CN111073304B - Fluorosilicone rubber composition and preparation method thereof - Google Patents
Fluorosilicone rubber composition and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
- C08L83/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
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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
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
- C08K2003/2213—Oxides; Hydroxides of metals of rare earth metal of cerium
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention belongs to the technical field of rubber, and particularly relates to a fluorosilicone rubber composition and a preparation method thereof. The composition is prepared from the following raw materials in parts by weight: 100 parts of fluorosilicone raw rubber, 1-8 parts of liquid fluororubber, 0.1-5 parts of chain extender, 30-70 parts of reinforcing filler, 1-15 parts of structure control agent, 2-8 parts of anti-aging agent, 0.5-10 parts of crosslinking agent and 1-4 parts of processing aid. According to the invention, the low molecular weight liquid fluorine rubber is chain-extended to fluorine silicon rubber molecules, so that the material is endowed with lower surface energy, and good lubricating property is provided for the composition, so that the material has excellent lubricating property, oil resistance and low compression permanent deformation property, and the cross-linking point distribution is adjusted by adjusting the vinyl content so that the material has good mechanical property; the preparation method is scientific, reasonable, simple and feasible.
Description
Technical Field
The invention belongs to the technical field of rubber, and particularly relates to a fluorosilicone rubber composition and a preparation method thereof.
Background
Fluorosilicone rubber (FMVQ) having a main chain composed of silicon and oxygen atoms and having a siloxane bond as a main chain structure, wherein poly (3,3, 3-trifluoropropylmethyl) silicone rubber is most widely used. The organic silicon rubber has the excellent performances of high and low temperature resistance, aging resistance, radiation resistance, ultraviolet ray resistance, electric insulation, wet skid resistance, low compression deformation rate and the like, and the fluororubber has the characteristics of good thermal stability, solvent resistance and the like. Therefore, the fluorosilicone rubber has excellent hydrogen solvent resistance, oil resistance, acid and alkali resistance and lower surface energy performance of the organic fluorine material due to the introduction of fluorine-containing groups on the basis of keeping excellent performances of the organic silicon material such as heat resistance, cold resistance, high voltage resistance, weather aging resistance and the like, and can work for a long time at the temperature of minus 55-200 ℃. Therefore, fluorosilicone rubber has been widely used in the automobile industry, the petrochemical industry, the medical care industry, and the military industry. It has a wide operating temperature range and is resistant to fuels, motor oils and many chemical solvents.
The cured surface of fluorosilicone rubber has a high coefficient of friction. In the assembly of some components such as electrical connector gaskets, it is desirable that the fluorosilicone rubber have good surface lubricity to allow for faster part assembly and to reduce off-specification parts due to tearing of the elastomer during the assembly operation. On the basis of ensuring the excellent performance of the fluorosilicone rubber, the lubricating grease has excellent lubricating property, is beneficial to processing and later use. The problem of lubricating property of the fluorosilicone rubber can be improved by mixing the fluororubber and the fluorosilicone rubber, but the fluororubber belongs to a carbon chain polymer, the fluorosilicone rubber is a silicone main chain polymer, the compatibility between the fluororubber and the silicone main chain polymer is poor, and the mechanical property of a blend is not high.
The silicon rubber, the fluorosilicone rubber and the fluororubber have excellent performances, and the development of blended rubber products with excellent performances is concerned by people. Chinese patent CN104530719A discloses a vinyl-terminated polymethyl trifluoropropyl siloxane fluorine rubber compatibilizer and a preparation method thereof, wherein the aim of improving the blending compatibility of fluorine rubber and fluorosilicone rubber is fulfilled by introducing vinyl-terminated polymethyl trifluoropropyl siloxane on a fluorine rubber main chain and utilizing the characteristic that the polymethyl trifluoropropyl siloxane can be well compatible with fluorine rubber and fluorine silicone rubber. But the performance is not greatly improved, the formula advantage is not obvious, and the molecular weight of the fluororubber is high and difficult to operate. Chinese patent CN104530610A discloses a blend of fluororubber and fluorosilicone rubber and a preparation method thereof, wherein the compatibility of the fluororubber and the fluorosilicone rubber is improved by introducing vinyl-terminated polymethyl trifluoropropyl siloxane on a fluororubber main chain; the viscosity difference between the fluororubber and the fluorosilicone rubber is reduced, and the blending uniformity is improved. However, the fluororubbers have high molecular weight, and need to be dissolved in an organic solvent, so that the process is complicated. Chinese patent CN107828165A discloses a silicone/fluoroether/fluorosilicone rubber composite rubber material and a preparation method thereof, wherein oil resistance cannot be well reflected due to the existence of silicone rubber, and the silicone rubber composite rubber material has a complex process and high operation difficulty.
How to endow the lubricating property of the fluororubber to the fluorosilicone rubber does not damage the excellent high and low temperature resistance, weather resistance, oil resistance, solvent resistance and low compression permanent deformation properties of the fluorosilicone rubber, and the fluororubber with low molecular weight can be extended into the molecular chain of the fluorosilicone rubber to endow the material with lower surface energy, so that the composition is provided with good lubricating property, and the material has more excellent mechanical property, lubricating property, oil resistance and low compression permanent deformation property, and becomes a technical problem to be solved urgently in the field.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art, and provides a fluorosilicone rubber composition which has excellent lubricating property, oil resistance, low compression set property and mechanical property; the invention also provides a preparation method of the composition, which is scientific, reasonable, simple and feasible.
The fluorosilicone rubber composition is prepared from the following raw materials in parts by weight:
100 parts of fluorosilicone raw rubber, 1-8 parts of liquid fluororubber, 0.1-5 parts of chain extender, 30-70 parts of reinforcing filler, 1-15 parts of structure control agent, 2-8 parts of anti-aging agent, 0.5-10 parts of crosslinking agent and 1-4 parts of processing aid.
Wherein:
the raw fluorosilicone rubber is vinyl-containing raw fluorosilicone rubber and vinyl-free raw fluorosilicone rubber, the viscosity average molecular weight of the vinyl-containing raw fluorosilicone rubber is 60-140 ten thousand, preferably 80-110 ten thousand, the vinyl content is 0.1-1% mol, and the viscosity average molecular weight of the vinyl-free raw fluorosilicone rubber is 60-140 ten thousand, preferably 80-110 ten thousand.
Preferably, the mass ratio of the vinyl-containing fluorosilicone raw rubber to the vinyl-free fluorosilicone raw rubber is (0.2-0.7): 1.
the liquid fluororubber is hydroxyl-terminated liquid fluororubber, and the number average molecular weight is 1000-.
The chain extender is one of dimethyl diazomethyl acetamide silane or phenyl methyl diazomethyl acetamide silane, and phenyl methyl diazomethyl acetamide silane is preferable.
The reinforcing filler is one or a mixture of more of fumed silica, precipitated silica, calcium carbonate, diatomite, titanium dioxide or kaolin. Preferably hydrophobic fumed silica with the specific surface area of 150-300m2(ii)/g; or hydrophobic fumed silica and other reinforcing fillersThe mixture achieves the purpose of reducing the cost.
The structure control agent is hydroxy fluorosilicone oil, wherein the viscosity of the adopted hydroxy fluorosilicone oil is 50-400cp at 25 ℃. Preferably, the structure control agent is hydroxy fluorosilicone oil, and the viscosity is 100-300cp at 25 ℃.
The anti-aging agent is one or a mixture of iron oxide and cerium dioxide, and the mixture of the iron oxide and the cerium dioxide is preferred.
The cross-linking agent is one or a mixture of high-vinyl fluorosilicone rubber and high-vinyl fluorosilicone oil, preferably the high-vinyl fluorosilicone rubber, and the vinyl content is 1-5 mol%.
The processing aid is one or a mixture of zinc stearate, sodium stearate or stearic acid, and preferably a mixture of stearic acid and sodium stearate.
The preparation method of the fluorosilicone rubber composition comprises the following steps:
(1) adding fluorosilicone raw rubber and liquid fluororubber into an internal mixer, adding a chain extender for internal mixing, adding a part of a structure control agent for internal mixing, then adding reinforcing filler in batches, adding the rest of the structure control agent, a crosslinking agent and a processing aid into the internal mixer for internal mixing in sequence after the addition is finished, heating and vacuumizing rubber materials, then discharging, and carrying out high-temperature treatment for 3-6 hours to obtain fluorosilicone rubber composition base rubber;
(2) cooling the base rubber to room temperature, standing for 24-48h, adding an anti-aging agent, thinly passing for 15-20 times, taking out the sheet, and packaging to obtain the fluorosilicone rubber composition.
Preferably, the preparation method of the fluorosilicone rubber composition specifically comprises the following steps:
(1) adding fluorosilicone raw rubber and liquid fluororubber into an internal mixer, adding a chain extender, carrying out internal mixing at 40 ℃ for 30min, adding a part of structure control agent, carrying out internal mixing for 10min, then adding reinforcing filler in batches, after the addition is finished, sequentially adding the rest of structure control agent, cross-linking agent and processing aid into the internal mixer, carrying out internal mixing for 30min, heating the rubber material to 135 ℃, vacuumizing for 1h, then discharging, and carrying out high-temperature treatment at 150 ℃ for 3-6h under the protection of nitrogen to obtain fluorosilicone rubber composition base rubber;
(2) and cooling the base rubber to room temperature, standing for 24h, adding an anti-aging agent through a double-roll mill, thinly passing for 15-20 times, and obtaining the fluorosilicone rubber composition after sheet discharge and packaging.
When the fluorosilicone rubber composition is used for processing products and evaluating the performance, a vulcanizing agent is added into the fluorosilicone rubber composition through a double-roll open mill, and the mixture is uniformly mixed and vulcanized, wherein the first-stage vulcanization comprises the following steps: pressurizing at 170 ℃ for 12min, and performing secondary vulcanization: air-dry oven at 200 ℃ for 4 h.
Wherein, the vulcanizing agent is one or a mixture of more of 2, 5-dimethyl-2, 5-di-tert-butyl peroxy hexane, dicumyl peroxide or di-tert-butyl peroxide, and 2, 5-dimethyl-2, 5-di-tert-butyl peroxy hexane is preferred. The adding amount is 0.5-2.0 parts.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention solves the problem of incompatible mixing of high molecular weight fluororubber and fluorosilicone rubber, changes the idea of extending the low molecular weight liquid fluororubber chain onto fluorosilicone rubber molecules, endows the material with lower surface energy, provides the composition with good lubricating property, enables the material to have excellent lubricating property, oil resistance and low compression permanent deformation performance, and enables the material to have good mechanical property by adjusting the vinyl content and adjusting the distribution of crosslinking points.
2. The rubber material prepared by the invention is not only beneficial to processing, but also beneficial to later-stage use, can work for a long time at the temperature of-55-200 ℃, and has wide application in the automobile industry, the petrochemical industry, the medical health and military industry.
3. The preparation method is scientific, reasonable, simple and feasible.
Detailed Description
The invention is further illustrated, but not limited, by the following examples.
The starting materials used in the examples are commercially available except as otherwise indicated.
Example 1
The fluorosilicone rubber composition is prepared from the following raw materials in parts by weight, and is specifically shown in table 1.
TABLE 1 raw Material composition of Fluorosilicone rubber composition
The preparation method comprises the following steps:
(1) adding fluorosilicone raw rubber and liquid fluororubber into an internal mixer, adding a chain extender, carrying out internal mixing at 40 ℃ for 30min, adding a part of structure control agent, carrying out internal mixing for 10min, then adding reinforcing filler in batches, after the addition is finished, sequentially adding the rest of structure control agent, cross-linking agent and processing aid into the internal mixer, carrying out internal mixing for 30min, heating the rubber material to 135 ℃, vacuumizing for 1h, and then carrying out high-temperature 150 ℃ treatment for 6h under the protection of discharged nitrogen to obtain the fluorosilicone rubber composition base rubber.
(2) Cooling the base rubber to room temperature, standing for 24h, adding anti-aging agents (ferric oxide and cerium dioxide) through a two-roll mill, thinly passing for 20 times, and obtaining the fluorosilicone rubber composition after sheet discharge and packaging.
(3) Adding 0.8 part of vulcanizing agent into the fluorosilicone rubber composition through a double-roll open mill, uniformly mixing, vulcanizing, and performing primary vulcanization: pressurizing at 170 ℃ for 12min, and performing secondary vulcanization: and (3) blowing the drying box for 4 hours at the temperature of 200 ℃ to prepare the fluorinated silicone rubber vulcanized rubber.
In the step (3), the vulcanizing agent is 2, 5-dimethyl-2, 5-di-tert-butyl peroxy hexane.
The properties of the vulcanized fluorosilicone rubber prepared in example 1 are shown in Table 3.
Example 2
The fluorosilicone rubber composition is prepared from the following raw materials in parts by weight, and is specifically shown in Table 2.
TABLE 2 raw Material composition of fluorosilicone rubber compositions
The preparation method is the same as that of the embodiment 1, and the vulcanizing agent adopted in the embodiment 2 is dicumyl peroxide.
The relevant properties of the fluorosilicone rubber vulcanizate prepared in example 2 are shown in Table 3.
Example 3
The specific operation was carried out in the same manner as in example 1 except that the hydroxyl-terminated liquid fluororubber had a number average molecular weight of 3400. The relevant properties of the fluorosilicone rubber vulcanizate prepared are shown in table 3.
Example 4
The specific operation was carried out in the same manner as in example 1 except that the amount of the hydroxyl-terminated liquid fluororubber was 5.3 parts by mass. The relevant properties of the fluorosilicone rubber vulcanizate prepared are shown in table 3.
Example 5
The specific operation method is the same as that of example 1, except that the adopted fluorosilicone raw rubber is different: 17.5 parts of vinyl-containing fluorosilicone rubber and 82.5 parts of non-vinyl silicone rubber. The relevant properties of the fluorosilicone rubber vulcanizate prepared are shown in table 3.
Example 6
The specific operation was carried out in the same manner as in example 1 except that the amount of the chain extender was 3.5 parts. The relevant properties of the fluorosilicone rubber vulcanizate prepared are shown in table 3.
Example 7
The specific operation was carried out in the same manner as in example 2 except that the amount of the chain extender was 0.5 part. The relevant properties of the fluorosilicone rubber vulcanizate prepared are shown in table 3.
Comparative example 1
The specific procedure was the same as in example 1, except that no chain extender was added. The relevant properties of the fluorosilicone rubber vulcanizate prepared are shown in table 4.
Comparative example 2
The specific procedure was the same as in example 2, except that no chain extender was added. The relevant properties of the fluorosilicone rubber vulcanizate prepared are shown in table 4.
Comparative example 3
The specific operation was carried out in the same manner as in example 1 except that the liquid fluororubber and the chain extender were not added. The relevant properties of the fluorosilicone rubber vulcanizate prepared are shown in table 4.
Comparative example 4
The specific operation is the same as that of example 1, except that the hydroxyl-terminated liquid fluororubber has a number average molecular weight of 20000. The relevant properties of the fluorosilicone rubber vulcanizate prepared are shown in table 4.
And (3) performance testing:
hardness, as tested in GB/T531-1999;
tensile strength and elongation at break, tested in GB/T528-;
tear strength, as measured by crescent test specimens as specified in GB/T529-1999;
compression set, testing according to the type A sample specified in GB/T7759 and 1996;
testing the oil-resistant volume change rate according to the liquid B specified in GB/T1690;
the surface friction coefficient adopts a friction coefficient tester friction surface felt, the load is 500g, and the traction speed is 50 mm/min.
Table 3 results of the relevant performance tests of the examples
Table 4 comparative example correlation performance test results
Claims (5)
1. A fluorosilicone rubber composition, characterized in that: the feed is prepared from the following raw materials in parts by weight:
100 parts of fluorosilicone raw rubber, 1-8 parts of liquid fluororubber, 0.1-5 parts of chain extender, 30-70 parts of reinforcing filler, 1-15 parts of structure control agent, 2-8 parts of anti-aging agent, 0.5-10 parts of crosslinking agent and 1-4 parts of processing aid;
wherein:
the raw fluorosilicone rubber is vinyl-containing raw fluorosilicone rubber and vinyl-free raw fluorosilicone rubber, and the mass ratio of the vinyl-containing raw fluorosilicone rubber to the vinyl-free raw fluorosilicone rubber is (0.2-0.7): 1, the viscosity average molecular weight of the vinyl-containing fluorosilicone crude rubber is 60-140 ten thousand, the vinyl content is 0.1-1% mol, and the viscosity average molecular weight of the vinyl-free fluorosilicone crude rubber is 60-140 ten thousand; the liquid fluororubber is hydroxyl-terminated liquid fluororubber, and the number average molecular weight is 1000-;
the chain extender is one of dimethyl diazomethyl acetamide silane or phenyl methyl diazomethyl acetamide silane;
the reinforcing filler is one or a mixture of more of fumed silica, precipitated silica, calcium carbonate, diatomite, titanium dioxide or kaolin;
the cross-linking agent is one or the mixture of high vinyl fluorosilicone rubber and high vinyl fluorosilicone oil.
2. The fluorosilicone rubber composition according to claim 1, wherein: the structure control agent is hydroxy fluorosilicone oil, and the viscosity of the structure control agent is 50-400cp at 25 ℃.
3. The fluorosilicone rubber composition according to claim 1, wherein: the anti-aging agent is one or a mixture of iron oxide and cerium dioxide.
4. The fluorosilicone rubber composition according to claim 1, wherein: the processing aid is one or a mixture of zinc stearate, sodium stearate or stearic acid.
5. A method for preparing a fluorosilicone rubber composition according to any one of claims 1 to 4, characterized by: the method comprises the following steps:
(1) adding fluorosilicone raw rubber and liquid fluororubber into an internal mixer, adding a chain extender for internal mixing, adding a part of a structure control agent for internal mixing, then adding reinforcing filler in batches, adding the rest of the structure control agent, a crosslinking agent and a processing aid into the internal mixer for internal mixing in sequence after the addition is finished, heating and vacuumizing rubber materials, then discharging, and carrying out high-temperature treatment for 3-6 hours to obtain fluorosilicone rubber composition base rubber;
(2) cooling the base rubber to room temperature, standing for 24-48h, adding an anti-aging agent, thinly passing for 15-20 times, taking out the sheet, and packaging to obtain the fluorosilicone rubber composition.
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| CN113755016B (en) * | 2021-08-31 | 2022-12-09 | 中海油田服务股份有限公司 | Fluorosilicone rubber composition, preparation method thereof and packer rubber barrel comprising fluorosilicone rubber composition |
| CN114395258A (en) * | 2022-01-22 | 2022-04-26 | 宁平 | Fluorosilicone rubber composition and preparation method thereof |
| CN115926476B (en) * | 2023-01-10 | 2024-04-19 | 山东大学 | High-strength oil-resistant fluorine-silicon sealing material for engine and preparation method thereof |
| CN116120749B (en) * | 2023-02-27 | 2023-12-05 | 昆山力普电子橡胶有限公司 | Fluorine silica gel material for watchband and preparation method thereof |
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| JPH0741627A (en) * | 1993-07-28 | 1995-02-10 | Toray Dow Corning Silicone Co Ltd | Rubber composition |
| US6035780A (en) * | 1998-04-13 | 2000-03-14 | Xerox Corporation | Compatibilized blend of fluoroelastomer and polysiloxane useful for printing machine component |
| CN1286899C (en) * | 2002-06-06 | 2006-11-29 | 陶氏康宁公司 | Fluorocarbon elastomer silicone vulcanizates |
| CN100575408C (en) * | 2003-12-15 | 2009-12-30 | 陶氏康宁公司 | Fluorocarbon elastomer silicone vulcanizates |
| GB0509467D0 (en) * | 2005-05-10 | 2005-06-15 | Dow Corning | Fluorosilicone rubber composition and adhering method thereof |
| CN1302048C (en) * | 2005-06-13 | 2007-02-28 | 上海三爱富新材料股份有限公司 | Fluorine-silicon compounded rubber stock and method for making same |
| CN101177486A (en) * | 2007-11-02 | 2008-05-14 | 广东信力特种橡胶制品有限公司 | Method for preparing fluorine silicon rubber base glue |
| CN101412835B (en) * | 2008-11-28 | 2011-01-19 | 华南理工大学 | Blend of fluorubber and silastic, and preparation thereof |
| CN102220014B (en) * | 2011-06-01 | 2013-04-03 | 山东大学 | High-strength fluorinated silicone rubber gross rubber and preparation method thereof |
| CN104530610A (en) * | 2014-12-29 | 2015-04-22 | 中国兵器工业集团第五三研究所 | Fluorine rubber-fluorosilicone rubber blend and preparation method thereof |
| CN104530719A (en) * | 2014-12-29 | 2015-04-22 | 中国兵器工业集团第五三研究所 | Vinyl blocked poly(trifluoropropyl)methylsiloxane fluororubber compatibilizer and preparation method thereof |
| CN106280495A (en) * | 2016-08-26 | 2017-01-04 | 山东华夏神舟新材料有限公司 | A kind of high strength and high hardness Fluorosilicone rubber composition and preparation method thereof |
| CN107903632A (en) * | 2017-12-15 | 2018-04-13 | 惠州市三岛新材料有限公司 | A kind of room temperature vulcanization high-temperature-resisting silicon rubber and preparation method thereof |
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