DD211720A5 - PROCESS FOR PRODUCING TONERDE CATALYSTS - Google Patents
PROCESS FOR PRODUCING TONERDE CATALYSTS Download PDFInfo
- Publication number
- DD211720A5 DD211720A5 DD83251339A DD25133983A DD211720A5 DD 211720 A5 DD211720 A5 DD 211720A5 DD 83251339 A DD83251339 A DD 83251339A DD 25133983 A DD25133983 A DD 25133983A DD 211720 A5 DD211720 A5 DD 211720A5
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- German Democratic Republic
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- sio
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
- B01J21/04—Alumina
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
- B01J23/04—Alkali metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/08—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of gallium, indium or thallium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
- C07C5/22—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by isomerisation
- C07C5/23—Rearrangement of carbon-to-carbon unsaturated bonds
- C07C5/25—Migration of carbon-to-carbon double bonds
- C07C5/2506—Catalytic processes
- C07C5/2512—Catalytic processes with metal oxides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
Ein mit Kieselsaeure stabilisierter gamma-Aluminiumoxid-Katalysator ist mit Oxiden zwei- oder dreiwertiger Metalle aus der Gruppe II A, III B, VII und /oder Lanthaniden impraegniert und dient als Isomerisierungskatalysator.A stabilized with silica acid gamma-alumina catalyst is impregnated with oxides of divalent or trivalent metals from the group II A, III B, VII and / or lanthanides and serves as an isomerization catalyst.
Description
._ Berlin, den 12.9.1983 AP B 01 j/ 251 339/6 62 501 11Berlin, 12.9.1983 AP B 01 j / 251 339/6 62 501 11
Verfahren zur Herstellung von Tonerde-KatalysatorenProcess for the preparation of alumina catalysts
Die Erfindung betrifft ein Verfahren zur Herstellung von Tonerde-Katalysatoren, stabilisiert mit Kieselsäure.The invention relates to a process for the preparation of alumina catalysts stabilized with silica.
Die erfindungQgemäß hergestellten Katalysatoren werden angewandt beispielsweise sur Isomerisierung olefinisch ungesättigter Verbindungen.The catalysts prepared according to the invention are used, for example, for isomerization of olefinically unsaturated compounds.
Katalysatoren auf der Basis von y-Tonerde sind bekannt; ebenso bekannt ist, daß sie für bestimmte Reaktionen, insbesondere für die Bindungs-Isomerisationsreaktionen eine su hohe Acidität aufweisen. Darüber hinaus steigt die Acidität von y~-Tonerde weiter, wenn diese zur Erhöhung der thermischen Stabilität mit Kieselsäure behandelt worden ist (US-PS 40 13 590 und 40 13 589 sowie US-Re 30 668). Andererseits ist eine Stabilisierung mit Kieselsäure erforderlich, um Tonerde einer Regenerierung bei hoher Temperatur ohne Verlust ihrer Aktivität zugänglich su machen.Catalysts based on y-alumina are known; It is also known that they have a high acidity for certain reactions, in particular for the binding isomerization reactions. Moreover, the acidity of y.sup.- clay further increases when it has been treated with silica to increase the thermal stability (US Pat. Nos. 4,013,590 and 4,013,589 and US Pat. No. Re. 30,668). On the other hand, stabilization with silica is required to render alumina susceptible to high temperature regeneration without loss of its activity.
Ziel der Srfindung ist die Bereitstellung eines Verfahrens zur Herstellung von Tonerde-Katalysatoren mit verbessertenThe object of the invention is to provide a process for the preparation of alumina catalysts with improved
ΔΡ Β 01 J/ 251 339/6 62 501 11ΔΡ Β 01 J / 251 339/6 62 501 11
Eigenschai"ten, die für Isomerisierung3reaktionen geeignet sind«Properties which are Suitable for Isomerization3 Reactions «
Der Erfindung liegt die Aufgabe zugrunde, einerseits die Äcidität von Katalysatoren auf der Basis von v- -Aluminiumoxid so weit herabzusetzen, daß sie sich für Isomerisierungsreaktionen eignet und andererseits nicht so weit su verringern, daß die thermische Stabilität infrage gestellt wäre·On the one hand, the object of the invention is to reduce the ubiquity of catalysts based on α-aluminum oxide to such an extent that it is suitable for isomerization reactions and, on the other hand, does not reduce it so far that the thermal stability would be called into question.
Dies erreicht man. erfindungsgemäß durch Zusatz von einem oder mehreren Oxid(en) von Metallen der Gruppe II λ und/oder Till und/oderThis is achieved. according to the invention by addition of one or more oxide (s) of metals of group II λ and / or Till and / or
AP B 01 J/ 251 339/β 62 501AP B 01 J / 251 339 / β 62 501
III B und/oder der Lanthan!den zu mit Kieselsäure stabilisierter y-Tonerde.III B and / or the lanthanum! To the silica-stabilized y-alumina.
Dem erfindungsgemäßen Katalysator kann man die allgemeine FormelThe catalyst of the invention can be the general formula
a Al2O3. b SiO2. c Me^O,.a Al 2 O 3 . b SiO 2 . c Me ^ O ,.
zuschreiben, worin Me 0 ein oder mehrere Oxid(e) der Metalle der Gruppen II A, III B, VIII und/oder der Lanthaniden bezeichnet und a, b und c die Mol-Anzahl der oxidischen Komponenten angeben, wobei die Relationin which Me 0 denotes one or more oxide (s) of the metals of the groups II A, III B, VIII and / or the lanthanides and a, b and c indicate the molar number of oxidic components, the relation
c = m.b + Bc = m.b + B
erfüllt sein muß;must be fulfilled;
B = 0,01,B = 0.01,
b 0,02 bis 0,25, (b+c)/a = 0,01 bis 9, m = 0,7 bis 0,1b 0.02 to 0.25, (b + c) / a = 0.01 to 9, m = 0.7 to 0.1
Im Falle eine3 calciuiahaltigen Katalysators soll das TSoI-verhältnis folgender Beziehung genügen:In the case of a catalyst containing three calciuli, the TSoI ratio should satisfy the following relationship:
Mole GaO I 0,500 . Mole SiO3 + 0,030.Mole GaO I 0.500. Mole SiO 3 + 0.030.
Ira Falle eines bariumhaltigen Katalysators soll das Molverhältnis folgender Besiehung genügen:Ira case of a barium-containing catalyst should satisfy the molar ratio of the following Besiehung:
Hole BaO = 0,500 . Hole SiO9 + 0,020.Get BaO = 0.500. Get SiO 9 + 0.020.
AP B 01 J/ 251 339/6 62 501 11AP B 01 J / 251 339/6 62 501 11
Im Falle von lanthaniialtigen Katalysatoren soll das MoI- verhältnis folgender Besiehung genügen:In the case of lanthanide catalysts, the moi ratio should satisfy the following occupation:
Mole La2O3 = 0,257 . Mole SiO2 + 0,014,Mole La 2 O 3 = 0.257. Mole SiO 2 + 0.014,
Im Falle von eisenhaltigen Katalysatoren soll das MoI-yerhältnis folgender Beziehung genügen:In the case of iron-containing catalysts, the MoI ratio should satisfy the following relationship:
Mole Fe2O3 = 0,290 , Mole SiO0 + 0,018.Mole Fe 2 O 3 = 0.290, moles SiO 0 + 0.018.
In obigen vier speziellen Fällen liegt die Mol-Anzahl SiO, und das Verhältnis (b+c)/a bei den oben angegebenen Werten.In the above four specific cases, the number of moles of SiO 2 and the ratio of (b + c) / a are those given above.
Der erfindungsgemäße Katalysator eignet sich insbesondere zur Isomerisierung von olefinischen Doppelbindungen, insbesondere zur Isomerisierung -von 2-Buten zu 1-Buten.The catalyst according to the invention is particularly suitable for the isomerization of olefinic double bonds, in particular for the isomerization of 2-butene to 1-butene.
Die Herstellung des erfindungsgemäßen stabilisierten y -Tonerde-Katalysators geschieht im Sinne obiger amerikanischer Patentschriften durch Tränken der Tonerde mit einer wäßrigen Lösung von Salzen der Metalle der Gruppen II A, III B, VIII und/oder der Lanthaniden, vorzugsweise Hitrate oder Acetate.The preparation of the stabilized y-toner earth catalyst according to the invention is carried out in the sense of the above US patents by impregnating the alumina with an aqueous solution of salts of the metals of groups II A, III B, VIII and / or the lanthanides, preferably Hitrate or acetates.
Die Erfindung wird an folgenden Beispielen weiter erläutert. B _e i 3 ρ i e 1 1 The invention will be further illustrated by the following examples. B _e i 3 ρ ie 1 1
20 g y-Tonerde (spezifische Oberfläche 200 rn /g) wurden20 g of y-clay (specific surface area 200 rn / g) were added
3 mit 15 cm einer alkoholischen Lösung enthaltend 0,75 g "Dynasil A 40", daß ist eine 40%ige Lösung von Ethylenorthosilicat, behandelt. 3 with 15 cm of an alcoholic solution containing 0.75 g of "Dynasil A 40" that is a 40% solution of ethylene orthosilicate treated.
IP B 01 J/ 251 339/6 62 501 11IP B 01 J / 251 339/6 62 501 11
Das Gemisch konnte bei 50 0C 2 h reagieren, dann wurde es dekantiert und mit Dampf zur Hydrolyse der Silanolgruppen behandelt gebrannt.The mixture was allowed to react at 50 ° C. for 2 hours, then it was decanted and fired with steam to hydrolyze the silanol groups.
behandelt. Anschließend wurde getrocknet und 4 h bei 500 0Ctreated. It was then dried and 4 h at 500 0 C.
Man erhielt ein Material enthaltend 1,5 % SiO0, welches mit 15 cnr einer wäßrigen Lösung von 5»9 S Lanthannitrat imprägniert, das imprägnierte Material getrocknet und 4 h bei 500 0C gebrannt wurde.This gave a material containing 1.5% SiO 0 , which impregnated with 15 cnr an aqueous solution of 5 »9 S lanthanum nitrate, the impregnated material was dried and fired at 500 0 C for 4 h.
Der so erhaltene Katalysator war eine mit 1,5 % SiOp stabilisierte y—Tonerde enthaltend 10 % La2O.,.The catalyst thus obtained was stabilized with 1.5% SiOp y- clays containing 10 % La 2 O.,.
Er wurde in einen Reaktor eingebracht und in diesem trans-2-Buten bei 4-70 0C unter Atmosphärendruck bei einer Durchsatzgeschwindigkeit von 6 m-Vm .h isomerisiert» Auf diese Weise erhielt man 1-Buten mit nur 14-0 ppm Isobuten.He was placed in a reactor and isomerizing .h in this trans-2-butene at 4-70 0 C under atmospheric pressure at a throughput speed of 6 m-Vm "In this manner, 1-butene obtained with only 14-0 ppm isobutene.
Nach 24 h bei 1 000 0C besaß der Katalysator eine spe-After 24 h at 1 000 0 C the catalyst had a spe-
p zifische Oberfläche von 113 21 /g und zeigte nach 40 Zyklen von Betriebszeit - insgesamt 332 h - und Regenerationsseit - insgesamt 152 h ·. keinen Aktivitätsverlust. Die .Regenerierung erfolgte bei einer Temperatur von 540 G,p surface of 113 21 / g and showed after 40 cycles of operating time - a total of 332 h - and Regenerationsseit - a total of 152 h ·. no loss of activity. The regeneration was carried out at a temperature of 540 G,
Entsprechend Beispiel 1 wurde ein Katalysator hergestellt, der in y--Tonerde 1,5 % SiO2 und 2,5 % CaO enthielt. Der Calciumgehalt wurde durch Tränken mit 15 cnr einer wäßrigen Lösung von 2,4 g Calciumnitrat, Trocknen und Brennen während 4 h bei 500 0C eingebracht,According to Example 1, a catalyst was prepared which contained 1.5 % SiO 2 and 2.5 % CaO in y-alumina. The calcium content was introduced by impregnation with 15 cnr an aqueous solution of 2.4 g of calcium nitrate, drying and firing for 4 h at 500 0 C,
Dieser Katalysator diente, wie oben, zur IsomerisierungThis catalyst served as above for isomerization
AP B 01 J/ 251 339/6 62 501 11AP B 01 J / 251 339/6 62 501 11
von 2-Buten bei 450 0G unter Atmosphärendruck bei einer Durchsatzgeschwindigkeit von 6 nr/m «h, wodurch man 1-Buten mit einem Isobutengehalt von nur 150 ppm erhielt.of 2-butene at 450 0 G under atmospheric pressure at a flow rate of 6 nr / m h, whereby 1-butene was obtained with an isobutene content of only 150 ppm.
Nach einer Wärmebehandlung von 24 h bei 1 000 0G hatteAfter a heat treatment of 24 h at 1 000 0 G had
2 der Katalysator eine spezifische Oberfläche 183 m /g und zeigte nach 40 Zyklen von Betriebszeit - insgesamt 332 h und Regenerationszeit - insgesamt 152 h--keinen Aktivitätsverlust. Die Regenerierung erfolgte bei 54-0 0G.2, the catalyst had a specific surface area of 183 m / g and showed no loss of activity after 40 cycles of operating time - a total of 332 h and regeneration time - 152 h in total. The regeneration was carried out at 54-0 0 G.
Claims (2)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| IT21512/82A IT1152198B (en) | 1982-05-27 | 1982-05-27 | ALBUMINE RANGE CATALYST AND ITS PREPARATION METHOD |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DD211720A5 true DD211720A5 (en) | 1984-07-25 |
Family
ID=11182900
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DD83251339A DD211720A5 (en) | 1982-05-27 | 1983-05-27 | PROCESS FOR PRODUCING TONERDE CATALYSTS |
| DD83266938A DD228538A5 (en) | 1982-05-27 | 1983-05-27 | METHOD FOR ISOMERIZING OLEFINICALLY UNSATURATED COMPOUNDS |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DD83266938A DD228538A5 (en) | 1982-05-27 | 1983-05-27 | METHOD FOR ISOMERIZING OLEFINICALLY UNSATURATED COMPOUNDS |
Country Status (29)
| Country | Link |
|---|---|
| JP (1) | JPS58216741A (en) |
| KR (1) | KR840004521A (en) |
| AU (1) | AU557471B2 (en) |
| BE (1) | BE896851A (en) |
| CA (1) | CA1193238A (en) |
| CS (1) | CS239938B2 (en) |
| DD (2) | DD211720A5 (en) |
| DE (1) | DE3319099A1 (en) |
| DK (1) | DK234483A (en) |
| EG (1) | EG16047A (en) |
| ES (1) | ES8505833A1 (en) |
| FR (1) | FR2527941A1 (en) |
| GB (1) | GB2121698B (en) |
| GR (1) | GR78565B (en) |
| HU (1) | HU200709B (en) |
| IT (1) | IT1152198B (en) |
| LU (1) | LU84824A1 (en) |
| NL (1) | NL8301873A (en) |
| NO (1) | NO158485C (en) |
| NZ (1) | NZ204199A (en) |
| PH (1) | PH17970A (en) |
| PL (1) | PL140654B1 (en) |
| PT (1) | PT76765B (en) |
| RO (1) | RO86664B (en) |
| SE (1) | SE452954B (en) |
| SU (1) | SU1440330A3 (en) |
| YU (1) | YU44435B (en) |
| ZA (1) | ZA833399B (en) |
| ZW (1) | ZW11383A1 (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61157345A (en) * | 1984-12-28 | 1986-07-17 | Toyo C C I Kk | Carrier for catalyst |
| DE3839580C1 (en) * | 1988-11-24 | 1990-07-05 | Condea Chemie Gmbh, 2212 Brunsbuettel, De | |
| US5187138A (en) * | 1991-09-16 | 1993-02-16 | Exxon Research And Engineering Company | Silica modified hydroisomerization catalyst |
| US5208200A (en) * | 1992-02-27 | 1993-05-04 | Exxon Research And Engineering Co. | Noble metal on rare earth modified silica alumina as hydrocarbon conversion catalyst |
| US5248409A (en) * | 1992-02-27 | 1993-09-28 | Exxon Research & Engineering Company | Metal on rare earth modified silica alumina as hydrocarbon conversion catalyst |
| DE4445680A1 (en) * | 1994-12-21 | 1996-06-27 | Huels Chemische Werke Ag | Catalyst and process for the isomerization of aliphatic C¶4¶-C¶1¶¶¶ monoolefins |
| DE102013226370A1 (en) | 2013-12-18 | 2015-06-18 | Evonik Industries Ag | Production of butadiene by oxidative dehydrogenation of n-butene after prior isomerization |
| DE102015200702A1 (en) | 2015-01-19 | 2016-07-21 | Evonik Degussa Gmbh | Preparation of butadiene from ethene |
| JP6571392B2 (en) | 2015-05-29 | 2019-09-04 | Ｊｘｔｇエネルギー株式会社 | Isomerization catalyst, linear olefin production method and compound production method |
| JP6736017B2 (en) * | 2015-11-05 | 2020-08-05 | Ｅｎｅｏｓ株式会社 | Isomerization catalyst, method for producing linear olefin and method for producing compound |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2461069A (en) * | 1944-06-10 | 1949-02-08 | Socony Vacuum Oil Co Inc | Simultaneous catalytic cracking and desulfurization of hydrocarbons |
| US3313858A (en) * | 1965-02-12 | 1967-04-11 | Phillips Petroleum Co | Isomerization of non-terminal olefins |
| US3925253A (en) * | 1973-03-19 | 1975-12-09 | Ethyl Corp | Catalysts |
| US4220559A (en) * | 1978-02-14 | 1980-09-02 | Engelhard Minerals & Chemicals Corporation | High temperature-stable catalyst composition |
| FR2424061A1 (en) * | 1978-04-25 | 1979-11-23 | Lyon Applic Catalytiques | NEW CONTACT MASS FOR HETEROGENOUS CATALYSIS |
| JPS6035174B2 (en) * | 1979-05-10 | 1985-08-13 | 株式会社日本触媒 | Catalyst for producing alkylene glycol ethers |
-
1982
- 1982-05-27 IT IT21512/82A patent/IT1152198B/en active
-
1983
- 1983-05-11 NZ NZ204199A patent/NZ204199A/en unknown
- 1983-05-11 ZA ZA833399A patent/ZA833399B/en unknown
- 1983-05-12 ZW ZW113/83A patent/ZW11383A1/en unknown
- 1983-05-17 GB GB08313562A patent/GB2121698B/en not_active Expired
- 1983-05-17 YU YU1099/83A patent/YU44435B/en unknown
- 1983-05-17 SE SE8302769A patent/SE452954B/en not_active IP Right Cessation
- 1983-05-18 PH PH28927A patent/PH17970A/en unknown
- 1983-05-18 KR KR1019830002174A patent/KR840004521A/en not_active Application Discontinuation
- 1983-05-19 GR GR71394A patent/GR78565B/el unknown
- 1983-05-20 AU AU14835/83A patent/AU557471B2/en not_active Expired - Fee Related
- 1983-05-24 RO RO111050A patent/RO86664B/en unknown
- 1983-05-25 NO NO831848A patent/NO158485C/en unknown
- 1983-05-25 FR FR8308649A patent/FR2527941A1/en not_active Withdrawn
- 1983-05-25 PL PL1983242188A patent/PL140654B1/en unknown
- 1983-05-25 DK DK234483A patent/DK234483A/en not_active Application Discontinuation
- 1983-05-25 EG EG323/83A patent/EG16047A/en active
- 1983-05-26 PT PT76765A patent/PT76765B/en unknown
- 1983-05-26 CA CA000428978A patent/CA1193238A/en not_active Expired
- 1983-05-26 SU SU833597798A patent/SU1440330A3/en active
- 1983-05-26 LU LU84824A patent/LU84824A1/en unknown
- 1983-05-26 NL NL8301873A patent/NL8301873A/en not_active Application Discontinuation
- 1983-05-26 HU HU831865A patent/HU200709B/en not_active IP Right Cessation
- 1983-05-26 CS CS833718A patent/CS239938B2/en unknown
- 1983-05-26 BE BE0/210854A patent/BE896851A/en not_active IP Right Cessation
- 1983-05-26 DE DE19833319099 patent/DE3319099A1/en active Granted
- 1983-05-27 JP JP58092564A patent/JPS58216741A/en active Pending
- 1983-05-27 DD DD83251339A patent/DD211720A5/en not_active IP Right Cessation
- 1983-05-27 ES ES523075A patent/ES8505833A1/en not_active Expired
- 1983-05-27 DD DD83266938A patent/DD228538A5/en not_active IP Right Cessation
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