-sticky, plastic, non-curable and randomly formed; the sealing device is suitable for sealing, lubricating and protecting valve rods of oil-gas field wellhead hydraulic control blowout preventers and hydraulic control gate valves and also suitable for sealing and lubricating valve rods of other high-temperature high-pressure liquid and gas medium valves.
The second purpose of the invention is to provide a preparation method of the low-temperature rod-shaped valve rod sealant.
The first purpose of the invention is realized by the following technical scheme:
the rod-shaped valve rod sealant composition is characterized by comprising the following components in parts by weight:
Figure BDA0002833343200000021
further, the methyl silicone oil is a linear chain structure, and the main technical index ranges of the methyl silicone oil are as follows: kinematic viscosity (25 ℃): 8000-20000 mm2And/s, a flash point (open) of not less than 300 ℃ and a pour point of not more than-50 ℃. The main functions are as follows: 1) the sealant has excellent low-temperature performance and viscosity-temperature coefficient, and reduces the rheological resistance of the sealant at low temperature; 2) the kinematic viscosity is large, the adhesion on the metal surface is strong, and the sealing performance is good.
Furthermore, the tackifier is one or a mixture of polymethyl methacrylate and low molecular polyisobutylene. The main technical index range of polymethyl methacrylate is as follows: kinematic viscosity (100 ℃): 850-2450 mm2(ii)/s, flash point (open) of not less than 240 ℃, acid value mgKOH/g of not more than 0.5; the main technical index range of the low molecular polyisobutylene is as follows: kinematic viscosity (100 ℃): 950 to 2900mm2(ii)/s, flash point (open) of not less than 250 ℃ and acid value mgKOH/g of not more than 0.1. The main functions are as follows: 1) the dynamic viscosity is high, the adhesion on the metal surface is strong, the bearing capacity is high, the valve rod is not easy to be extruded or washed away, and the sealing function is strong; 2) it has large molecular weight, large thickness of formed oil film, high strength and good lubricating property.
Further, the fumed silica is prepared byA vapor phase process hydrophilic silica. The main technical index range of the gas-phase method hydrophilic silicon dioxide is as follows: specific surface area: 100 to 400m2Water content (105 ℃ C.. times.2H) of not more than 0.5% by weight. The main functions are as follows: 1) the thermal stability is good, and the consistency of the grease does not change obviously at high temperature, namely the grease has good high-temperature characteristics; 2) the grease formed by thickening has excellent colloid stability and mechanical stability; 3) the oil distribution is small, and the structure of the grease can be kept stable for a long time.
Further, the structure improving agent adopts one of diphenyl dihydroxy silane, hexamethyl disilazane or octyl trimethoxy silane. The hydroxyl group in the structure improving agent can be reacted with SiO2The molecules are combined, so that the intersolubility of the thickening agent and the base oil is increased, the stability of the colloid structure of the lubricating grease is improved, and the shearing resistance and the rheologic resistance of the colloid are greatly improved.
Further, the polyethylene wax is white particles, and the main technical index ranges are as follows: kinematic viscosity (149 ℃): 40-100 mm2(s), softening point: 105 to 110 ℃. It has the following advantages: 1) the polyethylene wax has stable chemical property, good chemical stability and colloid stability, and is not easy to lose consistency due to high-temperature oxidation of a thickening agent and long-time contact with corrosive media, so that the lubricating grease is lost; 2) the polyethylene wax belongs to high molecular hydrocarbon, has good adhesiveness and plasticity, and is convenient for the molding of the rod-shaped sealant; 3) the sealant prepared by the polyethylene wax is hardly dissolved in water, is not emulsified, and has stronger capability of preventing moisture and gas medium from permeating.
Furthermore, the asbestos fiber adopts inorganic mineral chrysotile fiber, and the main technical index ranges are as follows: content not less than 98%, fiber length: 1-10 mm. The main functions are as follows: 1) the molding agent used as the rod-shaped valve rod sealing agent ensures that the rod-shaped valve rod sealing agent is not broken or deformed; 2) the composite material has the advantages of good heat resistance, high temperature resistance at 480 ℃, weak acid and strong base resistance, high strength, good adsorption performance and the like. The dosage of the low-temperature rod-shaped valve rod sealant is controlled to be 2-8%, and the requirements of the low-temperature rod-shaped valve rod sealant on the forming and sealing performance can be met.
Furthermore, the colloidal graphite adopts scaly colloidal graphite powder, and the main technical index ranges are as follows: fixed carbon content not less than 98%, average particle diameter: 5 μm. The colloidal graphite belongs to a lamellar crystal structure, the bonding force between atoms in the same layer is stronger, and the bonding force between atoms between layers is weaker. The lamination of lamellar crystals means that a large pressure can be applied in the direction perpendicular to the lamellae, and a small tangential force can easily act in the direction of the lamellae to displace the lamellae from one another, so that a large pressure can be applied and the friction factor is small. Meanwhile, the paint is high temperature resistant, and the use temperature can reach over 600 ℃; the graphite is corrosion resistant, and except strong oxidation media such as fuming sulfuric acid, concentrated nitric acid and the like, the colloidal graphite can resist all media. The dosage of the low-temperature rod-shaped valve rod sealant is controlled to be 10-20%, and the requirements of the low-temperature rod-shaped valve rod sealant on the lubricating performance and the sealing performance can be met.
Furthermore, the titanium dioxide adopts anatase titanium dioxide, and the main technical index range is as follows: the content is not less than 98%, and the volatile matter (105 ℃) is not more than 1.5%. Titanium dioxide belongs to a non-layered structure solid lubricant, can be accumulated on a friction surface to form a single-layer or multi-layer covering film with lower stress, can enhance the thickness and strength of an oil film, can reduce the friction coefficient and enhance the bearing capacity. Meanwhile, the chemical property is stable, and the compound hardly reacts with any substance at normal temperature. The dosage of the low-temperature rod-shaped valve rod sealant is controlled to be 1-5%, and the requirements of the low-temperature rod-shaped valve rod sealant on the lubricating performance and the sealing performance can be met.
Furthermore, the corrosion inhibitor adopts one or a mixture of two of benzotriazole and derivative thereof or thiadiazole derivative. The benzotriazole and the derivative thereof adopt benzotriazole (T706) or benzotriazole derivative (T551), and the thiadiazole derivative adopts 2, 5-dithio-1, 3, 4-thiadiazole derivative (T561). The corrosion inhibitor has the effects that a chemical film, namely a passivation layer, can be formed on the surface of metal by the corrosion inhibitor, and metal ions are prevented from entering lubricating grease, so that the catalytic oxidation effect on oil is weakened, the service life of the oil is prolonged, and meanwhile, the corrosion of sulfur and organic acid on nonferrous metals such as copper, lead, tin, silver and the like is prevented. The dosage of the corrosion inhibitor is controlled within the range of 0.1-1%, namely the requirement of corrosion resistance of the low-temperature rod-shaped valve rod sealant is met.
The second object of the invention is achieved by the following technical measures:
a preparation method of the low-temperature rod-shaped valve rod sealant composition comprises the following steps:
1) firstly, sequentially adding methyl silicone oil and tackifier into a reaction kettle, heating and stirring to 90 +/-5 ℃, stirring at constant temperature for 30 +/-5 minutes to uniformly disperse a system, then adding a structure improver, continuously heating to 160 +/-5 ℃, slowly adding fumed silica, then adding polyethylene wax, and stirring at constant temperature for 60 +/-5 minutes;
2) after the constant temperature is finished, sequentially adding asbestos fibers, colloidal graphite, titanium dioxide and a corrosion inhibitor, stirring and dispersing for 45 +/-5 minutes, then discharging, putting into a barrel, immediately carrying out hot grinding once through a three-roll grinding machine, and holding into a thick rod shape for later use;
3) and (3) preparing the crude rod-shaped semi-finished product into a cylinder by a circular hole forming machine, and then cutting the cylinder into rod-shaped objects with the diameter of 15 +/-1 mm and the length of 110 +/-5 mm to obtain the low-temperature rod-shaped valve rod sealant composition.
The invention has the technical advantages that:
1. the invention adopts hydrophilic silicon dioxide thickening methyl silicone oil, and is matched with the adhesion promoter and the solid lubricant, and simultaneously adopts a brand new technical route to creatively add polyethylene wax and asbestos fiber into the sealing agent composition, and the obtained sealing agent composition of the rod-shaped valve rod has excellent low-temperature performance, excellent thermal stability and chemical stability, strong medium erosion resistance, excellent sealing property, pressure resistance, adhesion and abrasion resistance. The gap that no low-temperature valve rod sealing agent exists in the market is filled. The sealing, lubricating and protecting device is suitable for sealing, lubricating and protecting the valve rods of the hydraulic control blowout preventer and the hydraulic control gate valve of the oil and gas extraction well in the cold or extremely cold climate area;
2. compared with most of blowout prevention valves using common sealing grease or lithium-based lubricating grease, the low-temperature rod-shaped valve rod sealing grease composition provided by the invention has thicker lubricating grease film and lower friction coefficient; the valve rod has lower opening torque, stronger medium erosion resistance and better sealing property. The switch of the blowout prevention valve is quicker and more sensitive, so that the safety of a wellhead device and personnel is ensured;
3. the low-temperature rod-shaped valve rod sealing grease compound provided by the invention is non-toxic, non-sticky, plastic, non-curable, randomly shaped and easier to fill a valve in use.
Detailed Description
The present invention is described in detail with reference to the following embodiments, however, the scope of the present invention is not limited to the following embodiments, and those skilled in the art can achieve the object of the present invention based on the disclosure of the present invention.
Example one
A low-temperature rod-shaped valve rod sealing grease composition is prepared by the following steps:
1) 43.5 parts of methyl silicone oil (V25-15000 mm)2S) and 5 parts of polymethyl methacrylate (V100. about.1050 mm)2/s) sequentially adding the mixture into a reaction kettle, heating and stirring the mixture to 90 +/-5 ℃, stirring the mixture at constant temperature for 30 +/-5 minutes to uniformly disperse the system, adding 2 parts of diphenyl dihydroxysilane, continuously heating the mixture to 160 +/-5 ℃, and slowly adding 6 parts of gas-phase hydrophilic silicon dioxide (the specific surface area is 200 m)2Per g) and 20 parts of polyethylene wax (V149. 85 mm) are then added2And/s) stirring at constant temperature for 60 +/-5 minutes.
2) After the constant temperature is finished, 5 parts of asbestos fiber, 15 parts of colloidal graphite, 3 parts of titanium dioxide and 0.5 part of T706 are sequentially added, stirred and dispersed for 45 +/-5 minutes, then discharged into a barrel, immediately and thermally ground once through a three-roll grinder, and held into a thick rod shape by a hand for later use.
3) And (3) preparing the crude rod-shaped semi-finished product into a cylinder by a circular hole forming machine, and then cutting the cylinder into rod-shaped objects with the diameter of 15 +/-1 mm and the length of 110 +/-5 mm to obtain the low-temperature rod-shaped valve rod sealant composition.
Example two
A low-temperature rod-shaped valve rod sealing grease composition is prepared by the following steps:
1) first, 36.7 parts of methyl silicone oil (V25-12500 mm)2S), 5 parts of polymethyl methacrylate (V100 ═ 1980 mm)2S) and 2 parts of low-molecular polyisobutene (V100 ═ 2870 mm)2/s) sequentially adding into a reaction kettle, heating to 90 +/-5 ℃, stirring at constant temperature for 30 +/-5 minutes to uniformly disperse the system, adding 3 parts of octyl trimethoxy silane, continuously heating to 160 +/-5 ℃, and slowly adding 8 parts of gas-phase hydrophilic silicon dioxide (the specific surface area is 150 m)2Per g) and then 22 parts of polyethylene wax (V149 ═ 97 mm) are added2And/s) stirring at constant temperature for 60 +/-5 minutes.
2) After the constant temperature is finished, 6 parts of asbestos fiber, 12 parts of colloidal graphite, 5 parts of titanium dioxide and 0.3 part of T561 are sequentially added, stirred and dispersed for 45 +/-5 minutes, then discharged into a barrel, immediately and thermally ground once through a three-roll grinder, and held into a thick rod shape by a hand for later use.
3) And (3) preparing the crude rod-shaped semi-finished product into a cylinder by a circular hole forming machine, and then cutting the cylinder into rod-shaped objects with the diameter of 15 +/-1 mm and the length of 110 +/-5 mm to obtain the low-temperature rod-shaped valve rod sealant composition.
EXAMPLE III
A low-temperature rod-shaped valve rod sealing grease composition is prepared by the following steps:
1) 33.8 parts of methyl silicone oil (V25-9500 mm)2S) and 8 parts of low-molecular polyisobutene (V100: 1030 mm)2/s) sequentially adding the mixture into a reaction kettle, heating and stirring the mixture to 90 +/-5 ℃, stirring the mixture at constant temperature for 30 +/-5 minutes to uniformly disperse the system, adding 3 parts of diphenyl dihydroxysilane, continuously heating the mixture to 160 +/-5 ℃, and slowly adding 9 parts of gas-phase hydrophilic silicon dioxide (the specific surface area is 260 m)2Per g) and then 16 parts of polyethylene wax (V149 ═ 55 mm) are added2And/s) stirring at constant temperature for 60 +/-5 minutes.
2) After the constant temperature is finished, sequentially adding 8 parts of asbestos fiber, 20 parts of colloidal graphite, 2 parts of titanium dioxide and 0.2 part of T551, stirring and dispersing for 45 +/-5 minutes, then discharging into a barrel, immediately carrying out hot grinding once through a three-roll grinding machine, and holding into a thick rod shape for later use.
3) And (3) preparing the crude rod-shaped semi-finished product into a cylinder by a circular hole forming machine, and then cutting the cylinder into rod-shaped objects with the diameter of 15 +/-1 mm and the length of 110 +/-5 mm to obtain the low-temperature rod-shaped valve rod sealant composition.
Example four
A low-temperature rod-shaped valve rod sealing grease composition is prepared by the following steps:
1) 44.2 parts of methyl silicone oil (V25-10900 mm)2S), 3 parts of polymethyl methacrylate (V100 ═ 1530 mm)2S) and 3 parts of low-molecular polyisobutene (V100 ═ 980 mm)2/s) sequentially adding the mixture into a reaction kettle, heating and stirring the mixture to 90 +/-5 ℃, stirring the mixture at constant temperature for 30 +/-5 minutes to uniformly disperse the system, adding 1 part of hexamethyldisilazane, continuously heating the mixture to 160 +/-5 ℃, and slowly adding 3 parts of gas-phase hydrophilic silicon dioxide (the specific surface area is 380 m)2Per g) and then 25 parts of polyethylene wax (V149. 79 mm)2And/s) stirring at constant temperature for 60 +/-5 minutes.
2) After the constant temperature is finished, 5 parts of asbestos fiber, 11 parts of colloidal graphite, 4 parts of titanium dioxide and 0.8 part of T706 are sequentially added, stirred and dispersed for 45 +/-5 minutes, then discharged into a barrel, immediately and thermally ground once through a three-roll grinder, and held into a thick rod shape by a hand for later use.
3) And (3) preparing the crude rod-shaped semi-finished product into a cylinder by a circular hole forming machine, and then cutting the cylinder into rod-shaped objects with the diameter of 15 +/-1 mm and the length of 110 +/-5 mm to obtain the low-temperature rod-shaped valve rod sealant composition.
EXAMPLE five
A low-temperature rod-shaped valve rod sealing grease composition is prepared by the following steps:
1) 50.8 parts of methyl silicone oil (V25-16600 mm)2S), 2 parts of polymethyl methacrylate (V100: 930 mm)2S) and 5 parts of low-molecular polyisobutene (V100 ═ 1460mm2/s) sequentially adding the mixture into a reaction kettle, heating and stirring the mixture to 90 +/-5 ℃, stirring the mixture at constant temperature for 30 +/-5 minutes to uniformly disperse the system, adding 2.7 parts of diphenyl dihydroxy silane, continuously heating the mixture to 160 +/-5 ℃, and slowly adding 8 parts of gas-phase hydrophilic silicon dioxide (the specific surface area is 320 m)2Per g) and then 15 parts of polyethylene wax (V149. 79 mm)2And/s) stirring at constant temperature for 60 +/-5 minutes.
2) After the constant temperature is finished, 4 parts of asbestos fiber, 10 parts of colloidal graphite, 2 parts of titanium dioxide and 0.5 part of T706 are sequentially added, stirred and dispersed for 45 +/-5 minutes, then discharged into a barrel, immediately and thermally ground once through a three-roll grinder, and held into a thick rod shape by a hand for later use.
3) And (3) preparing the crude rod-shaped semi-finished product into a cylinder by a circular hole forming machine, and then cutting the cylinder into rod-shaped objects with the diameter of 15 +/-1 mm and the length of 110 +/-5 mm to obtain the low-temperature rod-shaped valve rod sealant composition.
EXAMPLE six
A low-temperature rod-shaped valve rod sealing grease composition is prepared by the following steps:
1) 31.7 parts of methyl silicone oil (V25-12500 mm)2S) and 6 parts of polymethyl methacrylate (V100 ═ 1980 mm)2/s) sequentially adding into a reaction kettle, heating to 90 +/-5 ℃, stirring at constant temperature for 30 +/-5 minutes to uniformly disperse the system, adding 2 parts of octyl trimethoxy silane, continuously heating to 160 +/-5 ℃, and slowly adding 5 parts of gas-phase hydrophilic silicon dioxide (the specific surface area is 200 m)2Per g) and 24 parts of polyethylene wax (V149 ═ 95 mm) are then added2And/s) stirring at constant temperature for 60 +/-5 minutes.
2) After the constant temperature is finished, sequentially adding 8 parts of asbestos fiber, 18 parts of colloidal graphite, 5 parts of titanium dioxide and 0.3 part of T561, stirring and dispersing for 45 +/-5 minutes, then discharging into a barrel, immediately carrying out hot grinding once through a three-roll grinding machine, and holding into a thick rod shape for later use.
3) And (3) preparing the crude rod-shaped semi-finished product into a cylinder by a circular hole forming machine, and then cutting the cylinder into rod-shaped objects with the diameter of 15 +/-1 mm and the length of 110 +/-5 mm to obtain the low-temperature rod-shaped valve rod sealant composition.
EXAMPLE seven
A low-temperature rod-shaped valve rod sealing grease composition is prepared by the following steps:
1) 39.85 parts of methyl silicone oil (V25-13800 mm)2S) and 2 parts of polymethyl methacrylate (V100 ═ 2360 mm)2S) and 3 parts of low-molecular polyisobutene (V100 ═ 1890 mm)2S) sequential addition of the reactantsHeating and stirring to 90 +/-5 ℃ in a kettle, stirring at constant temperature for 30 +/-5 minutes to uniformly disperse the system, adding 2 parts of diphenyl dihydroxy silane, continuously heating to 160 +/-5 ℃, and slowly adding 6 parts of gas-phase hydrophilic silicon dioxide (the specific surface area is 180 m)2Per g) and then 22 parts of polyethylene wax (V149 ═ 95 mm) are added2And/s) stirring at constant temperature for 60 +/-5 minutes.
2) After the constant temperature is finished, 6 parts of asbestos fiber, 16 parts of colloidal graphite, 3 parts of titanium dioxide and 0.15 part of T551 are sequentially added, stirred and dispersed for 45 +/-5 minutes, then discharged into a barrel, immediately and thermally ground once through a three-roll grinder, and held into a thick rod shape by a hand for later use.
3) And (3) preparing the crude rod-shaped semi-finished product into a cylinder by a circular hole forming machine, and then cutting the cylinder into rod-shaped objects with the diameter of 15 +/-1 mm and the length of 110 +/-5 mm to obtain the low-temperature rod-shaped valve rod sealant composition.
The technical parameters of the low temperature stem sealant composition obtained in examples one to seven are shown in the following table:
Figure BDA0002833343200000091
Figure BDA0002833343200000101
the low-temperature rod-shaped valve rod sealant provided by the invention has the advantages of excellent low-temperature performance, excellent thermal stability and chemical stability, strong medium erosion resistance, excellent sealing property, pressure resistance and adhesion and long service life, and can completely meet the requirements of sealing, lubricating and protecting the valve rods of the wellhead hydraulic control blowout preventer and the hydraulic control gate valve of the oil and gas field in a low-temperature environment.
The above description is only for the specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.

Claims (11)

1. The low-temperature rod-shaped valve rod sealant composition comprises the following components in parts by weight:
Figure FDA0002833343190000011
2. the low temperature stick valve stem sealant composition as claimed in claim 1, wherein the methyl silicone oil is linear chain structure, and the methyl silicone oil has the following main technical indexes: kinematic viscosity (25 ℃): 8000-20000 mm2And/s, a flash point (open) of not less than 300 ℃ and a pour point of not more than-50 ℃.
3. The low temperature rod-shaped valve stem sealing agent composition as claimed in claim 1, wherein the tackifier is one or a mixture of polymethyl methacrylate and low molecular polyisobutylene, and the main technical index range of the polymethyl methacrylate is as follows: kinematic viscosity (100 ℃): 850-2450 mm2(ii)/s, flash point (open) of not less than 240 ℃, acid value mgKOH/g of not more than 0.5; the main technical index range of the low molecular polyisobutylene is as follows: kinematic viscosity (100 ℃): 950 to 2900mm2(ii)/s, flash point (open) of not less than 250 ℃ and acid value mgKOH/g of not more than 0.1.
4. The low temperature stem sealant composition as claimed in claim 1, wherein the thickening agent is fumed hydrophilic silica, which has a main specification range: specific surface area: 100 to 400m2Water content (105 ℃ C.. times.2H) of not more than 0.5% by weight.
5. The low temperature stem sealant composition as claimed in claim 1, wherein the structure-improving agent is one of diphenyldihydroxysilane, hexamethyldisilazane, or octyltrimethoxysilane.
6. The low temperature stick valve stem sealant composition of claim 1, wherein the polyethylene wax is white particles having a main specification range of: kinematic viscosity (149 ℃): 40-100 mm2(s), softening point: 105 to 110 ℃.
7. The low temperature stick valve stem sealant composition as claimed in claim 1, wherein the asbestos fiber is mineral chrysotile fiber, and the main technical index ranges thereof are as follows: content not less than 98%, fiber length: 1.0-10.0 mm.
8. The low-temperature stem sealant composition as claimed in claim 1, wherein the colloidal graphite is a flaky colloidal graphite powder, and the main technical index range is as follows: fixed carbon content not less than 98%, average particle diameter: 5 μm.
9. The low-temperature rod-shaped valve rod sealant composition as claimed in claim 1, wherein the titanium dioxide is anatase titanium dioxide, and the main technical index ranges are as follows: the content is not less than 98%, and the volatile matter (105 ℃) is not more than 1.5%.
10. The stem seal composition of claim 1, wherein the corrosion inhibitor is benzotriazole or a derivative thereof or a thiadiazole derivative, the benzotriazole or a derivative thereof is benzotriazole (T706) or a derivative thereof (T551), and the thiadiazole derivative is a 2, 5-dithio-1, 3, 4-thiadiazole derivative (T561).
11. A method of making a cryogenic stem sealant composition according to any one of claims 1 to 10 comprising the steps of:
1) firstly, sequentially adding methyl silicone oil and tackifier into a reaction kettle, heating and stirring to 90 +/-5 ℃, stirring at constant temperature for 30 +/-5 minutes to uniformly disperse a system, then adding a structure improver, continuously heating to 160 +/-5 ℃, slowly adding fumed silica, then adding polyethylene wax, and stirring at constant temperature for 60 +/-5 minutes;
2) after the constant temperature is finished, sequentially adding asbestos fibers, colloidal graphite, titanium dioxide and a corrosion inhibitor, stirring and dispersing for 45 +/-5 minutes, then discharging, putting into a barrel, immediately carrying out hot grinding once through a three-roll grinding machine, and holding into a thick rod shape for later use;
3) and (3) preparing the crude rod-shaped semi-finished product into a cylinder by a circular hole forming machine, and then cutting the cylinder into rod-shaped objects with the diameter of 15 +/-1 mm and the length of 110 +/-5 mm to obtain the low-temperature rod-shaped valve rod sealant composition.
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