CN101375027A - Method of improving an engine using a lubricating composition comprising a colloidal dispersion of a rare earth to catalyse the combustion of soot - Google Patents
Method of improving an engine using a lubricating composition comprising a colloidal dispersion of a rare earth to catalyse the combustion of soot Download PDFInfo
- Publication number
- CN101375027A CN101375027A CNA2007800039226A CN200780003922A CN101375027A CN 101375027 A CN101375027 A CN 101375027A CN A2007800039226 A CNA2007800039226 A CN A2007800039226A CN 200780003922 A CN200780003922 A CN 200780003922A CN 101375027 A CN101375027 A CN 101375027A
- Authority
- CN
- China
- Prior art keywords
- acid
- particle
- rare earth
- colloidal dispersion
- lubricating composition
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 42
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 39
- 238000001246 colloidal dispersion Methods 0.000 title claims abstract description 31
- 238000002485 combustion reaction Methods 0.000 title claims abstract description 8
- 230000001050 lubricating effect Effects 0.000 title claims description 35
- 150000002910 rare earth metals Chemical class 0.000 title abstract description 6
- 239000004071 soot Substances 0.000 title description 25
- 239000002245 particle Substances 0.000 claims abstract description 40
- 150000001875 compounds Chemical class 0.000 claims abstract description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 51
- 229910052684 Cerium Inorganic materials 0.000 claims description 28
- 239000003921 oil Substances 0.000 claims description 27
- 235000019198 oils Nutrition 0.000 claims description 27
- 229910052742 iron Inorganic materials 0.000 claims description 24
- 239000002253 acid Substances 0.000 claims description 11
- 239000003153 chemical reaction reagent Substances 0.000 claims description 11
- 125000004432 carbon atom Chemical group C* 0.000 claims description 9
- 239000000314 lubricant Substances 0.000 claims description 9
- 238000006555 catalytic reaction Methods 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000000446 fuel Substances 0.000 claims description 6
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 5
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 claims description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 4
- FBUKVWPVBMHYJY-UHFFFAOYSA-N nonanoic acid Chemical compound CCCCCCCCC(O)=O FBUKVWPVBMHYJY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002912 waste gas Substances 0.000 claims description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 3
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 3
- OBETXYAYXDNJHR-SSDOTTSWSA-M (2r)-2-ethylhexanoate Chemical compound CCCC[C@@H](CC)C([O-])=O OBETXYAYXDNJHR-SSDOTTSWSA-M 0.000 claims description 2
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 claims description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- LDMOEFOXLIZJOW-UHFFFAOYSA-N 1-dodecanesulfonic acid Chemical compound CCCCCCCCCCCCS(O)(=O)=O LDMOEFOXLIZJOW-UHFFFAOYSA-N 0.000 claims description 2
- LBLYYCQCTBFVLH-UHFFFAOYSA-N 2-Methylbenzenesulfonic acid Chemical compound CC1=CC=CC=C1S(O)(=O)=O LBLYYCQCTBFVLH-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 claims description 2
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 239000005639 Lauric acid Substances 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- JMKATISBVVWRSS-UHFFFAOYSA-N OP(O)=O.CC1=CC=CC=C1 Chemical class OP(O)=O.CC1=CC=CC=C1 JMKATISBVVWRSS-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- 150000007513 acids Chemical class 0.000 claims description 2
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- SVMUEEINWGBIPD-UHFFFAOYSA-N dodecylphosphonic acid Chemical class CCCCCCCCCCCCP(O)(O)=O SVMUEEINWGBIPD-UHFFFAOYSA-N 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 2
- 239000004519 grease Substances 0.000 claims description 2
- SSILHZFTFWOUJR-UHFFFAOYSA-N hexadecane-1-sulfonic acid Chemical compound CCCCCCCCCCCCCCCCS(O)(=O)=O SSILHZFTFWOUJR-UHFFFAOYSA-N 0.000 claims description 2
- JDPSFRXPDJVJMV-UHFFFAOYSA-N hexadecylphosphonic acid Chemical class CCCCCCCCCCCCCCCCP(O)(O)=O JDPSFRXPDJVJMV-UHFFFAOYSA-N 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- 235000021313 oleic acid Nutrition 0.000 claims description 2
- 235000012424 soybean oil Nutrition 0.000 claims description 2
- 239000003549 soybean oil Substances 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- 239000003784 tall oil Substances 0.000 claims description 2
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 claims description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 2
- 150000001735 carboxylic acids Chemical class 0.000 claims 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims 1
- 239000006185 dispersion Substances 0.000 abstract description 22
- 238000002156 mixing Methods 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 239000010687 lubricating oil Substances 0.000 abstract 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 27
- -1 rare-earth compound Chemical class 0.000 description 14
- 239000000654 additive Substances 0.000 description 12
- 208000035126 Facies Diseases 0.000 description 10
- 230000000996 additive effect Effects 0.000 description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 239000002199 base oil Substances 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 5
- 239000006229 carbon black Substances 0.000 description 5
- 235000019241 carbon black Nutrition 0.000 description 5
- 125000000219 ethylidene group Chemical group [H]C(=[*])C([H])([H])[H] 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 235000021317 phosphate Nutrition 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 238000004627 transmission electron microscopy Methods 0.000 description 5
- XDOFQFKRPWOURC-UHFFFAOYSA-N 16-methylheptadecanoic acid Chemical group CC(C)CCCCCCCCCCCCCCC(O)=O XDOFQFKRPWOURC-UHFFFAOYSA-N 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 4
- 125000001931 aliphatic group Chemical group 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 4
- 150000002148 esters Chemical group 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- 239000003209 petroleum derivative Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Chemical group 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000002480 mineral oil Substances 0.000 description 3
- 235000010446 mineral oil Nutrition 0.000 description 3
- 239000010705 motor oil Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
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- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
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- 239000003085 diluting agent Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- NAGJZTKCGNOGPW-UHFFFAOYSA-N dithiophosphoric acid Chemical class OP(O)(S)=S NAGJZTKCGNOGPW-UHFFFAOYSA-N 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- SQNZJJAZBFDUTD-UHFFFAOYSA-N durene Chemical compound CC1=CC(C)=C(C)C=C1C SQNZJJAZBFDUTD-UHFFFAOYSA-N 0.000 description 1
- ODLMAHJVESYWTB-UHFFFAOYSA-N ethylmethylbenzene Natural products CCCC1=CC=CC=C1 ODLMAHJVESYWTB-UHFFFAOYSA-N 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- IPCSVZSSVZVIGE-UHFFFAOYSA-M hexadecanoate Chemical compound CCCCCCCCCCCCCCCC([O-])=O IPCSVZSSVZVIGE-UHFFFAOYSA-M 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 125000001183 hydrocarbyl group Chemical group 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- SHOJXDKTYKFBRD-UHFFFAOYSA-N mesityl oxide Natural products CC(C)=CC(C)=O SHOJXDKTYKFBRD-UHFFFAOYSA-N 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- ZCYXXKJEDCHMGH-UHFFFAOYSA-N nonane Chemical compound CCCC[CH]CCCC ZCYXXKJEDCHMGH-UHFFFAOYSA-N 0.000 description 1
- BKIMMITUMNQMOS-UHFFFAOYSA-N normal nonane Natural products CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000008041 oiling agent Substances 0.000 description 1
- 125000001117 oleyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])/C([H])=C([H])\C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229940107700 pyruvic acid Drugs 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- WTGQALLALWYDJH-WYHSTMEOSA-N scopolamine hydrobromide Chemical compound Br.C1([C@@H](CO)C(=O)OC2C[C@@H]3N([C@H](C2)[C@@H]2[C@H]3O2)C)=CC=CC=C1 WTGQALLALWYDJH-WYHSTMEOSA-N 0.000 description 1
- 150000003333 secondary alcohols Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Chemical group 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-N sulfonic acid Chemical compound OS(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-N 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
- F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
- F01N3/023—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters using means for regenerating the filters, e.g. by burning trapped particles
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M141/00—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
- C10M141/02—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic oxygen-containing compound
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M141/00—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
- C10M141/08—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic sulfur-, selenium- or tellurium-containing compound
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M141/00—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
- C10M141/10—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic phosphorus-containing compound
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/02—Well-defined aliphatic compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/02—Well-defined aliphatic compounds
- C10M2203/022—Well-defined aliphatic compounds saturated
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/06—Well-defined aromatic compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/102—Aliphatic fractions
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/104—Aromatic fractions
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/04—Phosphate esters
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/06—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having phosphorus-to-carbon bonds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2225/00—Organic macromolecular compounds containing phosphorus as ingredients in lubricant compositions
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2010/00—Metal present as such or in compounds
- C10N2010/06—Groups 3 or 13
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2010/00—Metal present as such or in compounds
- C10N2010/14—Group 7
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2010/00—Metal present as such or in compounds
- C10N2010/16—Groups 8, 9, or 10
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/38—Catalyst protection, e.g. in exhaust gas converters
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/50—Emission or smoke controlling properties
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/01—Emulsions, colloids, or micelles
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Lubricants (AREA)
- Lubrication Of Internal Combustion Engines (AREA)
Abstract
The invention relates to a method of improving an engine equipped with an exhaust line fitted with a particulate filter, in which the particulates contained in the exhaust gas are trapped on said filter, and the trapped particulates are periodically burnt off, which method is characterized in that, for the purpose of catalysing the combustion of said particles, a composition resulting from mixing a lubricating oil with a colloidal dispersion is used as engine-lubricating composition, which dispersion comprises particles of a compound of at least one rare earth and an amphiphilic agent.
Description
Technical field
The present invention relates to use the operation method of the motor of the lubricating composition catalysed soot burning that comprises the rare earth elements colloidal dispersion.
Background technique
Be known that in the process that diesel fuel (gazole) burns in diesel engine carbonaceous products has the trend that forms soot, soot it is said to environment and all harmful to health.For a long time in the technology of the discharging of seeking to reduce these soots or carbonaceous particles.Petrol engine (poor burn engine) for the operation under poor combustion pattern (m é lange pauvre) of itself also discharging this class particle also faces same problem.
At present widely used a kind of gratifying solution is in regular regeneration in case collecting granules on the plugged sereen.When soot spontaneous ignition temperature low (this can obtain by in combustion process catalyzer being introduced the soot center), can promote the regeneration of filter more.This technology of " Fuel Borne Catalysis (fuel combustion catalysis) " by name or FBC also is extensive use of.The soot that has so added additive has low to the spontaneous ignition temperature that is enough in the motor normal course of operation or frequently reaches in the cycle in specific regeneration.
Although the FBC technology is gratifying, but still need other alternative technologies so that can have the solution of as far as possible wide range and can solve the problem that reduces the deleterious particle discharging thus, and the condition that faces regardless of this problem.
Summary of the invention
Therefore purpose of the present invention provides a kind of such new technique.
For this reason, the present invention relates to produce the waste gas that contains particle and be furnished with the operation method of motor of the muffler (pot d ' é chappement) of band particulate filter, wherein on described filter, capture particle, and regularly carry out the burning of the particle that captured, the method is characterized in that, for the burning of the described particle of catalysis, use composition that the mixture by following material obtains lubricating composition as motor:
-lubricant oil;
-comprise the particle of compound of at least a rare earth elements and the colloidal dispersion of amphiphilic reagent.
With the method for using the FBC technology different, the advantage of method of the present invention has been to eliminate specific reservoir that the soot burnt catalyzer uses and the existence that this catalyzer is metered into the device in the fuel.
Reading following description and be used for its various concrete of illustration but after the non-limiting example, can more completely find out further feature of the present invention, details and advantage.
It is element in the group that element constituted of 57 to 71 (comprising 57 and 71) that term " rare earth elements " is understood to mean by yttrium, scandium and cycle atom ordinal number in this manual.
Composition of the present invention is available from the mixture of two kinds of solvents: lubricant oil and colloidal dispersion.
Lubricant oil is well known to a person skilled in the art.Can reaffirm that these products contain the base oil with lubricating property.This base oil can be derived from oil, especially based on the mineral oil of the mixture of paraffin, aromatic hydrocarbons or isoparaffin and these compounds.Mineral oil can obtain by the vacuum distillation of crude oil, and hydrocrack, hydrotreatment and dewaxing subsequently subsequently of gained distillate and/or hydroisomerization are to improve the character as viscosity and flowability and so on of thus obtained base oil.
These base oils also can be based on the artificial oil of polyalphaolefin or organic ester.
The viscosity index of mineral oil can be for example 90 to 100 (index that records according to ASTM D2270 standard), the hydrotreatment product be 120 to 130, for the artificial oil based on polyalphaolefin, this index can be higher than 140, for based on those of organic ester, even can reach 200.
Equally in a known way; lubricant oil contains the different additive that can be divided into three classes in addition: the additive that is used to improve the chemical stability of oil or suppresses the influence of degradation product; improve the additive and the protective money metal surface of the rheological equationm of state and have the additive of wear-resistant effect.
For example comprise in the first kind based on phenol, based on substituted aromatic amines or based on sulfur-containing compound or based on the anti-oxidant additives of zinc dialkyl dithiophosphate.Also comprise acylate or phenol or divalent metal Orvus Gardinol additive and organic surface active agent type dispersant additives.
The second class additive is those of pour point that act on oil, and for having the oligomer types of alkyl chain or the product of so-called Fluhyzon type, long-chain polyalcohols acrylate or alkylation polystyrene type antifreezing solution.Also comprise the additive that improves viscosity index in second class.These additives are based on hydrocarbyl polymers (for example ethylene/propene copolymer) or based on the polymer with ester functional group (polymethacrylate type).At last, also comprise anti-foam product in the second class additive, for example based on organosilicon.
The 3rd class additive comprises the product with wear-resistant effect.These are the organic products of sulfur-bearing, chlorine or the phosphorus of phosphordithiic acid derivative or phosphomolybdate derivative type normally.
Second solvent of composition of the present invention is a colloidal dispersion.
Term " colloidal dispersion " is meant any system that is suspended in the liquid phase to be constituted by the fine solid particles based on the colloid size of rare-earth compound in this manual, described particle may be chosen bonding or the adion that contains residual quantity, for example nitrate anion, acetate, citrate or ammonium in addition wantonly.Term " colloid size " is understood to mean the size of about 1 nanometer to about 500 nanometers.Particle is more special to have about 250 nanometers at most, especially maximum 100 nanometers, preferred maximum 20 nanometers, the average-size of more preferably maximum 15 nanometers.It is to be noted that in this class dispersion, rare-earth compound can preferably be entirely colloidal form, or be that colloidal form and part are ionic species.
Unless indicate separately, above the size distribution of mentioning with this specification remainder is by traditionally to dry and be deposited on the transmission electron microscopy (TEM) that the sample on the carbon film that loads on the copper grid carries out and measure in advance.
Rare earth elements can more particularly be selected from cerium, lanthanum, yttrium, neodymium, gadolinium and praseodymium.The most special selection cerium.
According to first version of the present invention, colloidal dispersion is characterised in that this dispersion comprises the particle of the compound of cerium and other rare earth elements.
According to another version, colloidal dispersion of the present invention is characterised in that, this dispersion comprises the particle based on the compound of cerium, optional other rare earth elements and iron.
More particularly; when the particle of dispersion of the present invention during based on the compound of several elements (being cerium, other rare earth elements and/or iron); these elements are blended in each particle, and these elements are generally the form of mixed oxide and/or hydration mixed oxide (oxyhydroxide).
Under the situation of the colloidal dispersion of cerium, this element preferably is mainly the form of cerium IV.For example, with respect to cerium IV, the content of cerium III (content of representing by the total Ce atomic ratio of CeIII/) is generally maximum 40%.Therefore it can become with the specific embodiments of used dispersion and can be into maximum 20%, and is maximum more especially 10%, and more maximum more especially 1%.
Under the situation of above-mentioned first version, the rare earth elements beyond the cerium is lanthanum or praseodymium more especially.Certainly, the present invention includes the situation of compound that particle wherein is several other rare earth elementss of cerium and combination.
With respect in the cerium of oxide and the total mole number of rare earth elements, the ratio of the rare earth elements beyond the cerium is preferably at least 10 moles of %, more special at least 20 moles of %, maximum more especially again 50 moles of %.
Under the situation of second version, it is maximum 50% that the ratio of cerium is preferably, maximum more especially 20%, maximum more especially again 10%, and this ratio is with cerium oxide CeO
2Molal quantity with respect to cerium oxide and iron oxide Fe
2O
3Total moles is represented.
These two kinds of versions can be combined, and that is to say, particle can be the compound of cerium, at least a other rare earth elements and iron.
As mentioned above, the particle of colloidal dispersion is suspended in the liquid phase, and this liquid phase is an organic facies at this.
This organic facies can be made of above-mentioned base oil with lubricating property, or its also can be this base oil and with the mixture of miscible another organic facies of this oil.Find out that particularly and subsequently lubricating composition of the present invention can obtain by lubricant oil is mixed with ready-made colloidal dispersion.In this case, it can be hydrocarbon that this dispersion comprises, more especially the organic facies of non-polar hydrocarbon.
As the example of organic facies, can mention aliphatic hydrocarbon, for example hexane, heptane, octane, nonane, inertia clicyclic hydrocarbon, for example cyclohexane, cyclopentane, cycloheptane, aromatic hydrocarbons, for example benzene, toluene, ethylo benzene, dimethylbenzene, liquid ring alkane.Same suitable is Isopar or Solvesso type (trade mark of EXXON company) petroleum distillate, especially mainly the Solvesso 100 that contains the mixture of ethyl methyl benzene and trimethylbenzene, contain alkylbenzene, the Solvesso 150 of the mixture of dimethyl benzene and durol and mainly contain C-11 and the Isopar of C-12 isoparaffin and cycloalkane particularly.As other petroleum distillate, also can mention from Petrolink company
Type petroleum distillate or from Total company
The type petroleum distillate.
For organic facies, also can use chlorinated hydrocabon, for example chlorobenzene or dichlorobenzene, or chlorotoluene.Can consider ether and aliphatic series and alicyclic ketone, for example Di Iso Propyl Ether, dibutyl ethers, MEK, methyl iso-butyl ketone (MIBK), DIBK and Mesityl oxide.
Can consider ester, but they has the shortcoming of possibility hydrolysis.As the ester of energy usefulness, can mention those that make by the acid and the reaction of C1 to C8 alcohol, especially the palmitate of secondary alcohol such as isopropanol.For example, can mention butyl acetate.
Certainly, organic facies can be based on the mixture of the compound of two or more hydrocarbon or the above-mentioned type.
At last, as mentioned above, from the example that has just provided, select organic facies according to the compatibility or the compatibility of itself and lubricant oil.
In addition, colloidal dispersion comprises amphiphilic reagent.
This amphiphilic reagent to small part interacts via grafting or via the particle of the compound of electrostatic bonding and rare earth elements and optional iron.
This reagent is acid more especially.
More special being selected from of acid comprises at least 6 carbon atoms, more special 10 to 60 carbon atoms, preferred 10 to 50 carbon atoms, the more preferably organic acid of 15 to 25 carbon atoms.
These acid can be straight or brancheds.They can be aryl, aliphatic series or aryl aliphatic acid, and optional other functional group that has needs only these functional groups and stablizes in medium (need use dispersion of the present invention in this medium).Thus, can for example use to have about 10 aliphatic carboxylic acids to about 40 carbon atoms, aliphatic sulfonic acid, aliphatic phosphonic acids, alkylaryl phosphonic acids and alkyl aryl sulphonic acid, they are natural or synthetic.Certainly use the acid of form of mixtures.
Also can use its carbon back chain to have the carboxylic acid of ketone, for example pyruvic acid that is replaced by ketone at alpha position.These also can be alpha-halogen-carboxylic acid or alpha-hydroxy carboxylic acid compounds.The chain that is connected on the carboxyl can have degree of unsaturation.This chain can be interrupted by ether or ester functional group, as long as it is excessively not impaired to have the lipophilicity of chain of carboxyl.
For example, can mention the fatty acid of tall oil, soybean oil, grease (suif), lax seed oil, oleic acid, linoleic acid, stearic acid and isomer thereof, n-nonanoic acid, capric acid, lauric acid, myristic acid, DBSA, 2 ethyl hexanoic acid, aphthenic acids, caproic acid, toluenesulfonic acid, toluene phosphonic acids, lauryl sulfonic acid, lauryl phosphonic acids, palmityl sulfonic acid and palmityl phosphonic acids.
As amphiphilic reagent, also can mention polyoxyethylene alkyl ether phosphate.These are understood that it is the organic phosphate of following formula at this:
Or the polyoxygenated ethylene alkylphosphonic of following formula:
Wherein:
■ R
1, R
2, R
3Identical or different, representative especially has the straight or branched alkyl of 2 to 20 carbon atoms; Phenyl; Alkylaryl is more particularly alkyl phenyl, especially has the alkyl chain with 8 to 12 carbon atoms; Aryl alkyl is more particularly the phenyl aryl;
■ n is an oxidation ethylidene number, for example can be 0 to 12; And
■ M represents hydrogen, sodium or potassium atom.
Radicals R
1Especially can be hexyl, octyl group, decyl, dodecyl, oleyl, nonyl phenyl.
As the example of this type of amphipathic compound, can mention Rhodia with trade mark
With
Those that sell, especially following products:
-
RA 600 polyoxygenated ethylidene (C8-C10) alkyl ether phosphates;
-
RS 710 or RS 410 polyoxygenated ethylidene tridecyl ether phosphates;
-
PA 35 polyoxygenated ethylidene oil cetyl (ol é oc é tyl) ether phosphate;
-
PA 17 polyoxygenated ethylidene nonylplenyl ether phosphate esters; With
-
RE 610 polyoxygenated ethylidene (branching) nonyl ethers phosphate esters.
The amount of the amphiphilic reagent that exists in the dispersion can be determined by molar ratio r:
The molal quantity of the molal quantity of r=amphiphilic reagent/E compound
E is meant the summation of these one or more rare earth elementss or one or more rare earth elementss and iron at this.
This molar ratio can be 0.2-1, preferred 0.4-0.8.
Available in the method for the invention dispersion can present according to a kind of particular.
According to this embodiment, dispersion makes that at least 90% particle is a single crystal grain.Term " monocrystalline " particle is understood to mean and looks like particle individual and that be made of single crystallite when checking dispersion by TEM (high-resolution transmission electron microscopy).
Also can use cryogenic refrigeration TEM technology to measure the state of aggregation of basic granules.This technology can be observed via transmission electron microscopy (TEM) and keep freezing sample in its natural medium, and this medium is water or organic diluent, for example aromatics or aliphatic solvents, for example Solvesso and Isopar or some alcohol, for example ethanol.
For aqueous sample, in liquid ethane, or, in liquid nitrogen, on the film of about 50 to 100 nanometer thickness, carry out freezing for other sample.
By cryogenic refrigeration TEM, keep the dispersed state of particle well, and represent the state that in real medium, exists.
According to this embodiment, particle has thin and narrow size distribution.This is because they have 1 to 5 nanometer, the d of preferred 2 to 3 nanometers
50
Usually and only as an example, the concentration of the dispersion of rare earth elements and optional iron is one or more rare earth oxides or one or more rare earth oxides and the ferriferous oxide Fe of 1 to 40 weight %
2O
3, with respect to the gross weight meter of dispersion.
At last, for the colloidal dispersion and the preparation thereof of the compound of rare earth elements, optional rare earth metal and iron, usually and as an example, can be with reference to patent application EP 0 671 205, WO01/10545 and WO 97/19022 whole description separately.
Lubricating composition available in the method for the present invention can prepare by lubricant oil is mixed with the colloidal dispersion of the compound of rare-earth compound or rare earth elements and iron.The ratio of this mixing is inessential and can change in wide range.For example, these ratios can be so that be maximum 15 quality % of total composition in the rare earth elements from colloidal dispersion of metallic element, optional rare earth elements and the content of iron in lubricating composition, maximum more especially 10%, only the ratio of a few percent is possible.
According to observations, so the composition that obtains is stable, that is to say, does not observe the sedimentation of dispersion, therefore, does not have the deposition of cerium or iron particle in the bottom of the reservoir that contains lubricating composition.In addition, even lubricating composition exposes at high temperature (this is to use said composition as the situation in the engine operation process of oiling agent), also keep this stability.In addition, unexpectedly observe, this composition is in the use burning of catalysed soot beyond the question of engine operation.
Method of the present invention is applicable to such motor, and this motor can produce the deleterious particle that is present in the waste gas, for example soot in its running.It is diesel engine or with the petrol engine of poor combustion mode operation more especially.
This method is applicable to the motor of being furnished with outlet pipe or muffler in a known way, has integrated particulate filter in this outlet pipe or muffler.Traditionally, this filter comprises the filter of the type with filter wall of being made by pottery or made by silicon carbide, and waste gas circulation is by this filter wall.But it also can be one or more sieves of being made by metallic sieve or the foam type filter being made or made by lamination coating by pottery.
The particle that method of the present invention is intended to capture on the catalysed particulate filter or the burning of soot.Within the scope of the invention, use the catalyzer of the compound of rare earth elements or iron and rare earth elements as these soot burnt, and its carry by lubricating composition rather than in the method for prior art carry by fuel.For example in (vidange) process of changing oil, introduce this lubricating composition in engine oil tank, this lubricating composition prepared and therefore comprises the dispersion of rare earth elements or iron and rare earth elements before it is used in the motor.Lubricating composition passes through in the lubricated circuit of motor thus.According to observations, the compound of the rare earth elements of being introduced by lubricating composition or rare earth elements and iron is found in soot and therefore helps its burning of catalysis.
Certainly, can under the situation that does not deviate from scope of the present invention, when using the operating fuel motor that also contains the soot burnt catalyzer, implement said method.This catalyzer also can be aforesaid colloidal dispersion.Can be similarly in being furnished with the system of particulate filter of catalysis, muffler implements method of the present invention.This filter is known, and it is a filter of introducing the oxidation catalyst of particle or soot in its manufacture process.
Embodiment
Provide embodiment now.
Embodiment 1
This embodiment relates to the preparation of available lubricating composition in the method for the invention.
For this preparation, use according to the method for embodiment's 4 described types of patent application EP 671205 but use 160 ℃ of autoclaves to handle the colloidal dispersion of making based on cerium.The organic facies of this dispersion is Isopar, and amphiphilic reagent is isostearic acid.The content of regulating used ceric nitrate is to obtain to contain the colloidal dispersion of 25 weight % metallic ceriums.Colloid has the average-size of 5 nanometers.
In this dispersion, add tank oil (Total Activa Diesel 10W40) to obtain to contain the lubricating composition of this tank oil of 43 weight % and 57 weight % colloidal dispersions.
Embodiment 2
This embodiment relates to the preparation of available second lubricating composition in the method for the invention.
For this preparation, using what make according to the method for embodiment's 3 described types of patent application WO 01/10545 is 50/50 the cerium and the colloidal dispersion of iron based on the metal molar ratio.The organic facies of this dispersion is Isopar, and amphiphilic reagent is isostearic acid.This dispersion contains 10 weight % metals (cerium and iron).Colloid has the size of 3 to 4 nanometers and is individual fully.
In this dispersion, add tank oil (Total Activa Diesel 10W40) to obtain to contain the lubricating composition of this tank oil of 28 weight % and 72 weight % colloidal dispersions.
Embodiment 3
This embodiment relates to the catalyzed oxidation test of the soot that carries out in the presence of available lubricating composition in the method for the invention.Measure the catalytic performance of soot oxidation by thermogravimetry.The Setaram thermobalance that use is furnished with quartz boat wherein is equipped with the sample that contains about 20 milligrams of samples.
Sample is made of from embodiment 1 the lubricating composition and the mixture of 80 weight % carbon blacks 20 weight %.The carbon black that is used to simulate the soot of diesel emission is the carbon black that Cabot company sells with label Elftex 125.With the mixture of lubricating composition and carbon black by mixing to come homogenizing with scraper.Thus obtained thickener is dry under 60 ℃ in draft furnace in advance, reaches 120 ℃ then.
20 milligrams of samples of making thus and handling are introduced in the boat of thermobalances, making then by volume ratio separately is 87% and 13% the circulation of air flow that air/water mixture constituted.150 ℃ down keep 30 minutes after, begin to heat up with 10 ℃/minute increasing degrees, and with the mass loss of thermograph sample until 900 ℃.
Embodiment 4
According to the program identical but use the lubricating composition described in the embodiment 2 to carry out this embodiment with embodiment 3.
The comparative example 5
This embodiment relates to the soot oxidation test of carrying out in the presence of the lubricating composition of prior art.The program that this experimental evidence is identical but use pure tank oil Total Activa Diesel10W40 to carry out.Therefore Ping Ce sample is made of pure tank oil of 20 weight % and 80 weight % carbon blacks thus.
The results are shown in the table 1: they are expressed as half oxidizing temperature (T50% (soot)) of soot, and it is corresponding to half required temperature of the mass loss of measuring between 200 ℃ to 900 ℃ for acquisition.
Table 1
| Embodiment | T50% (soot) ℃ |
| 3 | 510℃ |
| 4 | 515℃ |
| 5 contrasts | 610℃ |
| Independent soot | 620℃ |
Can see that the interpolation of pure tank oil does not have the half way around temperature of soot or almost not influence, and the use of lubricating composition that contains tank oil and contain the colloidal dispersion of cerium or cerium and iron can reduce the combustion temperature of soot very significantly.
Embodiment 6
In this embodiment, re-use from the colloidal dispersion of embodiment 2 cerium and iron and with this dispersion that 10 grams contain 10 quality % metallic ceriums and iron and add in the 160 gram engine oils (ElfPrestigrade 15W40) to obtain to contain the lubricating composition of 94 these tank oils of quality % and the commercial colloidal dispersion of 6 quality %.Therefore the metal Ferrum content of this lubricating composition is 0.20 weight %, and the content of metallic cerium is 0.45 weight %.
Then this lubricating composition is introduced in the container that partly clogs, this container itself is placed in the air bells chamber that keeps 110 ℃.Then via iron and the cerium content of chemometric techniques (ICP) in this container top periodic measurement said composition.
Following table 2 is given in the chamber at iron that records after the various waiting time under 110 ℃ and cerium content.
Table 2
| Heating time under 110 ℃ (fate) | Weight % cerium | Weight % iron |
| 0 | 0.45 | 0.20 |
| 1 | 0.45 | 0.20 |
| 3 | 0.45 | 0.20 |
| 6 | 0.45 | 0.20 |
| 10 | 0.45 | 0.20 |
| 13 | 0.45 | 0.20 |
| 17 | 0.45 | 0.20 |
| 28 | 0.45 | 0.20 |
| 38 | 0.45 | 0.20 |
| 55 | 0.45 | 0.20 |
| 79 | 0.45 | 0.20 |
Therefore can see that consider iron and cerium content through not changing 110 ℃ of continuous heating in following 79 days, the thermostability of this lubricating composition is very high.Can be considered to the stability of sufficient to guarantee lubricating composition between twice of engine oil path changed oil this stabilization time that records under these conditions.
Claims (12)
1. can produce the waste gas that contains particle and be furnished with the operation method of motor of the muffler of band particulate filter, wherein on described filter, capture particle, and regularly carry out the burning of the particle that captured, the method is characterized in that, for the burning of the described particle of catalysis, use composition that the mixture by following material obtains lubricating composition as motor:
-lubricant oil;
-comprise the particle of compound of at least a rare earth elements and the colloidal dispersion of amphiphilic reagent.
2. the method for claim 1 is characterized in that rare earth elements is selected from cerium, lanthanum, yttrium, neodymium, gadolinium, praseodymium.
3. method as claimed in claim 1 or 2 is characterized in that colloidal dispersion comprises the particle of the compound of iron and rare earth elements.
4. the described method of one of claim as described above is characterized in that amphiphilic reagent is acid.
5. method as claimed in claim 4 is characterized in that aforementioned acid is to comprise 10 to 60 carbon atoms, the carboxylic acid of more special 15 to 25 carbon atoms.
6. as claim 4 or 5 described methods, it is characterized in that described acid is selected from the fatty acid of tall oil, soybean oil, grease, lax seed oil, oleic acid, linoleic acid, stearic acid and isomer thereof, n-nonanoic acid, capric acid, lauric acid, myristic acid, DBSA, 2 ethyl hexanoic acid, aphthenic acids, caproic acid, toluenesulfonic acid, toluene phosphonic acids, lauryl sulfonic acid, lauryl phosphonic acids, palmityl sulfonic acid and palmityl phosphonic acids.
7. the described method of one of claim as described above is characterized in that colloidal dispersion comprises the particle of the compound of rare earth elements, and at least 90% is single crystal grain in these particles.
8. method as claimed in claim 7 is characterized in that particle has 1 to 5 nanometer, the d of preferred 2 to 3 nanometers
50Value.
9. the described method of one of claim as described above is characterized in that, is maximum 15 quality % of total composition in the rare earth elements from colloidal dispersion of metallic element, optional rare earth elements and the content of iron in lubricating composition.
10. the described method of one of claim as described above is characterized in that, uses the lubricating composition that comprises lubricant oil and colloidal dispersion, and this lubricating composition prepared before it uses in motor.
11. the described method of one of claim as described above is characterized in that motor is a diesel engine or with the petrol engine of poor combustion mode operation.
12. the described method of one of claim is characterized in that as described above, it is on the motor of operating fuel that contains the particle burning catalyzer or be furnished with on the motor of muffler of the particulate filter that comprises catalysis and implementing.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR0600838A FR2896824B1 (en) | 2006-01-30 | 2006-01-30 | METHOD OF OPERATING AN ENGINE USING A LUBRICATING COMPOSITION COMPRISING A COLLOIDAL DISPERSION OF A RARE EARTH FOR CATALYZING SOOT COMBUSTION |
| FR0600838 | 2006-01-30 | ||
| PCT/EP2007/050493 WO2007085561A1 (en) | 2006-01-30 | 2007-01-18 | Method of improving an engine using a lubricating composition comprising a colloidal dispersion of a rare earth to catalyse the combustion of soot |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101375027A true CN101375027A (en) | 2009-02-25 |
| CN101375027B CN101375027B (en) | 2011-09-07 |
Family
ID=36589232
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007800039226A Expired - Fee Related CN101375027B (en) | 2006-01-30 | 2007-01-18 | Method of improving an engine using a lubricating composition comprising a colloidal dispersion of a rare earth to catalyse the combustion of soot |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US20090241523A1 (en) |
| EP (1) | EP1989407B1 (en) |
| CN (1) | CN101375027B (en) |
| AT (1) | ATE462875T1 (en) |
| DE (1) | DE602007005615D1 (en) |
| ES (1) | ES2343759T3 (en) |
| FR (1) | FR2896824B1 (en) |
| WO (1) | WO2007085561A1 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108690688A (en) * | 2018-05-16 | 2018-10-23 | 上海金兆节能科技有限公司 | A kind of corrosion-resistant lubricating grease and preparation method thereof |
| CN108728225A (en) * | 2018-07-10 | 2018-11-02 | 上海金兆节能科技有限公司 | Health environment-friendly lubricating grease and preparation method thereof |
| CN108753412A (en) * | 2018-07-10 | 2018-11-06 | 上海金兆节能科技有限公司 | Environmentally friendly autonomous reparation micro lubricating oil and preparation method thereof |
| CN108893139A (en) * | 2018-08-01 | 2018-11-27 | 李成霞 | A kind of method of use amphipathic catalyst fuel desulfuration containing neodymium |
| CN109054926A (en) * | 2018-07-10 | 2018-12-21 | 上海金兆节能科技有限公司 | Health environment-friendly micro cutting liquid and preparation method thereof |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2853261B1 (en) * | 2003-04-04 | 2006-06-30 | Rhodia Elect & Catalysis | COLLOIDAL DISPERSION OF A RARE EARTH COMPOUND COMPRISING AN ANTI-OXIDANT AGENT AND ITS USE AS A GAS ADJUVANT FOR INTERNAL COMBUSTION ENGINES |
| US8741821B2 (en) | 2007-01-03 | 2014-06-03 | Afton Chemical Corporation | Nanoparticle additives and lubricant formulations containing the nanoparticle additives |
| FR2913431B1 (en) * | 2007-03-06 | 2009-04-24 | Rhodia Recherches & Tech | METHOD FOR OPERATING A DIESEL ENGINE TO FACILITATE THE REGENERATION OF A PARTICLE FILTER ON THE EXHAUST LINE |
| US8333945B2 (en) | 2011-02-17 | 2012-12-18 | Afton Chemical Corporation | Nanoparticle additives and lubricant formulations containing the nanoparticle additives |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3809307A1 (en) * | 1988-03-19 | 1989-09-28 | Veba Oel Ag | ENGINE LUBRICANE FOR DIESEL ENGINES AND METHOD FOR OPERATING A DIESEL ENGINE |
| DE3926817A1 (en) * | 1989-08-14 | 1991-02-21 | Miltiathis Markou | Lubricant contg. lubricating oil and rare earth element esp. cerium - used in internal combustion engines for reducing pollutant content in exhaust gases |
| DE4133137A1 (en) * | 1991-10-07 | 1992-04-23 | Bernd Fischer | Assisting oxidn. of particles in diesel engine - by addn. of catalytically supportive to lubricating oil |
| GB0126663D0 (en) * | 2001-11-06 | 2002-01-02 | Oxonica Ltd | Cerium oxide nanoparticles |
| FR2833862B1 (en) * | 2001-12-21 | 2004-10-15 | Rhodia Elect & Catalysis | ORGANIC COLLOIDAL DISPERSION OF IRON PARTICLES, PROCESS FOR PREPARING THE SAME, AND ITS USE AS A FUEL ADJUVANT FOR INTERNAL COMBUSTION ENGINES |
| US6892531B2 (en) * | 2003-04-02 | 2005-05-17 | Julius J. Rim | System for and methods of operating diesel engines to reduce harmful exhaust emissions and to improve engine lubrication |
| FR2853261B1 (en) * | 2003-04-04 | 2006-06-30 | Rhodia Elect & Catalysis | COLLOIDAL DISPERSION OF A RARE EARTH COMPOUND COMPRISING AN ANTI-OXIDANT AGENT AND ITS USE AS A GAS ADJUVANT FOR INTERNAL COMBUSTION ENGINES |
| US7615519B2 (en) * | 2004-07-19 | 2009-11-10 | Afton Chemical Corporation | Additives and lubricant formulations for improved antiwear properties |
-
2006
- 2006-01-30 FR FR0600838A patent/FR2896824B1/en not_active Expired - Fee Related
-
2007
- 2007-01-18 DE DE602007005615T patent/DE602007005615D1/en active Active
- 2007-01-18 ES ES07703988T patent/ES2343759T3/en active Active
- 2007-01-18 WO PCT/EP2007/050493 patent/WO2007085561A1/en active Application Filing
- 2007-01-18 US US12/162,585 patent/US20090241523A1/en not_active Abandoned
- 2007-01-18 EP EP07703988A patent/EP1989407B1/en not_active Not-in-force
- 2007-01-18 CN CN2007800039226A patent/CN101375027B/en not_active Expired - Fee Related
- 2007-01-18 AT AT07703988T patent/ATE462875T1/en not_active IP Right Cessation
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108690688A (en) * | 2018-05-16 | 2018-10-23 | 上海金兆节能科技有限公司 | A kind of corrosion-resistant lubricating grease and preparation method thereof |
| CN108728225A (en) * | 2018-07-10 | 2018-11-02 | 上海金兆节能科技有限公司 | Health environment-friendly lubricating grease and preparation method thereof |
| CN108753412A (en) * | 2018-07-10 | 2018-11-06 | 上海金兆节能科技有限公司 | Environmentally friendly autonomous reparation micro lubricating oil and preparation method thereof |
| CN109054926A (en) * | 2018-07-10 | 2018-12-21 | 上海金兆节能科技有限公司 | Health environment-friendly micro cutting liquid and preparation method thereof |
| CN108728225B (en) * | 2018-07-10 | 2020-08-11 | 江苏省健尔康医用敷料有限公司 | Lubricating grease and preparation method thereof |
| CN108893139A (en) * | 2018-08-01 | 2018-11-27 | 李成霞 | A kind of method of use amphipathic catalyst fuel desulfuration containing neodymium |
| CN108893139B (en) * | 2018-08-01 | 2020-12-04 | 嘉兴笼列电子商务有限公司 | Method for desulfurizing fuel oil by using amphiphilic catalyst containing neodymium |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101375027B (en) | 2011-09-07 |
| ATE462875T1 (en) | 2010-04-15 |
| EP1989407B1 (en) | 2010-03-31 |
| FR2896824B1 (en) | 2008-03-07 |
| DE602007005615D1 (en) | 2010-05-12 |
| FR2896824A1 (en) | 2007-08-03 |
| EP1989407A1 (en) | 2008-11-12 |
| WO2007085561A1 (en) | 2007-08-02 |
| ES2343759T3 (en) | 2010-08-09 |
| US20090241523A1 (en) | 2009-10-01 |
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