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. 2021 Jul 8;6(28):18248-18252.
doi: 10.1021/acsomega.1c02119. eCollection 2021 Jul 20.

Production of cis-Na2N2O2 and NaNO3 by Ball Milling Na2O and N2O in Alkali Metal Halide Salts

Jack V Davis  1 , Oswaldo Guio  1 , Burjor Captain  1 , Carl D Hoff  1
Affiliations

Production of cis-Na2N2O2 and NaNO3 by Ball Milling Na2O and N2O in Alkali Metal Halide Salts

Jack V Davis et al. ACS Omega. .

Abstract

Ball milling of sodium oxides and alkali metal halide salts under a pressure of 2 atm nitrous oxide at temperatures of 38 ± 4 °C is reported. After 2.5 h of ball milling, FTIR data for both 14N2O and 15N2O additions show conclusively that cis-Na2N2O2 is formed based on excellent agreement with data reported earlier by Jansen and Feldmann who prepared pure crystalline cis-Na2N2O2 by reaction of sodium oxide and nitrous oxide for 2 h at 360 °C in a tube furnace. Continued ball milling under nitrous oxide leads to slow buildup of NaNO3 with yields on the order of 24% achieved in 20 h. Production of nitrate only occurs during active ball milling. Studies over the first 10 h reveal a trend among potassium halide salts: KBr ≅ KCl > KI ≫ KF. Ball milling of sodium oxide alone under an atmosphere of N2O gives much lower yields than ball milling in the presence of added alkali metal halide salt. Ball milling of sodium oxide and nitrous oxide in fluorocarbon oil, silicone oil, calcium fluoride, clinoptilolite, molecular sieves, and silica gel does not lead to significant yields of either cis-Na2N2O2 or NaNO3.

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Conflict of interest statement

The authors declare no competing financial interest.

Figures

Figure 1
Figure 1
Comparison of FTIR data for ball milling results of Na2O/KBr under 3 atm 14N2O (red) and 15N2O (black). The spectra shown were obtained after ≈6 h time ball milling.
Figure 2
Figure 2
KBr pellet FTIR spectra as a function of time for ball milling of Na2O (0.5 g) in KBr (1.5 g) under 30 psi, 2.0 ATM N2O.
Figure 3
Figure 3
Initial rates of production of nitrate as a function of time (h) for KF, KBr, KCl, and KI.
Figure 4
Figure 4
Mole fraction in total Na distribution for the first 20.5 h of ball milling 0.5 g Na2O in 1.5 g KBr in standard conditions.
See this image and copyright information in PMC

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