JPH0217482B2 - - Google Patents

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Publication number
JPH0217482B2
JPH0217482B2 JP1030077A JP3007789A JPH0217482B2 JP H0217482 B2 JPH0217482 B2 JP H0217482B2 JP 1030077 A JP1030077 A JP 1030077A JP 3007789 A JP3007789 A JP 3007789A JP H0217482 B2 JPH0217482 B2 JP H0217482B2
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JP
Japan
Prior art keywords
silicon
silica
modified silica
boron
crystalline modified
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 - Lifetime
Application number
JP1030077A
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English (en)
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JPH01275417A (ja
Inventor
Kuramatsuso Maruko
Manaara Jobanni
Fuatsutoore Bitsutorio
Notaari Buruuno
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SnamProgetti SpA
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SnamProgetti SpA
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Publication date
Priority claimed from IT24844/78A external-priority patent/IT1096596B/it
Priority claimed from IT2263879A external-priority patent/IT1166822B/it
Application filed by SnamProgetti SpA filed Critical SnamProgetti SpA
Publication of JPH01275417A publication Critical patent/JPH01275417A/ja
Publication of JPH0217482B2 publication Critical patent/JPH0217482B2/ja
Granted legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H04—ELECTRIC COMMUNICATION TECHNIQUE
    • H04N—PICTORIAL COMMUNICATION, e.g. TELEVISION
    • H04N3/00—Scanning details of television systems; Combination thereof with generation of supply voltages
    • H04N3/10—Scanning details of television systems; Combination thereof with generation of supply voltages by means not exclusively optical-mechanical
    • H04N3/16—Scanning details of television systems; Combination thereof with generation of supply voltages by means not exclusively optical-mechanical by deflecting electron beam in cathode-ray tube, e.g. scanning corrections
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/09—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis
    • C07C29/10—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis of ethers, including cyclic ethers, e.g. oxiranes
    • 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
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/08—Silica
    • 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
    • B01J29/00—Catalysts comprising molecular sieves
    • B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00—Boron; Compounds thereof
    • C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
    • C01B35/10—Compounds containing boron and oxygen
    • C01B35/1009—Compounds containing boron and oxygen having molecular-sieve properties
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00—Boron; Compounds thereof
    • C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
    • C01B35/10—Compounds containing boron and oxygen
    • C01B35/12—Borates
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
    • C07C1/20—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon starting from organic compounds containing only oxygen atoms as heteroatoms
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2/00—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms
    • C07C2/54—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by addition of unsaturated hydrocarbons to saturated hydrocarbons or to hydrocarbons containing a six-membered aromatic ring with no unsaturation outside the aromatic ring
    • C07C2/64—Addition to a carbon atom of a six-membered aromatic ring
    • C07C2/66—Catalytic processes
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2/00—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms
    • C07C2/86—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by condensation between a hydrocarbon and a non-hydrocarbon
    • C07C2/862—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by condensation between a hydrocarbon and a non-hydrocarbon the non-hydrocarbon contains only oxygen as hetero-atoms
    • C07C2/864—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by condensation between a hydrocarbon and a non-hydrocarbon the non-hydrocarbon contains only oxygen as hetero-atoms the non-hydrocarbon is an alcohol
    • H—ELECTRICITY
    • H04—ELECTRIC COMMUNICATION TECHNIQUE
    • H04N—PICTORIAL COMMUNICATION, e.g. TELEVISION
    • H04N3/00—Scanning details of television systems; Combination thereof with generation of supply voltages
    • H04N3/10—Scanning details of television systems; Combination thereof with generation of supply voltages by means not exclusively optical-mechanical
    • H04N3/16—Scanning details of television systems; Combination thereof with generation of supply voltages by means not exclusively optical-mechanical by deflecting electron beam in cathode-ray tube, e.g. scanning corrections
    • H04N3/22—Circuits for controlling dimensions, shape or centering of picture on screen
    • H04N3/223—Controlling dimensions
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2521/00—Catalysts comprising the elements, oxides or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium or hafnium
    • C07C2521/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • C07C2521/08—Silica
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P30/00—Technologies relating to oil refining and petrochemical industry
    • Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P30/00—Technologies relating to oil refining and petrochemical industry
    • Y02P30/40—Ethylene production

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Multimedia (AREA)
  • Signal Processing (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Catalysts (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Silicon Compounds (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)

Description

【発明の詳細な説明】 本発明は、結晶性シリカに関連する新規合成物
質に係る。さらに詳述すれば、本発明は、ケイ素
及びホウ素の酸化物でなりかつ多孔性の結晶構造
を有する合成物質、該合成物質の製法及び該合成
物質の使用に関するものである。 各種文献によれば、ホウ素が平面配位又は四面
体配位を有しうる稠密な天然のホウケイ酸塩（非
多孔性物質である）が知られている。多孔性ガラ
スも公知であり、かかるガラス様物質を化学的に
作用せしめることにより得られる。これらの物質
はその原材料に応じて、シリカ、アルカリ、アル
ミナ及びB2O3を含みうる。文献は、ホウ素の配
位がゼオライト形構造、すなわち規則正しい多孔
性の結晶構造であることを教示しているが、これ
までのところ、かかる構造は得られていない
（Breck、ゼオライト・モレキユラー・シーブス
（Zeolite Molecular Sieves）J.Wiley and Sons
社、ニユーヨーク、1974、第322頁）。 公知の方法は、米国特許第4049573号に記載の
如く、アルミニウム及びケイ素の酸化物からなる
ゼオライトにホウ酸を含浸せしめることのみであ
る。この場合、ホウ素は結晶格子の一部を構成す
るよう格子内に入るものではない。 発明者らは、ケイ素に代わる置換体としてホウ
素を結晶格子に導入せしめることによつて変性せ
しめた結晶性シリカを開発した。 さらに、発明者らは、ホウ素がケイ素に代わる
置換用元素となる以外にも、多孔質であり、よく
制御されかつゼオライト構造に近似した結晶構造
を有する新規物質を生成し得るとの知見を得て本
発明に至つた。 該物質（本明細書の以下の記載では、簡略化の
ため「ボラリツト（Boralite）Ｂと称する）は、
酸化物のモル比として、かつ無水状態として次式
により特徴づけられる。 （０−１）R2O・（０−１）C2/oＯ・B2O3・（
５−50）SiO2 （式中、Ｒはテトラエチルアンモニウムカチオン
（TEA）であり、ＣはH+、NH4 +又は原子価ｎの
金属の如きカチオンである。） なお、ボラリツトＢの熱安定性はモル比
SiO2／B2O3が大きいことに関連する。 特に、か焼された後ではR2Oが存在しないこと
が望ましい（ただし、必ずしも厳密な意味ではな
い。） 上記式に相当するボラリツトＢは特定の結晶構
造を有し、高温度（450℃ないし750℃）でか焼し
たH+形のものに関するＸ線回折スペクトルは第
１表に記載の特徴的なピークを示す。 第 １ 表 面 間 隔 ｄ（Å） 相対強度 11.23 Ｓ 6.52 Ｗ 5.98 Ｗ 4.08 MW 3.90 Ｓ 3.46 MW 3.26 MW 3.05 Ｗ 2.98 MW 2.65 Ｗ 2.05 Ｗ 記号の説明：VS＝非常に強い Ｓ＝強い MW＝中程度弱い Ｗ＝弱い モル比SiO2／B2O3、焼成温度及びカチオンの
性質の変化に伴つて、上記数値は若干変化する。 H+の代わりに他のカチオンが存在する場合に
は、通常のゼオライトのものと類似してスペクト
ルにわずかな変化を生ずる。 赤外線吸収スペクトルでは、導入されたホウ素
の量を関数として910ないし925cm-1の領域に特徴
的な吸収を示す。 ボラリツトＢの製法は、水熱反応条件下、ケイ
素誘導体、ホウ素誘導体及び包接化剤（テトラエ
チルアンモニウム化合物）を、PH９ないし14、温
度110ないし220℃、期間１ないし30日間で反応さ
せることを特徴とする。 ホウ素及びケイ素の有機誘導体（たとえばホウ
酸トリアルキル及びオルトケイ酸テトラアルキル
エステル）を使用し、テフロン（登録商標）容
器、又はポリプロピレン、白金、その他の材料の
容器（アルカリ性溶液が結晶化容器から不純物を
抽出することを防止するため）において、水熱反
応を行なうことにより、高純度のボラリツトＢが
得られる。 不純物が存在しないことは、ボラリツトＢの特
有な性質（たとえば疎水性であること、このため
脱水力を持たないこと）を保証する。 非常に高い純度が要求されない場合には、各成
分について安価な原料を使用できる。たとえばホ
ウ素については、ホウ酸、ホウ酸ナトリウム及び
ホウ砂を使用でき、ケイ素については、コロイド
状シリカ、シリカゲル、ケイ酸ナトリウム、エア
ロジルなどを使用できる。さらに結晶化には、ガ
ラス、ステンレス鋼などで形成された容器を使用
できる。 かかる場合、ボラリツトＢは反応体又は結晶化
容器に由来する不純物を含む場合がある。たとえ
ば、市販のシリカはAl2O32000ppm以下を含む
が、10000ppm程度のアルミナ含量では、他の性
質、たとえば疎水性及び脱水力が変化されること
があつたとしても、構造及び結晶学上の特性を変
化させるものではない。 アルカリ金属又はアルカリ土類金属の水酸化物
又はハロゲン化物の如き鉱化剤を添加することも
できる。 ボラリツトＢは、高温度での熱処理及び水蒸気
の存在下における熱処理のいずれにおいても非常
に安定である。 本発明によるボラリツトＢは、そのままで又は
好ましくはシリカ、アルミナ及びクレー様物質か
ら選ばれる不活性担体上に分散担持された状態で
触媒反応又は吸収処理で使用される。一般に、下
記の多数の反応で利用される。 １ トルエンをメタノールでアルキル化してキシ
レン、主としてパラ−キシレンを生成する反応 ２ トルエンを不均化して主としてパラ−キシレ
ンを生成する反応 ３ ジメチルエーテル及び／又はメタノール又は
他の低級アルコールのオレフイン類及び芳香族
類の如き炭化水素への変換反応 ４ クラツキング及び水素化分解 ５ ノルマル−パラフイン及びナフテンの異性化 ６ オレフイン結合又はアセチレン結合を有する
化合物の重合 ７ 改質反応 ８ オルト−キシレンの如きポリアルキル置換芳
香族化合物の異性化 ９ 芳香族類、特にトルエンの不均化 10 脂肪族カルボニル化合物の少なくとも部分的
芳香族炭化水素への変換反応 11 他のC8芳香族炭化水素からエチルベンゼン
の分離 12 炭化水素の水素添加及び脱水素 13 メタン化 14 酸化、特に内燃機関排出物の酸化 15 含酸素脂肪族化合物の脱水 16 オレフインの高オクタン価燃料への変換 特に、本発明のボラリツトＢは、メチル第３級
ブチルエーテルからメタノール及びイソブチレン
を生成する反応における触媒として有効に使用さ
れる。 上述した本発明の目的を説明するために、次に
実施例について述べるが、これに限定されるもの
ではない。 実施例 CO2を含有しない雰囲気に維持したパイレツク
スガラス容器に、水酸化テトラエチルアンモニウ
ムの25％（重量）溶液110gを導入し、ついで撹
拌しながらホウ酸12gを加えた。 溶解後、なお撹拌を続けながら40％LudoxA.S.
コロイド状シリカ100gを添加した。 反応混合物を撹拌しながら80℃に１時間加熱し
た。 その後、水熱反応を、テフロン内張り静置オー
トクレーブ（300ml）内において150℃で９日間実
施した。ついで、このようにして得られた反応生
成物を室温まで冷却し、フイルター上で集め、蒸
留水で注意深く洗浄し、乾操及びか焼することに
よつて得られた結晶性生成物は、平均直径1.3μm
の球状粒子よりなるものであつた。 化学分析では、モル比SiO2／B2O3＝6.86を示
した。550℃でか焼したH+形のもののＸ線回折ス
ペクトルは、第１表に示すデータと一致した。赤
外線吸収スペクトルでは、921cm-1に特徴的な吸
収バンドを示した。 比表面積（BET法に従い、窒素ガス中で測定）
は421m2/gであつた。 細孔容積は0.18cm3/gであり、実測密度（ヘリウ
ム法）は2.32g/cm3である。酸性度（CsCl法で測
定）はPH1.8である。 参考例 内径８mmの電気加熱式管状反応器に、上記実施
例に従つて調製した粒径30ないし50メツシユ
（ASTM、米国シリーズ）のボラリツトＢ触媒３
mlを充填した。 定量ポンプにより、反応器に、予熱管で予熱し
たメチル第３級ブチルエーテルを導入した。 反応器の下流に、６バールに設定した圧力チエ
ツク弁を設けた。このチエツク弁に、適当に加熱
される試料採集装置を具備せしめ、圧力が低下す
る際、反応器の流出物をガスクロマトグラフイー
に導入するようにした。 第２表に示す温度に加熱し、メチル第３級ブチ
ルエーテルを各種の液空間速度（LHSV）で導入
した。得られた結果を同じく第２表に示す。 【表】

Claims (1)

  1. 【特許請求の範囲】 １ 結晶性シリカの結晶格子内に、ケイ素に代わ
    る置換元素としてホウ素を導入させてなる結晶性
    変性シリカであつて、無水状態で、式 （０−１）R2O・（０−１）C2/oＯ・B2O3・（
    ５−50）SiO2 （式中、Ｒはテトラエチルアンモニウムカチオン
    であり、ＣはH+、NH4 +又は原子価ｎの金属の
    如きカチオンである）に相当し、H+形の場合、
    下記データに相当するＸ線回折スペクトルを有す
    ることを特徴とする、結晶性変性シリカ。 面 間 隔 ｄ（Å） 相対強度 11.23 Ｓ 6.52 Ｗ 5.98 Ｗ 4.08 MW 3.90 Ｓ 3.46 MW 3.26 MW 3.05 Ｗ 2.98 MW 2.65 Ｗ 2.05 Ｗ 記号の説明：VS＝非常に強い Ｓ＝強い MW＝多少弱い Ｗ＝弱い ２ 結晶性シリカの結晶格子内に、ケイ素に代わ
    る置換元素としてホウ素を導入させてなる結晶性
    変性シリカであつて、無水状態で、式 （０−１）R2O・（０−１）C2/oＯ・B2O3・（
    ５−50）SiO2 （式中、Ｒはテトラエチルアンモニウムカチオン
    であり、ＣはH+、NH4 +又は原子価ｎの金属の
    如きカチオンである）に相当し、H+形の場合、
    下記データに相当するＸ線回折スペクトルを有す
    る結晶性変性シリカの製法において、ケイ素誘導
    体、ホウ素誘導体及びテトラエチルアンモニウム
    化合物を、水熱条件下、PH９ないし14、温度110
    ないし220℃で１ないし30日間反応させることを
    特徴とする、結晶性変性シリカの製法。 面 間 隔 ｄ（Å） 相対強度 11.23 Ｓ 6.52 Ｗ 5.98 Ｗ 4.08 MW 3.90 Ｓ 3.46 MW 3.26 MW 3.05 Ｗ 2.98 MW 2.65 Ｗ 2.05 Ｗ 記号の説明：VS＝非常に強い Ｓ＝強い MW＝多少弱い Ｗ＝弱い ３ 特許請求の範囲第２項記載の製法において、
    前記ケイ素誘導体がケイ素のコロイド状シリカで
    ある、結晶性変性シリカの製法。 ４ 特許請求の範囲第２項記載の製法において、
    前記ホウ素誘導体がホウ酸である、結晶性変性シ
    リカの製法。
JP1030077A 1978-06-22 1989-02-10 結晶性変性シリカ及びその製法 Granted JPH01275417A (ja)

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IT24844/78A IT1096596B (it) 1978-06-22 1978-06-22 Materiale sintetico a base di silice
IT24844A/78 1978-06-22
IT22638A/79 1979-05-14
IT2263879A IT1166822B (it) 1979-05-14 1979-05-14 Materiali sintetici costrituiti da ossidi di silicio e boro avente struttura cristallina porosa loro metodo di preparazione ed uso degli stessi

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IE48198B1 (en) 1984-10-31
DK165173B (da) 1992-10-19
AT381483B (de) 1986-10-27
SE445521B (sv) 1986-06-30
PH15865A (en) 1983-04-13
ES482161A0 (es) 1980-12-16
BG39638A3 (en) 1986-07-15
JPH0223481B2 (ja) 1990-05-24
GR66589B (ja) 1981-03-30
PT69799A (en) 1979-07-01
AU4787479A (en) 1980-01-03
SE8803721D0 (sv) 1988-10-18
SE7905452L (sv) 1979-12-23
TR21215A (tr) 1984-01-02
SE8803722L (sv) 1988-10-18
IL57582A (en) 1983-09-30
GB2078704A (en) 1982-01-13
IN151534B (ja) 1983-05-14
NO792059L (no) 1979-12-28
ES8101921A1 (es) 1980-12-16
NL190144C (nl) 1993-11-16
FR2429182A1 (fr) 1980-01-18
DK240379A (da) 1979-12-23
LU81415A1 (fr) 1979-09-12
SE8403805D0 (sv) 1984-07-20
DK164813C (da) 1993-01-11
DK165174C (da) 1993-03-01
ATA438279A (de) 1986-03-15
DK149839B (da) 1986-10-13
SE8403805L (sv) 1984-07-20
IE791169L (en) 1979-12-22
JPH01275417A (ja) 1989-11-06
DK3692A (da) 1992-01-10
FR2429182B1 (ja) 1984-10-12
SE462845B (sv) 1990-09-10
NO156125B (no) 1987-04-21
YU148479A (en) 1983-01-21
PL216527A1 (ja) 1980-04-21
CH643803A5 (it) 1984-06-29
CA1155824A (en) 1983-10-25
DE2924915A1 (de) 1980-01-03
SE464248B (sv) 1991-03-25
GB2024790B (en) 1982-11-24
DK164813B (da) 1992-08-24
NL190144B (nl) 1993-06-16
SE464249B (sv) 1991-03-25
AR225417A1 (es) 1982-03-31
NL7904909A (nl) 1979-12-28
US4666692A (en) 1987-05-19
IL57582A0 (en) 1979-10-31
AU531123B2 (en) 1983-08-11
SE8803722D0 (sv) 1988-10-18
RO78795B (ro) 1983-07-30
DK3592A (da) 1992-01-10
GB2078704B (en) 1983-04-07
JPH0230612A (ja) 1990-02-01
DK165173C (da) 1993-03-01
HU181955B (en) 1983-11-28
DK149839C (da) 1987-03-16
DK165174B (da) 1992-10-19
DK3692D0 (da) 1992-01-10
PL118686B1 (en) 1981-10-31
NO156125C (no) 1987-07-29
US4656016A (en) 1987-04-07
RO78795A (ro) 1983-08-03
GB2024790A (en) 1980-01-16
EG13934A (en) 1983-03-31
SE8803721L (sv) 1988-10-18
DK3592D0 (da) 1992-01-10
DD144398A5 (de) 1980-10-15
DK593084D0 (da) 1984-12-11
DK593084A (da) 1984-12-11
DE2924915C2 (de) 1983-11-17

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