Preparation method and device of trimethyl borate-10
A technology of trimethyl borate and esterification reaction, applied in the field of trimethyl boron-10 acid, can solve the problems of large loss of trimethyl borate, difficulty in single treatment, complicated process, etc. Beautiful, good separation effect
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[0067] Example 1
[0068] 1 Esterification reaction
[0069] (a) Purge the reaction kettle with high-purity nitrogen for 5-10 minutes, and adjust the reactants in a molar ratio 10 BF 3 :CaCl 2 :CH 3 The ratio of ONa=1:1.5:3.0 is added to the reactor, and methanol is used as the solvent to make the raw materials evenly distributed in it, which is conducive to stirring. Turn on the stirring device and set the speed to about 150r / min;
[0070] (b) Set the reaction temperature to 70°C and the reaction time to 30h;
[0071] 2 azeotropic distillation
[0072] (a) The reaction product is subjected to azeotropic distillation at a temperature of 70°C;
[0073] (b) Collect 50-60°C fractions, then continue to increase the temperature, recover methanol, and recycle.
[0074] 3 Extractive distillation
[0075] (a) Put the distillate into the extractive distillation tower kettle, turn on the 6 heating pack power supply and 1 condensate water switch. In order to ensure the heat transfer performance of th...
Example Embodiment
[0079] Example 2
[0080] 1 Esterification reaction
[0081] (a) Purge the reactor with high-purity nitrogen for about 5 to 10 minutes, and adjust the reactants to the molar ratio of the reactants 10 BF 3 :CaCl 2 :CH 3 The ratio of ONa=1:1.7:3.4 is added to the reactor, and methanol is used as the solvent to make the raw materials evenly distributed in it, which is good for stirring. Turn on the stirring device and set the speed to about 200r / min;
[0082] (b) Set the reaction temperature to 60°C and the reaction time to 35h.
[0083] 2 azeotropic distillation
[0084] (a) The reaction product is subjected to azeotropic distillation, and the temperature is set to 80°C;
[0085] (b) Collect 50-60°C fractions, then continue to increase the temperature, recover methanol, and recycle.
[0086] 3 Extractive distillation
[0087] (a) Add the distillate to the extractive distillation tower kettle, turn on the 6 heating pack power supply and 1 condensate water switch. In order to ensure the heat t...
Example Embodiment
[0091] Example 3
[0092] 1 Esterification reaction
[0093] (a) Purge the reactor with high-purity nitrogen for about 5 to 10 minutes, and adjust the reactants to the molar ratio of the reactants 10 BF 3 :CaCl 2 :CH 3 The ratio of ONa=1:1.8:3.6 is added to the reactor, and methanol is used as the solvent to make the raw materials evenly distributed in it, which is good for stirring. Turn on the stirring device and set the speed to about 300r / min;
[0094] (b) Set the reaction temperature to 50°C and the reaction time to 45h;
[0095] 2 azeotropic distillation
[0096] (a) The reaction product is subjected to azeotropic distillation at a temperature of 90°C,
[0097] (b) Collect 50-60°C fractions, then continue to increase the temperature, recover methanol, and recycle.
[0098] 3 Extractive distillation
[0099] (a) Put the distillate into the extractive distillation tower kettle, turn on the 6 heating pack power supply and 1 condensate water switch. In order to ensure the heat transfer p...
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