Purification and preparation of phosphorus-containing compounds
A compound and iron compound technology, applied in the field of purification and preparation of phosphorus-containing compounds, can solve problems such as ineffective distillation
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[0056] While various aspects of the invention are exemplified by the preparation of various organophosphorus compounds, it is believed that the methods described are generally applicable to the preparation or purification of any phosphorus-containing compound that can be subjected to the reflux and fractionation conditions described herein. It should be noted that the phosphorous rocks from which commercial phosphorous compounds are derived contain at least trace levels of arsenic as a contaminant. In many applications it is desirable to remove arsenic contamination in order to purify the phosphorus-containing compound for further use. In various aspects, the phosphorus-containing compounds are also used to synthesize many phosphorus-containing compounds such as organophosphorus compounds, or they are used directly as purified in various applications such as chip fabrication processes.
[0057] While the invention is not limited by theory, it is believed that treatment with at...
Embodiment
[0060] The invention has been described above with respect to various embodiments. Further non-limiting descriptions are given below as examples.
[0061] Example 1 - TEPO co-distilled with Cu(I)Cl
[0062] A 50L three-neck distillation flask was equipped with a 50L heating mantle with a built-in pneumatic magnetic stirrer, using 0.24 in 2 Pro-Pak packed 3-foot, silver-coated, vacuum-jacketed distillation columns and fractionation heads. After charging 42.5 kg of commercial TEPO and Cu(I)Cl (100 g) into the distillation flask, the resulting green slurry was stirred under nitrogen flow for about 1 hour to release CuCl that may have accumulated inside the distillation flask when it came into contact with TEPO pressure. With vigorous stirring, the distillation flask was refluxed for 24 hours under a head pressure of 30-35 mmHg, and the head temperature rose to 115°C-116°C. About 4.5 kg of the volatile fraction was collected slowly to remove low boilers including ethanol az...
Embodiment 3
[0071] Example 3 - TEPO co-distilled with water and sodium sulfate
[0072] A 2 L multi-neck flask was equipped with a mechanical stirrer and charged with TEPO (1000 mL) and DI water (5 mL). The colorless solution was stirred at room temperature for 6 hours, dried over anhydrous sodium sulfate (100.0 g) for 24 hours and filtered through a filter stick. Use fill with 0.24 in 2 The filtrate was fractionated on a Pro-Pak 2 foot, silver-coated, vacuum-jacketed distillation column. A volatile fraction of about 145 g was collected and a main fraction of 757 g (76%) exhibited low arsenic contamination and >99.0% GC purity (at 27 mmHg. Both fractions were at a head pressure of 27 mmHg and 113-114 collected at the top temperature of °C). Impurity concentrations are very low (in the ppb range), so temperature differences between fractions are very small.
[0073] TEPO samples were sent to Applied Analytical, Inc. (16713 Picadilly Court, Round Rock, Texas 78664-8545) for ICP Mass t...
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