A kind of production technology of acid-sensitive phosphite
A phosphite and production process technology, which is applied in the field of acid-sensitive phosphite production process, can solve the problems of high operating cost, incomplete dehydration, and reduced yield, and achieve easy management, good reaction selectivity, and avoidance of The effect of low temperature operation
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Embodiment 1
[0042] (1) Synthesis: in the 5000mL four-neck flask reactor equipped with constant pressure dropping funnel, stirrer, thermometer and reflux condenser, add the solution of 101g (3.15mol) methanol in 2024g (20mol) triethylamine, Cool the reactor with an ice-salt bath, control the stirring speed to 100r / min, start to add 137g of phosphorus trichloride dropwise, control the drop rate, keep the reaction temperature at 20-40°C, drop the material for 2 hours, and continue stirring for 0.5 h;
[0043] (2) Alkali washing: control the stirring speed at 80r / min and the temperature at 20-40°C, add 500mL of 20% sodium hydroxide dilute alkali to the crude product synthesized in the first step, stir for 2min, let stand for 5min, separate the water phase, retain the oil phase;
[0044] (3) Drying: In the oil phase of the second step, add 215mL of 40% sodium hydroxide concentrated alkali for extraction and dehydration, stir for 2 minutes, let stand for 5 minutes, separate layers, and recover...
Embodiment 2
[0047] (1) synthesis: in the 5000mL four-neck flask reactor equipped with constant pressure dropping funnel, stirrer, thermometer and reflux condenser, add the solution of 145g (3.15mol) ethanol in 2024g (20mol) triethylamine, Cool the reactor with an ice-salt bath, control the stirring speed to 100r / min, start to add 137g of phosphorus trichloride dropwise, control the drop rate, keep the reaction temperature at 20-40°C, drop the material for 2 hours, and continue stirring for 0.5 h;
[0048] (2) Alkali washing: control the stirring speed at 80r / min and the temperature at 20-40°C, add 500mL of 20% sodium hydroxide dilute alkali to the crude product synthesized in the first step, stir for 2min, let stand for 5min, separate the water phase, retain the oil phase;
[0049] (3) Drying: In the oil phase of the second step, add 215mL of 40% sodium hydroxide concentrated alkali for extraction and dehydration, stir for 2 minutes, let stand for 5 minutes, separate layers, and recover ...
Embodiment 3
[0052] (1) Synthesis: In a 5000mL four-necked flask reactor equipped with a constant pressure dropping funnel, agitator, thermometer and reflux condenser, according to tertiary amine: alcohol: phosphorus trichloride=22:3:1, add 3mol For the solution of ethanol in 22mol triethylamine, cool the reactor with an ice-salt bath, control the stirring speed to 100r / min, start to add 1mol phosphorus trichloride dropwise, control the drop rate, keep the reaction temperature at 20-40°C, drop The feeding time is 2h, and the stirring is continued for 0.5h after dropping;
[0053] (2) Alkali washing: control the stirring speed at 80r / min and the temperature at 30°C, add 500mL of 20% sodium hydroxide dilute alkali to the crude product synthesized in the first step, stir for 8min, let stand for 10min, separate the water phase, and keep the oil Mutually;
[0054] (3) Drying: In the oil phase of the second step, according to the volume ratio of concentrated alkali and oil phase of 0.08:1, add ...
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