DE1266288B - Carbonyl diisocyanate and process for its preparation - Google Patents

Carbonyl diisocyanate and process for its preparation

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Publication number
DE1266288B
DE1266288B DEN27093A DEN0027093A DE1266288B DE 1266288 B DE1266288 B DE 1266288B DE N27093 A DEN27093 A DE N27093A DE N0027093 A DEN0027093 A DE N0027093A DE 1266288 B DE1266288 B DE 1266288B
Authority
DE
Germany
Prior art keywords
carbonyl
diisocyanate
preparation
carbonyl diisocyanate
temperatures
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
Application number
DEN27093A
Other languages
German (de)
Inventor
Dr Edgar Nachbaur
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
EDGAR NACHBAUR DR
Original Assignee
EDGAR NACHBAUR DR
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by EDGAR NACHBAUR DR filed Critical EDGAR NACHBAUR DR
Priority to DEN27093A priority Critical patent/DE1266288B/en
Publication of DE1266288B publication Critical patent/DE1266288B/en
Pending legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C265/00—Derivatives of isocyanic acid
    • C07C265/16—Derivatives of isocyanic acid having isocyanate groups acylated
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C263/00—Preparation of derivatives of isocyanic acid
    • C07C263/08—Preparation of derivatives of isocyanic acid from or via heterocyclic compounds, e.g. pyrolysis of furoxans
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C275/00—Derivatives of urea, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
    • C07C275/44—Derivatives of urea, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups having nitrogen atoms of urea groups doubly-bound to carbon atoms

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

Carbonyldiisocyanat und Verfahren zu dessen Herstellung Gegenstand der Erfindung ist Carbonyldiisocyanat der Formel CO(NCO)2 und ein Verfahren zu dessen Herstellung durch Thermolyse von Trichlorisocyanursäure.Carbonyl diisocyanate and process for its preparation subject matter of the invention is carbonyl diisocyanate of the formula CO (NCO) 2 and a process for the same Manufactured by thermolysis of trichloroisocyanuric acid.

Es wurde gefunden, daß man Carbonyldiisocyanat erhält, wenn man Trichlorisocyanursäure bei Temperaturen von 200 bis 400"C in einer Inertgasatmosphäre thermisch zersetzt. Das Verfahren läßt sich durch die folgende Reaktionsgleichung wiedereben: Trichlorisocyanursäure Im Verlauf der Reaktion traten als Nebenprodukte Spuren von Cl2 und CO auf.It has been found that carbonyl diisocyanate is obtained if trichloroisocyanuric acid is thermally decomposed at temperatures of 200 to 400 ° C. in an inert gas atmosphere. The process can be represented by the following reaction equation: Trichloroisocyanuric acid In the course of the reaction, traces of Cl2 and CO appeared as by-products.

Die Durchführbarkeit dieses Verfahrens ist sehr überraschend, da Chlor-Stickstoff-Verbindungen im allgemeinen beim Erhitzen explosionsartig und völlig unkontrollierbar zerfallen. The feasibility of this procedure is very surprising since Chlorine-nitrogen compounds in general explosive and completely when heated disintegrate uncontrollably.

Das Verfahren kann im allgemeinen so durchgeführt werden, daß man Trichlorisocyanursäure in einem geschlossenen Gefäß unter Hindurchleiten eines inerten Gases auf die Reaktionstemperatur erhitzt. The process can generally be carried out so that one Trichloroisocyanuric acid in a closed vessel while an inert one is passed through Gas heated to the reaction temperature.

Diese Temperatur liegt oberhalb des Zersetzungspunktes von Trichlorisocyanursäure, d. h. oberhalb von 200"C und kann bis 400"C ansteigen, vorzugsweise verwendet man Temperaturen zwischen 250 und 270"C. Das mit dem Inertgas übergehende Gemisch aus Carbonyldiisocyanat, NCl3 und Chlor kann gereinigt werden, indem man es durch eine Säule mit festem, wasserfreiem Kupfer(I)-chlorid leitet. Diese Reinigungsoperation kann vorzugsweise bei Temperaturen von 150 bis 180"C durchgeführt werden und-ist leicht an der fortschreitenden Verfärbung der zunächst schwach grünen Säulenfüllung nach Braunschwarz zu verfolgen.This temperature is above the decomposition point of trichloroisocyanuric acid, d. H. above 200 "C and can rise to 400" C, is preferably used Temperatures between 250 and 270 "C. The mixture passing over with the inert gas Carbonyl diisocyanate, NCl3 and chlorine can be purified by passing it through a Column with solid, anhydrous copper (I) chloride passes. This cleaning operation can preferably be carried out at temperatures of 150 to 180 ° C. and is slightly by the progressive discoloration of the initially pale green column filling to pursue to Braunschwarz.

Inerte Gase, die für das Verfahren geeignet sind, sind beispielsweise Stickstoff oder Edelgase. Eine für das Verfahren geeignete Vorrichtung wird in der Figur gezeigt. Es bedeutet 1 Reaktionsgefäß, 2 Zuführung für Inergas, 3 Heizmantel, 4 Heizbad (Metallbad), 5 Produktleitung, 6 U-Rohr (enthaltend CuCl), 7 Heizbad (Öl), 8 Leitung für Endprodukt. Inert gases that are suitable for the process are, for example Nitrogen or noble gases. An apparatus suitable for the method is disclosed in Figure shown. It means 1 reaction vessel, 2 feeds for inert gas, 3 heating mantles, 4 heating bath (metal bath), 5 product line, 6 U-tube (containing CuCl), 7 heating bath (oil), 8 End product line.

Das Carbonyldiisocyanat ist neu. Es ist eine stark lichtbrechende wasserklare Flüssigkeit von erstickendem Geruch mit einem Siedepunkt von 103,5° Cl 705mm Hg. Die Verbindung ist löslich in inerten organischen Lösungsmitteln. Sie kann für eine Vielzahl von chemischen Umsetzungen benutzt werden. The carbonyl diisocyanate is new. It is a highly refractive one water-clear liquid with a suffocating odor with a boiling point of 103.5 ° Cl 705mm Hg. The compound is soluble in inert organic solvents. she can be used for a variety of chemical reactions.

So reagiert sie z. B. mit Ammoniak zum Carbonyldiharnstoff gemäß mit Alkohol zum Carbonyldiurethan gemäß Beispiel 10 g Trichlorisocyanursäure (Reinheit 95 bis 9901, aktives Chlor) wurde in das Reaktionsgefäß 1 der Figur eingetragen. Das Gefäß wird dann auf eine Temperatur von 260"C geheizt, während durch die Leitung 2 ein langsamer Stickstoffstrom zugeführt wird. Die aus dem Reaktionsgefäß 1 abströmenden Gase werden über Kupfer(I)-chlorid gereinigt. Nach dem Abkühlen der Reaktionsgase wird das Carbonyl- diisocaynat als stark lichtbrechende wasserklare Flüssigkeit vom Siedepunkt 103,5°Cl705mm Hg in einer Ausbeute von 73010 der Theorie erhalten.So she reacts z. B. with ammonia to the carbonyl diurea according to with alcohol to the carbonyl diurethane according to Example 10 g of trichloroisocyanuric acid (purity 95 to 9901, active chlorine) were introduced into reaction vessel 1 in the figure. The vessel is then heated to a temperature of 260 "C, while a slow stream of nitrogen is fed in through line 2. The gases flowing out of the reaction vessel 1 are cleaned using copper (I) chloride. After the reaction gases have cooled, the carbonyl Diisocaynate was obtained as a highly refractive, water-clear liquid with a boiling point of 103.5 ° Cl705mm Hg in a yield of 73010 of theory.

Claims (3)

Patentansprüche: 1. Carbonyldiisocyanat. Claims: 1. Carbonyl diisocyanate. 2. Verfahren zur Herstellung von Carbonyldiisocyanat, dadurch gekennzeichnet, daß man Trichlorisocyanursäure bei Temperaturen von 200 bis 400"C in einer Inertgasatmosphäre thermisch zersetzt. 2. Process for the preparation of carbonyl diisocyanate, characterized in that that he Trichloroisocyanuric acid at temperatures from 200 to 400 "C in an inert gas atmosphere thermally decomposed. 3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß man das rohe Carbonyldiisocyanat durch Überleiten über Kupfer(I)-chlorid bei Temperaturen von 150 bis 180O C von Nebenprodukten, besonders von Stickstofftrichlorid, befreit. 3. The method according to claim 2, characterized in that the crude carbonyl diisocyanate by passing over copper (I) chloride at temperatures freed from 150 to 180 ° C of by-products, especially nitrogen trichloride.
DEN27093A 1965-07-27 1965-07-27 Carbonyl diisocyanate and process for its preparation Pending DE1266288B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEN27093A DE1266288B (en) 1965-07-27 1965-07-27 Carbonyl diisocyanate and process for its preparation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEN27093A DE1266288B (en) 1965-07-27 1965-07-27 Carbonyl diisocyanate and process for its preparation

Publications (1)

Publication Number Publication Date
DE1266288B true DE1266288B (en) 1968-04-18

Family

ID=7344119

Family Applications (1)

Application Number Title Priority Date Filing Date
DEN27093A Pending DE1266288B (en) 1965-07-27 1965-07-27 Carbonyl diisocyanate and process for its preparation

Country Status (1)

Country Link
DE (1) DE1266288B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3941873A (en) * 1974-03-12 1976-03-02 Bayer Aktiengesellschaft Process for the preparation of carbonyl diisocyanate

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3941873A (en) * 1974-03-12 1976-03-02 Bayer Aktiengesellschaft Process for the preparation of carbonyl diisocyanate

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