CH210742A - Process for the production of nickel phthalocyanine. - Google Patents

Process for the production of nickel phthalocyanine.

Info

Publication number
CH210742A
CH210742A CH210742DA CH210742A CH 210742 A CH210742 A CH 210742A CH 210742D A CH210742D A CH 210742DA CH 210742 A CH210742 A CH 210742A
Authority
CH
Switzerland
Prior art keywords
production
nickel
paratoluene
phthalimide
nickel phthalocyanine
Prior art date
Application number
Other languages
German (de)
Inventor
Montecatini Societa G Agricola
Original Assignee
Montedison Spa
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 Montedison Spa filed Critical Montedison Spa
Publication of CH210742A publication Critical patent/CH210742A/en

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B47/00—Porphines; Azaporphines
    • C09B47/04—Phthalocyanines abbreviation: Pc
    • C09B47/06—Preparation from carboxylic acids or derivatives thereof, e.g. anhydrides, amides, mononitriles, phthalimide, o-cyanobenzamide

Landscapes

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

Description

  

  Zusatzpatent zum Hauptpatent     Nr.    207346.    Verfahren zur Herstellung von     Nickelphtbaloeyanin.       Im Hauptpatent ist ein Verfahren zur  Herstellung von     Kupferphthaloeyanin    be  schrieben, bei welchem man     Phthalsäure    oder  deren     Anhydride    mit Kupfer oder Kupfer  abgebenden Stoffen in Gegenwart von     Di-          eyandiamid    erhitzt.  



  Nach dem Zusatzpatent     Nr.   <B>208879</B> -wird  analog     Kupferplithaloeyanin    erhalten, wenn  man     Phthalsäure    durch     Phthalimid    ersetzt.  



  Es wurde nun gefunden, da man eben  falls     Nickelphthaloeyanin    herstellen kann,  wenn man     Phthalimid    mit Nickel oder  nickelabgebenden Stoffen in Gegenwart von       Dieyandiamid    erhitzt.  



  Das Verfahren kann wie das Verfahren  des Hauptpatentes durchgeführt werden.  Man kann auch ein gewisses Quantum     Para-          toluolsulfamid    und Stoffe, die das     Sehmel-          zen    und die Kondensation begünstigen, wie  zum Beispiel     Paratoluolsulfochlorid,    hinzu  fügen.    Die erhaltenen Rohprodukte lassen sich  leicht reinigen, zum Beispiel durch siedende  Extraktion mit verdünnter Salzsäure und  darauf mit verdünnter Natronlauge.  



  <I>Beispiel:</I>  In einem eisernen, mit starkem     Rührer     versehenen offenen Gefäss, werden<B>100 g</B>       Phthalimid,   <B>80 g</B>     Dieyandiamid    und 40<B>g</B>  kristallisiertes Nickelchlorid oder<B>100 g</B>       Phthalimid,    120<B>g</B> einer Mischung von     Di-          cyandiamid    und     Paratoluolsulfamid    und  40<B>g</B> kristallisiertes Nickelchlorid gemischt  und langsam auf zirka     240-260'   <B>C</B> er  hitzt, bis die     Farbstoffbildung    nicht mehr  zunimmt. Die anfänglich flüssige Masse  wird immer     diekflüssiger    und zuletzt fest.

    Nach erfolgter Abkühlung wird die Masse  aus dem Apparat herausgenommen, gemah  len und mit verdünnter Salzsäure und an  schliessend mit verdünnter Natronlauge     ko-          cliend    extrahiert. Man erhält eine gute Aus-      beute an     blauo-rünliellem    Farbstoff.

   Wenn  man ihn in<B>10-15</B> Teilen Schwefelsäure  löst und allmählich Wasser bis zu einer  Säurekonzentration von<B>78%</B> zufügt, so  scheidet das Pigment als     Sulfat    aus, welches  nach     Filfrieren    auf einem Porzellanfilter  und eventuellem Waschen mit<B>60'</B> N  Schwefelsäure sich mit Wasser zu schönen  Kristallen mit metallischem Glanz     und    in  chemisch reinem Zustand     hydrolysiert.  



  Additional patent to main patent No. 207346. Process for the production of Nickelphtbaloeyanin. In the main patent, a process for the production of copper phthaloeyanine is described in which phthalic acid or its anhydrides are heated with copper or copper-releasing substances in the presence of di-eyandiamide.



  According to additional patent no. <B> 208879 </B> - copper plithaloeyanine is obtained analogously when phthalic acid is replaced by phthalimide.



  It has now been found that nickel phthaloeyanine can also be produced if phthalimide is heated with nickel or nickel-releasing substances in the presence of dieyandiamide.



  The method can be carried out like the method of the main patent. You can also add a certain amount of paratoluene sulphamide and substances that promote simmering and condensation, such as paratoluene sulphonyl chloride. The crude products obtained can be easily cleaned, for example by boiling extraction with dilute hydrochloric acid and then with dilute sodium hydroxide solution.



  <I> Example: </I> In an iron open vessel equipped with a powerful stirrer, <B> 100 g </B> phthalimide, <B> 80 g </B> dieyandiamide and 40 <B> g </ B> crystallized nickel chloride or <B> 100 g </B> phthalimide, 120 <B> g </B> of a mixture of dicyandiamide and paratoluene sulfamide and 40 <B> g </B> crystallized nickel chloride and mixed slowly to approx 240-260 '<B> C </B> until the dye no longer forms. The initially liquid mass becomes more and more liquid and finally solid.

    After cooling, the mass is removed from the apparatus, ground and extracted with a co-solution with dilute hydrochloric acid and then with dilute sodium hydroxide solution. A good yield of blue-green dye is obtained.

   If you dissolve it in <B> 10-15 </B> parts of sulfuric acid and gradually add water up to an acid concentration of <B> 78% </B>, the pigment separates out as sulfate, which after filtering on a porcelain filter and possibly washing with <B> 60 '</B> N sulfuric acid hydrolyzes with water to beautiful crystals with a metallic sheen and in a chemically pure state.

Claims (1)

PATENTANSPRUCH: Verfahren zur Herstellung von Nichel- phthaloeyanin, dadurch gekennzeiehnet, dass man Phthalimid mit Nickel oder mit nickel abgebenden Stoffen in Gegenwart von Di- cyandiamid erhitzt. PATENT CLAIM: Process for the production of nichelphthaloeyanine, characterized in that phthalimide is heated with nickel or with nickel-releasing substances in the presence of dicyandiamide. <B>UNTERANSPRUCH:</B> <B>1.</B> Verfahren nach Patentansprueh, dadurch gekennzeichnet, dass die Reaktion in Ge- genwart einer Mischung von Dieyandi- amid und Paratoluolsulfamid stattfindet. 2. Verfahren nach Patentanspruch, dadurch gekennzeichnet" dass man Stoffe hinzu fügt, die das Schmelzen und die Konden sation beLrünstigen. <B>3.</B> Verfahren nad Patentanspruch und Un teranspruch 2, dadurch gekennzeichnet, dass man Paratoluolsulfochlorid hinzu fügt. 4. SUBCLAIM: 1. Method according to patent claim, characterized in that the reaction takes place in the presence of a mixture of dieyandiamide and paratoluene sulfamide. 2. The method according to claim, characterized in that substances are added which promote melting and condensation. 3. Method according to claim and claim 2, characterized in that paratoluene sulfochloride is added. 4th Verfahren nach Patentanspruch und Un teransprüchen<B>1,</B> 2 und<B>3,</B> dadurch ge kennzeichnet, dass man die gewonnenen Produkte durch saure und alkalische Ex traktion reinigt. Method according to patent claim and sub-claims <B> 1, </B> 2 and <B> 3, </B> characterized in that the products obtained are cleaned by acidic and alkaline extraction.
CH210742D 1937-07-03 1937-08-26 Process for the production of nickel phthalocyanine. CH210742A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
IT207346X 1937-07-03

Publications (1)

Publication Number Publication Date
CH210742A true CH210742A (en) 1940-07-31

Family

ID=11171235

Family Applications (5)

Application Number Title Priority Date Filing Date
CH207346D CH207346A (en) 1937-07-03 1937-08-26 Process for the production of copper phthalocyanine.
CH210743D CH210743A (en) 1937-07-03 1937-08-26 Process for the production of magnesium phthalocyanine.
CH208880D CH208880A (en) 1937-07-03 1937-08-26 Process for the production of copper phthalocyanine.
CH210742D CH210742A (en) 1937-07-03 1937-08-26 Process for the production of nickel phthalocyanine.
CH208879D CH208879A (en) 1937-07-03 1937-08-26 Process for the production of copper phthalocyanine.

Family Applications Before (3)

Application Number Title Priority Date Filing Date
CH207346D CH207346A (en) 1937-07-03 1937-08-26 Process for the production of copper phthalocyanine.
CH210743D CH210743A (en) 1937-07-03 1937-08-26 Process for the production of magnesium phthalocyanine.
CH208880D CH208880A (en) 1937-07-03 1937-08-26 Process for the production of copper phthalocyanine.

Family Applications After (1)

Application Number Title Priority Date Filing Date
CH208879D CH208879A (en) 1937-07-03 1937-08-26 Process for the production of copper phthalocyanine.

Country Status (4)

Country Link
BE (1) BE423293A (en)
CH (5) CH207346A (en)
FR (1) FR826017A (en)
GB (1) GB503029A (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2657139A1 (en) * 1976-12-16 1978-06-22 Bayer Ag PROCESS FOR THE PRODUCTION OF COPPER PHTHALOCYANINE
TW325476B (en) * 1995-06-21 1998-01-21 Kawasaki Kasei Chemicals Method for producing copper phthalocyanine
WO2008079356A2 (en) 2006-12-22 2008-07-03 Dow Global Technologies Inc. Tetra-sulfo iron-phthalocyanine and related methods

Also Published As

Publication number Publication date
CH207346A (en) 1939-10-31
CH208879A (en) 1940-02-29
CH208880A (en) 1940-02-29
CH210743A (en) 1940-07-31
BE423293A (en) 1937-09-30
GB503029A (en) 1939-03-30
FR826017A (en) 1938-03-21

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