Preparation method of phosphomonoester
A phosphoric acid monoester and temperature control technology, which is applied in chemical instruments and methods, phosphorus organic compounds, compounds of group 5/15 elements of the periodic table, etc., can solve the problem of low content of phosphoric acid monoester and complex preparation process of phosphoric acid monoester, etc. problem, to achieve the effect of good technical effect
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Embodiment 1
[0040] Preparation of Tetradecyl Phosphate Monoester: 200.00 g of tetradecyl mixed alcohol (mass ratio of dodecyl alcohol to tetradecyl alcohol is 70:30), 0.42 g of hypophosphorous acid and pure water are added to a round bottom flask 14.80g, open and stir and heat up; Add catalyst (the described catalyst is SnCl4, MnO2 and CuSO4 mass ratio is the mixture of 0.9: 1: 0.3) 0.88g in round-bottomed flask when temperature rises to 70 DEG C, then segmental drop Phosphorus pentoxide 74.28g, the temperature is controlled at 75±5°C, and the feeding time is controlled at 1.5 hours; after the addition, it is kept at 85°C for 4.5 hours, then 5.18g of pure water is added, the temperature is controlled at 85°C, and at this temperature After 2 hours of heat preservation, the temperature was lowered to 75° C. and filtered to obtain the phosphate ester product. Analysis by double indicator titration method: monoester: 92.3%, diester: 5.0%, phosphoric acid 2.7%.
Embodiment 2
[0048] The difference from Example 1 is that the catalyst is SnCl4.
[0049] Add 200.00g of tetradecyl alcohol (mass ratio of dodecanol to tetradecyl alcohol is 70:30), 0.42g of hypophosphorous acid and 14.80g of pure water in the round bottom flask, start stirring and heat up; when the temperature rises to Add 40.88g of SnCl to the round bottom flask at 70°C, then add 74.28g of phosphorus pentoxide in stages, control the temperature at 75±5°C, and control the feeding time for 1.5 hours; Then add 5.18g of pure water, control the temperature at 85±2°C, keep at this temperature for 2 hours, then cool down to 75°C and filter to obtain the phosphate ester product. Analysis by double indicator titration: monoester: 83.9%, diester: 12.6%, phosphoric acid 3.5%.
Embodiment 3
[0051] The difference from Example 1 is that the catalyst is MnO2.
[0052] Add 200.00g of tetradecyl alcohol (mass ratio of dodecanol to tetradecyl alcohol is 70:30), 0.42g of hypophosphorous acid and 14.80g of pure water in the round bottom flask, start stirring and heat up; when the temperature rises to Add 20.88g of MnO to the round bottom flask at 70°C, then add 74.28g of phosphorus pentoxide in stages, control the temperature at 75±5°C, and control the feeding time for 1.5 hours; after adding, keep warm at 85°C for 4.5 hours, Then add 5.18g of pure water, control the temperature at 85±2°C, keep at this temperature for 2 hours, then cool down to 75°C and filter to obtain the phosphate ester product. Analysis by double indicator titration method: monoester: 84.3%, diester: 11.4%, phosphoric acid 4.3%.
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