CN108948749A - A kind of bullet O-shaped rubber seal and preparation method thereof - Google Patents
A kind of bullet O-shaped rubber seal 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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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
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
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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
- C08K3/02—Elements
- C08K3/04—Carbon
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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
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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
- C08K3/28—Nitrogen-containing compounds
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/14—Peroxides
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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
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The present invention relates to a kind of bullet O-shaped rubber seal and preparation method thereof, belong to technical field of sealing technology.The present invention is using fluorine silicone rubber due to introducing trifluoro propyl in siloxane chain, so that fluorine silicone rubber is in the resistant of high or low temperature for maintaining methyl silicone rubber, weatherability, compression recovery, resilience, on the basis of a series of excellent performances such as release property, simultaneously again with the resistance to fuel oil of fluorubber, the performances such as solvent resistant, and by polymerizeing with vinyltriethoxysilane, the stable high molecular weight fluorine silicon raw rubber of quality is made, again by addition modified hydrotalcite as constitution controller, the O-shaped rubber seal of bullet is made in the auxiliary agents such as heat-resisting stabilizing agent, with heat-resisting well, wear-resisting and ageing-resistant performance, addition modified hydrotalcite can increase the internal bond strength of rubber seal, effectively improve the stretch-proof of rubber seal, it is ageing-resistant, it is wear-resisting, it is heat-resisting, with metal adhesion and physical property, so that sealing ring compression set is small, Elasticity is good.
Description
Technical field
The present invention relates to a kind of bullet O-shaped rubber seal and preparation method thereof, belong to technical field of sealing technology.
Background technique
Modern pharmaceutical machinery mostly uses silicon rubber O-ring seal to be sealed greatly.Silicon rubber O-ring seal has preferable
High and low temperature resistance and excellent sealing performance, it is harsh that the silicon rubber of special compounding can also better meet food, pharmaceuticals industry
Hygienic requirements, the always preferred sealing material of food pharmaceuticals industry for a long time.But many compounding agents of silicon rubber and
Component can still enter in the media such as food, medicine during equipment application, so that the purity of medium is reduced, especially to Gao Pin
The purity of matter drug generates adverse effect, to influence the quality of product；And silicon rubber resistance to low temperature, solvent resistance compared with
Difference, resistance to water vapor seal performance is relatively low, has some limitations in the process of manufacture of some extraordinary drugs.For this purpose,
Developmental research is a kind of with good comprehensive performance and to be able to satisfy the high-quality O-ring seal of medical and health requirement be always medical row
One pursuit direction of industry, and improve a main improvement direction of pharmaceutical equipment product quality.
O-ring seal is usually known as O-ring by us, its cross sectional shape is circle.O-ring seal is hydraulic and pneumatic
Very widely used in system: the sealing performance of O-ring is very good, is all in daily use in static seal and dynamic sealing；It in addition to
Combined seal structure can also be formed with other kinds of sealing element other than independent use；Appropriate in material selection
Under the premise of, O-ring seal can meet the requirement of many different operating conditions, medium and moving condition.
O-ring is widely used in mechanical industry, however often will appear some problems in actual production: O-shaped
It is big to enclose compression set, O-ring belongs to extrusion pressing type sealing, it is easy to appear after a period of use in seal groove becomes flat
Situation causes to leak after loss of elasticity, and therefore, urgent need develops a kind of O-ring that compression set is small.
Summary of the invention
The technical problems to be solved by the invention: for the big problem of existing sealing ring compression set, one is provided
Kind bullet O-shaped rubber seal and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of O-shaped rubber seal of bullet, including following weight parts raw material: 100~120 parts of fluorine silicon raw rubbers, 30~50 parts of hard charcoals
It is black, 20~30 parts of modified hydrotalcites, 2~4 parts of cumyl peroxides, 3~5 parts of zinc oxide, 1~3 part of anti-aging agent, 1~3 part of rush
Into agent, 1~3 part of vulcanizing agent.
Decompression dehydration in polymer reactor is added by fluorine silicone rubber in the fluorine silicon raw rubber, then heats up and add under nitrogen atmosphere
Enter vinyltriethoxysilane, platinum catalyst is stirred to react 2~3h, heating is vacuumized and is made after 2~3h.
The fluorine silicone rubber, vinyltriethoxysilane, the parts by weight of platinum catalyst are 500~600 parts of fluorine silicone rubber,
2~3 parts of vinyltriethoxysilane, 4~5 parts of platinum catalysts.
The decompression dehydration process is to be dehydrated to moisture content less than 0.1%, and the warming temperature is 120~130 DEG C, heating
Temperature is 160~180 DEG C, and the vacuum degree is 0~0.1kPa.
The modified hydrotalcite is that magnesium nitrate, aluminum nitrate, flake graphite are added in deionized water and are stirred, add carbon
Sour sodium, poly-vinyl alcohol solution, sodium hydroxide solution, be fitted into after being stirred and evenly mixed at 50~60 DEG C in hydrothermal reaction kettle reaction 20~
For 24 hours, dry after filtering washing to be made.
Weight of material part is 4~6 parts of magnesium nitrates, 3.0~4.5 parts of aluminum nitrates, 1~2 part of sheet in the modified hydrotalcite
Graphite, 80~100 parts of deionized waters, 2.0~2.5 parts of sodium carbonate, 20~25 parts of mass fractions are 2% poly-vinyl alcohol solution, 10~
20 parts of mass fractions are 10% sodium hydroxide solution.
Temperature is 120~130 DEG C in the hydrothermal reaction kettle.
A kind of preparation method of bullet with O-shaped rubber seal, specific steps are as follows:
(1) it takes fluorine silicone rubber that decompression dehydration in polymer reactor is added, then heats up under nitrogen atmosphere and three second of vinyl is added
Oxysilane, platinum catalyst are stirred to react 2~3h, and heating obtains fluorine silicon raw rubber after vacuumizing 2~3h；
(2) take magnesium nitrate, aluminum nitrate, flake graphite, be added in deionized water and stir, add sodium carbonate, poly-vinyl alcohol solution,
Sodium hydroxide solution stirs 15~20min at 50~60 DEG C, obtains mixed liquor；
(3) mixed liquor is fitted into hydrothermal reaction kettle reaction 20~for 24 hours, it is dry after filtering washing, obtain modified hydrotalcite；
(4) it takes fluorine silicon raw rubber to be packed on double roll mill to plasticate repeatedly 2~3 times, add white carbon black, modified hydrotalcite, peroxide
It is thin 5~10 times logical to change diisopropylbenzene (DIPB), zinc oxide, anti-aging agent, add vulcanizing agent it is thin it is 5~10 times logical after is fitted into during compression original mold has
It is placed in vulcanizing treatment on vulcanizing press, then 1~2h of drying and processing, obtains bullet with O-shaped rubber seal.
The present invention is compared with other methods, and advantageous effects are:
The present invention using fluorine silicone rubber due to introducing trifluoro propyl in siloxane chain so that fluorine silicone rubber is maintaining methyl
On the basis of a series of excellent performances such as resistant of high or low temperature, weatherability, compression recovery, resilience, the release property of silicon rubber, together
When there are the performances such as resistance to fuel oil, the solvent resistant of fluorubber again, and by polymerizeing with vinyltriethoxysilane, it is steady that quality is made
Fixed high molecular weight fluorine silicon raw rubber, then it is obtained as auxiliary agents such as constitution controller, heat-resisting stabilizing agents by addition modified hydrotalcite
The O-shaped rubber seal of bullet, has good heat-resisting, wear-resisting and ageing-resistant performance, and addition modified hydrotalcite can increase rubber
The internal bond strength of sealing ring, effectively improve rubber seal stretch-proof, it is ageing-resistant, wear-resisting, heat-resisting, with metal adhesion and
Physical property, so that sealing ring compression set is small, elasticity is good.
Specific embodiment
It takes 500~600g fluorine silicone rubber, decompression dehydration is added in polymer reactor to moisture content less than 0.1%, then in nitrogen
Under atmosphere, 120~130 DEG C are warming up to, 2~3g vinyltriethoxysilane is added, 4~5g platinum catalyst is continually fed into nitrogen
Gas agitating reacts 2~3h, is heated to 160~180 DEG C and is evacuated to 0~0.1kPa, and fluorine silicon raw rubber is obtained after 2~3h of pressure maintaining, takes 4
~6g magnesium nitrate, 3.0~4.5g aluminum nitrate, 1~2g flake graphite are added in 80~100mL deionized water, with 300~400r/
Min stirs 20~30min, adds 2.0~2.5g sodium carbonate, and 20~25g mass fraction is 2% poly-vinyl alcohol solution, 10~
20g mass fraction is 10% sodium hydroxide solution, and 15~20min is stirred at 50~60 DEG C, mixed liquor is obtained, mixed liquor is packed into
In hydrothermal reaction kettle, the hydro-thermal reaction 20~for 24 hours at 120~130 DEG C filters to obtain filter residue, filter residue 3~5 is washed with deionized
It is secondary, then filter residue is placed in drying box, it dries at 105~110 DEG C to constant weight, obtains modified hydrotalcite, take 100~120g fluorine silicon
Raw rubber is packed on double roll mill, is plasticated fluorine silicon raw rubber 2~3 times repeatedly at 100~130 DEG C, is added 30~50g hard charcoal
Black, 20~30g modified hydrotalcite, 2~4g cumyl peroxide, 3~5g zinc oxide, 1~3g anti-aging agent is thin 5~10 times logical,
Add 1~3g vulcanizing agent, it is thin it is 5~10 times logical after is fitted into during compression original mold has, on vulcanizing press, with 140~160 DEG C into
Row 30~40min of vulcanizing treatment, then bullet is obtained with O-shaped rubber seal in high temperature oven with 160~180 DEG C of 1~2h of drying and processing
Circle.
It takes 500g fluorine silicone rubber, decompression dehydration is added in polymer reactor to moisture content less than 0.1%, then in nitrogen atmosphere
Under, 120 DEG C are warming up to, 2g vinyltriethoxysilane is added, 4g platinum catalyst is continually fed into nitrogen gas stirring reaction 2h, adds
Heat is to 160 DEG C and is evacuated to 0.05kPa, and fluorine silicon raw rubber is obtained after pressure maintaining 2h, takes 4g magnesium nitrate, 3.0g aluminum nitrate, 1g sheet stone
Ink is added in 80mL deionized water, stirs 20min with 300r/min, adds 2.0g sodium carbonate, and 20g mass fraction is 2% poly-
Glycohol solution, 10g mass fraction are 10% sodium hydroxide solution, stir 15min at 50 DEG C, obtain mixed liquor, mixed liquor is filled
Enter in hydrothermal reaction kettle, the hydro-thermal reaction 20h at 120 DEG C filters to obtain filter residue, is washed with deionized filter residue 3 times, then by filter residue
It is placed in drying box, dries at 105 DEG C to constant weight, obtain modified hydrotalcite, 100g fluorine silicon raw rubber is taken to be packed on double roll mill,
It plasticates repeatedly at 100 DEG C fluorine silicon raw rubber 2 times, adds 30g white carbon black, 20g modified hydrotalcite, 2g cumyl peroxide,
3g zinc oxide, 1g anti-aging agent is logical 5 times thin, adds 1g vulcanizing agent, it is thin it is 5 times logical after is fitted into during compression original mold has, in compression molding
On machine, with 140 DEG C of progress vulcanizing treatment 30min, then in high temperature oven it is close with O-shaped rubber to obtain bullet with 160 DEG C of drying and processing 1h
Seal.
It takes 550g fluorine silicone rubber, decompression dehydration is added in polymer reactor to moisture content less than 0.1%, then in nitrogen atmosphere
Under, 125 DEG C are warming up to, 2g vinyltriethoxysilane is added, 4g platinum catalyst is continually fed into nitrogen gas stirring reaction 2h, adds
Heat is to 170 DEG C and is evacuated to 0.05kPa, and fluorine silicon raw rubber is obtained after pressure maintaining 2h, takes 5g magnesium nitrate, 3.5g aluminum nitrate, 1g sheet stone
Ink is added in 90mL deionized water, stirs 25min with 350r/min, adds 2.2g sodium carbonate, and 22g mass fraction is 2% poly-
Glycohol solution, 15g mass fraction are 10% sodium hydroxide solution, stir 18min at 55 DEG C, obtain mixed liquor, mixed liquor is filled
Enter in hydrothermal reaction kettle, the hydro-thermal reaction 22h at 125 DEG C filters to obtain filter residue, is washed with deionized filter residue 4 times, then by filter residue
It is placed in drying box, dries at 108 DEG C to constant weight, obtain modified hydrotalcite, 110g fluorine silicon raw rubber is taken to be packed on double roll mill,
It plasticates repeatedly at 115 DEG C fluorine silicon raw rubber 2 times, adds 40g white carbon black, 25g modified hydrotalcite, 3g cumyl peroxide,
4g zinc oxide, 2g anti-aging agent is logical 8 times thin, adds 2g vulcanizing agent, it is thin it is 8 times logical after is fitted into during compression original mold has, in compression molding
On machine, with 150 DEG C of progress vulcanizing treatment 35min, then in high temperature oven it is close with O-shaped rubber to obtain bullet with 170 DEG C of drying and processing 1h
Seal.
It takes 600g fluorine silicone rubber, decompression dehydration is added in polymer reactor to moisture content less than 0.1%, then in nitrogen atmosphere
Under, 130 DEG C are warming up to, 3g vinyltriethoxysilane is added, 5g platinum catalyst is continually fed into nitrogen gas stirring reaction 3h, adds
Heat is to 180 DEG C and is evacuated to 0.1kPa, and fluorine silicon raw rubber is obtained after pressure maintaining 3h, takes 6g magnesium nitrate, 4.5g aluminum nitrate, 2g sheet stone
Ink is added in 100mL deionized water, stirs 30min with 400r/min, adds 2.5g sodium carbonate, and 25g mass fraction is 2% poly-
Glycohol solution, 20g mass fraction are 10% sodium hydroxide solution, stir 20min at 60 DEG C, obtain mixed liquor, mixed liquor is filled
Enter in hydrothermal reaction kettle, hydro-thermal reaction for 24 hours, filters to obtain filter residue at 130 DEG C, is washed with deionized filter residue 5 times, then by filter residue
It is placed in drying box, dries at 110 DEG C to constant weight, obtain modified hydrotalcite, 120g fluorine silicon raw rubber is taken to be packed on double roll mill,
It plasticates repeatedly at 130 DEG C fluorine silicon raw rubber 3 times, adds 50g white carbon black, 30g modified hydrotalcite, 4g cumyl peroxide,
5g zinc oxide, 3g anti-aging agent is logical 10 times thin, adds 3g vulcanizing agent, it is thin it is 10 times logical after is fitted into during compression original mold has, in plate sulphur
On change machine, with 160 DEG C of progress vulcanizing treatment 40min, then in high temperature oven bullet is obtained with O-shaped rubber with 180 DEG C of drying and processing 2h
Sealing ring.
Reference examples: the O-shaped rubber seal of Dongguan company production.
The O-shaped rubber seal of example and reference examples is detected, specific detection is as follows:
Mechanics Performance Testing: using electronic tensile machine, by national standard GB/T528-2009, " vulcanized rubber or thermoplastic elastomer stretching are answered
The measurement of stress-strain performance " testing conductive silicon rubber tensile property, tensile speed 500mm/min.
Conducting performance test: the intercepted length 50mm on the sheet specimens of molding vulcanization, sectional area are 6mm × 1mm batten,
Volume resistance is measured by GB/T2439-1989.
Specific testing result such as table 1.
1 performance characterization contrast table of table
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Tensile strength/MPa | 3.70 | 3.25 | 3.14 | 0.77 |
| Elongation at break/% | 561 | 468 | 310 | 182 |
| Volume resistivity/Ω cm | 1.14 | 1.04 | 1.09 | 0.07 |
As shown in Table 1, O-shaped rubber seal prepared by the present invention has good mechanical property and electric conductivity.
Claims (8)
1. a kind of O-shaped rubber seal of bullet, which is characterized in that including following weight parts raw material:
100~120 parts of fluorine silicon raw rubbers, 30~50 parts of white carbon blacks, 20~30 parts of modified hydrotalcites, 2~4 parts of peroxidating diisopropyls
Benzene, 3~5 parts of zinc oxide, 1~3 part of anti-aging agent, 1~3 part of promotor, 1~3 part of vulcanizing agent.
2. a kind of O-shaped rubber seal of bullet as described in claim 1, which is characterized in that the fluorine silicon raw rubber is by fluorine silicon rubber
Decompression dehydration in polymer reactor is added in glue, then heats up under nitrogen atmosphere and vinyltriethoxysilane, platinum catalysis is added
Agent is stirred to react 2~3h, and heating is made after vacuumizing 2~3h.
3. a kind of O-shaped rubber seal of bullet as claimed in claim 2, which is characterized in that the fluorine silicone rubber, vinyl three
Ethoxysilane, platinum catalyst parts by weight be 500~600 parts of fluorine silicone rubber, 2~3 parts of vinyltriethoxysilane, 4~5
Part platinum catalyst.
4. a kind of O-shaped rubber seal of bullet as claimed in claim 3, which is characterized in that the decompression dehydration process is de-
Water is to moisture content less than 0.1%, and the warming temperature is 120~130 DEG C, and heating temperature is 160~180 DEG C, and the vacuum degree is
0~0.1kPa.
5. a kind of O-shaped rubber seal of bullet as described in claim 1, which is characterized in that the modified hydrotalcite is by nitre
Sour magnesium, aluminum nitrate, flake graphite are added in deionized water and stir, it is molten to add sodium carbonate, poly-vinyl alcohol solution, sodium hydroxide
Liquid is fitted into hydrothermal reaction kettle reaction 20~for 24 hours after stirring and evenly mixing at 50~60 DEG C, dry after filtering washing to be made.
6. a kind of O-shaped rubber seal of bullet as claimed in claim 5, which is characterized in that material in the modified hydrotalcite
Parts by weight be 4~6 parts of magnesium nitrates, 3.0~4.5 parts of aluminum nitrates, 1~2 part of flake graphite, 80~100 parts of deionized waters, 2.0~
2.5 parts of sodium carbonate, 20~25 parts of mass fractions are 2% poly-vinyl alcohol solution, and 10~20 parts of mass fractions are that 10% sodium hydroxide is molten
Liquid.
7. a kind of O-shaped rubber seal of bullet as claimed in claim 5, which is characterized in that temperature in the hydrothermal reaction kettle
It is 120~130 DEG C.
8. a kind of preparation method of the O-shaped rubber seal of bullet as described in claim 1~7 any one, which is characterized in that
Specific steps are as follows:
(1) it takes fluorine silicone rubber that decompression dehydration in polymer reactor is added, then heats up under nitrogen atmosphere and three second of vinyl is added
Oxysilane, platinum catalyst are stirred to react 2~3h, and heating obtains fluorine silicon raw rubber after vacuumizing 2~3h；
(2) take magnesium nitrate, aluminum nitrate, flake graphite, be added in deionized water and stir, add sodium carbonate, poly-vinyl alcohol solution,
Sodium hydroxide solution stirs 15~20min at 50~60 DEG C, obtains mixed liquor；
(3) mixed liquor is fitted into hydrothermal reaction kettle reaction 20~for 24 hours, it is dry after filtering washing, obtain modified hydrotalcite；
(4) it takes fluorine silicon raw rubber to be packed on double roll mill to plasticate repeatedly 2~3 times, add white carbon black, modified hydrotalcite, peroxide
It is thin 5~10 times logical to change diisopropylbenzene (DIPB), zinc oxide, anti-aging agent, add vulcanizing agent it is thin it is 5~10 times logical after is fitted into during compression original mold has
It is placed in vulcanizing treatment on vulcanizing press, then 1~2h of drying and processing, obtains bullet with O-shaped rubber seal.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111534105A (en) * | 2020-04-02 | 2020-08-14 | 浙江翔宇密封件有限公司 | Anti-aging silicone rubber sealing material for high-speed rail sealing element and preparation method thereof |
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| CN111534105A (en) * | 2020-04-02 | 2020-08-14 | 浙江翔宇密封件有限公司 | Anti-aging silicone rubber sealing material for high-speed rail sealing element and preparation method thereof |
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Application publication date: 20181207 |
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