FR2525752A1 - Pyro-hydrolysis furnace, esp. for analysing samples - where superheated steam is used to achieve redn. in reaction time - Google Patents

Pyro-hydrolysis furnace, esp. for analysing samples - where superheated steam is used to achieve redn. in reaction time Download PDF

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Publication number
FR2525752A1
FR2525752A1 FR8206842A FR8206842A FR2525752A1 FR 2525752 A1 FR2525752 A1 FR 2525752A1 FR 8206842 A FR8206842 A FR 8206842A FR 8206842 A FR8206842 A FR 8206842A FR 2525752 A1 FR2525752 A1 FR 2525752A1
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sep
steam
tube
furnace
redn
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FR8206842A
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French (fr)
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FR2525752B1 (en
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Christian Poletiko
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Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
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Commissariat a lEnergie Atomique CEA
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
    • F27D7/02—Supplying steam, vapour, gases, or liquids
    • 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
    • B01J15/00—Chemical processes in general for reacting gaseous media with non-particulate solids, e.g. sheet material; Apparatus specially adapted therefor
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B17/00—Furnaces of a kind not covered by any preceding group
    • F27B17/02—Furnaces of a kind not covered by any preceding group specially designed for laboratory use
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Clinical Laboratory Science (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

Appts. includes an electric furnace made of refractory material and contg. a reaction chamber, which is esp. a tube (a). Tube (a) has an inlet/outlet for a boat contg. a sample, and also an outlet end for reaction prods., which are fed through a condenser. Tube (a) is surrounded by a helical tube (b) fed with steam from a boiler. The steam is heated in tube (b) to a temp. near to that of the sample boat before the steam enters tube (a). The result is a substantial redn. in the time required for pyrohydrolysis of the sample. Used e.g. to determine the amt. of the chlorides or fluorides of Na, K or Mg present as impurities in uranium oxides and Zr alloy sleeves, where the halides are converted by steam to hydroxides.

Description

La présente invention se rapporte à un four de pyrohydrolyse à vapeur surchauffée. The present invention relates to a superheated steam pyrohydrolysis furnace.

Dans les fours généralement utilisés pour effectuer les réactions de pyrohydrolyse dans les laboratoires et les installations industrielles, on fait pénétrer de la vapeur à iOO"C dans l'enceinte du four. In furnaces generally used for carrying out pyrohydrolysis reactions in laboratories and industrial installations, steam is introduced at 100 ° C. into the furnace enclosure.

Cette vapeur qui n'est que légèrement réchauffée dans le four n'a qu'une réactivité faible et les réactions ne s'effectuent que relativement lentement.This steam, which is only slightly warmed in the oven, has only a weak reactivity and the reactions take place only relatively slowly.

Le but de la présente invention est de fournir un four agencé de telle façon que la vapeur soit surchauffée notablement avant d'atteindre la nacelle contenant le produit à traiter afin de rendre le four plus performant. The object of the present invention is to provide a furnace arranged in such a way that the steam is significantly overheated before reaching the nacelle containing the product to be treated in order to make the furnace more efficient.

L'invention a pour objet un four de pyrohydrolyse comprenant un four proprement dit en matière réfractaire chauffé électriquement, comportant intérieurement une chambre réactionnelle équipée vers l'extérieur d'une ouverture d'entrée et de sortie d'une nacelle contenant un échantillon à traiter, cette chambre étant reliée en amont par un conduit d'arrivée de vapeur à une source de production de vapeur et en aval à un réfrigérant pour condenser les produits de la réaction, caractérisé en ce que le conduit d'arrivée de vapeur est enroulé en serpentin autour de la chambre réactionnelle de l'aval vers l'amont avant de déboucher en amont de la chambre réactionnelle, de telle sorte que la vapeur atteint le produit à traiter à une température voisine de celle de la nacelle. The subject of the invention is a pyrohydrolysis furnace comprising a furnace proper of electrically heated refractory material, internally comprising a reaction chamber equipped to the outside with an inlet and outlet opening of a nacelle containing a sample to be treated. this chamber being connected upstream by a steam inlet duct to a steam generation source and downstream to a condenser for condensing the products of the reaction, characterized in that the steam supply duct is wound in coil around the reaction chamber from downstream to upstream before opening upstream of the reaction chamber, so that the steam reaches the product to be treated at a temperature close to that of the nacelle.

Grâce à agencement de ce four, on obtient un rendement et une cinétique de réaction beaucoup plus élevés que dans le cas des fours utilisés jusqu'à présent. Thanks to the arrangement of this furnace, a much higher yield and reaction kinetics are obtained than in the case of furnaces used hitherto.

D'autres avantages et caractéristiques de
l'invention ressortiront d'ailleurs de la description qui suit d'un mode de réalisation donné à titre nullement limitatif, en référence aux dessins annexés dans lesquels :
- la figure 1 représente schématiquement un four électrique d'un type couramment utilisé pour effectuer les réactions de pyrohydrolyse
- la figure 2 représente schématiquement un four perfectionné conforme à l'invention.Other advantages and features of
the invention will become apparent from the following description of an embodiment given by way of non-limiting way, with reference to the accompanying drawings in which:
FIG. 1 schematically represents an electric furnace of a type commonly used for carrying out pyrohydrolysis reactions.
- Figure 2 shows schematically an improved furnace according to the invention.

Sur la figure I, on observe un four électrique 1 en matière réfractaire,chauffé électriquement et traversé longitudinalement par une chambre réactionnelle en forme de tube 3 dont l'entrée 5 est équipée d'un bouchon 7 pouvant être éventuellement refroidi, au moment du passage de la nacelle contenant le produit à traiter, par une arrivée d'eau annulaire 9. FIG. 1 shows an electric furnace 1 of refractory material, electrically heated and traversed longitudinally by a tube-shaped reaction chamber 3, the inlet 5 of which is equipped with a plug 7 which can be optionally cooled at the moment of the passage of the nacelle containing the product to be treated, by an annular water inlet 9.

A l'entrée 5, débouche un conduit d'arrivée de vapeur 11 issu d'un bouilleur 13. Le tube 3 est relié en aval à un réfrigérant 15 pour la condensation des produits de la réaction. At the inlet 5, opens a steam inlet conduit 11 from a boiler 13. The tube 3 is connected downstream to a refrigerant 15 for condensation of the reaction products.

La surveillance du four est effectuée à partir d'un pupitre de commande 17. On voit que dans ce four de type connu, la vapeur amenée par le conduit 11 pénètre dans le tube 3 en étant que partiellement chauffée et n'ayant de ce fait qu'une faible réactivité. Oven monitoring is carried out from a control console 17. It can be seen that in this known type furnace, the steam supplied by the duct 11 penetrates into the tube 3 while being only partially heated and therefore not being heated. that a low reactivity.

Dans le four conforme à 1'invention représenté à la figure 2, le conduit d'arrivée de vapeur 71 entoure le tube 3 sous la forme d'un serpentin 12 avant de déboucher en amont du tube 3. In the oven according to the invention shown in Figure 2, the steam inlet conduit 71 surrounds the tube 3 in the form of a coil 12 before opening upstream of the tube 3.

On comprend que de cette façon la vapeur se trouve surchauffée avant de pénétrer dans le tube. Cette vapeur surchauffée peut donc agir de façon plus énergique et plus rapide sur le produit à traiter qui est contenu dans la nacelle non représentée, placée au centre du four. It is understood that in this way the steam is superheated before entering the tube. This superheated steam can therefore act more forcefully and quickly on the product to be treated which is contained in the nacelle not shown, placed in the center of the oven.

Pour mettre en évidence le progrès technique apporté par l'invention, on a effectué des essais comparatifs à la fois sur un four de type courant et sur un four conforme à l'invention
On a utilisé à cet effet des oxydes d'uranium et des gaines métalliques essentiellement constituées d'alliages de zirconium en vue de déterminer qualitativement et quantitativement les impuretés se présentant sous forme de sels mdtalliques-de formule MX dans laquelle M représente des métaux comme le sodium, le potassium, le magnésium et X un halogène et plus parti culièrement le chlore et le fluor
il se produit la réaction suivante

Figure img00030001
In order to demonstrate the technical progress brought about by the invention, comparative tests were carried out both on a furnace of the standard type and on an oven according to the invention.
For this purpose, uranium oxides and metallic sheaths consisting essentially of alloys of zirconium have been used for the purpose of qualitatively and quantitatively determining the impurities in the form of metal salts of the formula MX in which M represent metals such as sodium, potassium, magnesium and X halogen and more particularly chlorine and fluorine
the following reaction occurs
Figure img00030001

Le dosage des éléments recueillis au pied du réfrigérant permet de connattre la naturé et les constituants des impuretés. The dosage of the elements collected at the foot of the refrigerant makes it possible to know the nature and the constituents of the impurities.

Les résultats obtenus ont été consignés dans le tableau suivant dans lequel ont été précisées notamment les durées nécessaires à la conduite des réactions. The results obtained were recorded in the following table in which were specified in particular the time required to conduct the reactions.

DUREES DES REACTIONS DE PYROHYDROLYSE

Figure img00030002
DURATION OF PYROHYDROLYSIS REACTIONS
Figure img00030002

<tb> <SEP> Echantillon <SEP> four <SEP> classique <SEP> four <SEP> conforme <SEP> facteur <SEP> ciné- <SEP>
<tb> <SEP> à <SEP> l'invention <SEP> tique
<tb> <SEP> voisin <SEP> de <SEP> de
<tb> <SEP> oxyde <SEP> d'ura- <SEP> 60 <SEP> Mn <SEP> 14 <SEP> mn <SEP> 5
<tb> <SEP> nium <SEP>
<tb> <SEP> O,5g <SEP>
<tb> <SEP> oxyde <SEP> d'urar <SEP> <SEP> 50 <SEP> mn <SEP> 7 <SEP> Mi <SEP> 8
<tb> <SEP> nium
<tb> <SEP> 0,1g <SEP>
<tb> gaines <SEP> 70 <SEP> mn <SEP> 15 <SEP> mn <SEP> 5
<tb> <SEP> tE'lliee's <SEP>
<tb>
il est bien entendu que les essais indiqués ci-dessus, n'ont aucun caractère limitatif et que le four conforme à l'invention peut s'appliquer sans exception à toutes les réactions de pyrohydrolyse et à toutes les réactions chimiques sous atmosphère de vapeur surchauffée. <tb><SEP> Sample <SEP> oven <SEP> classic <SEP> oven <SEP> compliant <SEP> factor <SEP> cine- <SEP>
<tb><SEP> to <SEP> the invention <SEP> tick
<tb><SEP> neighbor <SEP> of <SEP> from
<tb><SEP> oxide <SEP> of ura- <SEP> 60 <SEP> Mn <SEP> 14 <SEP> mn <SEP> 5
<tb><SEP> nium <SEP>
<tb><SEP> O, 5g <SEP>
<tb><SEP> oxide <SEP> of urar <SEP><SEP> 50 <SEP> mn <SEP> 7 <SEP> Mi <SEP> 8
<tb><SEP> nium
<tb><SEP> 0.1g <SEP>
<tb> sheaths <SEP> 70 <SEP> min <SEP> 15 <SEP> min <SEP> 5
<tb><SEP>tE'lliee's<SEP>
<Tb>
it is understood that the tests indicated above, are not limiting and that the oven according to the invention can be applied without exception to all pyrohydrolysis reactions and all chemical reactions under superheated steam atmosphere .

Claims (1)

REVENDICATIONS 7. Four de pyrohydrolwse comprenant un four (1) proprement dit en matière réfractaire chauffé électriquement, comportant intérieurement une chambre réactionnelle (3) équipée vers l'extérieur d'une-ouverture (5) d'entrée et de sortie d'une nacelle contenant un échantillon à traiter, cette chambre étant reliée en amont par un conduit d'arrivée de vapeur (11) à une source de production de vapeur (13) et en aval à un réfrigérant (15) pour condenser les produits de la réaction, caractérisé en ce que le conduit d'arrivée de vapeur est enroulé en serpentin (12) autour de la chambre réactionnelle de l'aval vers l'amont avant de déboucher en amont de la chambre réactionnelle, de telle sorte que la vapeur atteint le produit à traiter à une température voisine de celle de lanacelle,  7. Pyrohydrolwse furnace comprising a furnace (1) proper electrically heated refractory material, having internally a reaction chamber (3) equipped to the outside of an aperture (5) input and output of a nacelle containing a sample to be treated, this chamber being connected upstream by a steam inlet duct (11) to a steam generating source (13) and downstream to a refrigerant (15) for condensing the reaction products, characterized in that the steam supply duct is wound in a serpentine (12) around the reaction chamber from the downstream upstream before discharging upstream of the reaction chamber, so that the vapor reaches the product to be treated at a temperature close to that of the bucket,
FR8206842A 1982-04-21 1982-04-21 OVERHEATED STEAM PYROHYDROLYSIS OVEN Expired FR2525752B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
FR8206842A FR2525752B1 (en) 1982-04-21 1982-04-21 OVERHEATED STEAM PYROHYDROLYSIS OVEN

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Application Number Priority Date Filing Date Title
FR8206842A FR2525752B1 (en) 1982-04-21 1982-04-21 OVERHEATED STEAM PYROHYDROLYSIS OVEN

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FR2525752B1 FR2525752B1 (en) 1987-05-07

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11360064B2 (en) * 2016-03-30 2022-06-14 3M Innovative Properties Company Oxy-pyrohydrolysis system and method for total halogen analysis

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1033772A (en) * 1951-03-09 1953-07-15 Pechiney Prod Chimiques Sa Method and apparatus for treating powdery materials with gases and vice versa
US3389538A (en) * 1965-08-09 1968-06-25 Continental Oil Co Sample vaporizing apparatus
GB1340844A (en) * 1972-05-02 1973-12-19 Envirotech Corp Fluid sampler apparatus and method
FR2396289A1 (en) * 1977-07-01 1979-01-26 Bodenseewerk Perkin Elmer Co METHOD AND INSTALLATION FOR THE AUTOMATIC PRODUCTION AND MEASUREMENT OF GASEOUS ANALYSIS SAMPLES FROM A SERIES OF SAMPLE LIQUIDS

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1033772A (en) * 1951-03-09 1953-07-15 Pechiney Prod Chimiques Sa Method and apparatus for treating powdery materials with gases and vice versa
US3389538A (en) * 1965-08-09 1968-06-25 Continental Oil Co Sample vaporizing apparatus
GB1340844A (en) * 1972-05-02 1973-12-19 Envirotech Corp Fluid sampler apparatus and method
FR2396289A1 (en) * 1977-07-01 1979-01-26 Bodenseewerk Perkin Elmer Co METHOD AND INSTALLATION FOR THE AUTOMATIC PRODUCTION AND MEASUREMENT OF GASEOUS ANALYSIS SAMPLES FROM A SERIES OF SAMPLE LIQUIDS

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11360064B2 (en) * 2016-03-30 2022-06-14 3M Innovative Properties Company Oxy-pyrohydrolysis system and method for total halogen analysis

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