DE1216316B - Improved process for the continuous production of melamine - Google Patents
Improved process for the continuous production of melamineInfo
- Publication number
- DE1216316B DE1216316B DEST18064A DEST018064A DE1216316B DE 1216316 B DE1216316 B DE 1216316B DE ST18064 A DEST18064 A DE ST18064A DE ST018064 A DEST018064 A DE ST018064A DE 1216316 B DE1216316 B DE 1216316B
- Authority
- DE
- Germany
- Prior art keywords
- catalyst
- melamine
- layer
- vapors
- urea
- 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
- 229920000877 Melamine resin Polymers 0.000 title claims description 9
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 title claims description 9
- 238000000034 method Methods 0.000 title claims description 8
- 238000010924 continuous production Methods 0.000 title claims description 3
- 239000003054 catalyst Substances 0.000 claims description 29
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 239000004202 carbamide Substances 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 230000000284 resting effect Effects 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 1
- 239000011949 solid catalyst Substances 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
- C07D251/40—Nitrogen atoms
- C07D251/54—Three nitrogen atoms
- C07D251/56—Preparation of melamine
- C07D251/60—Preparation of melamine from urea or from carbon dioxide and ammonia
-
- 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
- C07D251/40—Nitrogen atoms
- C07D251/54—Three nitrogen atoms
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Description
BUNDESREPUBLIK DEUTSCHLAND DEUTSCHES 40JTWW PATENTAMTFEDERAL REPUBLIC OF GERMANY GERMAN 40JTWW PATENT OFFICE Int. α.:Int. α .:
C07dC07d
AUSLEGESCHRIFTEDITORIAL
Deutsche Kl.: 12 ρ -10/05 German class: 12 ρ - 10/05
Nummer: 1216 316Number: 1216 316
Aktenzeichen: St 18064IV d/12 ρFile number: St 18064IV d / 12 ρ
Anmeldetag: 12. Juli 1961Filing date: July 12, 1961
Auslegetag: 12. Mai 1966Opening day: May 12, 1966
: Die Erfindung betrifft eine Verbesserung des den Gegenstand des Patens 1102165 bildenden Verfahrens zur kontinuierlichen Herstellung von Melamin durch aufeinanderfolgendes Erhitzen von Harnstoff und bzw. oder einem durch thermische Zersetzung von Harnstoff gebildeten Produkt mit Ammoniak in Gegenwart eines Katalysators mit großer innerer Oberfläche in zwei getrennten Umsetzungsräumen, wobei der Harnstoff und bzw. oder sein thermisches Zersetzungsprodukt zusammen mit Ammoniak zunächst einer auf etwa 350° C erhitzten Katalysatorwirbelschicht, wie sie für die Melaminsynthese an sich bekanntermaßen gebraucht wird, zugeleitet wird und die abziehenden Gase und Dämpfe durch eine auf etwa 3300C gehaltene Katalysatorruheschicht geführt werden, worauf aus den die Katalysatorruheschicht verlassenden Gasen und Dämpfen das gebildete Melamin durch Abkühlen abgeschieden wird. : The invention relates to an improvement of the subject of patent 1102165 forming process for the continuous production of melamine by successive heating of urea and / or a product formed by thermal decomposition of urea with ammonia in the presence of a catalyst with a large internal surface in two separate reaction rooms wherein the urea and or or its thermal decomposition product together initially a heated to about 350 ° C catalyst fluidized bed, such as is used for the melamine synthesis per se known, is fed with ammonia and withdrawing gases and vapors through to about 330 0 C. The catalyst resting layer held, whereupon the melamine formed is deposited by cooling from the gases and vapors leaving the catalyst resting layer.
Dieses Verfahren weist den Nachteil auf, daß zur ao Erreichung eines möglichst hohen Umsetzungsgrades relativ große Katalysatormengen erforderlich sind. So braucht man z. B. in der Katalysatorruheschicht 1700 kg Kieselkörner, wenn diese Schicht durch Kühlung auf 330° C gehalten wird und wenn der Katalysatorwirbelschicht stündlich 100 kg Harnstoff zugesetzt wird. Der Umsetzungsgrad beträgt in diesem Fall 96%.This process has the disadvantage that in order to achieve the highest possible degree of conversion relatively large amounts of catalyst are required. So you need z. B. in the catalyst rest layer 1700 kg of silica grains if this layer is kept at 330 ° C by cooling and if the catalyst fluidized bed 100 kg of urea is added every hour. The degree of conversion in this case is 96%.
Wird die Katalysatorruheschicht auf einer Temperatur von 350° C gehalten, so muß diese Schicht 825 kg Kieselkörner enthalten, damit bei gleichen Harnstoffzusatz ein Umsetzungsgrad von 94% vom theoretisch möglichen Höchstwert erreicht" wird. Bei höheren Temperaturen geht der Umsetzungsgrad zurück.If the catalyst resting layer is kept at a temperature of 350 ° C., this layer must Contains 825 kg of silica grains, so with the same addition of urea a degree of conversion of 94% of Theoretically possible maximum value is reached ". At higher temperatures, the degree of conversion goes down return.
Aus der britischen Patentschrift 767 344 ist ein Verfahren zur Herstellung von Melamin bekannt, wobei man Harnstoff und/oder ein durch thermische Zersetzung von Harnstoff gebildetes Produkt in Anwesenheit von NH3 und eines Katalysators mit großer innerer Oberfläche auf Temperaturen von 220 bis 400° C erhitzt.A process for the production of melamine is known from British patent specification 767 344, in which urea and / or a product formed by thermal decomposition of urea is heated to temperatures of 220 to 400 ° C. in the presence of NH 3 and a catalyst with a large internal surface area .
Bei einer Ausführungsform dieses Verfahrens wurde erörtert, drei verschiedene z. B. hintereinandergeschaltete Katalysatorwirbelschichten mit steigenden Temperaturen anzuwenden, wobei dann der feste Katalysator von der einen nach der folgenden Wirbelschicht befördert wird.In one embodiment of this method it has been discussed to use three different e.g. B. cascaded To apply fluidized catalyst beds with increasing temperatures, then the solid catalyst from one to the next Fluidized bed is conveyed.
Dieser Feststofftransport und das Wirbeln des Katalysators in verschiedenen Schichten erfordert einen großen Energieaufwand.This transport of solids and the swirling of the catalyst in different layers requires a large amount of energy.
Gemäß der Erfindung sind große Einsparungen Verbessertes Verfahren zur kontinuierlichen
Herstellung von MelaminAccording to the Invention, Big Savings Are Improved Process For Continuous
Manufacture of melamine
Zusatz zum Patent: 1102 165Addendum to the patent: 1102 165
Anmelder:Applicant:
Stamicarbon N. V., Heerlen (Niederlande)Stamicarbon N.V., Heerlen (Netherlands)
Vertreter:Representative:
Dr. F. Zumstein,Dr. F. Zumstein,
Dipl.-Chem. Dr. rer. nat. E. AssmannDipl.-Chem. Dr. rer. nat. E. Assmann
und Dipl.-Chem. Dr. R. Koenigsberger,and Dipl.-Chem. Dr. R. Koenigsberger,
Patentanwälte, München 2, Bräuhausstr. 4Patent Attorneys, Munich 2, Bräuhausstr. 4th
Als Erfinder benannt:
Johannes Joseph Steggerda,
Geleen (Niederlande)Named as inventor:
Johannes Joseph Steggerda,
Geleen (Netherlands)
Beanspruchte Priorität:Claimed priority:
Niederlande vom 14. Juli 1960 (253 816)Netherlands of July 14, 1960 (253 816)
an Katalysator- und Energiekosten möglich, wenn man im zuerst von den Dämpfen durchströmten Teil der Katalysatorruheschicht oder im Fall mehrerer seriengeschalteter Katalysatorruheschichten in den zuerst durchströmten Schichten die Temperatur von etwa 350 bis zu 375 bis 425° C ansteigen läßt, worauf durch Kühlung des restlichen Teils der Katalysatorruheschicht oder der Katalysatorruheschichten die Temperatur der austretenden Dämpfe auf etwa 350° C oder darunter herabgesetzt wird.possible in terms of catalyst and energy costs if the vapors flowed through the first Part of the catalyst rest layer or in the case of several catalyst rest layers connected in series in the layers through which the air flows first, the temperature rises from around 350 to 375 to 425 ° C leaves, followed by cooling the remaining part of the catalyst rest layer or layers the temperature of the escaping vapors is reduced to about 350 ° C or below.
Wenn z. B. die mit einer Temperatur von 350° C eintretenden Dämpfe die Temperatur im unteren Teil der Ruheschicht bis zu 400° C ansteigen lassen, worauf durch Kühlung im oberen Teil die Temperatur der austretenden Dämpfe wieder auf 350° C zurückversetzt wird, so braucht die Ruheschicht nur kg Katalysator zu enthalten, dagegen aber kg, wenn die ganze Ruheschicht auf 350° C gehalten wird.If z. B. the entering with a temperature of 350 ° C vapors the temperature in the lower part Let the rest layer rise up to 400 ° C, whereupon the temperature is increased by cooling in the upper part the escaping vapors is set back to 350 ° C, the rest shift only needs kg of catalyst, but kg if the entire rest shift is kept at 350 ° C will.
Die Ersparung an Katalysatormenge beträgt also 38%.The amount of catalyst saved is therefore 38%.
Selbstverständlich kann man beim erfindungsgemäßen Verfahren statt nur einer Katalysatorruhe-Of course, in the process according to the invention, instead of just a catalyst rest
. - 609 568/549. - 609 568/549
schicht auch mehrere, ζ. B. zwei seriengeschaltete Katalysatorschichten-anwenden und in diesem Fall in der von den Dämpfen zuerst durchströmten Katalysatorschicht eine Temperatur von 375 bis 425° C und in der darauffolgenden Katalysatorschicht eine Temperatur von 350°'C (oder niedriger) aufrechterhalten, r; ;; ';■. \/_! -"_'_.""-. .■..;-.-.-layer several, ζ. B. use two series-connected catalyst layers and in this case maintain a temperature of 375 to 425 ° C. in the catalyst layer through which the vapors first flow and a temperature of 350 ° C. (or lower) in the subsequent catalyst layer, r; ;; '; ■. \ / _! - "_'_.""-.. ■ ..; -.-.-
Claims (1)
■Britische Patentschrift Nr. 767 344. .. - ..Considered publications:
■ British patent specification No. 767 344 ... - ..
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| NL1216316X | 1960-07-14 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1216316B true DE1216316B (en) | 1966-05-12 |
Family
ID=19872036
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEST18064A Pending DE1216316B (en) | 1960-07-14 | 1961-07-12 | Improved process for the continuous production of melamine |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE1216316B (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB767344A (en) * | 1952-01-17 | 1957-01-30 | American Cyanamid Co | Improvements relating to the production of melamine and/or cyanamide |
-
1961
- 1961-07-12 DE DEST18064A patent/DE1216316B/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB767344A (en) * | 1952-01-17 | 1957-01-30 | American Cyanamid Co | Improvements relating to the production of melamine and/or cyanamide |
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