Low temperature preparation method of boron trifluoride dimethyl carbonate complex compound
A technology of dimethyl carbonate and boron trifluoride, which is applied in the field of low-temperature preparation of boron trifluoride dimethyl carbonate complex, can solve the problems of high risk, high energy consumption, etc. Reaction temperature, safe and controllable effect of production process
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Embodiment 1
[0024] Add sulfur trioxide, boric acid, and anhydrous hydrofluoric acid into the gas generator at a weight ratio of 4:1:1, and react at 18°C for 15 hours. The vacuum pump evacuates the boron trifluoride gas, The degree of vacuum is 0.07MPa.
[0025] The derived boron trifluoride gas enters the purification tank filled with 85% concentrated sulfuric acid for purification, and the gauge pressure of the purification tank is 0.2MPa.
[0026] The purified boron trifluoride gas enters the complexing kettle, which is filled with dimethyl carbonate, and the mass ratio of the filling amount of dimethyl carbonate to the boron trifluoride gas produced by each kettle in the gas making kettle is 6 : 3, the complexation reaction temperature is 20°C, and the reaction time is 4 hours.
[0027] The complexation reaction liquid circulates in the complexation tank and the filter, the temperature of the filter is 8°C lower than the temperature of the complexation tank, and the reaction liquid ...
Embodiment 2
[0036] Add sulfur trioxide, boric acid, and anhydrous hydrofluoric acid into the gas generator at a mass ratio of 8:1:1, and react at 30° C. for 8 hours to generate boron trifluoride gas. The vacuum pump evacuates the boron trifluoride gas, and the vacuum degree is 0.08MPa.
[0037] The exported boron trifluoride gas enters the purification tank filled with concentrated sulfuric acid with a concentration of 93% for purification, and the gauge pressure of the purification tank is 0.4MPa.
[0038] The purified boron trifluoride gas enters the complexing kettle, which is filled with dimethyl carbonate, and the mass ratio of the filling amount of dimethyl carbonate to the boron trifluoride gas produced by each kettle in the gas making kettle is 6 : 4, the complexation reaction temperature is 30 DEG C, and the reaction time is 8 hours.
[0039] The filter temperature is 10° C. lower than the complexation reaction temperature, and the rest refer to Example 1. The product is a whit...
Embodiment 3
[0041] Add sulfur trioxide, boric acid, and anhydrous hydrofluoric acid into the gas generator at a weight ratio of 12:2:3, and react at 48° C. for 4 hours to generate boron trifluoride gas. The vacuum pump pumps out the boron trifluoride gas with a vacuum degree of 0.098MPa.
[0042] The exported boron trifluoride gas enters the purification tank filled with 98% concentrated sulfuric acid for purification, and the gauge pressure of the purification tank is 0.5MPa.
[0043] The purified boron trifluoride gas enters the complexing kettle, which is filled with dimethyl carbonate, and the mass ratio of the filling amount of dimethyl carbonate to the boron trifluoride gas produced by each kettle in the gas making kettle is 6 : 6, the complexation reaction temperature is 40 DEG C, and the reaction time is 12 hours.
[0044] The filter temperature is 15° C. lower than the complexation reaction temperature, and the rest refer to Example 1. The product is a white crystal with a boro...
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