CN103602018A - Method for improving oil resistance and high temperature resistance by blending desulfurized fluororubber micro-powder/acrylic rubber - Google Patents
Method for improving oil resistance and high temperature resistance by blending desulfurized fluororubber micro-powder/acrylic rubber Download PDFInfo
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- CN103602018A CN103602018A CN201310554756.6A CN201310554756A CN103602018A CN 103602018 A CN103602018 A CN 103602018A CN 201310554756 A CN201310554756 A CN 201310554756A CN 103602018 A CN103602018 A CN 103602018A
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- desulfurization
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Abstract
The invention discloses a method for improving oil resistance and high temperature resistance by blending desulfurized fluororubber micro-powder/acrylic rubber, which is characterized by comprising the following steps: in parts by weight, mixing 10-100 parts of desulfurized fluororubber micro-powder with a gel content of 70-80% and a particle size of 1-120mu m, 100 parts of acrylic rubber, 30-80 parts of carbon black, 0.5-3 parts of stearic acid, 0.5-3 parts of accelerant and 0.5-3 parts of vulcanizing agent by using a two-roll open mill; at a roll temperature of 50-60 DEG C, blending for 10-30 min so as to obtain a desulfurized fluororubber micro-powder/acrylic rubber blend; then vulcanizing the blend for 10-30 min at a vulcanizing temperature of 150-180 DEG C firstly, and then vulcanizing the blend for 2-12 h at a vulcanizing temperature of 200-250 DEG C, so that a desulfurized fluororubber micro-powder/acrylic rubber blended vulcanizate is obtained.
Description
Technical field
The present invention relates to a kind of method of improving oil resistant high thermal resistance with the blend of desulfurization viton micro mist/acrylic elastomer, belong to polymer processing field.
Background technology
Acrylic elastomer has higher thermostability, less ventilation property, the performances such as good oil resistant, resistance to ozone, ageing-resistant, proof stress is tired, be widely used in various high temperature, oil resistant environment, can be at 150 ℃ life-time service, become automotive industry in recent years and focus on a kind of sealing material of develop and spread, especially for the high temperature resistant oil sealing of automobile, bent axle, valve rod, head gasket, hydraulic oil pipeline etc.Compare with acrylic elastomer, viton has higher use temperature (can at 200 ℃ life-time service), but because its cost is far above acrylic elastomer, has greatly limited its range of application.
By by acrylic elastomer and viton use, to promote the resistance to elevated temperatures of acrylic elastomer, attracted domestic and international investigator's concern [M.A.Kader and A.K.Bhowmick, Journal of Applied Polymer Science, 2003,89,1442.].But how reducing and use the cost of viton, is a current difficult problem urgently to be resolved hurrily.
Summary of the invention
The object of the invention is provides a kind of method of improving oil resistant high thermal resistance with the blend of desulfurization viton micro mist/acrylic elastomer for the deficiencies in the prior art, be characterized in adopting solid state mechanochemistry reactor (ZL200410040237.9), realize superfine grinding and the power chemical desulfurization of waste and old viton, improve the interface compatibility of itself and acrylic elastomer, thereby provide a kind of cheap and easy to get, improve the functional filler of acrylic elastomer oil resistant, resistance to elevated temperatures.
Object of the present invention adopts following technical measures to realize, and wherein said raw material umber, except specified otherwise, is parts by weight.
The method of improving oil resistant high thermal resistance with the blend of desulfurization viton micro mist/acrylic elastomer comprises the following steps:
1) preparation of desulfurization viton micro mist
By the waste and old viton after post vulcanization just broken be micelle or oddments, add in solid state mechanochemistry reactor and pulverize and desulfurization, rotating speed 1000-3000rpm passes into circulating water simultaneously, and controlled circulation water temp is at 5-35 ℃, through repeatedly milling 3-10 time, under shearing force, pressure and frictional force acting in conjunction, realize stress induced power chemical desulfurization and superfine grinding, the gel content of desulfurization viton micro mist is 70-80%, particle diameter is 1-120 μ m, standby;
2) preparation of desulfurization viton micro mist/acrylic elastomer blend
By gel content, be 70-80%, particle diameter is desulfurization viton micro mist 10-100 part, 100 parts of acrylic elastomers, carbon black 30-80 part of 1-120 μ m, stearic acid 0.5-3 part, promotor 0.5-3 part and vulcanizing agent 0.5-3 part, with two roller mill mixings, roller temperature 50-60 ℃, blend 10-30min, obtains desulfurization viton micro mist/acrylic elastomer blend;
3) sulfuration of desulfurization viton micro mist/acrylic elastomer blend
By above-mentioned blend, in one step cure temperature, be 150-180 ℃, curing time 10-30min, post vulcanization temperature is 200-250 ℃, and curing time is 2-12h, and sulfuration obtains desulfurization viton micro mist/acrylic elastomer blended vulcanizate.
Described promotor is any in the blend of N cyclohexyl 2 benzothiazole sulfenamide, zinc dibutyl dithiocaarbamate or N cyclohexyl 2 benzothiazole sulfenamide and zinc dibutyl dithiocaarbamate.
Described vulcanizing agent is sulphur or trithiocyanuric acid.
The blend of desulfurization viton micro mist/acrylic elastomer improves desulfurization viton micro mist/acrylic elastomer blended vulcanizate that the method for oil resistant high thermal resistance prepares.
Desulfurization viton micro mist/acrylic elastomer blended vulcanizate is for sealing member, adhesive tape and the sebific duct field of automobile or precision instrument.
Performance test:
1. adopt ASTM D471 standard, by testing, at 150 ℃, in ASTM3# oil, soak the cubical expansivity of 72h and the oil-proofness that tensile strength velocity of variation is evaluated desulfurization viton micro mist/acrylic elastomer blended vulcanizate, as shown in Table 1 below, result shows to have improved its oil-proofness with the blend of desulfurization viton micro mist/acrylic elastomer.
2. adopt GB/T3512-2001 standard, by testing at 150 ℃, the velocity of variation of placing elongation at break after 72h and tensile strength in hot air aging case is evaluated the high thermal resistance of desulfurization viton micro mist/acrylic elastomer blended vulcanizate, as shown in Table 1 below, result shows to have improved its high thermal resistance with the blend of desulfurization viton micro mist/acrylic elastomer.
3. adopt tensile strength and the elongation at break of tension testing machine test cross-linked rubber, rate of extension 500mm/min, as shown in Table 1 below, result shows to have improved mechanical property with the blend of desulfurization viton micro mist/acrylic elastomer.
Tool of the present invention has the following advantages:
1. desulfurization viton micro mist addition is large, the highest 50% of the blend total mass that accounts for, and cost is lower, is widely used.
2. over-all properties is superior, has significantly improved the oil resistant of goods by add desulfurization viton micro mist in acrylic elastomer
Property and high thermal resistance.
3. technique is simple, easy and simple to handle, is conducive to suitability for industrialized production.
Embodiment
Below by embodiment, the present invention is specifically described; be necessary to be pointed out that at this following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment to the present invention according to foregoing.
Embodiment 1:
30 parts of the desulfurization viton micro mists that gel content is 80%, particle diameter is 120 μ m, 100 parts of acrylic elastomers, 80 parts of carbon blacks, 0.5 part of stearic acid, 2 parts of accelerant N-cyclohexyl-2-[4-morpholinodithio sulphenamides, 0.5 part, vulcanizing agent sulphur.Adopt two roller mill mixings, roller temperature 50-60 ℃, blend 30min, then adopt vulcanizing press sulfuration, 175 ℃ * 30min of one step cure condition, 200 ℃ * 6h of post vulcanization condition, sulfuration obtains desulfurization viton micro mist/acrylic elastomer blended vulcanizate.
Embodiment 2.
50 parts of the desulfurization viton micro mists that gel content is 75%, particle diameter is 100 μ m, 100 parts of acrylic elastomers, 60 parts of carbon blacks, 1.5 parts of stearic acid, 3 parts of promotor zinc dibutyl dithiocaarbamates, 1 part of vulcanizing agent trithiocyanuric acid.Adopt two roller mill mixings, roller temperature 50-60 ℃, blend 20min, then adopt vulcanizing press sulfuration, 170 ℃ * 15min of cure conditions, post vulcanization condition is 230 ℃ * 4h, sulfuration obtains desulfurization viton micro mist/acrylic elastomer blended vulcanizate.
Embodiment 3.
100 parts of the desulfurization viton micro mists that gel content is 75%, particle diameter is 100 μ m, 100 parts of acrylic elastomers, 30 parts of carbon blacks, 3 parts of stearic acid, 0.5 part of promotor zinc dibutyl dithiocaarbamate, 2 parts of vulcanizing agent trithiocyanuric acids.Adopt two roller mill mixings, roller temperature 50-60 ℃, blend 20min, then adopt vulcanizing press sulfuration, 180 ℃ * 10min of cure conditions, post vulcanization condition is 250 ℃ * 2h, sulfuration obtains desulfurization viton micro mist/acrylic elastomer blended vulcanizate.
Embodiment 4.
50 parts of the desulfurization viton micro mists that gel content is 70%, particle diameter is 1 μ m, 100 parts of acrylic elastomers, 50 parts of carbon blacks, 0.5 part of stearic acid, 2 parts of accelerant N-cyclohexyl-2-[4-morpholinodithio sulphenamides, 3 parts, vulcanizing agent sulphur.Adopt two roller mill mixings, roller temperature 50-60 ℃, blend 10min, then adopt vulcanizing press sulfuration, 150 ℃ * 20min of one step cure condition, 230 ℃ * 4h of post vulcanization condition, sulfuration obtains desulfurization viton micro mist/acrylic elastomer blended vulcanizate.
Application example 1
Adopt prepared desulfurization viton micro mist/acrylic elastomer blend in embodiment 4, through vulcanizing press sulfidization molding, obtain O type circle, excellent combination property, cost significantly reduces.
Comparison example 1
100 parts of acrylic elastomers, 50 parts of carbon blacks, 0.5 part of stearic acid, 2 parts of accelerant N-cyclohexyl-2-[4-morpholinodithio sulphenamides, 3 parts, vulcanizing agent sulphur.Adopt two roller mill mixings, roller temperature 50-60 ℃, blend 20min, then adopt vulcanizing press sulfuration, 150 ℃ * 20min of one step cure condition, 230 ℃ * 4h of post vulcanization condition, sulfuration obtains desulfurization viton micro mist/acrylic elastomer blended vulcanizate.
The Performance Ratio of table 1 embodiment and comparison example
Claims (5)
1. with the blend of desulfurization viton micro mist/acrylic elastomer, improve the method for oil resistant high thermal resistance, it is characterized in that the method comprises the following steps:
1) preparation of desulfurization viton micro mist
By the waste and old viton after post vulcanization just broken be micelle or oddments, add in solid state mechanochemistry reactor and pulverize and desulfurization, rotating speed 1000-3000rpm passes into circulating water simultaneously, and controlled circulation water temp is at 5-35 ℃, through repeatedly milling 3-10 time, under shearing force, pressure and frictional force acting in conjunction, realize stress induced power chemical desulfurization and superfine grinding, the gel content of desulfurization viton micro mist is 70-80%, particle diameter is 1-120 μ m, standby;
2) preparation of desulfurization viton micro mist/acrylic elastomer blend
By gel content, be 70-80%, particle diameter is desulfurization viton micro mist 10-100 weight part, acrylic elastomer 100 weight parts, the carbon black 30-80 weight part of 1-120 μ m, stearic acid 0.5-3 weight part, promotor 0.5-3 weight part and vulcanizing agent 0.5-3 weight part, with two roller mill mixings, roller temperature 50-60 ℃, blend 10-30min, obtains desulfurization viton micro mist/acrylic elastomer blend;
3) sulfuration of desulfurization viton micro mist/acrylic elastomer blend
By above-mentioned blend, in one step cure temperature, be 150-180 ℃, curing time 10-30min, post vulcanization temperature is 200-250 ℃, and curing time is 2-12h, and sulfuration obtains desulfurization viton micro mist/acrylic elastomer blended vulcanizate.
2. with the blend of desulfurization viton micro mist/acrylic elastomer, improve as claimed in claim 1 the method for oil resistant high thermal resistance, it is characterized in that promotor is any in the blend of N cyclohexyl 2 benzothiazole sulfenamide, zinc dibutyl dithiocaarbamate or N cyclohexyl 2 benzothiazole sulfenamide and zinc dibutyl dithiocaarbamate.
3. the blend of desulfurization viton micro mist/acrylic elastomer improves the method for oil resistant high thermal resistance as claimed in claim 1, it is characterized in that vulcanizing agent is sulphur or trithiocyanuric acid.
4. as described in one of claim 1~4, the blend of desulfurization viton micro mist/acrylic elastomer improves desulfurization viton micro mist/acrylic elastomer blended vulcanizate that the method for oil resistant high thermal resistance prepares.
As claimed in claim 4 desulfurization viton micro mist/acrylic elastomer blended vulcanizate for sealing member, adhesive tape and the sebific duct field of automobile or precision instrument.
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Cited By (6)
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CN105650157A (en) * | 2014-11-30 | 2016-06-08 | 衡阳市安骋汽车配件有限公司 | Particles having noise reduction and high-temperature declining resistance functions and preparation method of particles |
CN105650162A (en) * | 2014-11-30 | 2016-06-08 | 衡阳市安骋汽车配件有限公司 | Particles having high-temperature declining resistance function and high heat conductivity and preparation method of particles |
CN105650169A (en) * | 2014-11-30 | 2016-06-08 | 衡阳市安骋汽车配件有限公司 | Granules with noise reduction function and large porosity and preparation method of granules |
CN105650172A (en) * | 2014-11-30 | 2016-06-08 | 衡阳市安骋汽车配件有限公司 | Granules with high-temperature decay-resistant function and large porosity and preparation method of granules |
CN105650161A (en) * | 2014-11-30 | 2016-06-08 | 衡阳市安骋汽车配件有限公司 | Particles having larger porosity and excellent heat conductivity and preparation method of particles |
CN117024897A (en) * | 2023-07-11 | 2023-11-10 | 珠海优亿电子科技有限公司 | Oil-resistant sealing element for transformer and preparation process thereof |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105650157A (en) * | 2014-11-30 | 2016-06-08 | 衡阳市安骋汽车配件有限公司 | Particles having noise reduction and high-temperature declining resistance functions and preparation method of particles |
CN105650162A (en) * | 2014-11-30 | 2016-06-08 | 衡阳市安骋汽车配件有限公司 | Particles having high-temperature declining resistance function and high heat conductivity and preparation method of particles |
CN105650169A (en) * | 2014-11-30 | 2016-06-08 | 衡阳市安骋汽车配件有限公司 | Granules with noise reduction function and large porosity and preparation method of granules |
CN105650172A (en) * | 2014-11-30 | 2016-06-08 | 衡阳市安骋汽车配件有限公司 | Granules with high-temperature decay-resistant function and large porosity and preparation method of granules |
CN105650161A (en) * | 2014-11-30 | 2016-06-08 | 衡阳市安骋汽车配件有限公司 | Particles having larger porosity and excellent heat conductivity and preparation method of particles |
CN117024897A (en) * | 2023-07-11 | 2023-11-10 | 珠海优亿电子科技有限公司 | Oil-resistant sealing element for transformer and preparation process thereof |
CN117024897B (en) * | 2023-07-11 | 2024-02-20 | 珠海优亿电子科技有限公司 | Oil-resistant sealing element for transformer and preparation process thereof |
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