The preparation method of 15-crown ether-5
A technology of crown ether and dichloroethyl ether, applied in the field of preparation of 15-crown ether-5, can solve problems such as not seen, and achieve the effects of low cost, safe process operation and less three wastes
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Embodiment 1
[0024] A kind of preparation method of 15-crown ether-5, carries out according to the following steps:
[0025] Step 1: Open and close the relevant valves and buttons according to the operation steps of the vacuum system, pump 240 kg of triethylene glycol and 1200 kg of dioxane into a 3000L stainless steel reactor, stir for 5 minutes to make the mixture even;
[0026] Step 2: Pump 600 kg of dichloroethyl ether and 330 kg of dioxane into the high-level tank. After the pumping, close the vacuum system first, and then open each relevant valve to make the entire reaction system a reflux device. closure;
[0027] Step 3, stop stirring the triethylene glycol and dioxane in the step 1, open the manhole cover, slowly add 190 kilograms of sodium hydroxide in the 3000L stainless steel reactor, and close the manhole cover after adding;
[0028] Step 4, start stirring, and after about 5 minutes, after the temperature of the entire reaction system is constant, slowly add steam to 60°C and...
Embodiment 2
[0036] A kind of preparation method of 15-crown ether-5, carries out according to the following steps:
[0037] Step 1: Open and close the relevant valves and buttons according to the operation steps of the vacuum system, pump 240 kg of triethylene glycol and 1200 kg of dioxane into a 3000L stainless steel reactor, stir for 5 minutes to make the mixture even;
[0038] Step 2: Pump 600 kg of dichloroethyl ether and 330 kg of dioxane into the high-level tank. After the pumping, close the vacuum system first, and then open each relevant valve to make the entire reaction system a reflux device. closure;
[0039] Step 3, stop stirring the triethylene glycol and dioxane in the step 1, open the manhole cover, slowly add 190 kilograms of sodium hydroxide in the 3000L stainless steel reactor, and close the manhole cover after adding;
[0040] Step 4, start stirring, and after about 5 minutes, after the temperature of the entire reaction system is constant, slowly add steam to 60°C and...
Embodiment 3
[0048] A kind of preparation method of 15-crown ether-5, carries out according to the following steps:
[0049] Step 1: Open and close the relevant valves and buttons according to the operation steps of the vacuum system, pump 240 kg of triethylene glycol and 1200 kg of dioxane into a 3000L stainless steel reactor, stir for 5 minutes to make the mixture even;
[0050] Step 2: Pump 600 kg of dichloroethyl ether and 330 kg of dioxane into the high-level tank. After the pumping, close the vacuum system first, and then open each relevant valve to make the entire reaction system a reflux device. closure;
[0051]Step 3, stop stirring the triethylene glycol and dioxane in the step 1, open the manhole cover, slowly add 190 kilograms of sodium hydroxide in the 3000L stainless steel reactor, and close the manhole cover after adding;
[0052] Step 4, start stirring, and after about 5 minutes, after the temperature of the entire reaction system is constant, slowly add steam to 60°C and ...
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