Method and device for producing triruthenium dodecacarbonyl
A technology of triruthenium dodecacarbonyl and its manufacturing method, applied in the field of manufacturing triruthenium dodecacarbonyl, capable of solving problems such as burning of ruthenium thin films
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no. 1 approach
[0051] Place 1.5kg of DCR crude crystals on the sintered filter of the above-mentioned sublimation device, and carry out sublimation under the conditions of supply gas flow rate of 500sccm, heating temperature of 100°C, and vacuum degree of 26.6Pa, then cool the water at a temperature of 5°C DCR was precipitated (Test No. 1-4). The supply gas in this embodiment is CO only (CO concentration 100%). In addition, sublimation was performed in the same manner for each of Examples and Comparative Examples having the CO gas flow rate, heating temperature, sublimation time, etc. shown in Table 2.
[0052] [Table 2]
[0053]
[0054] *In Test No.1-3, DCR turned black after sublimation and could not be recovered.
[0055] When CO is supplied during sublimation, the sublimation rate is fast and DCR can be obtained with high yield even when the processing amount of crude DCR is large (1500g) (Test No. 1-4 to 1-9) . On the other hand, in the case of a small amount of crude DCR (130 g...
no. 2 approach
[0065] Crude DCR was purified in a sublimation apparatus with a sintered filter thickness of 3.0 mm (Test No. 2-1) and 1.7 mm (Test No. 2-2). The results are shown in Table 4. The sublimation conditions were the same as those of Test Nos. 1-4 of the first embodiment (DCR 1500 g, CO flow rate 500 sccm, heating temperature 100° C., pressure 26.6 Pa, sublimation time 18.5 hours). For Test No. 2-2, the measurement of impurity elements was also performed by ICP-MS.
[0066] [Table 4]
[0067] Test No.
Sintered filter
sublimation time
Yield
sublimation speed
2-1
3.0mm
18.5 hours
95
125
2-2
1.7mm
18.5 hours
87
100
[0068]As shown in Table 4, when the thickness of the sintered filter is 3.0 mm (Test No. 2-1), the sublimation rate is faster compared with the case of a thickness of 1.7 mm (Test No. 2-2). DCR was obtained in high yield. This is considered to be because by increasing the thickness of the filter, CO...
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