DE1134999B - Manufacture of cyanuric chloride that does not stick together with good flowability - Google Patents
Manufacture of cyanuric chloride that does not stick together with good flowabilityInfo
- Publication number
- DE1134999B DE1134999B DED34137A DED0034137A DE1134999B DE 1134999 B DE1134999 B DE 1134999B DE D34137 A DED34137 A DE D34137A DE D0034137 A DED0034137 A DE D0034137A DE 1134999 B DE1134999 B DE 1134999B
- Authority
- DE
- Germany
- Prior art keywords
- cyanuric chloride
- caking
- finely divided
- free
- gas
- 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
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 title claims description 24
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 239000000378 calcium silicate Substances 0.000 claims description 4
- 229910052918 calcium silicate Inorganic materials 0.000 claims description 4
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 4
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 3
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 150000003377 silicon compounds Chemical class 0.000 claims description 2
- 239000000047 product Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 3
- 229910002012 Aerosil® Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 150000004760 silicates Chemical class 0.000 description 2
- MCNLTUITFWBDSX-UHFFFAOYSA-N 4-chlorotriazin-5-amine Chemical class NC1=CN=NN=C1Cl MCNLTUITFWBDSX-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 1
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- QPJDMGCKMHUXFD-UHFFFAOYSA-N cyanogen chloride Chemical compound ClC#N QPJDMGCKMHUXFD-UHFFFAOYSA-N 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000005829 trimerization reaction Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/28—Only halogen atoms, e.g. cyanuric chloride
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
Description
DEUTSCHESGERMAN
PATENTAMTPATENT OFFICE
D34137IVd/12pD34137IVd / 12p
BEKANNTMACHUNG
DER ANMELDUNG
UND AUSGABE DER
AUSLEGESCHRIFT: 23. AUGUST 1962 NOTICE
THE REGISTRATION
AND ISSUE OF THE
EDITORIAL: AUGUST 23, 1962
Es ist bekannt, daß festes Cyanurchlorid in feinverteilter Form leicht zusammenbackt und daher bei der Lagerung oder Weiterverarbeitung Schwierigkeiten mit sich bringt.It is known that solid cyanuric chloride in finely divided form easily cakes and therefore contributes storage or further processing brings difficulties.
Es wurde nun gefunden, daß man nicht zusammenbackendes Cyanurchlorid mit einer ausgezeichneten Rieselfähigkeit und Weiterverarbeitbarkeit erhält, wenn man feinteiligem Cyanurchlorid geringe Mengen eines feinverteilten Siliciumdioxyds, Titandioxyds, Aluminiumdioxyds, Aluminiumsilikats oder Calciumsilicats zufügt. Besonders geeignet hierfür ist ein feinverteiltes Siliciumdioxyd, das durch Umsetzung einer flüchtigen Siliciumverbindung mit einem oxydierenden und/oder hydrolisierenden Gas oder Gasgemisch in der Gasphase bei erhöhter Temperatur gewonnen wurde. Ein derartiges Siliciumdioxyd ist unter dem warenzeichenrechtlich geschützten Namen »Aerosil« bekannt. Mit ähnlich gutem Erfolg lassen sich feinverteiltes, in der Gasphase gewonnenes Titandioxyd oder Aluminiumoxyd verwenden, ebenso Aluminiumsilicat oder Calciumsilicat, die durch Ausfällen aus Lösungen löslicher Alkalisilicate erhalten wurden. Meistens reichen schon Mengen von 0,3 bis 30Zo des Oxyds oder Silicats aus, um das Cyanurchlorid gut rieselfähig zu machen und ein Zusammenbacken zu verhindern.It has now been found that non-caking cyanuric chloride with excellent flowability and further processability is obtained if small amounts of a finely divided silicon dioxide, titanium dioxide, aluminum dioxide, aluminum silicate or calcium silicate are added to finely divided cyanuric chloride. A finely divided silicon dioxide obtained by reacting a volatile silicon compound with an oxidizing and / or hydrolyzing gas or gas mixture in the gas phase at elevated temperature is particularly suitable for this purpose. Such a silicon dioxide is known under the trademarked name "Aerosil". Finely divided titanium dioxide or aluminum oxide obtained in the gas phase can be used with similar success, as can aluminum silicate or calcium silicate obtained by precipitation from solutions of soluble alkali metal silicates. Mostly already amounts ranging from 0.3 to 3 0 Zo of the oxide or silicate of making free-flowing to the cyanuric chloride and prevent caking.
Man kann die feinverteilten Oxyde oder Silicate dem fertigen feinteiligen Cyanurchlorid zusetzen. Stellt man Cyanurchlorid durch Trimerisation von Chlorcyan in der Gasphase in Gegenwart eines Katalysators her, so kann man die erforderliche Menge des Oxyds oder Silikats mit Hilfe eines inerten Gases in den Produktionsgang einblasen, vorzugsweise an oder kurz vor der Stelle, wo das Cyanurchlorid kondensiert oder abgeschieden wird.The finely divided oxides or silicates can be added to the finished finely divided cyanuric chloride. If cyanuric chloride is produced by trimerization of cyanogen chloride in the gas phase in the presence of a catalyst here, the required amount of oxide or silicate can be obtained with the aid of an inert gas Blow into the production aisle, preferably at or just before the point where the cyanuric chloride condenses or is deposited.
Das erfindungsgemäß hergestellte, nicht zusammenbackende Cyanurchlorid kann mit ausgezeichnetem Erfolg zur Herstellung von Aminochlortriazinen verwendet werden. Diese Verbindungen werden durch Umsetzen von Cyanurchlorid mit Ammoniak, primären oder sekundären Aminen, vorzugsweise in Wasser, aber auch in Lösungsmitteln hergestellt. Bei der beschriebenen Umsetzung machte das Zusammenbacken des Cyanurchlorids bisher Schwierigkeiten. Es gelang häufig nicht, eine vollständige Reaktion zu erzielen, so daß das Endprodukt von nicht umgesetztem Cyanurchlorid getrennt werden mußte. Verwendet man dagegen Cyanurchlorid, das nach der Erfindung geringe Mengen von feinverteilten Oxyden oder Silikaten enthält, so ist es möglich, die Umsetzung quantitativ durchzuführen. Ein zusätzlicher Vorteil besteht darin, daß die Abfüllung der Produkte Herstellung von nicht zusammenbackendem, gut rieselfähigem CyanurchloridThe non-caking cyanuric chloride prepared according to the present invention can with excellent Success used to manufacture aminochlorotriazines. These connections are made through Reacting cyanuric chloride with ammonia, primary or secondary amines, preferably in Water, but also produced in solvents. In the implementation described, the caking made of the cyanuric chloride so far difficulties. Often a complete response was not found to achieve, so that the end product had to be separated from unreacted cyanuric chloride. If, on the other hand, cyanuric chloride is used, the small amounts of finely divided oxides according to the invention or contains silicates, it is possible to carry out the reaction quantitatively. An additional The advantage is that the filling of the products produces non-caking, free flowing cyanuric chloride
Anmelder:
Deutsche Gold- und Silber-ScheideanstaltApplicant:
German gold and silver separator
vormals Roessler,
Frankfurt/, Weißfrauenstr. 9formerly Roessler,
Frankfurt /, Weißfrauenstr. 9
TiIo Franz, Frankfurt/M.,TiIo Franz, Frankfurt / M.,
Dr. Robert Richter, Hochkirchen bei Köln,Dr. Robert Richter, Hochkirchen near Cologne,
und Dr. Gerhard Bach, Wesseling (Bez. Köln),and Dr. Gerhard Bach, Wesseling (Cologne district),
sind als Erfinder genannt wordenhave been named as inventors
infolge ihrer Rieselfähigkeit im Gegensatz zur bisherigen Arbeitsweise mühelos vonstatten geht. Bei der Arbeitsweise ohne Zusatz bereitet das Abfüllen des zusammenbackenden Produktes erhebliche Schwierigkeiten. due to its flowability, in contrast to the previous way of working, is effortless. at The method of working without additives causes considerable difficulties in filling the caked product.
Eine Menge von mehreren 100 kg feinteiligem Cyanurchlorid wird in einem dafür geeigneten Apparat mit 0,4 % Aerosil innig gemischt. Das Produkt wird durch diesen Zusatz voll rieselfähig. Diese Rieselfähigkeit bleibt dauernd erhalten, während Cyanurchlorid ohne diesen Zusatz rasch zusammenbacken würde.An amount of several 100 kg of finely divided cyanuric chloride is used in a suitable apparatus intimately mixed with 0.4% Aerosil. This additive makes the product fully free-flowing. These Flowability is permanently retained, while cyanuric chloride quickly cakes without this addition would.
Während der Kondensation von Cyanurchloriddampf wird kontinuierlich Calciumsilicat in einer Menge von 1 %, bezogen auf das Cyanurchlorid, mittels Inertgas vor der Sublimationskammer in die Dampfphase eingebracht. Das entstandene Produkt hat dieselben Eigenschaften wie das im Beispiel 1 erwähnte. During the condensation of cyanuric chloride vapor, calcium silicate is continuously in a Amount of 1%, based on the cyanuric chloride, using inert gas in front of the sublimation chamber into the Introduced vapor phase. The resulting product has the same properties as those mentioned in Example 1.
Claims (3)
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DED34137A DE1134999B (en) | 1960-08-31 | 1960-08-31 | Manufacture of cyanuric chloride that does not stick together with good flowability |
| CH918761A CH409984A (en) | 1960-08-31 | 1961-08-04 | Solid, finely divided cyanuric chloride, process for its preparation and its use for the preparation of aminochlorotriazines |
| BE607579A BE607579A (en) | 1960-08-31 | 1961-08-25 | Finely divided solid oyanuryl chloride, process for its preparation and use for the preparation of aminochlorinated triazines |
| GB30779/61A GB953590A (en) | 1960-08-31 | 1961-08-25 | A process for the production of solid, finely divided cyanuric chloride |
| SE859861A SE219752C1 (en) | 1960-08-31 | 1961-08-28 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DED34137A DE1134999B (en) | 1960-08-31 | 1960-08-31 | Manufacture of cyanuric chloride that does not stick together with good flowability |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1134999B true DE1134999B (en) | 1962-08-23 |
Family
ID=7042057
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DED34137A Pending DE1134999B (en) | 1960-08-31 | 1960-08-31 | Manufacture of cyanuric chloride that does not stick together with good flowability |
Country Status (5)
| Country | Link |
|---|---|
| BE (1) | BE607579A (en) |
| CH (1) | CH409984A (en) |
| DE (1) | DE1134999B (en) |
| GB (1) | GB953590A (en) |
| SE (1) | SE219752C1 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2435472A1 (en) * | 1978-09-11 | 1980-04-04 | Sueddeutsche Kalkstickstoff | CYANURYL CHLORIDE SUITABLE FOR A REACTION IN SOLUTION OR AQUEOUS SUSPENSION, AND METHOD FOR THE PRODUCTION THEREOF |
| EP0416584A1 (en) * | 1989-09-07 | 1991-03-13 | Lonza Ag | Process to improve the flowability of solid cyanuric chloride |
| EP1041069A1 (en) * | 1999-03-31 | 2000-10-04 | Degussa-Hüls Aktiengesellschaft | Free-flowing cyanuric chloride, process for its preparation and its use |
-
1960
- 1960-08-31 DE DED34137A patent/DE1134999B/en active Pending
-
1961
- 1961-08-04 CH CH918761A patent/CH409984A/en unknown
- 1961-08-25 BE BE607579A patent/BE607579A/en unknown
- 1961-08-25 GB GB30779/61A patent/GB953590A/en not_active Expired
- 1961-08-28 SE SE859861A patent/SE219752C1/sv unknown
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2435472A1 (en) * | 1978-09-11 | 1980-04-04 | Sueddeutsche Kalkstickstoff | CYANURYL CHLORIDE SUITABLE FOR A REACTION IN SOLUTION OR AQUEOUS SUSPENSION, AND METHOD FOR THE PRODUCTION THEREOF |
| DE2839384C2 (en) * | 1978-09-11 | 1988-09-08 | Skw Trostberg Ag, 8223 Trostberg | Mixture containing cyanuric chloride for the synthesis of cyanuric acid derivatives and process for their preparation |
| EP0416584A1 (en) * | 1989-09-07 | 1991-03-13 | Lonza Ag | Process to improve the flowability of solid cyanuric chloride |
| EP1041069A1 (en) * | 1999-03-31 | 2000-10-04 | Degussa-Hüls Aktiengesellschaft | Free-flowing cyanuric chloride, process for its preparation and its use |
| US6290925B1 (en) | 1999-03-31 | 2001-09-18 | Degussa Ag | Flowable cyanuric chloride, process for the production thereof and use thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CH409984A (en) | 1966-03-31 |
| BE607579A (en) | 1961-12-18 |
| SE219752C1 (en) | 1968-04-02 |
| GB953590A (en) | 1964-03-25 |
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