A kind of preparation method of methylene vinyl carbonate
A technology of methylene ethylene carbonate and tert-butyl carbonate, which is applied in the field of preparation of methylene ethylene carbonate, can solve the problems of purification method loss, long time consumption, low purity, etc., and achieve short time consumption and material loss Less, the effect of high product purity
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[0030] Meanwhile, the present invention also provides a preparation method of methylene ethylene carbonate, comprising the following steps:
[0031] Step 1: provide propargyl tert-butyl carbonate;
[0032] Step 2: mixing the propargyl tert-butyl carbonate with a mercury-containing catalyst, reacting and rectifying under stirring conditions to obtain a crude product of methylene ethylene carbonate;
[0033] Step 3: Purify the crude methylene ethylene carbonate by using the method described above to obtain the finished methylene ethylene carbonate.
[0034] According to the present invention, the above propargyl tert-butyl carbonate can be prepared by itself. The method in the prior art can be used to prepare the above-mentioned propargyl tert-butyl carbonate. However, the method for preparing propargyl tert-butyl carbonate in the prior art requires a large amount of catalyst, and the cost of raw materials and purification is high.
[0035] Preferably, according to the presen...
Embodiment 1
[0065] This example is used to illustrate the preparation method of the crude product of methylene ethylene carbonate disclosed by the present invention.
[0066] At room temperature, 350g (6.24mol) of propynyl alcohol and 325g (3.20mol) of triethylamine were sequentially added into a 2L three-necked flask, and after magnetic stirring for 5 minutes, 1360g (6.24mol) of di-tert-butyl dicarbonate was slowly added dropwise. After the drop, the temperature of the reaction oil bath was controlled at about 25°C. After the drop, the reaction progress was monitored by gas chromatography. The reaction was completed for 5 hours in total. Protected with a short pendant fractionation column, evaporated under reduced pressure to remove light components and triethylamine from the reaction, collected 878 g of the crude product of propargyl tert-butyl carbonate, the main content of the product was 92.3% as detected by gas chromatography, and the yield was 83.3%.
[0067] In a 1L three-neck fla...
Embodiment 2
[0069] This example is used to illustrate the preparation method of the crude product of methylene ethylene carbonate disclosed by the present invention.
[0070] At room temperature, add 100 g (1.78 mol) of propynyl alcohol and 338 g (3.56 mol) of triethylamine in a 1 L three-necked flask in sequence, and after magnetic stirring for 5 minutes, slowly drop in 400 g (1.83 mol) of di-tert-butyl dicarbonate, After the drop, the temperature of the reaction oil bath was controlled at about 45°C. After the drop, the reaction progress was monitored by gas chromatography. The reaction was completed for 4 hours in total. Protected with a short thorn fractionation column, evaporated under reduced pressure to remove light components and triethylamine from the reaction, collected 220 g of propargyl tert-butyl carbonate crude product, the main content of the product was 94.3% as detected by gas chromatography, and the yield was 74.6%.
[0071] In a 1L three-neck flask, under ice-water bath...
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