DE4009252C1 - Continuous measurement of chlorine in cyanuric chloride synthesis - by condensing part of the gas mixt. and sepg. it to measure chlorine using a photometer - Google Patents
Continuous measurement of chlorine in cyanuric chloride synthesis - by condensing part of the gas mixt. and sepg. it to measure chlorine using a photometerInfo
- Publication number
- DE4009252C1 DE4009252C1 DE19904009252 DE4009252A DE4009252C1 DE 4009252 C1 DE4009252 C1 DE 4009252C1 DE 19904009252 DE19904009252 DE 19904009252 DE 4009252 A DE4009252 A DE 4009252A DE 4009252 C1 DE4009252 C1 DE 4009252C1
- Authority
- DE
- Germany
- Prior art keywords
- chlorine
- photometer
- gas
- cyanuric chloride
- continuous measurement
- 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
Links
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 7
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 7
- 229910052801 chlorine Inorganic materials 0.000 title claims description 20
- 239000000460 chlorine Substances 0.000 title claims description 20
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title claims description 18
- 238000005259 measurement Methods 0.000 title abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract description 11
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 7
- QPJDMGCKMHUXFD-UHFFFAOYSA-N cyanogen chloride Chemical compound ClC#N QPJDMGCKMHUXFD-UHFFFAOYSA-N 0.000 claims description 6
- NCSHGROOCJHAFK-UHFFFAOYSA-N [Cl].N#CC#N Chemical compound [Cl].N#CC#N NCSHGROOCJHAFK-UHFFFAOYSA-N 0.000 claims 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 abstract 2
- 239000000126 substance Substances 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 230000002528 anti-freeze Effects 0.000 description 1
- 150000001804 chlorine Chemical class 0.000 description 1
- SJXIVKQAVJISKW-UHFFFAOYSA-N chloro cyanate Chemical compound ClOC#N SJXIVKQAVJISKW-UHFFFAOYSA-N 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/0052—Gaseous halogens
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/14—Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation
- G01N25/142—Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation by condensation
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
Die Erfindung betrifft ein Verfahren und eine Vorrichtung zur Bestimmung der Chlorgaskonzentration in Chlorcyangas bei der Cyanurchloridsynthese.The invention relates to a method and a Device for determining the chlorine gas concentration in chlorine cyanide gas during cyanuric chloride synthesis.
Das zur Synthese von Cyanurchlorid eingesetzte Chlorcyangas sollte 1 bis 2,5 Vol.-% freies Chlor enthalten. Dieser Chlorgehalt spielt eine wichtige Rolle für die Lebensdauer des Aktivkohle-Katalysators.The one used for the synthesis of cyanuric chloride Chlorine cyanide gas should contain 1 to 2.5 vol .-% free chlorine contain. This chlorine content plays an important role Roll for the life of the activated carbon catalyst.
Bisher wurde der Chlorgehalt in solchen Gasgemischen in periodischen Abständen meist naßchemisch bestimmt. Dieses Verfahren hat jedoch den Nachteil, daß kurzfristige Schwankungen von Prozeßparametern, wie Temperatur oder Druck, die sich auch auf die Chlorgaskonzentration auswirken, nicht erfaßt werden können und dadurch negative Auswirkungen auf die Standzeit des Katalysators hervorgerufen werden.So far, the chlorine content in such gas mixtures mostly determined periodically by wet chemistry. However, this method has the disadvantage that short-term fluctuations in process parameters, such as Temperature or pressure, which also affects the Chlorine gas concentration affect, not be detected can and thereby have negative effects on the Service life of the catalyst can be caused.
Aus der US-PS 38 97 541 ist es bekannt, Chlorcyan aus Blausäure und Chlor herzustellen. Die Ausbeute an Chlorcyan wird dabei durch IR-Spektrometrie der C-N- Bande und der C-H-Bande bestimmt. Weiterhin ist es aus der EP-OS 00 54 957 bekannt, Chlorkonzentrationen in Gasgemischen photometrisch zu messen. Aus keiner dieser Schriften ist jedoch ein Hinweis zu entnehmen, wie man die Chlorgaskonzentration in Chlorcyangas bei der Cyanurchloridsynthese bestimmen kann.From US-PS 38 97 541 it is known to chlorine from To produce hydrocyanic acid and chlorine. The yield at Chlorine cyanide is determined by IR spectrometry of the C-N Band and the C-H band determined. Furthermore it is over known from EP-OS 00 54 957, chlorine concentrations in Measure gas mixtures photometrically. None however, there is a note in these writings how to add the chlorine gas concentration in chlorine cyanide gas can determine the cyanuric chloride synthesis.
Es war daher die Aufgabe der vorliegenden Erfindung, ein Verfahren und eine Vorrichtung zur Bestimmung der Chlorgaskonzentration in Chlorcyangas bei der Cyanurchloridsynthese zu entwickeln, das eine kontinuierliche Messung mit kurzer Ansprechzeit gewährleistet.It was therefore the object of the present invention a method and an apparatus for determining the Chlorine gas concentration in chlorine cyanide at To develop cyanuric chloride synthesis, the one continuous measurement with short response time guaranteed.
Diese Aufgabe wird erfindungsgemäß dadurch gelöst, daß ein Teilstrom des Chlorcyan-/Chlorgasgemisches kondensiert und die Chlorkonzentration im Chlorcyankondensat photometrisch kontinuierlich gemessen wird.This object is achieved in that a partial stream of the chlorine / chlorine gas mixture condensed and the chlorine concentration in the Chlorine cyanate condensate continuously is measured.
Die entsprechende Meßvorrichtung ist gekennzeichnet durch einen Kondensator zur Kondensation des Chlorcyan-/Chlorgasgemisches und einer daran angekoppelten, mit einem Überlauf, einem Photometer und einem Ablauf versehenen Durchflußzelle.The corresponding measuring device is marked through a condenser to condense the Chlorine / chlorine gas mixture and one on it coupled, with an overflow, a photometer and a drainage flow cell.
Der Kondensator und die Durchflußzelle bestehen aus einem gegen Chlorgas und Chlorcyangas beständigen Material, vorzugsweise aus Glas. Als Photometer verwendet man vorteilhafterweise einen Zweistrahl-Prozeßphotometer. Der zur Gaskondensation benötigte Kühlkreislauf besteht aus einem Wasser/Frostschutzmittel-Gemisch, das mit Hilfe eines Durchlaufkühlers auf die erforderliche Kondensationstemperatur von 2 bis 4°C abgekühlt wird.The condenser and the flow cell consist of one resistant to chlorine gas and chlorine gas Material, preferably made of glass. As a photometer one advantageously uses one Two-beam process photometer. The one for gas condensation required cooling circuit consists of a Water / antifreeze mixture, which with the help of a Flow chiller to the required Condensation temperature of 2 to 4 ° C is cooled.
Die Abbildung zeigt schematisch eine beispielhafte Ausführungsform der erfindungsgemäßen Meßvorrichtung im Längsschnitt.The figure shows an example Embodiment of the measuring device according to the invention in longitudinal section.
Die Meßvorrichtung besteht aus einer an der Transportleitung des Chlorcyan-/ Chlorgasgemisches angebrachten Zuleitung (1) mit einer Fritte (2), deren Porengröße die Durchflußmenge des Teilstromgasgemisches bestimmt und feste Verunreinigungen zurückhält. Die Zuleitung (1) verläuft hinter der Fritte (2) wendelförmig in einem Kondensator (3), der mit Zu- (11) und Ableitung (12) für das Kühlmittelgemisch versehen ist. Die Zuleitung (1) endet in einem senkrecht stehenden Rohr (4), in das das Chlorcyan-/Chlorkondensat fließt.The measuring device consists of a feed line ( 1 ) attached to the transport line of the chlorine / chlorine gas mixture with a frit ( 2 ), the pore size of which determines the flow rate of the partial flow gas mixture and retains solid impurities. The supply line ( 1 ) extends behind the frit ( 2 ) in a spiral shape in a condenser ( 3 ) which is provided with supply ( 11 ) and discharge ( 12 ) for the coolant mixture. The feed line ( 1 ) ends in a vertical pipe ( 4 ) into which the chlorine / chlorine condensate flows.
Nichtkondensierbare, gasförmige Verunreinigungen entweichen nach oben und werden über eine Ableitung (10) abgeführt. Das Chlorcyan-/Chlorkondensat gelangt in die an das Rohr (4) angeflanschte Durchflußzelle (5), in die ein Überlauf (6) eingebaut ist. An dieser Meßstrecke (8) ist ein Photometer (7) an der Durchflußzelle (5) angebracht, das die Chlorkonzentration mißt. Das über den Überlauf (6) aus der Meßstrecke (8) abgelaufene Kondensat wird über einen Ablauf (9) aus der Durchflußzelle (5) entfernt und der Transportleitung wieder zugeführt.Non-condensable, gaseous contaminants escape upwards and are discharged via a discharge line ( 10 ). The chlorine / chlorine condensate enters the flow cell ( 5 ) flanged to the pipe ( 4 ), into which an overflow ( 6 ) is installed. At this measuring path (8) a photometer (7) is attached to the flow cell (5) which measures the concentration of chlorine. The past via the overflow (6) from the measuring section (8) the condensate is fed removed via an outlet (9) of the flow cell (5) and the transport line again.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19904009252 DE4009252C1 (en) | 1990-03-22 | 1990-03-22 | Continuous measurement of chlorine in cyanuric chloride synthesis - by condensing part of the gas mixt. and sepg. it to measure chlorine using a photometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19904009252 DE4009252C1 (en) | 1990-03-22 | 1990-03-22 | Continuous measurement of chlorine in cyanuric chloride synthesis - by condensing part of the gas mixt. and sepg. it to measure chlorine using a photometer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE4009252C1 true DE4009252C1 (en) | 1991-06-20 |
Family
ID=6402841
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19904009252 Expired - Lifetime DE4009252C1 (en) | 1990-03-22 | 1990-03-22 | Continuous measurement of chlorine in cyanuric chloride synthesis - by condensing part of the gas mixt. and sepg. it to measure chlorine using a photometer |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE4009252C1 (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3897541A (en) * | 1971-11-23 | 1975-07-29 | Bayer Ag | Process for preparing pure cyanogen chloride |
| EP0054957A1 (en) * | 1980-12-23 | 1982-06-30 | E.I. Du Pont De Nemours And Company | Method and apparatus for photometrically monitoring the concentration of both chlorine and chlorine dioxide |
-
1990
- 1990-03-22 DE DE19904009252 patent/DE4009252C1/en not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3897541A (en) * | 1971-11-23 | 1975-07-29 | Bayer Ag | Process for preparing pure cyanogen chloride |
| EP0054957A1 (en) * | 1980-12-23 | 1982-06-30 | E.I. Du Pont De Nemours And Company | Method and apparatus for photometrically monitoring the concentration of both chlorine and chlorine dioxide |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| 8100 | Publication of patent without earlier publication of application | ||
| D1 | Grant (no unexamined application published) patent law 81 | ||
| 8364 | No opposition during term of opposition | ||
| 8327 | Change in the person/name/address of the patent owner |
Owner name: DEGUSSA-HUELS AG, 60311 FRANKFURT, DE |
|
| 8327 | Change in the person/name/address of the patent owner |
Owner name: DEGUSSA AG, 40474 DUESSELDORF, DE |
|
| 8327 | Change in the person/name/address of the patent owner |
Owner name: DEGUSSA GMBH, 40474 DUESSELDORF, DE |
|
| 8327 | Change in the person/name/address of the patent owner |
Owner name: EVONIK DEGUSSA GMBH, 40474 DUESSELDORF, DE |