EP0284501A1 - Binder pitch with modified filtrability and its preparation - Google Patents
Binder pitch with modified filtrability and its preparation Download PDFInfo
- Publication number
- EP0284501A1 EP0284501A1 EP88400643A EP88400643A EP0284501A1 EP 0284501 A1 EP0284501 A1 EP 0284501A1 EP 88400643 A EP88400643 A EP 88400643A EP 88400643 A EP88400643 A EP 88400643A EP 0284501 A1 EP0284501 A1 EP 0284501A1
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- EP
- European Patent Office
- Prior art keywords
- pitch
- equal
- quinoline
- weight
- impregnation
- 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
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C1/00—Working-up tar
- C10C1/19—Working-up tar by thermal treatment not involving distillation
Definitions
- the present invention relates to pitches, in particular the pitches of coal tar, which are intended to be used as impregnating agents for carbon or graphite parts, with the aim of increasing their density and their mechanical strength.
- pitches in particular the pitches of coal tar, which are intended to be used as impregnating agents for carbon or graphite parts, with the aim of increasing their density and their mechanical strength.
- these pitches will be designated by the term “impregnation pitches”.
- the pitches are, generally, characterized by various analytical data, the knowledge of which makes it possible to assess their use value for the chosen application.
- IQ insoluble in quinoline
- IT insoluble in toluene
- a pitch deemed satisfactory for constituting an impregnation pitch generally complies with the following specifications: - a softening point KS of the order of 60 to 80 ° C; - a content of substances insoluble in quinoline generally less than or equal to 7% by weight; and - A fixed carbon content at least equal to 46%, for example between 46 and 54% by weight.
- the essential criterion for the success of an impregnation pitch is constituted by another measure specific to pitches of this type because it reflects the quality of impregnation of the pitch, namely, the filtration speed (or index of filterability).
- the filterability indices were determined here by the following method:
- the present invention firstly relates to an impregnation pitch having a softening point KS of between 60 ° and 80 ° C approximately, and a content of substances insoluble in quinoline less than or equal to 7% by weight approximately by weight , characterized in that its filterability index is greater than or equal to 4.5.
- the impregnation pitch according to the invention has a fixed carbon content at least equal to 46% by weight.
- the invention also relates to a method of manufacturing an impregnation pitch as defined above, characterized in that one submits in tar or else a soft pitch, that is to say a pitch having a softening point KS at most equal to 60 ° C, and a content of substances insoluble in quinoline at most equal to 7% by weight, to a heat treatment capable of removing a substantial part of its constituents of molecular mass less than 1200.
- the above-mentioned treatment comprises a heat treatment at a temperature between 350 ° C and 430 ° C and for a period of 1 to 50 hours, followed by flash distillation.
- the duration will be chosen the longer the lower the temperature.
- the temperature will be in particular between 400 ° C and 420 ° C and the duration of treatment will be in particular between 2 and 7 hours.
- impregnation pitches are prepared as follows: the pitch of Example 1 (comparative) is obtained by direct distillation of the coal tar, without heat treatment; the pitches of Examples 2 to 5 (in accordance with the invention) are prepared by subjecting the pitch of Example 1 to a heat treatment at temperature T (expressed in ° C) and for the duration t (expressed in hours) indicated in the table below, then a flash distillation.
- T expressed in ° C
- t expressed in hours
- the molar masses of the pitches are determined by gel permeation chromatography in 1,2,4,4-trichlorobenzene at 135 ° C.
- the calibration is carried out using pitch fractions which have been collected by preparative CPG and whose molecular weights have been determined by osmometry.
- the area S obtained is then calculated by integrating the peak (s) of the curve in FIG. 1c and the corresponding curves for the pitches of Examples 2 to 4, between the values 300 and 1200 of the molecular masses; these surfaces are plotted on the ordinate, with, on the abscissa, in a corresponding manner, the filterability indices I, which makes it possible to plot the curve of FIG. 2. It can be seen that the improvement in the filterability index of a pitch is all the greater as the elimination of the aforementioned products is important.
- the percentages of the largest particles are plotted on the ordinate for each of the pitches analyzed, and, on the abscissa, the filterability indices I correspondingly, which gives the curve of the figure. 3. It can thus be seen that the filterability index I gradually increases with the percentage of these particles, which are representative of the mesophase.
Abstract
Description
La présente invention concerne les brais, en particulier les brais de goudrons de houille, qui sont destinés à être utilisés comme agents d'imprégnation de pièces de carbone ou de graphite, dans le but d'augmenter leur densité et leur résistance mécanique. Dans le présent mémoire descriptif, on désignera ces brais par l'expression "brais d'imprégnation".The present invention relates to pitches, in particular the pitches of coal tar, which are intended to be used as impregnating agents for carbon or graphite parts, with the aim of increasing their density and their mechanical strength. In this specification, these pitches will be designated by the term "impregnation pitches".
Les brais sont, d'une manière générale, caractérisés par différentes données analytiques, dont la connaissance permet d'apprécier leur valeur d'usage pour l'application choisie. On donnera ci-après une définition des différentes caractéristiques des brais, qui seront évoquées ici :
- la teneur en substances insolubles dans la quinoléine (IQ), et la teneur en substances insolubles dans le toluène (IT), ces teneurs, exprimées en % en poids, étant obtenues par les modes opératoires indiqués dans les normes respectivement ISO 6791 et ISO 6376 :
- le point de ramollissement Kraemer-Sarnow (KS), exprimé en °C, qui est déterminé selon le procédé au mercure spécifié dans la norme DIN 52025 ;
- la teneur en carbone fixe (exprimée en % en poids), qui traduit le rendement en coke ou le pouvoir en carbone du brai, cette teneur étant calculée selon la méthode décrite dans la norme ISO 6988.The pitches are, generally, characterized by various analytical data, the knowledge of which makes it possible to assess their use value for the chosen application. We will give below a definition of the different characteristics of pitches, which will be discussed here:
the content of substances insoluble in quinoline (IQ), and the content of substances insoluble in toluene (IT), these contents, expressed in% by weight, being obtained by the procedures indicated in the standards respectively ISO 6791 and ISO 6376:
- the Kraemer-Sarnow softening point (KS), expressed in ° C, which is determined according to the mercury process specified in standard DIN 52025;
- the fixed carbon content (expressed in% by weight), which translates the coke yield or the carbon power of the pitch, this content being calculated according to the method described in standard ISO 6988.
Un brai jugé satisfaisant pour constituer un brai d'imprégnation respecte généralement les spécifications suivantes :
- un point de ramollissement KS de l'ordre de 60 à 80°C ;
- une teneur en substances insolubles dans la quinoléine généralement inférieure ou égale à 7% en poids ; et
- une teneur en carbone fixe au moins égale à 46%, par exemple comprise entre 46 et 54% en poids.A pitch deemed satisfactory for constituting an impregnation pitch generally complies with the following specifications:
- a softening point KS of the order of 60 to 80 ° C;
- a content of substances insoluble in quinoline generally less than or equal to 7% by weight; and
- A fixed carbon content at least equal to 46%, for example between 46 and 54% by weight.
Toutefois, le critère essentiel de succès d'un brai d'imprégnation est constitué par une autre mesure propre aux brais de ce type parce qu'elle traduit la qualité d'imprégnation du brai, à savoir, la vitesse de filtration (ou indice de filtrabilité). Les indices de filtrabilité ont ici été déterminés par la méthode suivante :However, the essential criterion for the success of an impregnation pitch is constituted by another measure specific to pitches of this type because it reflects the quality of impregnation of the pitch, namely, the filtration speed (or index of filterability). The filterability indices were determined here by the following method:
Dans une cellule de filtration, identique à celle décrite par Clarke J.W., Rantell T.D., dans la revue "Fuel", 1980, 59, 35-41, on soumet à une filtration, sur un disque fritté métallique, à une pression constante de 5 x 10⁵ Pa et à une température constante de 225°C, un échantillon de 50 g environ du brai à analyser préalablement chauffé en étuve. On enregistre la courbe m = f (t) (où m est la masse de brai filtré exprimée en grammes et t est le temps exprimé en minutes), et on calcule l'indice de filtrabilité I suivant la formule :
m₁ = masse recueillie au temps t₁
m₂ = masse recueillie au temps t₂In a filtration cell, identical to that described by Clarke JW, Rantell TD, in the review "Fuel", 1980, 59 , 35-41, is subjected to filtration, on a metallic sintered disc, at a constant pressure of 5 x 10⁵ Pa and at a constant temperature of 225 ° C, a sample of approximately 50 g of pitch to be analyzed, previously heated in an oven. The curve m = f (t) is recorded (where m is the mass of filtered pitch expressed in grams and t is the time expressed in minutes), and the filterability index I is calculated according to the formula:
m₁ = mass collected at time t₁
m₂ = mass collected at time t₂
Jusqu'à présent, l'homme du métier était persuadé que le traitement thermique de maturation d'un brai d'imprégnation était sand influence, voire même désavantageux, pour la vitesse de filtration.Up to now, the person skilled in the art was convinced that the thermal treatment of maturation of an impregnation pitch was sand influence, or even disadvantageous, for the speed of filtration.
La Société déposante a maintenant découvert que, contrairement à ce préjugé, la filtrabilité d'un brai d'imprégnation pouvait être considérablement améliorée par une maturation modérée de celui-ci.The Depositing Company has now discovered that, contrary to this prejudice, the filterability of an impregnation pitch could be considerably improved by a moderate maturation of it.
Par ailleurs, l'analyse par chromatographie par perméation de gel (CPG) de brais d'imprégnation ayant et n'ayant pas été traités thermiquement a permis à la Société déposante de constater que l'amélioration de l'indice de filtrabilité d'un brai est corrélée, d'une part, à une élimination des produits de masse moléculaire inférieure à 1200, et de préférence comprise entre 500 et 1100 et, d'autre part, à une augmentation de la fraction des particules insolubles dans la quinoléine, présentant une taille de l'ordre de 8-10 µm, autrement dit des particules représentatives de la mésophase. Tout se passe donc comme si les molécules, dont on constate qu'elles disparaissent de la matrice du brai, se retrouvaient en mésophase. L'observation en microscopie électronique des substances insolubles dans la quinoléine vient confirmer que les particules insolubles dans la quinoléine qui sont de toute petite taille, viennent, dans le cas des brais ayant été traités thermiquement, s'adsorber sur les particules de mésophase. Il en résulte que les phénomènes de colmatage, nuisant à l'obtention d'un bon indice de filtrabilité, qui étaient provoqués par ces particules de petite taille, se trouvent supprimés.In addition, analysis by gel permeation chromatography (GPC) of impregnation pitches which have and have not been heat-treated has enabled the applicant company to note that the improvement in the filterability index of a pitch is correlated, on the one hand, with an elimination of the products of molecular mass lower than 1200, and preferably between 500 and 1100 and, on the other hand, an increase in the fraction of particles insoluble in quinoline, having a size of the order of 8-10 μm, in other words particles representative of the mesophase. Everything therefore happens as if the molecules, which we see that they disappear from the pitch matrix, are found in mesophase. Observation by electron microscopy of substances insoluble in quinoline confirms that the insoluble particles in quinoline which are very small, come, in the case of pitches having been heat treated, to adsorb on the particles of mesophase. As a result, the clogging phenomena, hindering the obtaining of a good filterability index, which were caused by these small particles, are eliminated.
La présente invention a d'abord pour objet un brai d'imprégnation possédant un point de ramollissement KS compris entre 60° et 80°C environ, et une teneur en substances insolubles dans la quinoléine inférieure ou égale à 7% en poids environ en poids, caractérisé en ce que son indice de filtrabilité est supérieur ou égal à 4,5. De préférence, le brai d'imprégnation selon l'invention possède une teneur en carbone fixe au moins égale à 46% en poids.The present invention firstly relates to an impregnation pitch having a softening point KS of between 60 ° and 80 ° C approximately, and a content of substances insoluble in quinoline less than or equal to 7% by weight approximately by weight , characterized in that its filterability index is greater than or equal to 4.5. Preferably, the impregnation pitch according to the invention has a fixed carbon content at least equal to 46% by weight.
L'invention a également pour objet un procédé de fabrication d'un brai d'imprégnation tel que défini ci-dessus, caractérisé en ce qu'on soumet en goudron ou bien un brai mou, c'est-à-dire un brai possédant un point de ramollissement KS au plus égal à 60°C, et une teneur en substances insolubles dans la quinoléine au plus égale à 7% en poids, à un traitement thermique capable d'éliminer une partie substantielle de ses constituants de masse moléculaire inférieure à 1200.The invention also relates to a method of manufacturing an impregnation pitch as defined above, characterized in that one submits in tar or else a soft pitch, that is to say a pitch having a softening point KS at most equal to 60 ° C, and a content of substances insoluble in quinoline at most equal to 7% by weight, to a heat treatment capable of removing a substantial part of its constituents of molecular mass less than 1200.
Conformément à un mode de réalisation préféré du procédé selon l'invention, le traitement susindiqué comprend un traitement thermique à une température comprise entre 350°C et 430°C et pendant une durée de 1 à 50 heures, suivi d'une distillation éclair. Pour des raisons évidentes de cinétique, la durée sera choisie d'autant plus longue que la température sera moins élevée. La température sera notamment comprise entre 400°C et 420°C et la durée de traitement se situera notamment entre 2 et 7 heures.In accordance with a preferred embodiment of the method according to the invention, the above-mentioned treatment comprises a heat treatment at a temperature between 350 ° C and 430 ° C and for a period of 1 to 50 hours, followed by flash distillation. For obvious kinetic reasons, the duration will be chosen the longer the lower the temperature. The temperature will be in particular between 400 ° C and 420 ° C and the duration of treatment will be in particular between 2 and 7 hours.
La présente invention sera maintenant illustrée comme suit :The present invention will now be illustrated as follows:
A partir d'un même goudron de houille, on prépare des brais d'imprégnation comme suit : le brai de l'exemple 1 (comparatif) est obtenu par distillation directe du goudron de houille, sans traitement thermique ; les brais des exemples 2 à 5 (conformes à l'invention) sont préparés en faisant subir au brai de l'exemple 1, un traitement thermique à la température T (exprimée en °C) et pendant la durée t (exprimée en heures) indiquées dans le tableau ci-après, puis une distillation éclair. Dans le tableau ci-après, sont rapportées les caractéristiques des brais ainsi obtenus, telles qu'elles sont définies ci-dessus, ainsi que la valeur numérique (en unité arbitraire) de la surface S obtenue par intégration de la courbe de la figure 1c comme précisé ci-après.
On détermine les masses molaires des brais par chromatographie à perméation de gel dans le trichloro-1,2,4 benzène à 135°C.The molar masses of the pitches are determined by gel permeation chromatography in 1,2,4,4-trichlorobenzene at 135 ° C.
L'étalonnage est réalisé à l'aide de fractions de brai qui ont été recueillies par CPG préparative et dont les masses moléculaires ont été déterminées par osmométrie.The calibration is carried out using pitch fractions which have been collected by preparative CPG and whose molecular weights have been determined by osmometry.
En soustrayant de la courbe CPG du brai de l'exemple 5 (Figure 1a), celle du brai de l'exemple 1 (Figure 1b), on obtient la courbe, représentée sur la Figure 1c. L'examen de ces courbes fait apparaître que toute amélioration de l'indice de filtrabilité d'un brai est en rapport direct avec une élimination de produits de masses moléculaires comprises entre 300 et 1200 environ.By subtracting from the CPG curve of the pitch of Example 5 (Figure 1a), that of the pitch of Example 1 (Figure 1b), we obtain the curve, shown in Figure 1c. Examination of these curves shows that any improvement in the filterability index of a pitch is directly related to the elimination of products with molecular weights between 300 and 1200 approximately.
On calcule alors la surface S obtenue par intégration du (ou des) pic(s) de la courbe de la Figure 1c et des courbes correspondantes pour les brais des exemples 2 à 4, entre les valeurs 300 et 1200 des masses moléculaires ; on porte ces surfaces en ordonnées, avec, en abscisses, de façon correspondante, les indices de filtrabilité I, ce qui permet de tracer la courbe de la Figure 2. On constate que l'amélioration de l'indice de filtrabilité d'un brai est d'autant plus grande que l'élimination des produits précités est importante.The area S obtained is then calculated by integrating the peak (s) of the curve in FIG. 1c and the corresponding curves for the pitches of Examples 2 to 4, between the
Enfin, on étudie la distribution granulométrique des particules insolubles dans la quinoléine.Finally, we study the particle size distribution of particles insoluble in quinoline.
On porte, en ordonnées, les pourcentages des plus grandes particules (diamètre compris entre 8 et 10 µm) pour chacun des brais analysés, et, en abscisses, de façon correspondante, les indices de filtrabilité I, ce qui donne la courbe de la figure 3. On peut ainsi constater que l'indice de filtrabilité I augmente progressivement avec le pourcentage de ces particules, lesquelles sont représentatives de la mésophase.The percentages of the largest particles (diameter between 8 and 10 μm) are plotted on the ordinate for each of the pitches analyzed, and, on the abscissa, the filterability indices I correspondingly, which gives the curve of the figure. 3. It can thus be seen that the filterability index I gradually increases with the percentage of these particles, which are representative of the mesophase.
Parallèlement à cette étude, on observe, par microscopie électronique à balayage, l'aspect de ces particules. On remarque, sur les représentations photographiques obtenues concernant les brais des exemples 1 et 5 (Figure 4), une variation de la nature des substances insolubles dans la quinoléine, lesquelles passent de particules de type "noir de carbone" de taille de 1-2 µm environ (exemple 1) à des agglomérates mésophasiques de taille de 8-10 µm environ, ayant adsorbé les particules précédentes (exemple 5). Ces agglomérats proviennent des phénomènes de polycondensation consécutifs au traitement thermiques de l'invention.In parallel with this study, the appearance of these particles is observed by scanning electron microscopy. Note, on the photographic representations obtained concerning the pitches of Examples 1 and 5 (Figure 4), a variation in the nature of the substances insoluble in quinoline, which pass from particles of the “carbon black” type of size 1-2 approximately µm (example 1) to mesophasic agglomerates of size 8-10 µm approximately, having adsorbed the preceding particles (example 5). These agglomerates originate from the polycondensation phenomena consecutive to the thermal treatment of the invention.
Claims (7)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT88400643T ATE58549T1 (en) | 1987-03-20 | 1988-03-18 | WATERPROOFING PITCH WITH IMPROVED FILTERABILITY AND ITS MANUFACTURE. |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR8703927A FR2612525B1 (en) | 1987-03-20 | 1987-03-20 | IMPREGNATION PITCH WITH IMPROVED FILTERABILITY AND METHOD OF MANUFACTURING SAME |
| FR8703927 | 1987-03-20 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0284501A1 true EP0284501A1 (en) | 1988-09-28 |
| EP0284501B1 EP0284501B1 (en) | 1990-11-22 |
Family
ID=9349268
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP19880400643 Expired - Lifetime EP0284501B1 (en) | 1987-03-20 | 1988-03-18 | Binder pitch with modified filtrability and its preparation |
Country Status (10)
| Country | Link |
|---|---|
| US (1) | US4997542A (en) |
| EP (1) | EP0284501B1 (en) |
| JP (1) | JPS6414296A (en) |
| AT (1) | ATE58549T1 (en) |
| BR (1) | BR8801342A (en) |
| CA (1) | CA1304198C (en) |
| DE (1) | DE3861103D1 (en) |
| ES (1) | ES2018618B3 (en) |
| FR (1) | FR2612525B1 (en) |
| GR (1) | GR3001462T3 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5326457A (en) * | 1992-08-06 | 1994-07-05 | Aristech Chemical Corporation | Process for making carbon electrode impregnating pitch from coal tar |
| US5695631A (en) * | 1993-06-04 | 1997-12-09 | Mitsubishi Chemical Corporation | Process for producing petroleum needle coke |
| JP6274390B2 (en) * | 2012-10-24 | 2018-02-07 | 東海カーボン株式会社 | Method for producing graphite powder for negative electrode material of lithium secondary battery |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3692663A (en) * | 1971-03-19 | 1972-09-19 | Osaka Gas Co Ltd | Process for treating tars |
| US4086156A (en) * | 1974-12-13 | 1978-04-25 | Exxon Research & Engineering Co. | Pitch bonded carbon electrode |
| FR2370784A1 (en) * | 1976-11-12 | 1978-06-09 | Nippon Oil Co Ltd | CONTINUOUS OIL BRAI PRODUCTION PROCESS |
| FR2418269A1 (en) * | 1978-02-28 | 1979-09-21 | Union Carbide Corp | SUPERIOR QUALITY BRAI PREPARATION PROCESS |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3835024A (en) * | 1971-03-19 | 1974-09-10 | Osaka Gas Co Ltd | Method for manufacturing pitch |
| US3970542A (en) * | 1971-09-10 | 1976-07-20 | Cindu N.V. | Method of preparing electrode pitches |
| NL7305172A (en) * | 1973-04-13 | 1974-10-15 | ||
| NL183771C (en) * | 1976-06-23 | 1989-01-16 | Cindu Chemie Bv | PROCESS FOR THE PREPARATION OF A BINDER MEAT, AND FORMED ARTICLES, OBTAINED USING AN BINDER MEAT PREPARED BY THE METHOD. |
| JPS533764A (en) * | 1976-07-01 | 1978-01-13 | Seiko Instr & Electronics Ltd | Low power consumption oscillating circuit |
| US4096056A (en) * | 1976-10-21 | 1978-06-20 | Witco Chemical Corporation | Method of producing an impregnating petroleum pitch |
| US4369171A (en) * | 1981-03-06 | 1983-01-18 | Great Lakes Carbon Corporation | Production of pitch and coke from raw petroleum coke |
| GB2110232B (en) * | 1981-11-18 | 1986-05-08 | Nippon Oil Co Ltd | Process for the production of ethane |
| US4664774A (en) * | 1984-07-06 | 1987-05-12 | Allied Corporation | Low solids content, coal tar based impregnating pitch |
-
1987
- 1987-03-20 FR FR8703927A patent/FR2612525B1/en not_active Expired
-
1988
- 1988-03-18 DE DE8888400643T patent/DE3861103D1/en not_active Expired - Lifetime
- 1988-03-18 US US07/170,332 patent/US4997542A/en not_active Expired - Fee Related
- 1988-03-18 ES ES88400643T patent/ES2018618B3/en not_active Expired - Lifetime
- 1988-03-18 CA CA000561878A patent/CA1304198C/en not_active Expired - Fee Related
- 1988-03-18 AT AT88400643T patent/ATE58549T1/en not_active IP Right Cessation
- 1988-03-18 EP EP19880400643 patent/EP0284501B1/en not_active Expired - Lifetime
- 1988-03-21 BR BR8801342A patent/BR8801342A/en not_active Application Discontinuation
- 1988-03-22 JP JP63068021A patent/JPS6414296A/en active Pending
-
1991
- 1991-02-11 GR GR91400175T patent/GR3001462T3/en unknown
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3692663A (en) * | 1971-03-19 | 1972-09-19 | Osaka Gas Co Ltd | Process for treating tars |
| US4086156A (en) * | 1974-12-13 | 1978-04-25 | Exxon Research & Engineering Co. | Pitch bonded carbon electrode |
| FR2370784A1 (en) * | 1976-11-12 | 1978-06-09 | Nippon Oil Co Ltd | CONTINUOUS OIL BRAI PRODUCTION PROCESS |
| FR2418269A1 (en) * | 1978-02-28 | 1979-09-21 | Union Carbide Corp | SUPERIOR QUALITY BRAI PREPARATION PROCESS |
Non-Patent Citations (1)
| Title |
|---|
| JAPANESE PATENTS REPORT, section Chemical, vol. 78, no. 7, 17 mars 1978, Derwent Publications Ltd, Londres, GB; & JP-A-78 003 764 (NIPPON STEEL CORP.) 09-02-1978 * |
Also Published As
| Publication number | Publication date |
|---|---|
| BR8801342A (en) | 1988-11-01 |
| ATE58549T1 (en) | 1990-12-15 |
| DE3861103D1 (en) | 1991-01-03 |
| US4997542A (en) | 1991-03-05 |
| ES2018618B3 (en) | 1991-04-16 |
| FR2612525A1 (en) | 1988-09-23 |
| GR3001462T3 (en) | 1992-10-08 |
| EP0284501B1 (en) | 1990-11-22 |
| FR2612525B1 (en) | 1989-05-19 |
| CA1304198C (en) | 1992-06-30 |
| JPS6414296A (en) | 1989-01-18 |
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