CN114015103A - Surface fluorination treatment method for silicone rubber ring and anti-sticking application - Google Patents
Surface fluorination treatment method for silicone rubber ring and anti-sticking application Download PDFInfo
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- CN114015103A CN114015103A CN202111388047.6A CN202111388047A CN114015103A CN 114015103 A CN114015103 A CN 114015103A CN 202111388047 A CN202111388047 A CN 202111388047A CN 114015103 A CN114015103 A CN 114015103A
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- silicon rubber
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- silicone rubber
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 93
- 238000003682 fluorination reaction Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000004945 silicone rubber Substances 0.000 title claims description 32
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 58
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 58
- 239000011737 fluorine Substances 0.000 claims abstract description 58
- 238000007789 sealing Methods 0.000 claims abstract description 35
- 125000001153 fluoro group Chemical group F* 0.000 claims abstract description 5
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 5
- 239000002344 surface layer Substances 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 18
- 238000012360 testing method Methods 0.000 description 12
- 229920001971 elastomer Polymers 0.000 description 9
- 239000005060 rubber Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 150000003376 silicon Chemical class 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229920001903 high density polyethylene Polymers 0.000 description 1
- 239000004700 high-density polyethylene Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
- C08J7/126—Halogenation
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16J—PISTONS; CYLINDERS; SEALINGS
- F16J15/00—Sealings
- F16J15/02—Sealings between relatively-stationary surfaces
- F16J15/06—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces
- F16J15/10—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces with non-metallic packing
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16J—PISTONS; CYLINDERS; SEALINGS
- F16J15/00—Sealings
- F16J15/02—Sealings between relatively-stationary surfaces
- F16J15/06—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces
- F16J15/10—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces with non-metallic packing
- F16J15/108—Special methods for making a non-metallic packing
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- Engineering & Computer Science (AREA)
- General Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Sealing Material Composition (AREA)
- Treatments Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a silicon rubber surface fluorination treatment method and anti-sticking application, wherein silicon rubber is put into a fluorine-containing atmosphere for fluorination treatment so as to realize fluorination of the surface layer of the silicon rubber, and fluorine atoms are used for replacing hydrogen atoms in a silicon rubber molecular chain. The invention provides a surface fluorination treatment method of silicon rubber and application of the silicon rubber as a sealing ring, wherein the application effectively avoids the sticking phenomenon of the existing silicon rubber sealing ring, and further improves the service performance of the silicon rubber sealing ring.
Description
Technical Field
The invention relates to the technical field of silicone rubber, in particular to a surface fluorination treatment method of a silicone rubber sealing ring and anti-sticking application.
Background
Silicone rubber refers to rubber having a backbone composed of alternating silicon and oxygen atoms, with the silicon atoms typically having two organic groups attached to them.
Conventional silicone rubbers consist predominantly of siloxane segments containing methyl groups and small amounts of vinyl groups.
The silicon rubber has outstanding low-temperature resistance and can still normally work under the working condition of-55 ℃. Meanwhile, the silicon rubber also has certain heat resistance, can work for a long time under the working condition of 150 ℃, can still have elasticity for weeks or longer even if the temperature is slightly higher than 200 ℃, and can instantaneously resist the high temperature of more than 300 ℃.
In addition, the silicon rubber also has the outstanding characteristics of physiological inertia and no coagulation, so the silicon rubber is widely applied in the medical field.
Based on the excellent characteristics of the silicon rubber, particularly the low-temperature resistance, the silicon rubber is used as a key sealing structural part and has a wide application field. For example, in the field of weapons and equipment, two silicone rubber seals are typically used to seal against each other due to the necessity of sealing in cold environments. Similarly, in maritime works and oceanographic arts, the environment involved is severe, such as the arctic circle, the antarctic continental region, etc., and low temperature resistant silicone rubber is also required to be used as a sealing member.
In the application, the silicon rubber ring can cause the situation that two silicon rubber sealing rings are sticky based on the characteristics of silicon rubber, so that the use is inconvenient, and the sealing ring base body can be damaged by forcibly separating the two silicon rubber sealing rings when the two silicon rubber sealing rings are sticky. In the existing treatment mode, the physical mode of smearing the talcum powder on the silicon rubber is generally adopted to prevent sticking, but the talcum powder is not easy to adhere to the surface of the silicon rubber, is easy to drop and cannot be repeatedly used, so that the problems of low surface cleanliness of a silicon rubber ring and poor adhesion consistency of the talcum powder on the surface of the silicon rubber are caused. Therefore, the treatment with talc is still not ideal.
Disclosure of Invention
In view of the above problems, it is an object of the present invention to provide a method for fluorination treatment of a silicone rubber surface.
The technical scheme of the invention is as follows: a silicon rubber surface fluorination treatment method comprises the steps of putting silicon rubber into a fluorine-containing atmosphere for fluorination treatment so as to realize fluorination of the surface layer of the silicon rubber, and replacing hydrogen atoms in a silicon rubber molecular chain with fluorine atoms.
In some embodiments, the fluorine gas concentration in the fluorine-containing atmosphere ranges from 0.5% VOL to 5% VOL.
In some embodiments, the concentration value of fluorine gas in the fluorine-containing atmosphere is 0.5% VOL, 0.8% VOL, 1% VOL, 1.5% VOL, 2% VOL, 2.8% VOL, 3% VOL, 3.8% VOL, 4.2% VOL, 4.5% VOL, or 5% VOL.
In some embodiments, the silicone rubber is treated in the fluorine-containing atmosphere for a time period ranging from 30min to 240 min.
In some embodiments, the silicone rubber is treated in the fluorine-containing atmosphere for 30min, 40min, 60min, 80min, 120min, 140min, 160min, 180min, 200min, 220min, 240 min.
The other purpose of the invention is to adopt two silicon rubbers which are processed by fluorination as sealing rings and to avoid sticking when the two silicon rubber rings are pressed and attached.
The invention has the beneficial effects that:
the invention provides a surface fluorination treatment method of silicon rubber and an application of the silicon rubber as a sealing ring, wherein the adhesion phenomenon of the existing silicon rubber ring is effectively avoided in the application, and the service performance of the silicon rubber ring is further improved.
Drawings
FIG. 1 is a graph comparing the fluorinated rubber surface with the rubber surface that has not been fluorinated during the practice of the present invention.
FIG. 2 is a comparative schematic of an EDS test conducted on a rubber surface that has not been subjected to a fluorination treatment in the practice of the present invention.
FIG. 3 is a comparative schematic of the EDS test conducted on a fluorinated rubber surface in the practice of the invention.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings:
a silicon rubber ring surface fluorination treatment method comprises the steps of putting the silicon rubber ring into a fluorine-containing atmosphere for fluorination treatment, so that the surface layer of the silicon rubber ring is fluorinated, and fluorine atoms are used for replacing hydrogen atoms in a silicon rubber molecular chain.
A fluorination box is adopted, and fluorine gas is flushed into the fluorination box to form a fluorine-containing atmosphere.
In the fluorination box, fluorine gas is contacted with the surface of the silicon rubber ring at normal temperature to react. Fluorine atoms replace hydrogen atoms in a silica gel molecular chain, so that the material generated on the surface of the silicone rubber ring is denatured.
In some embodiments, to ensure fluorination, the fluorine gas concentration in the fluorine-containing atmosphere is in the range of 0.5% VOL to 5% VOL.
Further, in one embodiment, the concentration of fluorine gas in the fluorine-containing atmosphere is 0.5% VOL. Further, in one embodiment, the concentration of fluorine gas in the fluorine-containing atmosphere is 0.8% VOL. Further, the air conditioner is provided with a fan,
in one embodiment, the concentration value of fluorine gas in the fluorine-containing atmosphere is 1% VOL.
Further, in one embodiment, the concentration of fluorine gas in the fluorine-containing atmosphere is 1.5% VOL. Further, in an embodiment, the concentration value of fluorine gas in the fluorine-containing atmosphere is 2% VOL.
Further, in one embodiment, the concentration of fluorine gas in the fluorine-containing atmosphere is 2.8% VOL. Further, in an embodiment, the concentration value of fluorine gas in the fluorine-containing atmosphere is 3% VOL.
Further, in one embodiment, the concentration of fluorine gas in the fluorine-containing atmosphere is 3.8% VOL. Further, in one embodiment, the concentration of fluorine gas in the fluorine-containing atmosphere is 4.2% VOL. Further, in one embodiment, the concentration of fluorine gas in the fluorine-containing atmosphere is 4.5% VOL. Further, in an embodiment, the concentration value of fluorine gas in the fluorine-containing atmosphere is 5% VOL.
In some embodiments, in order to ensure the fluorination effect, the silicone rubber ring is treated in the fluorine-containing atmosphere for a time ranging from 30min to 240 min.
Further, in one embodiment, the silicone rubber is treated in the fluorine-containing atmosphere for 30 min.
Further, in one embodiment, the silicone rubber is treated in the fluorine-containing atmosphere for 40 min.
Further, in one embodiment, the silicone rubber is treated in the fluorine-containing atmosphere for 60 min.
Further, in one embodiment, the silicone rubber is treated in the fluorine-containing atmosphere for 80 min.
Further, in one embodiment, the silicone rubber is treated in the fluorine-containing atmosphere for 120 min.
Further, in one embodiment, the silicone rubber is treated in the fluorine-containing atmosphere for 140 min.
Further, in one embodiment, the silicone rubber is treated in the fluorine-containing atmosphere for 160 min.
Further, in one embodiment, the silicone rubber is treated in the fluorine-containing atmosphere for 180 min.
Further, in one embodiment, the silicone rubber is treated in the fluorine-containing atmosphere for 200 min.
Further, in one embodiment, the silicone rubber is treated in the fluorine-containing atmosphere for 220 min.
Further, in one embodiment, the silicone rubber is treated in the fluorine-containing atmosphere for 240 min.
The silicon rubber is subjected to fluorination treatment, so that the surface of the silicon rubber uniformly shows material performance, and the material has good performance durability.
In some embodiments, a fluorine-containing detection step is added, and after the fluorination reaction is completed, the HDPE test piece treated simultaneously with the silicone rubber sealing ring is detected, and the fluorine content of the test piece is detected by an electrochemical method.
After the fluorination treatment, the required fluorine content is controlled within 100-200 mu g/cm2。
In some embodiments, the adhesion effect is tested using a high temperature accelerated test. Specifically, a common silicon rubber sealing ring and a silicon sealing ring which is subjected to fluorination treatment in the invention are placed in a forced air drying oven together, the temperature is set to be 91 ℃, and the heating time is 80 hours. And (4) calculating and comparing the sticking effect of the sealing ring after the simulated room-temperature sealing compression is carried out for 9.5 years according to the corrected Alaninius equation. In the present embodiment, high temperature is an accelerated verification process under normal temperature conditions.
Through the contrast, the sticky condition of being stained with of ordinary silicon rubber sealing washer is serious, and two rubber rings through fluoridizing in this scheme produce mutual repulsion, are not stained with and glue.
In some embodiments, the pick-up effect test is increased under high temperature and high humidity conditions. The method specifically comprises the steps of placing a common silicon rubber sealing ring and a silicon sealing ring which is subjected to fluorination treatment in the invention in a high-low temperature damp-heat test box together, simulating a high-temperature and high-humidity working condition at the temperature of 60 ℃ and the relative humidity of 90% RH, and comparing the sealing and sticking effects after the treatment time is 100 hours.
Through the contrast, the sticky condition of being stained with of ordinary silicon rubber sealing washer is serious, and two rubber rings through fluoridizing in this scheme produce mutual repulsion, are not stained with and glue.
In some embodiments, the adhesion effectiveness test under high temperature and corrosive conditions is increased.
The surfaces of the common silicon rubber sealing ring and the fluorinated silicon sealing ring are respectively wiped by ethyl acetate for 400 times, and then the common silicon rubber sealing ring and the fluorinated silicon sealing ring are placed in a blast drying oven, the temperature is set to be 91 ℃ for high-temperature treatment, and the heating time is 80 hours, so that the repeated use function and the durability are checked. And comparing the sticking effect after the test is finished.
Through the contrast, the sticky condition of being stained with of ordinary silicon rubber sealing washer is serious, and two rubber rings through fluoridizing in this scheme produce mutual repulsion, are not stained with and glue.
In some embodiments, the adhesion effect is tested using a low temperature test. Specifically, a common silicon rubber sealing ring and a silicon sealing ring which is subjected to fluorination treatment in the invention are placed in a low-temperature box together, the temperature is set to be-20 ℃, and the time is 30 hours.
Through the contrast, the sticky condition of being stained with of ordinary silicon rubber sealing washer is serious, and two rubber rings through fluoridizing in this scheme produce mutual repulsion, are not stained with and glue. In the specific implementation process, as shown in fig. 1, it is a microscopic topography of a common silicon rubber which is not fluorinated and a silicon rubber which is fluorinated according to the scheme of the present invention.
In the specific implementation, as shown in fig. 2, the EDS test result of the non-fluorinated silicone rubber surface is shown.
In the specific implementation process, as shown in fig. 3, the result of the EDS test on the surface of the fluorinated silicone rubber is shown.
According to the invention, the pair of silicon rubber surfaces are subjected to fluorination treatment and applied to the sealing ring with strong anti-sticking property. When the product is used as a sealing ring, the low-temperature resistance characteristic of the silicon rubber is reserved, the anti-sticking characteristic is realized through fluorination treatment, the application performance is greatly improved, and all the defects of the talcum powder serving as an anti-sticking treatment mode are overcome.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations can be devised by those skilled in the art in light of the above teachings. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (6)
1. A surface fluorination treatment method of silicon rubber is characterized in that: and (3) putting the silicon rubber into a fluorine-containing atmosphere for fluorination treatment so as to fluorinate the surface layer of the silicon rubber and replace hydrogen atoms in the molecular chain of the silicon rubber with fluorine atoms.
2. The method for fluorinating a surface of a silicone rubber according to claim 1, wherein: the concentration range of fluorine gas in the fluorine-containing atmosphere is 0.5-5% VOL.
3. The method for fluorinating a surface of a silicone rubber according to claim 2, wherein: the concentration value of fluorine gas in the fluorine-containing atmosphere is 0.5% VOL, 0.8% VOL, 1% VOL, 1.5% VOL, 2% VOL, 2.8% VOL, 3% VOL, 3.8% VOL, 4.2% VOL, 4.5% VOL or 5% VOL.
4. The method for fluorinating a surface of a silicone rubber according to claim 1, wherein: the time range of the silicon rubber treated in the fluorine-containing atmosphere is 30min-240 min.
5. The method for fluorinating a surface of a silicone rubber according to claim 4, wherein: the treatment time of the silicon rubber in the fluorine-containing atmosphere is 30min, 40min, 60min, 80min, 120min, 140min, 160min, 180min, 200min, 220min and 240 min.
6. Use of a silicone rubber according to any one of claims 1 to 5, wherein: the two fluorinated silicone rubbers are used as sealing rings and are not sticky when the two silicone rubber sealing rings are pressed and attached.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111388047.6A CN114015103A (en) | 2021-11-22 | 2021-11-22 | Surface fluorination treatment method for silicone rubber ring and anti-sticking application |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111388047.6A CN114015103A (en) | 2021-11-22 | 2021-11-22 | Surface fluorination treatment method for silicone rubber ring and anti-sticking application |
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| CN114015103A true CN114015103A (en) | 2022-02-08 |
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| CN202111388047.6A Pending CN114015103A (en) | 2021-11-22 | 2021-11-22 | Surface fluorination treatment method for silicone rubber ring and anti-sticking application |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104356418A (en) * | 2014-10-17 | 2015-02-18 | 同济大学 | Method for remarkably improving surface hydrophobicity of silicone rubber |
| CN110504074A (en) * | 2019-07-30 | 2019-11-26 | 同济大学 | A method of for improving silicon rubber flashover voltage |
| CN112292420A (en) * | 2018-06-25 | 2021-01-29 | 三菱电线工业株式会社 | Silicone rubber molded body and method for producing same |
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2021
- 2021-11-22 CN CN202111388047.6A patent/CN114015103A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104356418A (en) * | 2014-10-17 | 2015-02-18 | 同济大学 | Method for remarkably improving surface hydrophobicity of silicone rubber |
| CN112292420A (en) * | 2018-06-25 | 2021-01-29 | 三菱电线工业株式会社 | Silicone rubber molded body and method for producing same |
| CN110504074A (en) * | 2019-07-30 | 2019-11-26 | 同济大学 | A method of for improving silicon rubber flashover voltage |
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