Preparation method of diethyl phosphinic acid without monoethyl phosphinic acid group and salt thereof
A technology of monoethylphosphinic acid and diethylphosphinic acid, which is applied in the field of preparation of diethylphosphinic acid and its salts, can solve the problems of complex process, high cost, waste water, etc., and achieve good removal effect, Ease of recycling and simple waste liquid treatment
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[0055] Example 1
[0056] Dissolve sodium hypophosphite monohydrate (2mol) and acetic anhydride (2mol) in 44ml ethylene glycol monomethyl ether, then add a catalytic amount of glacial acetic acid (0.1mol) with stirring, and add anhydrous after stirring at room temperature for 2 hours Sulfuric acid (1mol), after adding anhydrous sulfuric acid, cool to 15°C and let stand for 1 hour, filter and recover sodium sulfate to obtain anhydrous hypophosphorous acid solution;
[0057] Transfer the anhydrous hypophosphorous acid solution into an acid-resistant and pressure-resistant reactor with a constant-pressure dripping device, pass ethylene gas, and make the pressure in the kettle reach 1MPa, and separate from the constant-pressure dripping device under stirring at 1800r / min. Add in batches an initiating mixture composed of 20g of azobisisobutyronitrile, 0.4g of copper complex and 44ml of ethylene glycol monomethyl ether. During the dripping of the initiating mixture, keep the ethylene pre...
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[0064] Example 2
[0065] Dissolve sodium hypophosphite monohydrate (2mol) and acetic anhydride (2mol) in 44ml ethylene glycol monomethyl ether, then add catalytic amount of propionic acid (0.05mol) under stirring, and add 98% after stirring for 3 hours at room temperature Concentrated sulfuric acid (1mol), after adding 98% concentrated sulfuric acid, cool to 10°C and stand for 2.5 hours, filter and recover sodium sulfate to obtain anhydrous hypophosphorous acid solution;
[0066] Transfer the anhydrous hypophosphorous acid solution to an acid-resistant and pressure-resistant reactor with a constant-pressure dripping device, pass ethylene gas, and make the pressure in the kettle reach 1.2MPa, and stir from the constant-pressure dripping device at 800r / min. Add in batches an initiating mixture composed of 20g of azobisisobutyronitrile, 0.4g of copper complex and 44ml of ethylene glycol monomethyl ether, and keep the ethylene pressure in the reactor not less than 0.6 during the dripp...
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[0072] Example 3
[0073] Dissolve sodium hypophosphite monohydrate (2mol) and acetic anhydride (2.2mol) in 55ml dioxane, then add a catalytic amount of isovaleric acid (2mol) under stirring, and add 98.4% of isovaleric acid (2mol) under stirring at room temperature for 0.5 hours Concentrated sulfuric acid (1.2mol), after adding concentrated sulfuric acid, cool down to 5°C and let stand for 6 hours, filter and recover sodium sulfate to obtain anhydrous hypophosphorous acid solution;
[0074] Transfer the anhydrous hypophosphorous acid solution into an acid-resistant and pressure-resistant reactor with a constant-pressure dripping device, pass ethylene gas, and make the pressure in the kettle reach 0.1MPa, and stir from the constant-pressure dripping device at 1800r / min. Add in batches an initiation mixture composed of 20g azobisisobutyronitrile, 0.4g copper complex and 44ml ethylene glycol monomethyl ether, and keep the ethylene pressure in the reactor not less than 0.1 during the ...
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