CN1056155C - 齐格勒-纳塔型催化剂体系、制备方法及其用途 - Google Patents
齐格勒-纳塔型催化剂体系、制备方法及其用途 Download PDFInfo
- Publication number
- CN1056155C CN1056155C CN96113267A CN96113267A CN1056155C CN 1056155 C CN1056155 C CN 1056155C CN 96113267 A CN96113267 A CN 96113267A CN 96113267 A CN96113267 A CN 96113267A CN 1056155 C CN1056155 C CN 1056155C
- Authority
- CN
- China
- Prior art keywords
- catalyst system
- compound
- passage
- silicon gel
- space
- 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.)
- Expired - Fee Related
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title description 12
- 239000007787 solid Substances 0.000 claims abstract description 43
- 150000001875 compounds Chemical class 0.000 claims abstract description 31
- 239000002245 particle Substances 0.000 claims abstract description 30
- 239000010936 titanium Substances 0.000 claims abstract description 29
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 26
- 150000002681 magnesium compounds Chemical class 0.000 claims abstract description 10
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 5
- 150000002367 halogens Chemical class 0.000 claims abstract description 5
- 150000003609 titanium compounds Chemical class 0.000 claims abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 25
- 229910052710 silicon Inorganic materials 0.000 claims description 25
- 239000010703 silicon Substances 0.000 claims description 25
- 238000006116 polymerization reaction Methods 0.000 claims description 16
- 239000004615 ingredient Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 15
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 14
- 229920001155 polypropylene Polymers 0.000 claims description 10
- 239000011954 Ziegler–Natta catalyst Substances 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 5
- 125000000753 cycloalkyl group Chemical group 0.000 claims description 3
- 125000006737 (C6-C20) arylalkyl group Chemical group 0.000 claims description 2
- 239000004480 active ingredient Substances 0.000 claims description 2
- 150000001399 aluminium compounds Chemical class 0.000 claims description 2
- 125000003710 aryl alkyl group Chemical group 0.000 claims description 2
- 150000001721 carbon Chemical group 0.000 claims description 2
- 125000005234 alkyl aluminium group Chemical group 0.000 claims 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims 1
- -1 aluminum compound Chemical class 0.000 abstract description 21
- 229910052782 aluminium Inorganic materials 0.000 abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000741 silica gel Substances 0.000 abstract description 7
- 229910002027 silica gel Inorganic materials 0.000 abstract description 7
- 125000003262 carboxylic acid ester group Chemical class [H]C([H])([*:2])OC(=O)C([H])([H])[*:1] 0.000 abstract 1
- 239000011164 primary particle Substances 0.000 abstract 1
- 239000000499 gel Substances 0.000 description 21
- 239000000126 substance Substances 0.000 description 16
- 239000000843 powder Substances 0.000 description 14
- 239000011777 magnesium Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 239000000203 mixture Substances 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 229910052749 magnesium Inorganic materials 0.000 description 11
- 239000011148 porous material Substances 0.000 description 10
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 8
- 239000000460 chlorine Substances 0.000 description 8
- 125000001891 dimethoxy group Chemical group [H]C([H])([H])O* 0.000 description 8
- 239000000155 melt Substances 0.000 description 8
- IMNFDUFMRHMDMM-UHFFFAOYSA-N n-heptane Substances CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 7
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 6
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 238000012685 gas phase polymerization Methods 0.000 description 5
- 238000012725 vapour phase polymerization Methods 0.000 description 5
- 239000008096 xylene Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 150000001733 carboxylic acid esters Chemical class 0.000 description 4
- 229910052801 chlorine Inorganic materials 0.000 description 4
- 239000012442 inert solvent Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000012265 solid product Substances 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000004453 electron probe microanalysis Methods 0.000 description 3
- 150000002170 ethers Chemical class 0.000 description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 150000002576 ketones Chemical class 0.000 description 3
- 150000002596 lactones Chemical class 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 150000001244 carboxylic acid anhydrides Chemical class 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- IRRVTIDUSZWLNF-UHFFFAOYSA-N cyclopentylsilane Chemical compound [SiH3]C1CCCC1 IRRVTIDUSZWLNF-UHFFFAOYSA-N 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229920001519 homopolymer Polymers 0.000 description 2
- 239000000017 hydrogel Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 150000002901 organomagnesium compounds Chemical class 0.000 description 2
- FGTYTUFKXYPTML-UHFFFAOYSA-N 2-benzoylbenzoic acid Chemical class OC(=O)C1=CC=CC=C1C(=O)C1=CC=CC=C1 FGTYTUFKXYPTML-UHFFFAOYSA-N 0.000 description 1
- 229910000951 Aluminide Inorganic materials 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 125000005055 alkyl alkoxy group Chemical group 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229920005601 base polymer Polymers 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- NVHCKYSIRWGHRB-UHFFFAOYSA-N butan-2-yl-dimethoxy-(2-methylpropyl)silane Chemical compound CCC(C)[Si](OC)(OC)CC(C)C NVHCKYSIRWGHRB-UHFFFAOYSA-N 0.000 description 1
- 125000004106 butoxy group Chemical group [*]OC([H])([H])C([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- MYBJXSAXGLILJD-UHFFFAOYSA-N diethyl(methyl)alumane Chemical compound CC[Al](C)CC MYBJXSAXGLILJD-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- NHYFIJRXGOQNFS-UHFFFAOYSA-N dimethoxy-bis(2-methylpropyl)silane Chemical compound CC(C)C[Si](OC)(CC(C)C)OC NHYFIJRXGOQNFS-UHFFFAOYSA-N 0.000 description 1
- VHPUZTHRFWIGAW-UHFFFAOYSA-N dimethoxy-di(propan-2-yl)silane Chemical compound CO[Si](OC)(C(C)C)C(C)C VHPUZTHRFWIGAW-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910000039 hydrogen halide Inorganic materials 0.000 description 1
- 239000012433 hydrogen halide Substances 0.000 description 1
- 150000002680 magnesium Chemical class 0.000 description 1
- 235000011147 magnesium chloride Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 150000003021 phthalic acid derivatives Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F10/00—Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Transition And Organic Metals Composition Catalysts For Addition Polymerization (AREA)
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19529240A DE19529240A1 (de) | 1995-08-09 | 1995-08-09 | Katalysatorsysteme vom Typ der Ziegler-Natta-Katalysatoren |
| DE19529240.5 | 1995-08-09 | ||
| DE19545497.9 | 1995-12-06 | ||
| DE1995145497 DE19545497A1 (de) | 1995-12-06 | 1995-12-06 | Verbesserte Propylenhomopolymerisate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1152580A CN1152580A (zh) | 1997-06-25 |
| CN1056155C true CN1056155C (zh) | 2000-09-06 |
Family
ID=26017556
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96113267A Expired - Fee Related CN1056155C (zh) | 1995-08-09 | 1996-08-08 | 齐格勒-纳塔型催化剂体系、制备方法及其用途 |
Country Status (9)
| Country | Link |
|---|---|
| EP (1) | EP0761696B1 (enExample) |
| JP (1) | JPH09110916A (enExample) |
| CN (1) | CN1056155C (enExample) |
| AR (1) | AR003227A1 (enExample) |
| AT (1) | ATE164598T1 (enExample) |
| AU (1) | AU708459B2 (enExample) |
| DE (1) | DE59600133D1 (enExample) |
| ES (1) | ES2114335T3 (enExample) |
| TW (1) | TW367337B (enExample) |
Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19545499A1 (de) * | 1995-12-06 | 1997-06-12 | Basf Ag | Verbesserte statistische Propylencopolymerisate |
| DE69717440T2 (de) | 1996-06-21 | 2003-10-02 | W.R. Grace & Co.-Conn., New York | Aggregatträger und darauf angebrachte olefinpolymerisationskatalysatoren |
| DE19637367A1 (de) * | 1996-09-13 | 1998-03-19 | Basf Ag | Bei ihrer Herstellung modifizierte Ziegler-Natta-Katalysatorsysteme |
| DE19710761A1 (de) * | 1997-03-14 | 1998-09-17 | Basf Ag | Hochkristalline Propylenhomopolymerisate |
| DE19722569A1 (de) | 1997-05-28 | 1998-12-03 | Basf Ag | Statistische Propylencopolymerisate |
| DE19728141A1 (de) * | 1997-07-02 | 1999-01-07 | Basf Ag | Verfahren zur Polymerisation von C2-C8-Alk-1-enen mittels eines Ziegler-Natta-Katalysatorsystems |
| US7022795B1 (en) | 1998-03-13 | 2006-04-04 | Novolen Technology Holdings, C.V. | Highly crystalline propylene homopolymers |
| US6313061B1 (en) | 1998-12-22 | 2001-11-06 | W. R. Grace & Co.-Conn. | Method of making frangible spray dried agglomerated supports and olefin polymerization catalysts supported thereon |
| DE10002653A1 (de) * | 2000-01-21 | 2001-07-26 | Targor Gmbh | Neuartige Katalysatorsysteme vom Typ der Ziegler-Natta-Katalysatoren |
| EP1336625A1 (en) | 2002-02-14 | 2003-08-20 | Novolen Technology Holdings C.V. | Solid catalytic component and catalytic system of the Ziegler-Natta type, process for their preparation and their use in the polymerisation of alk-1-enes |
| DE10306893A1 (de) | 2003-02-18 | 2004-08-26 | Basf Ag | Verfahren zur Hydrophobierung von textilen Materialien |
| DE102004025368A1 (de) | 2004-05-19 | 2005-12-08 | Basf Ag | Verfahren zur Herstellung von strukturierten Oberflächen |
| US7329626B2 (en) | 2004-09-07 | 2008-02-12 | Lummus Novolen Technology Gmbh | Ziegler-Natta catalyst, preparation, and use for the polymerization of alkenes |
| JP2007297371A (ja) * | 2006-04-07 | 2007-11-15 | Colcoat Kk | ジアルコキシマグネシウム粒状物、その合成及び利用 |
| CN111094362B (zh) * | 2017-09-15 | 2021-04-16 | 巴塞尔聚烯烃意大利有限公司 | 用于烯烃聚合的催化剂组分的制备方法 |
| CN114957519A (zh) * | 2022-07-19 | 2022-08-30 | 吉化集团吉林市天龙催化剂有限公司 | 固体钛系催化剂、制备方法及用于丙烯聚合的催化剂组分 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2001043A (en) * | 1977-07-18 | 1979-01-24 | Stamicarbon | Process of preparing a porous pure silica |
| EP0243165A2 (en) * | 1986-04-24 | 1987-10-28 | Unilever Plc | Porous silica structures |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02293314A (ja) * | 1989-05-01 | 1990-12-04 | Mitsubishi Kasei Corp | 粒子凝集体及びその製造法 |
| US5661097A (en) * | 1994-08-12 | 1997-08-26 | The Dow Chemical Company | Supported olefin polymerization catalyst |
-
1996
- 1996-08-01 DE DE59600133T patent/DE59600133D1/de not_active Revoked
- 1996-08-01 EP EP96112429A patent/EP0761696B1/de not_active Revoked
- 1996-08-01 AT AT96112429T patent/ATE164598T1/de not_active IP Right Cessation
- 1996-08-01 ES ES96112429T patent/ES2114335T3/es not_active Expired - Lifetime
- 1996-08-06 TW TW085109534A patent/TW367337B/zh active
- 1996-08-07 AU AU61958/96A patent/AU708459B2/en not_active Ceased
- 1996-08-08 CN CN96113267A patent/CN1056155C/zh not_active Expired - Fee Related
- 1996-08-09 JP JP8210863A patent/JPH09110916A/ja active Pending
- 1996-09-08 AR ARP960103936A patent/AR003227A1/es unknown
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2001043A (en) * | 1977-07-18 | 1979-01-24 | Stamicarbon | Process of preparing a porous pure silica |
| EP0243165A2 (en) * | 1986-04-24 | 1987-10-28 | Unilever Plc | Porous silica structures |
Also Published As
| Publication number | Publication date |
|---|---|
| ATE164598T1 (de) | 1998-04-15 |
| EP0761696B1 (de) | 1998-04-01 |
| EP0761696A1 (de) | 1997-03-12 |
| DE59600133D1 (de) | 1998-05-07 |
| ES2114335T3 (es) | 1998-05-16 |
| AU708459B2 (en) | 1999-08-05 |
| JPH09110916A (ja) | 1997-04-28 |
| TW367337B (en) | 1999-08-21 |
| AU6195896A (en) | 1997-02-13 |
| AR003227A1 (es) | 1998-07-08 |
| CN1152580A (zh) | 1997-06-25 |
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| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
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