Photoluminescent heteronuclear metal cluster compound fluorescent materials and preparing method thereof
A fluorescent material and photoluminescence technology, applied in the directions of luminescent materials, chemical instruments and methods, can solve problems such as limited application, and achieve the effects of simple preparation method, stable chemical properties, and easy separation and purification
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Embodiment 1
[0019] In the first step, 250g of K 2 PdCl 4 Dissolve in 1L distilled water, add 160g sodium pyrrolidine dithiocarbamate (NaS 2 CNC 4 h 8 ) to generate a precipitate, which was filtered and dried to obtain a khaki solid Pd(S 2 CNC 4 h 8 ) 2 .
[0020] In the second step, at room temperature (operating pressure is one atmosphere), add equal volumes of acetonitrile and chloroform to the feed tank, and then add AgSbF 6 , solid Pd(S 2 CNC 4 h 8 ) 2 and dppm, the reaction mass ratio is AgSbF 6 :Pd(S 2 CNC 4 h 8 ) 2 : dppm=3.5: 4: 3, the mass volume ratio of the reaction material to acetonitrile and chloroform is respectively 2.1kg / L, after stirring rapidly for 5 minutes, add the reaction kettle, obtain a yellow solution after 2 hours of reaction, and recrystallize with ether, After filtering and drying, the photoluminescent heteronuclear metal cluster fluorescent material is obtained. Yield: 85%.
Embodiment 2
[0022] In the first step, 250g of K 2 PdCl 4 Dissolve in 1L distilled water, add 240g ammonium pyrrolidine dithiocarbamate (NH 4 S 2 CNC 4 h 8 ) to generate a precipitate, which was filtered and dried to obtain a khaki solid Pd(S 2 CNC 4 h 8 ) 2 .
[0023] In the second step, at room temperature, equal volumes of acetonitrile and chloroform were added to the feed tank, followed by the addition of AgSbF 6 , solid Pd(S 2 CNC 4 h 8 ) 2 and dppm, the reaction mass ratio is AgSbF 6 :Pd(S 2 CNC 4 h 8 ) 2 : dppm=3.5: 5: 3, the mass-volume ratio of reaction material and acetonitrile and chloroform is respectively 2.2kg / L, after rapid stirring, add reaction kettle in 5 minutes, obtain yellow solution after reacting for 2 hours, recrystallize with ether, After filtering and drying, the photoluminescent heteronuclear metal cluster fluorescent material is obtained. Yield: 81%.
Embodiment 3
[0025] In the first step, 300g of K 2 PdCl 4 Dissolve in 1L distilled water, add 160g sodium pyrrolidine dithiocarbamate (NaS 2 CNC 4 h 8 ) to generate a precipitate, which was filtered and dried to obtain a khaki solid Pd(S 2 CNC 4 h 8 ) 2 .
[0026] In the second step, at a temperature of -10°C, add equal volumes of acetonitrile and chloroform to the feed tank, and then add AgSbF in sequence. 6 , solid Pd(S 2 CNC 4 h 8 ) 2 and dppm, the reaction mass ratio is AgSbF 6 :Pd(S 2 CNC 4 h 8 ) 2 : dppm=3.5: 5: 4, the mass volume ratio of the reaction material to acetonitrile and chloroform is respectively 2.3kg / L, after rapid stirring for 5 minutes, add to the reaction kettle, obtain a yellow solution after 2 hours of reaction, recrystallize with ether, After filtering and drying, the photoluminescent heteronuclear metal cluster fluorescent material is obtained. Yield 85%.
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