A preparation method of fluoro phosphate materials
A technology of fluorophosphate and ethyl phosphate, which is applied in the field of preparation of fluorophosphate materials, to achieve the effects of precise control of reaction conditions, low cost and easy realization
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Embodiment 1
[0022] The invention uses a constant temperature water bath to carry out the reaction, and adopts a sealed polytetrafluoroethylene-lined corrosion-resistant austenitic stainless steel container. The volume of the container content space is 2L. First add 140g of ethyl phosphate and 1.4g of high-purity iron powder (in high-purity iron powder, the iron purity is greater than 99%) in the container, when heated to 80 ° C, feed nitrogen to replace the air, and then slowly (dropping speed is 1-2 drops) / sec) dropwise the hydrofluoric acid liquid 300ml of 10M concentration, this moment according to molar ratio HF: (CH 3 CH 2 O)PO 4 It is 3:1. After the addition, continue to feed nitrogen until the internal pressure reaches 2 atmospheres. After constant temperature and pressure for 6 hours, release the pressure to atmospheric pressure to end the reaction. Then use 0.01Mpa vacuum, distill under reduced pressure at 60°C to remove water, put 1.4g of dried 4A molecular sieve into it, l...
Embodiment 2
[0025] The invention uses a constant temperature water bath for the reaction, adopts a sealed polytetrafluoroethylene-lined corrosion-resistant austenitic stainless steel container, and the internal space volume of the container is 20L. First add 1.4Kg ethyl phosphate and 24g high-purity iron powder in the container, when heated to 92°C, feed nitrogen to replace the air, then slowly add 1.75L of hydrofluoric acid liquid with a concentration of 20M, according to the molar ratio HF:( CH 3 CH 2 O)PO 4 The ratio is 3.5:1. After the addition, continue to feed nitrogen until the internal pressure reaches 3 atmospheres. After constant temperature for 2 hours, release the pressure to atmospheric pressure to end the reaction. Then use 0.01Mpa vacuum, 70 ℃ vacuum distillation to remove water, continue to put in 70g of dried 4A molecular sieve, let it stand for 1h, use 4A molecular sieve to further remove water, filter the liquid with a 1um precision filter, that is what you need The ...
Embodiment 3
[0028] The invention uses a constant temperature water bath for the reaction, adopts a sealed polytetrafluoroethylene-lined corrosion-resistant austenitic stainless steel container, and the internal space volume of the container is 1000L. First add 140Kg ethyl phosphate and 2100g high-purity iron powder in the container, when heated to 90°C, feed nitrogen to replace the air, then slowly add 200L of hydrofluoric acid liquid with a concentration of 15M, molar ratio HF:(CH 3 CH 2 O)PO 4 After the addition, continue to feed nitrogen until the internal pressure reaches 2.5 atmospheres, keep the temperature for 3 hours, release the pressure to atmospheric pressure, and end the reaction. Then use 0.01Mpa vacuum, distill under reduced pressure at 65°C to remove water, continue to put in 4.2Kg dried 4A molecular sieve, let it stand for 1h, use 4A molecular sieve to further remove water, and filter the liquid with a 0.5um precision filter, that is The desired product trifluorophosphat...
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