EP0000748A1 - Procédé de préparation de polymères d'éthylène - Google Patents
Procédé de préparation de polymères d'éthylène Download PDFInfo
- Publication number
- EP0000748A1 EP0000748A1 EP78100534A EP78100534A EP0000748A1 EP 0000748 A1 EP0000748 A1 EP 0000748A1 EP 78100534 A EP78100534 A EP 78100534A EP 78100534 A EP78100534 A EP 78100534A EP 0000748 A1 EP0000748 A1 EP 0000748A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- oxygen
- catalyst
- stage
- carbon monoxide
- chromium
- 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.)
- Withdrawn
Links
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 4
- 229920000573 polyethylene Polymers 0.000 title claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 54
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000012159 carrier gas Substances 0.000 claims abstract description 28
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229940117975 chromium trioxide Drugs 0.000 claims abstract description 23
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 19
- 239000012018 catalyst precursor Substances 0.000 claims abstract description 18
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 17
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000005977 Ethylene Substances 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 13
- 150000001845 chromium compounds Chemical class 0.000 claims abstract description 12
- 239000000178 monomer Substances 0.000 claims abstract description 12
- 229910000423 chromium oxide Inorganic materials 0.000 claims abstract description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 10
- 229920000642 polymer Polymers 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 230000000379 polymerizing effect Effects 0.000 claims abstract description 4
- 229930195734 saturated hydrocarbon Natural products 0.000 claims abstract description 3
- 239000010412 oxide-supported catalyst Substances 0.000 claims description 6
- 229920001577 copolymer Polymers 0.000 claims description 5
- 229920001519 homopolymer Polymers 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 abstract description 29
- 239000000047 product Substances 0.000 abstract 3
- 239000013067 intermediate product Substances 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 description 8
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- -1 polyethylene Polymers 0.000 description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N Propene Chemical compound CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 2
- GYQWAOSGJGFWAE-UHFFFAOYSA-N azane tetrafluorosilane Chemical compound N.[Si](F)(F)(F)F GYQWAOSGJGFWAE-UHFFFAOYSA-N 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 description 1
- WSSSPWUEQFSQQG-UHFFFAOYSA-N 4-methyl-1-pentene Chemical compound CC(C)CC=C WSSSPWUEQFSQQG-UHFFFAOYSA-N 0.000 description 1
- 240000002989 Euphorbia neriifolia Species 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229940070337 ammonium silicofluoride Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 230000002040 relaxant effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 238000003260 vortexing Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 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
Definitions
- Processes of this type are known to have a number of advantageous aspects compared to comparable other processes, but on the other hand also leave one or two wishes unfulfilled.
- This desire is particularly understandable in that, with increasing catalyst yield, polymers with a decreasing content of residual catalyst are obtained; - The latter should be as small as possible that a - complex - cleaning step to remove the residues can be omitted.
- the centerpiece is the use of a special chromium oxide supported catalyst, which is obtained from a specific intermediate catalyst product in two stages in a specific way.
- the catalyst intermediate as such is not associated with any special features; it can be one which is customary in the polymerization of olefins by means of supported chromium oxide catalysts.
- the preliminary product is based on a carrier which has a particle size of 0.02 to 3, in particular of C, 04 to 1.5 mm.
- the carrier consists of silicon dioxide or is a silicon dioxide which is chemically or physically linked to a component consisting of the elements aluminum, titanium, zirconium, molybdenum, vanadium or thor, which component is an oxide of the element concerned or one under the conditions step (1) into an oxide composition of the affected element.
- this (calculated as oxide) can make up to 20, in particular up to 15, percent by weight, based on the total weight of the carrier.
- Silicon dioxide mixed oxides which contain 0.1 to 15 percent by weight, based on the total weight of the carrier, of aluminum oxide are particularly suitable as carriers.
- the catalyst precursor i.e. the carrier loaded with a chromium compound, which is chromium trioxide or a chromium compound which converts to chromium trioxide under the conditions of stage (1), is treated in a known manner with oxygen in a first stage (1) in a certain manner as defined above . It is of particular importance that the solid is left in the form of a fluidized bed; - Where you can use such devices and procedures, as are common in fluidized bed processes. As has been shown, air is the preferred carrier gas. As has also been shown, the period of whirling is not critical, apart from the minimum period of 30 minutes, but should generally be 2 to 15 hours for convenience.
- the oxygen treatment in stage (1) is combined with treatment by a promoter.
- the promoters can be the relevant ones be usual, such as in particular ammonium silicofluoride '(NH 4 ) 2 SiF 6 , and can be added to the catalyst precursor before or during the vortexing.
- stage (2) the product obtained from stage (1), which is preferably flushed free of oxygen, is treated with carbon monoxide in a specific manner defined above and thus converted into the actual supported chromium oxide catalyst.
- stage (1) which is preferably flushed free of oxygen
- carbon monoxide in a specific manner defined above and thus converted into the actual supported chromium oxide catalyst.
- the solid is left in the form of a fluidized bed, and that the carrier gas is anhydrous and oxygen-free.
- Polymers of ethylene are produced using the new catalysts by means of the so-called “solution polymerization process”, cyclohexane in particular being considered as a solvent.
- solution polymerization process cyclohexane in particular being considered as a solvent.
- the polymerization process as such has no special features and can be carried out in the relevant customary technological configurations.
- a catalyst precursor consists of a homogeneously loaded silica / alumina mixed oxide containing chromium trioxide in a weight ratio of carrier: chromium trioxide of 100: 4.4, which contains 0.4 percent by weight, based on the total weight of the mixed oxide, and one Has particle size of 0.04 to 1.5 mm.
- This preliminary product is mixed with a promoter (ammonium silicon fluoride) in a weight ratio of catalyst preliminary product: promoter of 100: 2.5.
- promoter ammonium silicon fluoride
- a stirred autoclave is charged with 1000 parts by weight of cyclohexane, whereupon it is flushed with nitrogen and 0.1 part by weight of catalyst is added.
- a thermostatically controlled temperature of 150 ° C. pure ethylene is pressed up to a pressure of 35 bar, the process is continued until the pressure has dropped to 25 bar due to the formation of polyethylene, and then ethylene is pressed again up to a pressure of 35 bar and so on for 90 minutes.
- the polymerization is then terminated by cooling to room temperature and relaxing.
- a preliminary catalyst product consists of a silica / alumina mixed oxide loaded homogeneously with chromium trioxide in a weight ratio of carrier: chromium trioxide of 100: 2.0, which contains 0.1 percent by weight, based on the total weight of the mixed oxide, and one Has particle size of 0.04 to 1.5 mm.
- This preliminary product is mixed with a promoter (ammonium silicon fluoride) in a weight ratio of catalyst preliminary product: promoter of 100: 1.5.
- promoter ammonium silicon fluoride
- a catalyst pre-product consists of a silica / alumina mixed oxide loaded homogeneously with chromium trioxide in a weight ratio of carrier: chromium trioxide of 100: 4.5, which is 0.3% by weight, based on the total weight of the mixed oxide-aluminum oxide contains and has a particle size of 0.04 to 1.5 mm.
- Example 3 The procedure is as in Example 3, with the exception that the first stage (1) is carried out at a temperature of 570 ° C. (instead of 680 ° C.).
- Example 2 The procedure is as in Example 1, with the exceptions that a temperature of 146 ° C. (instead of 150 ° C.) is used and that instead of ethylene, a mixture of 98.5 parts by weight of ethylene and 1.5 parts by weight of butene-1 is polymerized .
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)
- Polymerization Catalysts (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19772734909 DE2734909A1 (de) | 1977-08-03 | 1977-08-03 | Verfahren zum herstellen von polymerisaten des aethylens |
| DE2734909 | 1977-08-03 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP0000748A1 true EP0000748A1 (fr) | 1979-02-21 |
Family
ID=6015486
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP78100534A Withdrawn EP0000748A1 (fr) | 1977-08-03 | 1978-07-28 | Procédé de préparation de polymères d'éthylène |
Country Status (9)
| Country | Link |
|---|---|
| EP (1) | EP0000748A1 (fr) |
| JP (1) | JPS5428380A (fr) |
| AT (1) | ATA559578A (fr) |
| DE (1) | DE2734909A1 (fr) |
| DK (1) | DK342078A (fr) |
| ES (1) | ES472325A1 (fr) |
| FI (1) | FI782362A7 (fr) |
| IT (1) | IT7825982A0 (fr) |
| NO (1) | NO782639L (fr) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0279890A3 (en) * | 1986-06-16 | 1989-09-13 | Phillips Petroleum Company | In situ comonomer generation in olefin polymerization |
| EP0307907A3 (en) * | 1987-09-18 | 1989-09-27 | Phillips Petroleum Company | Process for olefin polymerization |
| WO1989012662A1 (fr) * | 1988-06-23 | 1989-12-28 | Mobil Oil Corporation | Oligomeres olefiniques ayant des proprietes lubrifiantes et leur procede de production |
| EP0361363A3 (fr) * | 1988-09-26 | 1991-08-07 | Phillips Petroleum Company | Procédé de polymérisation de polyéthylène basse densité à haute résistance mécanique et film à partir de celui-ci (film phénoménal) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5866661A (en) * | 1996-12-13 | 1999-02-02 | Phillips Petroleum Company | Ethylene polymerization processes and products thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1115023B (de) * | 1955-10-14 | 1961-10-12 | Phillips Petroleum Co | Verfahren und Vorrichtung zum Aktivieren oder Regenerieren eines chromoxydhaltigen Olefin-polymerisationskatalysators |
| FR1302764A (fr) * | 1960-10-07 | 1962-08-31 | Phillips Petroleum Co | Procédé de polymérisation des oléfines et catalyseur utilisé dans ce procédé |
| US3362946A (en) * | 1964-06-01 | 1968-01-09 | Phillips Petroleum Co | Method of treating supported chromium oxide catalyst and polymerization therewith |
| DE1906175B1 (de) * | 1968-02-08 | 1970-08-27 | Phillips Petroleum Co | Verfahren zur Aktivierung eines Chromoxyd-Traegerkatalysators |
| SU373986A1 (ru) * | 1971-06-01 | 1975-02-05 | Институт Катализа Сибирского Отделения Ан Ссср | Способ приготовлени катализатора дл полимеризации этилена |
-
1977
- 1977-08-03 DE DE19772734909 patent/DE2734909A1/de active Pending
-
1978
- 1978-07-21 IT IT7825982A patent/IT7825982A0/it unknown
- 1978-07-28 EP EP78100534A patent/EP0000748A1/fr not_active Withdrawn
- 1978-07-31 FI FI782362A patent/FI782362A7/fi not_active Application Discontinuation
- 1978-08-02 DK DK342078A patent/DK342078A/da unknown
- 1978-08-02 AT AT559578A patent/ATA559578A/de not_active Application Discontinuation
- 1978-08-02 JP JP9371178A patent/JPS5428380A/ja active Pending
- 1978-08-02 NO NO782639A patent/NO782639L/no unknown
- 1978-08-03 ES ES472325A patent/ES472325A1/es not_active Expired
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1115023B (de) * | 1955-10-14 | 1961-10-12 | Phillips Petroleum Co | Verfahren und Vorrichtung zum Aktivieren oder Regenerieren eines chromoxydhaltigen Olefin-polymerisationskatalysators |
| FR1302764A (fr) * | 1960-10-07 | 1962-08-31 | Phillips Petroleum Co | Procédé de polymérisation des oléfines et catalyseur utilisé dans ce procédé |
| US3362946A (en) * | 1964-06-01 | 1968-01-09 | Phillips Petroleum Co | Method of treating supported chromium oxide catalyst and polymerization therewith |
| DE1906175B1 (de) * | 1968-02-08 | 1970-08-27 | Phillips Petroleum Co | Verfahren zur Aktivierung eines Chromoxyd-Traegerkatalysators |
| SU373986A1 (ru) * | 1971-06-01 | 1975-02-05 | Институт Катализа Сибирского Отделения Ан Ссср | Способ приготовлени катализатора дл полимеризации этилена |
Non-Patent Citations (1)
| Title |
|---|
| DERWENT "Soviet inventtions illustrated", Chemical Seection 1, vol. W, Nr. 31 (1975) & SU-A-373 986 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0279890A3 (en) * | 1986-06-16 | 1989-09-13 | Phillips Petroleum Company | In situ comonomer generation in olefin polymerization |
| EP0307907A3 (en) * | 1987-09-18 | 1989-09-27 | Phillips Petroleum Company | Process for olefin polymerization |
| WO1989012662A1 (fr) * | 1988-06-23 | 1989-12-28 | Mobil Oil Corporation | Oligomeres olefiniques ayant des proprietes lubrifiantes et leur procede de production |
| EP0361363A3 (fr) * | 1988-09-26 | 1991-08-07 | Phillips Petroleum Company | Procédé de polymérisation de polyéthylène basse densité à haute résistance mécanique et film à partir de celui-ci (film phénoménal) |
Also Published As
| Publication number | Publication date |
|---|---|
| FI782362A7 (fi) | 1979-02-04 |
| IT7825982A0 (it) | 1978-07-21 |
| DE2734909A1 (de) | 1979-02-15 |
| ATA559578A (de) | 1980-08-15 |
| ES472325A1 (es) | 1979-02-16 |
| JPS5428380A (en) | 1979-03-02 |
| NO782639L (no) | 1979-02-06 |
| DK342078A (da) | 1979-02-04 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
| AK | Designated contracting states |
Designated state(s): BE CH DE FR GB NL SE |
|
| 17P | Request for examination filed | ||
| RAP1 | Party data changed (applicant data changed or rights of an application transferred) |
Owner name: SCHULZE, KURT |
|
| STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN |
|
| 18D | Application deemed to be withdrawn |
Effective date: 19810729 |