CN103013012B - A kind of auto pump caulking gum and preparation method thereof - Google Patents
A kind of auto pump caulking gum and preparation method thereof Download PDFInfo
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- CN103013012B CN103013012B CN201210485259.0A CN201210485259A CN103013012B CN 103013012 B CN103013012 B CN 103013012B CN 201210485259 A CN201210485259 A CN 201210485259A CN 103013012 B CN103013012 B CN 103013012B
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Abstract
The invention discloses a kind of auto pump caulking gum, be made up of following raw materials in part by weight: acrylic elastomer 50-60, trifluoropropyl siloxane 10-15, chlorohydrin rubber T3100 10-15, brominated butyl rubber 22110-15, high abrasion furnace carbon black N330 30-36, precipitated silica 20-24, light calcium carbonate 4-6, wollastonite powder 5-10, Zirconium tetrafluoride 3-5, barium sulfate 5-7, molybdenumdisulphide 3-5, Modified Iron mine tailing ground-slag 9-11, vulcanizing agent DCBP1 ~ 2, anti-aging agent TPPD 1-2, vulkacit H 0.5 ~ 1, magnesium oxide 4-6, 2-thiol group benzimidazolyl 1-2, paraffin 1-2, sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester 1-2, acetyl tributyl citrate three (2-ethylhexyl) ester 17-19.Rubber size of the present invention has excellent ozone resistance and resistance to low temperature, resistance toheat, and use temperature scope is large, technique environmental protection, can make various gasket with this sizing material.
Description
Technical field
The present invention relates to synthetic rubber field, be specifically related to a kind of car-valve gasket sizing material and preparation method thereof.
Background technology
The riding stability and riding comfort etc. of automobile rubber component to the vibrationproof of automobile, noise abatement, raising vehicle play great role.The conventional rubber material usage of automobile is larger, but along with engine be in recent years tending towards high-power, miniaturization development, the envrionment temperature of engine environment raises, gas exhaust inspecting laws and regulations requirement is stricter, in addition the use of alcohol fuel, forces rubber component to improve heat-resisting, cold-resistant, oil resistant, the properties such as ageing-resistant.So the elastomeric consumption of high-performance special constantly increases, automobile is the principal market of these special synthetic rubbers.Therefore, the glue kind of automobile rubber is by the special gelatin future development with premium properties.
Acrylic elastomer (hereinafter referred to as ACM) take acrylate as the elastomerics that main monomer obtains through copolymerization, and its main chain is saturated carbon chains, and side base is polar ester groups.Because its many excellence given by special construction, as heat-resisting, ageing-resistant, oil resistant, resistance to ozone, uvioresistant etc., mechanical property and processing characteristics are better than viton and silicon rubber, and it is heat-resisting, ageing resistance and oil-proofness are better than paracril.ACM is widely used in various high temperature, resistance to oil environment, become a kind of sealing material that automotive industry in recent years focuses on develop and spread, especially for the high temperature resistant oil sealing, bent axle, valve rod, head gasket, hydraulic oil pipeline etc. of automobile, current domestic needs is whole dependence on import almost.
Cause engine room temperature rise because car speed improves, the envrionment temperature of auto parts machinery will reach 150 DEG C even more than 180 DEG C usually, therefore how to obtain the focus that the ACM rubber that can use in higher temperature environment for a long time becomes industry concern.In order to give prominence to or improve the processing characteristics of ACM, in recent years modification carried out to ACM or select ACM to one of other elastomer-modified study hotspots becoming processed and applied.Existing rubber seal is under the operating modes such as high temperature, low temperature, the large temperature difference, corrosive medium and long lifetime, and its sealing property is difficult to satisfactory, works out the trend that high performance rubber unvulcanizate becomes current domestic rubber industry development.
Summary of the invention
The invention provides a kind of auto pump caulking gum and preparation method thereof, sizing material of the present invention has excellent high-low temperature resistant, oil resistant, solvent resistant and chemical resistance, simultaneously good mechanical property.
The present invention adopts following technical scheme:
A kind of auto pump caulking gum, be made up of following raw materials in part by weight: acrylic elastomer 50-60, trifluoropropyl siloxane rubber 10-15, chlorohydrin rubber T3100 10-15, american exxon brominated butyl rubber 2211 10-15, high abrasion furnace carbon black N330 30-36, precipitated silica 20-24, light calcium carbonate 4-6, wollastonite powder 5-10, Zirconium tetrafluoride 3-5, barium sulfate 5-7, molybdenumdisulphide 3-5, Modified Iron mine tailing ground-slag 9-11, vulcanizing agent DCBP1 ~ 2, anti-aging agent TPPD 1-2, vulkacit H 0.5 ~ 1, magnesium oxide 4-6, 2-thiol group benzimidazolyl 1-2, paraffin 1-2, sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester 1-2, acetyl tributyl citrate three (2-ethylhexyl) ester 17-19.
Described a kind of auto pump caulking gum, it is characterized in that, be made up of following raw materials in part by weight: acrylic elastomer 59, trifluoropropyl siloxane rubber 14, chlorohydrin rubber T3100 13, brominated butyl rubber 2,211 14, high abrasion furnace carbon black N330 32, precipitated silica 22, light calcium carbonate 5, wollastonite powder 6, Zirconium tetrafluoride 4, barium sulfate 6, molybdenumdisulphide 4, Modified Iron mine tailing ground-slag 10, vulcanizing agent DCBP1.5, anti-aging agent TPPD 1.2, vulkacit H 0.8, magnesium oxide 5, 2-thiol group benzimidazolyl 1.5, paraffin 1.5, sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester 1.5, acetyl tributyl citrate three (2-ethylhexyl) ester 18.
The preparation method of described a kind of auto pump caulking gum, is characterized in that, comprise the following steps:
(1) preparation method of modification tree ash:
The potter's clay of tree ash weight 1-2% is joined in tree ash and mixes, with 15-20% salt acid soak 1-2 hour, wash with water to neutrality, after oven dry, add the trisodium phosphate of aluminate coupling agent DL-411, the 1-2% being equivalent to solid weight 0.5-1.0%, 1-2% iso-octyl Soxylat A 25-7,3-5% zinc oxide, with the speed high-speed stirring of 1200-1500 rev/min, obtain dispersion liquid, dispersion liquid is dried, is ground into powder, obtains modification tree ash;
(2) preparation of Modified Iron mine tailing ground-slag:
By scaling loss 4-6 hour at iron tailings 900-1000 DEG C, then nanometer powder is ground to form, admix the ptfe micropowder, the sodium lignosulfonate of 1-2%, the 1-2% different tridecanol polyoxyethylene ether agitating that are equivalent to powder weight 1-2% more even, dry, grind to form nanometer powder, obtain Modified Iron mine tailing ground-slag;
(3) 1:1 mass ratio dilution sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester is pressed with machine oil;
(4) by formula rate, modification tree ash, high abrasion furnace carbon black N330, precipitated silica are dropped in high-speed mixer, with the speed high-speed stirring of 1000-1200 rev/min, the coupling agent that step (2) has been diluted is sprayed onto in mixed fillers simultaneously, continue to stir 5-6 minute, discharging cooling is for subsequent use, obtains mixture;
(5) by acrylic elastomer, trifluoropropyl siloxane rubber, chlorohydrin rubber T3100, american exxon brominated butyl rubber 2211, Modified Iron mine tailing, drop in Banbury mixer, plasticate at the temperature of 65-73 DEG C, after plasticating 10-14 minute, when temperature reaches 82-95 DEG C, start discharge, after discharge, park cooling 10-12 hour;
(6) by formula rate, above-mentioned cooled broken-(down)rubber is joined in Banbury mixer, add the compound of step (4) again, after mixing 2-3 minute, after adding the mixing 10-15 of other leftover materials minute in formula beyond sulphur removal agent and promotor class again, when temperature reaches 90-128 DEG C, start discharge, after discharge, park cooling 12-14 hour;
(7) above-mentioned mixing materials is dropped in mill, then vulcanizing agent, promotor class are added in rubber unvulcanizate, thin-pass 6-8 time, processing temperature≤56 DEG C of mill.
Beneficial effect
The present invention is by acrylic elastomer and other several compounding rubber, improve the over-all properties of rubber unvulcanizate, tree ash is improved, tail iron ore is carried out modification simultaneously, then mix with carbon black, use coupling agent treatment again, use as strengthening agent, improve the dispersiveness of filler at rubber unvulcanizate, improve ozone resistance and the resistance to low temperature of rubber unvulcanizate, resistance toheat, than acrylic elastomer itself and butadiene-acrylonitrile rubber, there is wider use temperature scope simultaneously, better processing performance, lower starting material and production cost, meet the performance requriements of production domesticization component.
Embodiment
A preparation for auto pump caulking gum,
Take acrylic elastomer AR-100 59kg, trifluoropropyl siloxane 14kg, chlorohydrin rubber T310013kg, brominated butyl rubber 2211 14kg, high abrasion furnace carbon black N330 32kg, precipitated silica 22kg, light calcium carbonate 5kg, wollastonite powder 6kg, Zirconium tetrafluoride 4kg, barium sulfate 6kg, molybdenumdisulphide 4kg, Modified Iron mine tailing ground-slag 10kg, vulcanizing agent DCBP1.5kg, anti-aging agent TPPD1.2kg, vulkacit H 0.8kg, magnesium oxide 5kg, 2-thiol group benzimidazolyl 1.5kg, paraffin 1.5kg, sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester 1.5kg, acetyl tributyl citrate three (2-ethylhexyl) ester 18kg,
Preparation method comprises the following steps:
(1) preparation method of modification tree ash:
The potter's clay of tree ash weight 1-2% is joined in tree ash and mixes, with 15-20% salt acid soak 1-2 hour, wash with water to neutrality, after oven dry, add the trisodium phosphate of aluminate coupling agent DL-411, the 1-2% being equivalent to solid weight 0.5-1.0%, 1-2% iso-octyl Soxylat A 25-7,3-5% zinc oxide, with the speed high-speed stirring of 1200-1500 rev/min, obtain dispersion liquid, dispersion liquid is dried, is ground into powder, obtains modification tree ash;
(2) preparation of Modified Iron mine tailing ground-slag:
By scaling loss 4-6 hour at iron tailings 900-1000 DEG C, then nanometer powder is ground to form, admix the ptfe micropowder, the sodium lignosulfonate of 1-2%, the 1-2% different tridecanol polyoxyethylene ether agitating that are equivalent to powder weight 1-2% more even, dry, grind to form nanometer powder, obtain Modified Iron mine tailing ground-slag;
(3) 1:1 mass ratio dilution sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester is pressed with machine oil;
(4) by formula rate, modification tree ash, high abrasion furnace carbon black N330, precipitated silica are dropped in high-speed mixer, with the speed high-speed stirring of 1000-1200 rev/min, the coupling agent that step (2) has been diluted is sprayed onto in mixed fillers simultaneously, continue to stir 5-6 minute, discharging cooling is for subsequent use, obtains mixture;
(5) by acrylic elastomer, trifluoropropyl siloxane rubber, chlorohydrin rubber T3100, brominated butyl rubber 221, Modified Iron mine tailing, drop in Banbury mixer, plasticate at the temperature of 65-73 DEG C, after plasticating 10-14 minute, when temperature reaches 82-95 DEG C, start discharge, after discharge, park cooling 10-12 hour;
(6) by formula rate, above-mentioned cooled broken-(down)rubber is joined in Banbury mixer, add the compound of step (4) again, after mixing 2-3 minute, after adding the mixing 10-15 of other leftover materials minute in formula beyond sulphur removal agent and promotor class again, when temperature reaches 90-128 DEG C, start discharge, after discharge, park cooling 12-14 hour;
(7) above-mentioned mixing materials is dropped in mill, then vulcanizing agent, promotor class are added in rubber unvulcanizate, thin-pass 6-8 time, processing temperature≤56 DEG C of mill.
Experimental data
Make sizing material by the formula for raw stock of embodiment to make a service test detection, detected result is in table 1.
Table 1
The lower temperature resistance of sizing material of the present invention, resistance toheat and resistance to tearing are all good than conventional gaskets material as can be seen from the table, can be used as various sealing member material.
Claims (2)
1. an auto pump caulking gum, it is characterized in that, be made up of following raw materials in part by weight: acrylic elastomer 50-60, trifluoropropyl siloxane 10-15, chlorohydrin rubber T3100 10-15, american exxon brominated butyl rubber 2211 10-15, high abrasion furnace carbon black N330 30-36, precipitated silica 20-24, light calcium carbonate 4-6, wollastonite powder 5-10, Zirconium tetrafluoride 3-5, barium sulfate 5-7, molybdenumdisulphide 3-5, Modified Iron mine tailing ground-slag 9-11, vulcanizing agent DCBP1 ~ 2, anti-aging agent TPPD 1-2, vulkacit H 0.5 ~ 1, magnesium oxide 4-6, 2-thiol group benzimidazolyl 1-2, paraffin 1-2, sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester 1-2, acetyl tributyl citrate three (2-ethylhexyl) ester 17-19,
The preparation method of described auto pump caulking gum comprises the following steps:
(1) preparation of Modified Iron mine tailing ground-slag: by scaling loss 4-6 hour at iron tailings 900-1000 DEG C, then nanometer powder is ground to form, admix the ptfe micropowder, the sodium lignosulfonate of 1-2%, the 1-2% different tridecanol polyoxyethylene ether agitating that are equivalent to powder weight 1-2% more even, dry, grind to form nanometer powder, obtain Modified Iron mine tailing ground-slag;
(2) 1:1 mass ratio dilution sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester is pressed with machine oil;
(3) by formula rate, high abrasion furnace carbon black N330, precipitated silica are dropped in high-speed mixer, with the speed high-speed stirring of 1000-1200 rev/min, sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester of simultaneously step (2) having been diluted is sprayed onto in mixed fillers, continue to stir 5-6 minute, discharging cooling is for subsequent use, obtains mixture;
(4) by acrylic elastomer, trifluoropropyl siloxane rubber, chlorohydrin rubber T3100, brominated butyl rubber 2211, Modified Iron mine tailing, drop in Banbury mixer, plasticate at the temperature of 65-73 DEG C, after plasticating 10-14 minute, when temperature reaches 82-95 DEG C, start discharge, after discharge, park cooling 10-12 hour;
(5) by formula rate, above-mentioned cooled broken-(down)rubber is joined in Banbury mixer, add the compound of step (4) again, after mixing 2-3 minute, after adding the mixing 10-15 of other leftover materials minute in formula beyond sulphur removal agent and vulkacit H again, when temperature reaches 90-128 DEG C, start discharge, after discharge, park cooling 12-14 hour;
(6) above-mentioned mixing materials is dropped in mill, then vulcanizing agent, vulkacit H are added in rubber unvulcanizate, thin-pass 6-8 time, processing temperature≤56 DEG C of mill.
2. a kind of auto pump caulking gum according to claim 1, be made up of following raw materials in part by weight: acrylic elastomer 59, trifluoropropyl siloxane rubber 14, chlorohydrin rubber T3100 13, american exxon brominated butyl rubber 2,211 14, high abrasion furnace carbon black N330 32, precipitated silica 22, light calcium carbonate 5, wollastonite powder 6, Zirconium tetrafluoride 4, barium sulfate 6, molybdenumdisulphide 4, Modified Iron mine tailing ground-slag 10, vulcanizing agent DCBP1.5, anti-aging agent TPPD 1.2, vulkacit H 0.8, magnesium oxide 5, 2-thiol group benzimidazolyl 1.5, paraffin 1.5, sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester 1.5, acetyl tributyl citrate three (2-ethylhexyl) ester 18.
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CN101784749A (en) * | 2007-08-20 | 2010-07-21 | 国际壳牌研究有限公司 | Method of creating an annular seal around a tubular element |
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