CN108929544A - A kind of fluorine silicone rubber material and preparation method thereof for oil pumping in oil fields pump seal - Google Patents
A kind of fluorine silicone rubber material and preparation method thereof for oil pumping in oil fields pump seal Download PDFInfo
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- CN108929544A CN108929544A CN201810865457.7A CN201810865457A CN108929544A CN 108929544 A CN108929544 A CN 108929544A CN 201810865457 A CN201810865457 A CN 201810865457A CN 108929544 A CN108929544 A CN 108929544A
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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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
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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
- C08K3/34—Silicon-containing compounds
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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
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Abstract
The fluorine silicone rubber material and preparation method thereof that the present invention relates to a kind of for oil pumping in oil fields pump seal, belongs to oil well pump equipment technology field.The fluorine silicone rubber that the present invention is prepared using surface there is the Fullerol compared with polyhydroxy to be activated, allow to carry out graft reaction with silane coupling agent, obtain the fullerene of surface modification siloxanes；And polymerization reaction can be hydrolyzed with D4 and fluorosilicone in siloxanes, so that fullerene modification is in the network of polysiloxanes, in this, as the base-material of silicon rubber, after silicon rubber base-material is mixed and vulcanized with filler, the silicon rubber of obtained fullerene modification has apparent oil resistance and mechanical performance.
Description
Technical field
The fluorine silicone rubber material and preparation method thereof that the present invention relates to a kind of for oil pumping in oil fields pump seal belongs to oil pump dress
Standby technical field.
Background technique
Oil well pump is that the common downhole hardware for crude oil in well being extracted into ground is driven by pumping unit.Common oil well pump mainly by
The most of composition of pump barrel, inlet valve, piston, drain four.Fixed form according to oil well pump in underground, can be divided into tubing pump and
Insert pump.Oil well pump is the underground equipment of oil pumping.Contain sand, wax, water, gas and corrosive substance in the liquid of its institute's pumping, again
In hundreds of meters of underground works to upper km, pump pressure may be up to 10MPa or more.So its working environment is complicated, item
Part is severe, and the quality of pump work directly influences oil well output.Therefore oil well pump should generally meet following requirements: (1) tying
Structure is simple, intensity is high, high-quality, coupling part sealed reliable；(2) manufacture material is wear-resisting and corrosion resistance is good, long service life；
(3) specification type is able to satisfy the needs of oil well lifting rate, adaptable；(4) it is convenient for removing；(5) be considered as in structure sand control,
Gas-tight, and have necessary ancillary equipment.
Usually the sealing material used in oil well pump is in materials such as silicon rubber, with stronger surface polarity, therefore
It can play the role of oil resistant.Silicon rubber refers to that main chain is alternately made of silicon and oxygen atom, usually connects that there are two have on silicon atom
The rubber of machine group.Common silicon rubber is mainly made of the silicon oxygen chain link containing methyl and a small amount of vinyl.
But when due to oil pumping in oil fields operation, conditions down-hole is severe, under high pressure, high oil and hot conditions, can make fluorine
Silicon rubber after long-term use, there is intensity decline, poor sealing the problem of.
Summary of the invention
The purpose of the present invention is: long-time use intensity existing for the fluorine silicone rubber used for high temperature oil pump declines, close
The bad problem of envelope property proposes oil resistant, the fluorine silicone rubber sealing material resistant to high temperature of a kind of fullerene enhancing.
Technical solution is:
A kind of fluorine silicone rubber material for oil pumping in oil fields pump seal, including following component by weight:
100 parts of fluorosilicon oil, 20~25 parts of the white carbon black, 10~12 parts of mica powder, 0.5~1 part of vulcanizing agent of fullerene modification.
Further, the preparation method of the fluorosilicon oil of fullerene modification, includes the following steps:
S1:
Wherein,Refer to Fullerol.
Further, the preparation method, includes the following steps:
S1: Fullerol, sodium hydride, n,N-Dimethylformamide are added extremely according to weight ratio 10:0.5~1:300~400
In reactor, 30~60min is handled at 20~35 DEG C, after product is centrifugated, uses ethanol washing；
S2: according to weight ratio 1:80~100, product obtained in step S1 is added to the KH560 containing 1~5wt%
Dimethylbenzene in, 1~5h is reacted at 85~95 DEG C in a nitrogen atmosphere, product is centrifuged, and with ethanol washing,
Obtain the fullerene of silane coupling agent modification；
S3: eight methoxy cyclotetrasiloxanes (D4), the dimethyl silicone polymer of ethenyl blocking, silane coupling agent are modified
Fullerene, catalyst are uniformly mixed according to weight ratio 1:5~8:0.5~1:0.05~0.06, are warming up to 85 in a nitrogen atmosphere
~90 DEG C, γ-trifluoro propyl methyl cyclotrisiloxane (D3F) is then added dropwise, weight ratio 1:3~5 of D3F and D4 are added dropwise
Afterwards, it is warming up to 2~4h of reaction at 105~160 DEG C, then is warming up to 175~185 DEG C of decompressions and steams low-boiling point material, obtains fowler
The fluorosilicon oil of alkene modification.
Further, the catalyst is Pt catalyst.
The preparation method of fluorine silicone rubber material for oil pumping in oil fields pump seal, includes the following steps:
Step 1, the fluorosilicon oil of fullerene modification and white carbon black, mica powder are kneaded uniformly on a mill, are then carried out
Mixing；
Step 2, vulcanizing agent is added in mixing material carries out back mixing；
Step 3, back mixing material is vulcanized in a mold, obtains fluorine silicone rubber material.
Further, temperature is 135~145 DEG C in the internal mixing pass, and vacuum degree is 1000~1500pa of absolute pressure, close
The time of refining is 3~6h.
Further, the temperature of sulfidation is 165~180 DEG C, and vulcanization time is 15~20min, and sulfide stress is 10
~15Mpa.
Beneficial effect
The fluorine silicone rubber that the present invention is prepared using surface there is the Fullerol compared with polyhydroxy to be activated, make it
Graft reaction can be carried out with silane coupling agent, obtain the fullerene of surface modification siloxanes；And siloxanes can with
Polymerization reaction is hydrolyzed in D4 and fluorosilicone, so that fullerene is modified in the network of polysiloxanes, in this, as silicon rubber
Base-material, after silicon rubber base-material is mixed and vulcanized with filler, since the surface of fullerene has relatively much stronger hydroxyl
Base, polarity is stronger, and the silicon rubber of obtained fullerene modification has apparent oil resistance and mechanical performance.
Detailed description of the invention
Fig. 1 is the influence curve figure that methyl-silicone oil impregnates number of days confrontation amount variation △ W (%).
Fig. 2 is that methyl-silicone oil impregnates number of days to the influence curve figure of tearing strength (kN/m).
Fig. 3 is that methyl-silicone oil impregnates number of days to the influence curve figure of elongation rate of tensile failure (%).
Fig. 4 is that methyl-silicone oil impregnates number of days to the influence curve figure of tensile strength (MPa).
Fig. 5 is that methyl-silicone oil impregnates number of days to the influence curve figure of hardness (shore A).
Specific embodiment
Below by specific embodiment, invention is further described in detail.But those skilled in the art will manage
Solution, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Specific skill is not specified in embodiment
Art or condition person described technology or conditions or carry out according to the literature in the art according to product description.Examination used
Production firm person is not specified in agent or instrument, and being can be with conventional products that are commercially available.
Heretofore described percentage all refers to mass percent in the absence of special instructions.
Embodiment 1
The fluorosilicon oil of fullerene modification is prepared first.
S1: Fullerol, sodium hydride, n,N-Dimethylformamide are added according to weight ratio 10:0.5:300 to reactor
In, 30min is handled at 20 DEG C, after product is centrifugated, uses ethanol washing；
S2: according to weight ratio 1:80, product obtained in step S1 is added to the dimethylbenzene of the KH560 containing 1wt%
In, 1h is reacted at 85 DEG C in a nitrogen atmosphere, product is centrifuged, and with ethanol washing, obtains silane coupling agent
The fullerene of modification；
S3: eight methoxy cyclotetrasiloxanes (D4), the dimethyl silicone polymer of ethenyl blocking, silane coupling agent are modified
Fullerene, Pt catalyst are uniformly mixed according to weight ratio 1:5:0.5:0.05, are warming up to 85 DEG C in a nitrogen atmosphere, are then added dropwise
γ-trifluoro propyl methyl cyclotrisiloxane (D3F), the weight ratio 1:3 of D3F and D4 after being added dropwise, are warming up at 105 DEG C anti-
2h is answered, then is warming up to 175 DEG C of decompressions and steams low-boiling point material, obtains the fluorosilicon oil of fullerene modification.
After the fluorosilicon oil for obtaining fullerene modification, it is prepared into silicon rubber with filler and vulcanizing agent.
Step 1,100 parts of the fluorosilicon oil of fullerene modification are kneaded on a mill with 22 parts of white carbon black, 11 parts of mica powder
Uniformly, mixing is then carried out, temperature is 135 DEG C in internal mixing pass, and vacuum degree is absolute pressure 1000pa, and the time of mixing is 3h；
Step 2,0.5~1 part of progress back mixing of vulcanizing agent is added in mixing material, back mixing temperature is 145 DEG C, the back mixing time
It is 2h；
Step 3, back mixing material being vulcanized in a mold, the temperature of sulfidation is 165 DEG C, and vulcanization time is 15min,
Sulfide stress is 10Mpa, obtains fluorine silicone rubber material.
Embodiment 2
The fluorosilicon oil of fullerene modification is prepared first.
S1: Fullerol, sodium hydride, n,N-Dimethylformamide are added according to weight ratio 10:1:400 into reactor,
60min is handled at 35 DEG C, after product is centrifugated, uses ethanol washing；
S2: according to weight ratio 1:100, product obtained in step S1 is added to the dimethylbenzene of the KH560 containing 5wt%
In, 5h is reacted at 95 DEG C in a nitrogen atmosphere, product is centrifuged, and with ethanol washing, obtains silane coupling agent
The fullerene of modification；
S3: eight methoxy cyclotetrasiloxanes (D4), the dimethyl silicone polymer of ethenyl blocking, silane coupling agent are modified
Fullerene, Pt catalyst are uniformly mixed according to weight ratio 1:8:1:0.06, are warming up to 90 DEG C in a nitrogen atmosphere, are then added dropwise
γ-trifluoro propyl methyl cyclotrisiloxane (D3F), the weight ratio 1:5 of D3F and D4 after being added dropwise, are warming up at 160 DEG C anti-
4h is answered, then is warming up to 185 DEG C of decompressions and steams low-boiling point material, obtains the fluorosilicon oil of fullerene modification.
After the fluorosilicon oil for obtaining fullerene modification, it is prepared into silicon rubber with filler and vulcanizing agent.
Step 1,100 parts of the fluorosilicon oil of fullerene modification are kneaded on a mill with 25 parts of white carbon black, 12 parts of mica powder
Uniformly, mixing is then carried out, temperature is 145 DEG C in internal mixing pass, and vacuum degree is absolute pressure 1500pa, and the time of mixing is 6h；
Step 2,1 part of progress back mixing of vulcanizing agent is added in mixing material, back mixing temperature is 155 DEG C, and the back mixing time is 4h；
Step 3, back mixing material being vulcanized in a mold, the temperature of sulfidation is 180 DEG C, and vulcanization time is 20min,
Sulfide stress is 15Mpa, obtains fluorine silicone rubber material.
Embodiment 3
The fluorosilicon oil of fullerene modification is prepared first.
S1: Fullerol, sodium hydride, n,N-Dimethylformamide are added according to weight ratio 10:0.6:350 to reactor
In, 40min is handled at 25 DEG C, after product is centrifugated, uses ethanol washing；
S2: according to weight ratio 1:90, product obtained in step S1 is added to the dimethylbenzene of the KH560 containing 2wt%
In, 3h is reacted at 90 DEG C in a nitrogen atmosphere, product is centrifuged, and with ethanol washing, obtains silane coupling agent
The fullerene of modification；
S3: eight methoxy cyclotetrasiloxanes (D4), the dimethyl silicone polymer of ethenyl blocking, silane coupling agent are modified
Fullerene, Pt catalyst are uniformly mixed according to weight ratio 1:7:0.8:0.05, are warming up to 88 DEG C in a nitrogen atmosphere, are then added dropwise
γ-trifluoro propyl methyl cyclotrisiloxane (D3F), the weight ratio 1:4 of D3F and D4 after being added dropwise, are warming up at 130 DEG C anti-
3h is answered, then is warming up to 180 DEG C of decompressions and steams low-boiling point material, obtains the fluorosilicon oil of fullerene modification.
After the fluorosilicon oil for obtaining fullerene modification, it is prepared into silicon rubber with filler and vulcanizing agent.
Step 1,100 parts of the fluorosilicon oil of fullerene modification are kneaded on a mill with 20 parts of white carbon black, 10 parts of mica powder
Uniformly, mixing is then carried out, temperature is 140 DEG C in internal mixing pass, and vacuum degree is absolute pressure 1200pa, and the time of mixing is 4h；
Step 2,0.5 part of progress back mixing of vulcanizing agent is added in mixing material, back mixing temperature is 150 DEG C, and the back mixing time is
3h；
Step 3, back mixing material being vulcanized in a mold, the temperature of sulfidation is 175 DEG C, and vulcanization time is 18min,
Sulfide stress is 12Mpa, obtains fluorine silicone rubber material.
Reference examples 1
Difference with embodiment 3 is: Fullerol does not carry out the modification of silane coupling agent.
By eight methoxy cyclotetrasiloxanes (D4), the dimethyl silicone polymer of ethenyl blocking, Fullerol, Pt catalyst according to
Weight ratio 1:7:0.8:0.05 is uniformly mixed, and is warming up to 88 DEG C in a nitrogen atmosphere, and γ-trifluoro propyl methyl ring three is then added dropwise
The weight ratio 1:4 of siloxanes (D3F), D3F and D4 after being added dropwise, are warming up at 130 DEG C and react 3h, then are warming up to 180 DEG C and subtract
Pressure steams low-boiling point material, obtains fluorosilicon oil.
After obtaining fluorosilicon oil, it is prepared into silicon rubber with filler and vulcanizing agent.
Step 1,100 parts of the fluorosilicon oil of fullerene modification are kneaded on a mill with 20 parts of white carbon black, 10 parts of mica powder
Uniformly, mixing is then carried out, temperature is 140 DEG C in internal mixing pass, and vacuum degree is absolute pressure 1200pa, and the time of mixing is 4h；
Step 2,0.5 part of progress back mixing of vulcanizing agent is added in mixing material, back mixing temperature is 150 DEG C, and the back mixing time is
3h；
Step 3, back mixing material being vulcanized in a mold, the temperature of sulfidation is 175 DEG C, and vulcanization time is 18min,
Sulfide stress is 12Mpa, obtains fluorine silicone rubber material.
Reference examples 2
Difference with embodiment 3 is: not being modified using fullerene in the KH560 not being added in rubber.
By eight methoxy cyclotetrasiloxanes (D4), the dimethyl silicone polymer of ethenyl blocking, KH560, Pt catalyst according to
Weight ratio 1:7:0.14:0.05 is uniformly mixed, and is warming up to 88 DEG C in a nitrogen atmosphere, and γ-trifluoro propyl methyl ring is then added dropwise
The weight ratio 1:4 of trisiloxanes (D3F), D3F and D4 after being added dropwise, are warming up at 130 DEG C and react 3h, then is warming up to 180 DEG C
Decompression steams low-boiling point material, obtains the fluorosilicon oil of fullerene modification.
After the fluorosilicon oil for obtaining fullerene modification, it is prepared into silicon rubber with filler and vulcanizing agent.
Step 1,100 parts of the fluorosilicon oil of fullerene modification are kneaded on a mill with 20 parts of white carbon black, 10 parts of mica powder
Uniformly, mixing is then carried out, temperature is 140 DEG C in internal mixing pass, and vacuum degree is absolute pressure 1200pa, and the time of mixing is 4h；
Step 2,0.5 part of progress back mixing of vulcanizing agent is added in mixing material, back mixing temperature is 150 DEG C, and the back mixing time is
3h；
Step 3, back mixing material being vulcanized in a mold, the temperature of sulfidation is 175 DEG C, and vulcanization time is 18min,
Sulfide stress is 12Mpa, obtains fluorine silicone rubber material.
Reference examples 3
Using commercially available usual silicone rubber product as control.
Characterization is tested
Tearing strength is tested using GB/T529-2008 standard；
Hardness is tested using GB/T531-2008 standard；
Tensile strength, elongation rate of tensile failure are tested using GB/T528-2008 standard；
Oil resistance is tested using GB/T1690-2010 standard；
△ W=(W2-W1)/W1 × 100%, wherein W1 is aerial quality before sample impregnates；W2 is that sample impregnates
Aerial quality afterwards.
After the fluorine silicone rubber that above embodiments and reference examples are prepared uses methyl-silicone oil different number of days, its object is measured
Rationality can be with volume/weight variation.As a result as shown in the table:
Methyl-silicone oil impregnates the influence of number of days confrontation amount variation △ W (%)
As can be seen from the table, after fluorine silicone rubber prepared by the present invention impregnates in methyl-silicone oil, swelling ratio it is small and
Stablize.And compared with reference examples 3 in the prior art, after impregnating in the oil, obvious swelling has occurred, weight increases
It is more.And due to being modified by silicon oxygen bond in polysiloxanes not by fullerene in reference examples 1, so that fullerene can not be preferably
Play the role of improving oil resistance to silicon rubber.
Methyl-silicone oil impregnates influence of the number of days to tearing strength (kN/m)
As can be seen from the table, it after fluorine silicone rubber prepared by the present invention impregnates in methyl-silicone oil, still can keep
Preferable tearing strength.And apparent intensity decline has occurred after dipping in common fluorine silicone rubber material in the prior art
The problem of.
Methyl-silicone oil impregnates influence of the number of days to elongation rate of tensile failure (%)
As can be seen from the table, after fluorine silicone rubber prepared by the present invention impregnates in methyl-silicone oil, although also occurring
The phenomenon that elongation rate of tensile failure declines, but compared with fluorine silicone rubber in the prior art, still can keep preferably tearing strong
Degree.
Methyl-silicone oil impregnates influence of the number of days to tensile strength (MPa)
As can be seen from the table, after fluorine silicone rubber prepared by the present invention impregnates in methyl-silicone oil, under tensile strength
Drop degree is significantly less than fluorine silicone rubber material in the prior art, after the immersion of 10d, the material of embodiment 1- embodiment 3
The rate of descent of the tensile strength of material only has 7.69-9.69%, and 3 fluorine silicone rubber material of reference examples in the prior art passes through 10 days
Immersion after, rate of descent has reached 48.34%；In addition, embodiment 3 and reference examples 1 are as can be seen that use silicon to fullerene
After alkane coupling agent grafting processing, it can be made to polymerize with the main chain of siloxanes, form tridimensional network, it can be obvious
Improve tensile strength in ground.
Methyl-silicone oil impregnates influence of the number of days to hardness (shore A)
As can be seen from the table, it after fluorine silicone rubber prepared by the present invention impregnates in methyl-silicone oil, still can keep
Preferable hardness.
Claims (7)
1. a kind of fluorine silicone rubber material for oil pumping in oil fields pump seal, which is characterized in that including by weight such as the following group
Point: 100 parts of fluorosilicon oil, 20~25 parts of the white carbon black, 10~12 parts of mica powder, 0.5~1 part of vulcanizing agent of fullerene modification.
2. the fluorine silicone rubber material according to claim 1 for oil pumping in oil fields pump seal, which is characterized in that the richness
The preparation method for strangling the fluorosilicon oil of alkene modification, includes the following steps:
S1:
S2:
S3:
Wherein,Refer to Fullerol.
3. the fluorine silicone rubber material according to claim 2 for oil pumping in oil fields pump seal, which is characterized in that the system
Preparation Method includes the following steps:
S1: Fullerol, sodium hydride, n,N-Dimethylformamide are added according to weight ratio 10:0.5~1:300~400 to reaction
In device, 30~60min is handled at 20~35 DEG C, after product is centrifugated, uses ethanol washing；
S2: according to weight ratio 1:80~100, product obtained in step S1 is added to two of the KH560 containing 1~5wt%
In toluene, 1~5h is reacted at 85~95 DEG C in a nitrogen atmosphere, product is centrifuged, and with ethanol washing, obtained
The fullerene of silane coupling agent modification；
S3: the fowler that eight methoxy cyclotetrasiloxanes (D4), the dimethyl silicone polymer of ethenyl blocking, silane coupling agent are modified
Alkene, catalyst are uniformly mixed according to weight ratio 1:5~8:0.5~1:0.05~0.06, are warming up to 85~90 in a nitrogen atmosphere
DEG C, γ-trifluoro propyl methyl cyclotrisiloxane (D3F) is then added dropwise, weight ratio 1:3~5 of D3F and D4 after being added dropwise, rise
Temperature is to reacting 2~4h at 105~160 DEG C, then is warming up to 175~185 DEG C of decompressions and steams low-boiling point material, obtains fullerene and modifies
Fluorosilicon oil.
4. the fluorine silicone rubber material according to claim 3 for oil pumping in oil fields pump seal, which is characterized in that described urges
Agent is Pt catalyst.
5. the preparation method of the fluorine silicone rubber material described in claim 1 for oil pumping in oil fields pump seal, which is characterized in that packet
Include following steps:
Step 1, the fluorosilicon oil of fullerene modification and white carbon black, mica powder are kneaded uniformly on a mill, then carry out mixing；
Step 2, vulcanizing agent is added in mixing material carries out back mixing；
Step 3, back mixing material is vulcanized in a mold, obtains fluorine silicone rubber material.
6. the preparation method of the fluorine silicone rubber material according to claim 5 for oil pumping in oil fields pump seal, feature exist
In, temperature is 135~145 DEG C in the internal mixing pass, and vacuum degree is 1000~1500pa of absolute pressure, the time of mixing is 3~
6h。
7. the preparation method of the fluorine silicone rubber material according to claim 5 for oil pumping in oil fields pump seal, feature exist
In the temperature of sulfidation is 165~180 DEG C, and vulcanization time is 15~20min, and sulfide stress is 10~15Mpa.
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| CN201810865457.7A CN108929544A (en) | 2018-08-01 | 2018-08-01 | A kind of fluorine silicone rubber material and preparation method thereof for oil pumping in oil fields pump seal |
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2018
- 2018-08-01 CN CN201810865457.7A patent/CN108929544A/en active Pending
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