Method for preparing phosphine and sodium trimetaphosphate simultaneously
A technology of sodium trimetaphosphate and phosphine, applied in chemical instruments and methods, phosphine, phosphorus compounds, etc., can solve the problems of low phosphine yield, consumption of large element phosphorus, and inability to completely decompose, etc. Achieve the effect of preventing oxidation and high temperature decomposition and dissolution, increasing the content, and reducing the production of long-chain high-molecular-weight chemicals
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Embodiment 1
[0022] Example 1 (A-10V-031 / A-10V-032-1)
[0023] A mixture of sodium phosphite and sodium phosphate prepared from 25 g of phosphorous acid, 26 g of phosphoric acid (85.7%) and 21 g of sodium hydroxide (96%) was evaporated to dryness under reduced pressure at 70°C to constant weight to obtain a theoretical amount of anhydrous mixed salt 55.8 g, P of the mixed salt Ⅲ / P VThe calculated value is 1.34, the sodium-phosphorus ratio is determined to be 0.923 (calculated value is 0.947), and the pH value of the solution (1%) is 3.34. Place 30 g of this mixed salt in a three-necked flask equipped with a nitrogen inlet and outlet, and replace the flask with nitrogen Neutral air, after half an hour, keep the nitrogen flow, the pressure is slightly higher than the standard atmospheric pressure, then the mixture is heated to 350 ° C, the material is melted and bubbled at this temperature, and the released phosphine is carried by nitrogen into the solution containing mercuric chloride ( ...
Embodiment 2
[0024] Example 2 (A-10V-013 / A-10V-014-1)
[0025] Sodium phosphite and sodium phosphate salt mixture (P Ⅲ / P V =1.001) evaporated to dryness under reduced pressure at 70°C to constant weight to obtain 54.3 grams of theoretical anhydrous mixed salt. The pH value is 3.48. Put 10 g of the mixed salt in a three-necked flask equipped with a nitrogen inlet and outlet, and replace the air in the flask with nitrogen. After half an hour, keep the nitrogen flow, and the pressure is slightly higher than the standard atmospheric pressure, and then the mixture is heated to 300 ° C. , the material melts and bubbles at this temperature, and the released phosphine is brought into the absorption bottle filled with mercuric chloride solution (2-3%) by nitrogen gas, and the released phosphine is obtained by the weight of the precipitate in the absorption solution after drying and the loss of mercury ions in the solution is determined. After the bubbling ends, continue heating at the same temp...
Embodiment 3
[0026] Example 3 (A-11V-064 / A-11-065-1)
[0027] Sodium phosphite and phosphate mixture (P Ⅲ / P V =1.33) evaporated to dryness under reduced pressure at 70°C to constant weight to obtain 104.3 grams of theoretical anhydrous mixed salt. ) has a pH value of 2.76. Place 20 g of the mixed salt in a three-necked flask equipped with a nitrogen inlet and outlet, and replace the air in the flask with nitrogen. After half an hour, keep the nitrogen flow, and the pressure is slightly greater than the standard atmospheric pressure. Then the mixture is heated to 350°C, the material melts and bubbles at this temperature, the released phosphine is brought into the absorption bottle filled with mercury chloride solution (2-3%) by nitrogen, and the released phosphine is dried by the precipitate in the absorption liquid The final weight and the loss of mercury ions in the solution were determined. After the bubbling ended, continue heating at the same temperature for 2 hours, stop heating a...
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