DE1047179B - Process for the production of pure graphite which can be used as a reactor material - Google Patents
Process for the production of pure graphite which can be used as a reactor materialInfo
- Publication number
- DE1047179B DE1047179B DES55671A DES0055671A DE1047179B DE 1047179 B DE1047179 B DE 1047179B DE S55671 A DES55671 A DE S55671A DE S0055671 A DES0055671 A DE S0055671A DE 1047179 B DE1047179 B DE 1047179B
- Authority
- DE
- Germany
- Prior art keywords
- graphite
- gas
- production
- reactor material
- flushing
- 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.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 17
- 229910002804 graphite Inorganic materials 0.000 title claims description 15
- 239000010439 graphite Substances 0.000 title claims description 15
- 238000000034 method Methods 0.000 title claims description 6
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 239000000463 material Substances 0.000 title claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 238000011010 flushing procedure Methods 0.000 claims description 8
- 238000010926 purge Methods 0.000 claims description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000460 chlorine Substances 0.000 claims description 4
- 229910052801 chlorine Inorganic materials 0.000 claims description 4
- 229910052736 halogen Inorganic materials 0.000 claims description 4
- 150000002367 halogens Chemical class 0.000 claims description 4
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 150000002366 halogen compounds Chemical class 0.000 claims 1
- 230000026030 halogenation Effects 0.000 claims 1
- 238000005658 halogenation reaction Methods 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 238000005087 graphitization Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052756 noble gas Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 230000002140 halogenating effect Effects 0.000 description 1
- 150000002835 noble gases Chemical class 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21C—NUCLEAR REACTORS
- G21C5/00—Moderator or core structure; Selection of materials for use as moderator
- G21C5/12—Moderator or core structure; Selection of materials for use as moderator characterised by composition, e.g. the moderator containing additional substances which ensure improved heat resistance of the moderator
- G21C5/126—Carbonic moderators
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/215—Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Landscapes
- Organic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- Plasma & Fusion (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Carbon And Carbon Compounds (AREA)
Description
Die Erfindung betrifft ein Verfahren zur Herstellung von Reinstgraphit, der als Reaktorwerkstoff verwendet werden soll.The invention relates to a method for producing ultra-pure graphite which is used as a reactor material shall be.
Es ist bekannt, den Graphit durch Behandeln mit Halogenen, wie Chlor oder Fluor, von seinen Verunreinigungen, wie Alkalien und Erdalkalien, Fe, Al, Si, Ti, B usw., zu befreien und die sich bildenden Chloroder Fluorverbindungen der zu entfernenden Aschenbestandteile durch ein Spülgas aus dem Graphit auszutreiben. Das restlose Herausspülen dieser dampfförmigen Verbindungen durch einen Spülgasstrom, der gleichzeitig auch eine Adsorption von Chlor und Fluor an Graphit verhindert, ist bekannt. Bisher verwendete man als Spülgas die teureren Edelgase, wie Argon und Helium, oder man benutzte den billigeren Reinststickstoff. Hierbei ist jedoch zu beachten, daß die Kosten für das Spülgas, auch wenn es sich nur um den billigeren Reinststickstoff handelt, die des Reinigungsgases bedeutend überwiegen.It is known to remove the impurities from graphite by treating them with halogens such as chlorine or fluorine. such as alkalis and alkaline earths, Fe, Al, Si, Ti, B etc., to free and the chlorine or To expel fluorine compounds of the ash components to be removed from the graphite by means of a flushing gas. The complete flushing out of these vaporous compounds by a flushing gas stream, which at the same time also prevents the adsorption of chlorine and fluorine on graphite is known. Previously used the more expensive noble gases such as argon and helium were used as the flushing gas, or the cheaper ones were used Pure nitrogen. It should be noted, however, that the cost of the purge gas, even if it is only The cheaper pure nitrogen is used, which significantly outweighs the cleaning gas.
Nun hat es sich gezeigt, daß Stickstoff einen verhältnismäßig hohen Absorptionsquerschnitt für langsame Neutronen besitzt. Bei 25% Porenvolumen des Graphits und völliger Stickstoffüllung der Poren ergibt sich eine Erhöhung des •Neutronenabsorptionsquerschnittes des Graphits von etwa 0,26 mbarn. Das ist der gleiche Wert, wie ihn ein Borgehalt von etwa. 0,3 ppm hervorrufen würde. Zur Erläuterung sei erwähnt, daß 1 mbarn einem Querschnitt von ΙΟ"27 cm2 entspricht. 1 ppm ist ein Maß für die Gewichtsprozente des Elementes und ist gleich 10-4Vo Gewicht.It has now been shown that nitrogen has a relatively high absorption cross-section for slow neutrons. With 25% pore volume of the graphite and complete nitrogen filling of the pores there is an increase in the • neutron absorption cross section of the graphite of about 0.26 mbarn. That is the same value as a boron content of about. 0.3 ppm would cause. 1 for explaining should be noted that a cross section of 1 mbarn ΙΟ "corresponds to 27 cm 2. Ppm is a measure of the weight percent of the element and is equal to 10- 4 Vo weight.
Wenn man also bei bestimmten Reaktortypen die Verbesserung durch die Borreinigung durch eine Verschlechterung des Stickstoffgehaltes nicht wieder aufgeben will, muß man mit teurerem Edelgas, wie Argon oder Helium, spülen. Es ist bekannt, daß Sauerstoff gegenüber dem hohen Absorptionsquerschnitt des Stickstoffes einen sehr geringen Absorptionsquerschnitt für langsame Neutronen besitzt. Sauerstoff kann jedoch als Spülgas wegen des Abbrandes des heißen Graphits nicht verwendet werden. Kohlenoxyd weist dagegen nur die geringe Neutronenabsorptionsfähigkeit des Kohlenstoffs und des Sauerstoffes auf und steht mit dem Kohlenstoff auch bei hohen Temperaturen im Gleichgewicht.So if you consider the improvement of the boron cleaning by a deterioration in certain reactor types If you don't want to give up the nitrogen content again, you have to use a more expensive noble gas such as argon or helium, purge. It is known that oxygen compared to the high absorption cross-section of the Nitrogen has a very small absorption cross-section for slow neutrons. oxygen however, it cannot be used as a purge gas because of the burn-off of the hot graphite. Carbon dioxide on the other hand has only the low neutron absorption capacity of carbon and oxygen and is in equilibrium with the carbon even at high temperatures.
Die Erfindung geht nun von dieser Erkenntnis aus und verwendet Koblenmonoxyd als Spülgas bei dem an sich bekannten Verfahren zur Reinigung des Graphits durch Halogenisierung der zu entfernenden Verunreinigungen des Graphits. Die Verwendung von Koblenmonoxyd als Spülgas hat den Vorteil, daß das bisher angewendete Reinigungsverfahren wesentlich verbilligt wird. Zu beachten ist jedoch dabei, daß Verfahren zur HerstellungThe invention is based on this knowledge and uses coblene monoxide as the purge gas in the known processes for cleaning graphite by halogenating the impurities to be removed of graphite. The use of coblen monoxide as a purge gas has the advantage that the previously used cleaning process is significantly cheaper. It should be noted, however, that Method of manufacture
von als Reaktorwerkstoff verwendbaremof that which can be used as a reactor material
ReinstgraphitPure graphite
Anmelder:Applicant:
Siemens-PlaniawerkeSiemens Planiawerke
Aktiengesellschaft für Kohlefabrikate,Joint stock company for coal products,
Meitingen bei AugsburgMeitingen near Augsburg
Dr. Erich Nedopil, Meitingen bei Augsburg,
ist als Erfinder genannt wordenDr. Erich Nedopil, Meitingen near Augsburg,
has been named as the inventor
Kohlenmonoxyd giftig ist und mit Luft ein explosib-Carbon monoxide is poisonous and an explosive
ao les Gasgemisch bildet. Um diese beiden Gefahrenmomente zu vermeiden, sieht die Erfindung vor, daß im ersten Spülintervall bei höchster Temperatur (2700° C) zunächst mit Stickstoff gespült wird, bis alle flüchtigen Halogenide und Halogengase durch die Abzugshaube, die sich über den Graphitierungsofen befindet, in dem die Reinigung des Graphits vorgenommen wird, entfernt sind. Eine solche Abzugshaube ist erforderlich, da die Halogengase gleichfalls gesundheitsschädlich sind und daher entsprechende Sicherungsmaßnahmen getroffen werden müssen. Nach der Stickstoffspülung wird nun die Abzugshaube gehoben oder entfernt und auf eine C O-Spülung umgeschaltet, damit sich unter der Abzugshaube kein explosibles Gasgemisch ansammeln kann. Das bei der CO-Spülung entweichende Gas wird nach seinem Durchtritt durch den Graphitierungsofen sofort abgebrannt. ao les gas mixture forms. About these two dangers to avoid, the invention provides that in the first rinsing interval at the highest temperature (2700 ° C) is first flushed with nitrogen until all volatile halides and halogen gases pass through the Extractor hood, which is located above the graphitization furnace, in which the graphite is cleaned are removed. Such a hood is necessary because the halogen gases are also used are harmful to health and therefore appropriate safety measures must be taken. After purging with nitrogen, the extractor hood is now lifted or removed and a CO purging is carried out switched so that no explosive gas mixture can collect under the extractor hood. That at the The gas escaping from CO flushing is burned off immediately after it has passed through the graphitization furnace.
Claims (2)
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DES55671A DE1047179B (en) | 1957-10-25 | 1957-10-25 | Process for the production of pure graphite which can be used as a reactor material |
| FR1205756D FR1205756A (en) | 1957-10-25 | 1958-10-15 | Process for preparing high purity graphite |
| GB33621/58A GB880547A (en) | 1957-10-25 | 1958-10-21 | Improvements in or relating to processes for the production of graphite of sufficient purity for use as a reactor material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DES55671A DE1047179B (en) | 1957-10-25 | 1957-10-25 | Process for the production of pure graphite which can be used as a reactor material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1047179B true DE1047179B (en) | 1958-12-24 |
Family
ID=7490606
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DES55671A Pending DE1047179B (en) | 1957-10-25 | 1957-10-25 | Process for the production of pure graphite which can be used as a reactor material |
Country Status (3)
| Country | Link |
|---|---|
| DE (1) | DE1047179B (en) |
| FR (1) | FR1205756A (en) |
| GB (1) | GB880547A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6881680B2 (en) | 2002-06-14 | 2005-04-19 | Toyo Tanso Co., Ltd. | Low nitrogen concentration carbonaceous material and manufacturing method thereof |
| RU2394758C2 (en) * | 2008-08-08 | 2010-07-20 | Общество с ограниченной ответственностью "ГрафитЭл-Московский электронный завод" | Method of obtaining pure graphite |
| CN108516544A (en) * | 2018-06-01 | 2018-09-11 | 中钢集团新型材料（浙江）有限公司 | It is electrolysed HF and KHF2Generate the method and system of fluorine gas purification graphite |
-
1957
- 1957-10-25 DE DES55671A patent/DE1047179B/en active Pending
-
1958
- 1958-10-15 FR FR1205756D patent/FR1205756A/en not_active Expired
- 1958-10-21 GB GB33621/58A patent/GB880547A/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| GB880547A (en) | 1961-10-25 |
| FR1205756A (en) | 1960-02-04 |
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