Process for the Synthesis of Precursor Complexes of Titanium Dioxide Sensitization Dyes Based on Ruthenium Polypyridine Complexes
AssigneeDyepower
InventorsRita BOARETTO, Eva BUSATTO, Stefano CARLI, Sandro FRACASSO, Stefano CARAMORI, Carlo Alberto BIGNOZZI
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Abstract
The present invention concerns a process for the synthesis of both precursor complexes and dye sensitizers for titanium dioxide based on ruthenium polypyridine complexes comprising microwave irradiation, under high pressure and in aqueous environment system
Claims11
Synthesis in aqueous media of both precursor complexes and dye sensitizers for titanium dioxide based on ruthenium polypyridine complexes of general formula RuLL′X2, RuLX3 or Ru LL′L″ where L, L′, L″ is a bidentate or tridentate organic ligand which can be chosen among H2dcbpy 4,4′-dicarboxy-2-2′-bipyridyl, 5,5′-dicarboxy-2,2′-bipyridyl, 4,4′,4″-tricarboxy-2,2′,6′,2″-terpyridyl, 4,4′-dinonyl-2,2′-bipyridyl, 4,4′-bis-3,4-dioctyloxystyryl-2,2′-bipyridyl, 6-phenyl-2,2′-bipyridyl, 6-(2,4-difluorophenyl)-2,2′-bipyridyl;
- the ruthenium precursor complexes can be RuCl3.3(H2O) [RuCl6]2−, [Ru(DMSO)6(Y)2] wherein Y is selected from PF6, ClO4, Cl, Br;
- X is an anionic ligand selected from NCS−, Cl−, CN−. The microwave irradiation, whose frequency is comprised from 300 MHz to 300 GHz, is applied in a high pressure vessel (HP500) contained in a multimodal or unimodal MW reactor, at pressure values of 690 kPa to 5500 kPa.
A process for the synthesis in aqueous media of precursor complexes and dye sensitizers for titanium dioxide based on ruthenium polypyridine complexes, the process comprising:
- i. selecting a ruthenium polypyridine complex selected from the group consisting of RuLL′X2, RuLX3 or Ru LL′L″, wherein
- a. each of L, L′, and L″ is a bidentate or tridentate organic ligand selected from the group consisting of H2dcbpy 4,4′-dicarboxy-2-2′-bipyridyl, 5,5′-dicarboxy-2,2′-bipyridyl, 4,4′,4″-tricarboxy-2,2′,6′,2″-terpyridyl, 4,4′-dinonyl-2,2′-bi pyridyl, 4,4′-bis-3,4-dioctyloxystyryl-2,2′-bipyridyl, 6-phenyl-2,2′-bipyridyl, 6-(2,4-difluorophenyl)-2,2′-bipyridyl;
- and
- b. X is an anionic ligand;
- and
- ii. irradiating said ruthenium polypyridine complex via microwave at a frequency of 300 MHz to 300 GHz in a high pressure vessel at a pressure of 690 kPa to 5500 kPa.
Dependencies are inferred from the claim text.