CN103772859B - Fluororubber compounded rubber of a kind of modification and preparation method thereof - Google Patents
Fluororubber compounded rubber of a kind of modification and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of fluororubber compounded rubber and preparation method thereof, viton of the present invention with modification binary fluorine rubber for raw material, use bis-phenol vulcanization system and peroxide vulcanizing system two kinds of vulcanizing agent modes to combine simultaneously and carry out sulfuration, and increase adapted auxiliary agent, mixing and obtain, it has excellent high heat resistance, winter hardiness, low-permeability and fuel resistance, be applicable to space flight, aviation, automobile, metallurgical, petrochemical complex, the industries such as electronics, and for sealing applications can not performance too low, also can not have problems because applied environment changes, can be used as the first-selection of sealing material.
Description
Technical field
The present invention relates to Materials Science and Engineering technical field, especially relate to fluororubber compounded rubber of a kind of low temperature resistant, chemical substance of improvement and preparation method thereof.
Background technology
Viton is novel macromolecular material, has excellent heat-resisting, media-resistant and oil-proofness and good physical and mechanical properties, electrical insulating property and radiation resistance etc., is known as " king of rubber ".
Viton 60 ~ 70% is for automotive industry.Now, along with the development of automotive light weight technology, high-performance, low oil consumption, automobile is containing alcohol and the widespread use of ethers green fuel, and vehicle emission standards improves constantly, to high performance fluorine rubber unvulcanizate sought-after with high heat resistance, winter hardiness, low-permeability and fuel resistance.But because of the restriction by current material sciemtifec and technical sphere current material, with regard to current elastomeric material, between the performances such as high heat resistance, winter hardiness, low-permeability and fuel resistance, there is conflict to a certain degree.
At present, domestic fluorine rubber compound sizing material can only meet some of performance, such as, for current known sizing material, is provided with resistance to low temperature, just not ability (containing alcohols) fuel performance.
Have developed synthesis and the applicating developing technology of high-performance rubber at present abroad, harsh low-temperature performance can have been met, the fuel oil containing alcohols or chemical substance performance can be met again.But this technical formula and concrete technology parameter are bottled up by abroad multinational, domestic relevant manufacturers can only to be correlated with high-performance rubber product from external import by paying great number import cost.
Perfluoroelastomers is a kind of new type rubber, its with tetrafluoroethylene, perfluoromethyl vinylether and general formula for CF
2(X is-COOR, CN, OC to=CF-ORFX
6h
5) terpolymer, be a kind of completely not containing the rubber of c h bond.It has the thermostability similar with tetrafluoroethylene and chemical resistant properties.Due to synthesis technique and the complexity thereof of perfluoroelastomers, production cost is too high, how obtaining the perfluoroelastomers simultaneously with premium propertiess such as high heat resistance, winter hardiness, low-permeability and fuel resistances, is the technical barrier perplexing China correlative technology field research staff for a long time.At present, China is not yet captured about the technology of perfluoroelastomers, and import can only be relied on to meet, and prices are rather stiff, so can not replace existing common viton kind.And adopt adjustment formula can not reach requirement, Just because of this, ensureing on excellent physicals, processing characteristics basis, by low temperature, alcohols fuel oil, the chemical substance performance of sizing material improved the adjustment of rubber in fluorine rubber compound and formula system, be that pole is necessary to adapt to the needs of all trades and professions.
Summary of the invention
The object of the invention is to meet material sciemtifec and technical sphere to the demand of perfluoroelastomers with performances such as excellent high heat resistance, winter hardiness, low-permeability and fuel resistances, thus provide a kind of formula preparing perfluoroelastomers material, and provide the preparation method of the perfluoroelastomers (fluororubber compounded rubber of the present invention) of low temperature resistant, the chemical series utilizing this formula production loading.
In order to realize the object of the invention, the fluororubber compounded rubber of low temperature resistant, the chemical series of improvement of the present invention with modification binary fluorine rubber for raw material, use bis-phenol vulcanization system and peroxide vulcanizing system two kinds of vulcanizing agent modes to combine simultaneously and carry out sulfuration, and increase adapted auxiliary agent, mixing and obtain.
The fluororubber compounded rubber of low temperature resistant, the chemical series of improvement of the present invention with two kinds of vulcanization systems: by the cross-linking density that the bis-phenol vulcanizing agent acquisition of higher dosage is higher, molecule chain end obtains crosslinked by superoxide and Calcium Fluoride (Fluorspan) auxiliary agent, molecule chain end is coupled together in this way, thus form the polymkeric substance of high molecular, reduce rubber unvulcanizate low-temperature performance while improving the physicals of rubber unvulcanizate, and do not change the process industrial art performance of sizing material.
The fluororubber compounded rubber of low temperature resistant, the chemical series of improvement of the present invention, adopts Calcium Fluoride (Fluorspan) auxiliary agent in its formula, utilizes the more effective combination of molecular structure of this auxiliary agent contain fluorine atoms and viton, the tensile strength of raising sizing material; Be equipped with modification infusorial earth auxiliary agent simultaneously, adding of modification infusorial earth auxiliary agent, make the elongation of its sizing material, low temperature flexibility further changed, simultaneously increase mobility man-hour adding, feeding is avoided to be " bridge formation ", increase substantially resistance to tearing and the elasticity of fluorine rubber compound, promote the vulcanization rate of sizing material.
The one that the invention provides the modification fluororubber compounded rubber of low temperature resistant, chemical species is specifically filled a prescription, and this is low temperature resistant, the modification fluororubber compounded rubber of chemical species is made by the rubber unvulcanizate comprising following raw material is mixing:
Modification binary fluorine rubber 100
Magnesium oxide 3-8
Calcium hydroxide 4-8
Carbon black filler 20-30
Releasing agent 1-3
Bisphenol AF 1.5-2.5
BPP 0.4-0.8
Modification infusorial earth auxiliary agent 5-10
Peroxide vulcanizing agent 3.0-4.5.
Wherein, peroxide vulcanizing agent is two 2.5 of 1.0-1.5 part, and the TAIC of 2.0-3.0 part.Described releasing agent is that Lay mattress falls apart and/or WS280(mono-kind take organosilicon as the new type rubber processing aid of base-material, can be commercially available from Structol company of the U.S.).。
Further, the present invention is low temperature resistant, the modification fluororubber compounded rubber raw material of chemical species can also comprise the Calcium Fluoride (Fluorspan) auxiliary agent of 0-40 part, more preferably, and the Calcium Fluoride (Fluorspan) auxiliary agent wherein containing 15-40 part.
In the modification fluororubber compounded rubber of low temperature resistant, chemical species of the present invention, described modification binary fluorine rubber is preferably REM260, and for containing a peroxide cure point monomer, Mooney is the modification binary fluorine rubber (CGREM260) of below 70MU, molecular weight is 7 ~ 120,000, and its concrete molecule is:
M(is the alkene of halogen atom-containing).
During modification fluororubber compounded rubber that is low temperature resistant, chemical species of the present invention is filled a prescription, described modification infusorial earth is a kind of inorganics, using the siliceous class inorganics of two or more vesicular structure as carrier, carry out physical treatment by silane coupling agent and obtain, the inorganics of described siliceous class is diatomite, tripoli, the strong powder of silicon.Preferred silane coupling agent is the amino silicane coupling agent containing four-functional group.
During modification fluororubber compounded rubber that is low temperature resistant, chemical species of the present invention is filled a prescription, described bisphenol AF is hexafluoro bisphenol-a.
During modification fluororubber compounded rubber that is low temperature resistant, chemical species of the present invention is filled a prescription, magnesium oxide preferably uses Japan's consonance high reactivity 170, and calcium hydroxide preferably uses the Caldic2000 calcium hydroxide of Japanese Jin Jiang company.The ultra-fine Calcium Fluoride (Fluorspan) that Calcium Fluoride (Fluorspan) preferred Shanghai Qiao Di company produces.The two 2.5/TAIC of peroxide vulcanizing agent is Jiangsu Japan Products, and TAIC is preferably Powdered.
About in component formula of the present invention, WS280 is a kind of Concentrated complexes of organo-siloxane/inorganic carrier; Bisphenol AF is two (4-hydroxy phenyl) HFC-236fa of 2.2-; Two 2.5 is 2.5-dimethyl-2.5 di-t-butyl peroxyhexane; TAIC is three triallyl isocyanurates.
Present invention also offers a kind of preparation method of modification fluororubber compounded rubber of low temperature resistant, chemical species, it is characterized in that, comprise the following steps:
1) modification binary fluorine rubber is plasticated in close rubber mixing machine;
2) two 2.5 and TAIC, modification infusorial earth to be weighed in advance and after mixing, join in Banbury mixer carry out mixing in advance.
3) in the sizing material after mixing in advance, add the mixture of bisphenol AF, BPP, magnesium oxide, calcium hydroxide, MTN990 carbon black, Calcium Fluoride (Fluorspan) and releasing agent, peroxide vulcanizing agent, auxiliary agent, mixing in close rubber mixing machine; Last in mill with triangle packet form back mixing thin-pass;
4) slice, detects, packaging.
Preferably, step (1) is: plasticated in close rubber mixing machine by modification binary fluorine rubber, and the time is 2.5min/30kg, and banburying temperature is no more than 70 DEG C;
Preferably, step (2) is: weighed in advance in two 2.5 and TAIC, modification infusorial earth and after mixing, and joins in Banbury mixer to carry out mixing in advance, and mixing time is 5min, and banburying temperature is no more than 100 DEG C; Batch turning, slice, room temperature, ventilation park 1-2 days.
Preferably, step (3) is: in the sizing material after mixing in advance, add bisphenol AF, BPP(BPP), magnesium oxide, calcium hydroxide, MTN990 carbon black, Calcium Fluoride (Fluorspan) and releasing agent, peroxide vulcanizing agent, auxiliary agent mixture, mixing in close rubber mixing machine, mixing time is 7min/30kg sizing material, and banburying terminates the preferred 24h of rear placement 20 ~ 28h(); Last in mill with triangle packet form back mixing thin-pass, mixing pass is 10 ~ 15 times (preferably 12 times), and melting temperature is no more than 60 DEG C.
The physical function parameter of the mixing fluororubber compounded rubber made of employing aforesaid method is: tensile strength can reach 16.0MPa, tensile yield can up to 250%, hardness is 70-80HA, the requirement of low temperature brittleness-50 DEG C can be met, resistance to (gasoline 75%: ethanol 25%) volumetric expansion is 3.0%, volumetric expansion in hydrocarbon medium is 4.9%, and compression set rate is 15-20%.
Fluororubber compounded rubber of the present invention adopts the binary fluorine rubber CGREM260(containing peroxide cure point of modification to synthesize below Mooney 70MU), the mode that bis-phenol vulcanization system and peroxide vulcanizing system two kinds of vulcanizing agents combine has been used in formula, the Calcium Fluoride (Fluorspan) of contain fluorine atoms is added in formula, adapted modification infusorial earth raw material simultaneously, mixing obtained a kind of fluorine rubber compound.
Wherein, in formula with two kinds of vulcanization systems be also, higher cross-linking density is obtained by the bis-phenol vulcanizing agent of higher dosage, molecule chain end can obtain crosslinked by superoxide and auxiliary agent again, molecule chain end is coupled together in this way the polymkeric substance that can form high molecular, reduce rubber unvulcanizate low-temperature performance while improving the physicals of rubber unvulcanizate, and do not change the process industrial art performance of sizing material.In addition, adopting Calcium Fluoride (Fluorspan) auxiliary agent in formula, is the more effective combination of molecular structure utilizing this auxiliary agent contain fluorine atoms and viton, improves the tensile strength of sizing material.Be equipped with adding of modification infusorial earth auxiliary agent simultaneously, the elongation of its sizing material can be made, low temperature flexibility further changed, simultaneously add especially inject extrusion way man-hour time, increase mobility, feeding is avoided to be " bridge formation ", resistance to tearing and the elasticity of fluorine rubber compound can be increased substantially, promote the vulcanization rate of sizing material.
Therefore, that is filled a prescription by whole rubber unvulcanizate is added, improve the physicals of sizing material on the one hand, reduce the low-temperature performance of sizing material on the other hand, meet the performance of the medium of resistance to harsh chemical of sizing material simultaneously, so the improvement fluororubber compounded rubber obtained according to the present invention, there is excellent tensile strength, elongation, outside low-temperature performance, there is the excellent fuel oil of resistance to alcohols and chemical mediator, and by the use of user, without the processing characteristics affecting product, pad can be widely used in, O type circle, sebific duct, offset plate, in the goods such as oil sealing, and it is suitable with external product technology, price material benefit.
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.If do not specialize, the conventional means that technique means used in embodiment is well known to those skilled in the art, is raw materials usedly commercial goods.
The preparation (1) of embodiment 1 fluororubber compounded rubber
There is fluororubber compounded rubber formula that is low temperature resistant, chemical mediator as follows.
Modification binary fluorine rubber (REM260) 100
Magnesium oxide 4
Calcium hydroxide 5
Carbon black filler 20
Calcium Fluoride (Fluorspan) 10
Releasing agent 1.5
Bisphenol AF 2.0
BPP 0.4
Modification infusorial earth 5
Two 2.51.0
TAIC2.0
Above-mentioned releasing agent is WS280.
Above-mentioned modification infusorial earth is that diatomite and tripoli are obtained by the amino silicane coupling agent physical treatment containing four-functional group.
The preparation (2) of embodiment 2 fluororubber compounded rubber
There is fluororubber compounded rubber formula that is low temperature resistant, chemical mediator as follows.
Modification binary fluorine rubber (REM260) 100
Magnesium oxide 6
Calcium hydroxide 7
Carbon black filler 25
Calcium Fluoride (Fluorspan) 20
Releasing agent 2.0
Bisphenol AF 2.2
BPP 0.5
Modification infusorial earth 7
Two 2.51.2
TAIC2.4
Above-mentioned releasing agent is that Lay mattress falls apart
Above-mentioned modification infusorial earth is that diatomite and the strong powder of silicon are obtained by the amino silicane coupling agent physical treatment containing four-functional group.
The preparation (3) of embodiment 3 fluororubber compounded rubber
There is fluororubber compounded rubber formula that is low temperature resistant, chemical mediator as follows.
Modification binary fluorine rubber (REM260) 100
Magnesium oxide 7
Calcium hydroxide 8
Carbon black filler 30
Calcium Fluoride (Fluorspan) 30
Releasing agent 3.0
Bisphenol AF 2.5
BPP 0.6
Modification infusorial earth 7
Two 2.51.5
TAIC2.8
Above-mentioned releasing agent is that Lay mattress falls apart and WS280 obtains by the mixing of 1:1 weight part.
Above-mentioned modification infusorial earth is that tripoli and the strong powder of silicon are obtained by the amino silicane coupling agent physical treatment containing four-functional group.
The preparation (4) of embodiment 4 fluororubber compounded rubber
There is fluororubber compounded rubber formula that is low temperature resistant, chemical mediator as follows.
Modification binary fluorine rubber (REM260) 100
Magnesium oxide 7
Calcium hydroxide 8
Carbon black filler 30
Calcium Fluoride (Fluorspan) 30
Releasing agent 3.0
Bisphenol AF 2.5
BPP 0.6
Modification infusorial earth does not add
Two 2.51.5
TAIC2.8
Above-mentioned releasing agent is that WS280 and Lay mattress are loose by 2:1 weight part mixing acquisition.
Above-mentioned modification infusorial earth is that the strong powder of diatomite, tripoli and silicon is obtained by the amino silicane coupling agent physical treatment of four-functional group.
The preparation method of the fluororubber compounded rubber in embodiment 1-4 is:
1) plasticated in close rubber mixing machine by modification binary fluorine rubber, the time is 2.5min/30kg, and banburying temperature is no more than 70 DEG C;
2) to be weighed in advance in two 2.5 and TAIC, modification infusorial earth and after mixing, join in Banbury mixer and carry out mixing in advance, mixing time is 5min, and banburying temperature is no more than 100 DEG C; Batch turning, slice, room temperature, ventilation park 1-2 days.
3) in the sizing material after mixing in advance, add the mixture of the auxiliary agents such as bisphenol AF, BPP, magnesium oxide, calcium hydroxide, MTN990 carbon black, Calcium Fluoride (Fluorspan) and releasing agent, mixing in close rubber mixing machine, mixing time is 7min/30kg sizing material, and banburying terminates the preferred 24h of rear placement 20-28h(); Last in mill with triangle packet form back mixing thin-pass, mixing pass be 10-15 all over (preferably 12 times), melting temperature is no more than 60 DEG C;
4) slice, detects, packaging.
The object blending together premixing glue is in advance to make liquid peroxide vulcanizing agent and the better vulcanization crosslinking of viton.Adopt follow-up mixing, the mode of thin-pass is intended to make sizing material quality more stable, reduces the loss of auxiliary agent in production process, production sizing material is disperseed evenly.
Wherein, modification infusorial earth is mainly for the deficiency of the various performance of modification viton mixing vulcanization system rubber unvulcanizate, a kind of auxiliary packing of exploitation, its specific surface area is about a kind of inorganics of 2.2m2/g, using the siliceous class inorganics of two or more vesicular structure as carrier, carry out physical treatment by silane coupling agent and obtain, the inorganics of described siliceous class is two or more in the materials such as diatomite, tripoli, the strong powder of silicon, Calucium Silicate powder.Preferred silane coupling agent is the amino silicane coupling agent containing four-functional group.The preparation technology of the diatomite auxiliary agent in embodiment 1-4 is:
Inorganics class (the strong powder of diatomite, silicon, Calucium Silicate powder, tripoli) any combination two kinds is mixed according to (1:1 weight ratio) in a reservoir, and airtight placement 4h, using this mixture as carrier, add the silane coupling agent of 5% ~ 10%, carry out physical treatment, surface is through amino modified process, and a kind of tip-like auxiliary packing material obtained.
The physicochemical property of embodiment 5 fluorine rubber compound of the present invention
Adopt national regulations method to detect, the physicals of the product obtained by the formula of embodiment 1-4 is as follows:
Table 1 fluorine rubber compound performance
As can be seen from Table 1, fluororubber compounded rubber of the present invention has excellent physicochemical property, except the tensile strength of its excellence, elongation, low-temperature performance, also there is the excellent fuel oil of resistance to alcohols and chemical mediator performance, and fluororubber compounded rubber production technique of the present invention is simple, mild condition, without the need to high temperature high pressure process, save energy, production technique is also very succinct, has good application prospect in scale operation.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (5)
1. the modification fluororubber compounded rubber of low temperature resistant a, chemical species, it is characterized in that, with modification binary fluorine rubber for raw material, use bis-phenol vulcanization system and peroxide vulcanizing system two kinds of vulcanizing agent modes to combine simultaneously and carry out sulfuration, and increase adapted auxiliary agent, mixing and obtain;
Wherein, and with two kinds of vulcanization systems, higher cross-linking density is obtained by the bis-phenol vulcanizing agent of higher dosage, molecule chain end obtains crosslinked by superoxide and Calcium Fluoride (Fluorspan) auxiliary agent, molecule chain end is coupled together in this way, thus form the polymkeric substance of high molecular, improve rubber unvulcanizate resistance to low temperature while improving the physicals of rubber unvulcanizate, and do not change the process industrial art performance of sizing material;
Wherein, described two kinds of vulcanization systems and raw material are made up of the component of following weight part:
Peroxide vulcanizing agent is wherein two 2.5 of 1.0-1.5 part, and the TAIC of 2.0-3.0 part;
Described modification binary fluorine rubber is for containing a peroxide cure point monomer, and Mooney is the modification binary fluorine rubber of below 70MU, and molecular weight is 7 ~ 120,000, and its concrete molecule is:
M is the alkene of halogen atom-containing;
Described modification infusorial earth is a kind of inorganics, using the siliceous class inorganics of two or more vesicular structure as carrier, carry out physical treatment by silane coupling agent and obtain, described siliceous class inorganics is diatomite, tripoli, the strong powder of silicon, and described silane coupling agent is the amino silicane coupling agent containing four-functional group.
2. fluororubber compounded rubber as claimed in claim 1, is characterized in that, described releasing agent is that Lay mattress falls apart and/or WS280.
3. a preparation method for the modification fluororubber compounded rubber of low temperature resistant, chemical species as claimed in claim 1, is characterized in that, comprise the following steps:
1) modification binary fluorine rubber is plasticated in close rubber mixing machine;
2) two 2.5 and TAIC, modification infusorial earth to be weighed in advance and after mixing, join in Banbury mixer carry out mixing in advance;
3) in the sizing material after mixing in advance, add the mixture of bisphenol AF, BPP, magnesium oxide, calcium hydroxide, MTN990 carbon black, Calcium Fluoride (Fluorspan) and releasing agent, mixing in close rubber mixing machine; Last in mill with triangle packet form back mixing thin-pass;
4) slice, detects, packaging.
4. preparation method as claimed in claim 3, is characterized in that, step 1) in modification binary fluorine rubber is plasticated in close rubber mixing machine, the time is 2.5min/30kg, and banburying temperature is no more than 70 DEG C.
5. preparation method as claimed in claim 3, is characterized in that, step 2) in mixing time mixing be in advance 5min, banburying temperature is no more than 100 DEG C; Batch turning, slice, room temperature, ventilation park 1-2 days.
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| CN104045949A (en) * | 2014-05-29 | 2014-09-17 | 江苏梅兰化工有限公司 | Ultra-low temperature resistant fluororubber mixed rubber and preparation method thereof |
| CN104558974A (en) * | 2014-12-12 | 2015-04-29 | 东莞市长安东阳光铝业研发有限公司 | Modified fluororubber compounded stock and preparation method thereof |
| CN104479263A (en) * | 2014-12-29 | 2015-04-01 | 江苏健神生物农化有限公司 | Preparation technology of perfluoro-elastomer rubber compound |
| CN105566820A (en) * | 2015-12-30 | 2016-05-11 | 崇夕山 | Shaft end O-shaped permanent compression set resisting rubber sealing ring |
| CN106633544B (en) * | 2016-11-17 | 2019-07-19 | 上海如实密封科技有限公司 | A kind of high temperature high voltage resistant sealing element fluorubber material and preparation method thereof |
| CN107501812A (en) * | 2017-09-02 | 2017-12-22 | 湖南梓唯汽车环保有限公司 | A kind of valve element fluorubber |
| CN107841072B (en) * | 2017-11-17 | 2019-09-27 | 江门市鑫辉密封科技有限公司 | A kind of fluorine rubber seal composition and preparation method thereof |
| CN114479319A (en) * | 2020-10-28 | 2022-05-13 | 中昊晨光化工研究院有限公司 | Fluororubber compound and preparation method and application thereof |
| CN112142902A (en) * | 2020-11-04 | 2020-12-29 | 段嘉敏 | Preparation method of special low-temperature-resistant fluororubber |
| CN112592548B (en) * | 2020-11-16 | 2023-02-24 | 上海如实密封科技有限公司 | Low-temperature-resistant fluororubber composition and application thereof |
| CN112852075A (en) * | 2021-02-03 | 2021-05-28 | 宁国市瑞普密封件有限公司 | Low-permeability fluororubber product material |
| CN116082775A (en) * | 2022-10-08 | 2023-05-09 | 山东东都汽车部件股份有限公司 | Axle hub oil seal product and preparation method thereof |
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| CN102875937A (en) * | 2012-09-12 | 2013-01-16 | 中昊晨光化工研究院有限公司 | Fluororubber rubber compound and preparation method thereof |
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