A kind of synthetic method of dichloropropanol
A technology of dichloropropanol and a synthesis method, applied in the directions of organic chemistry, introduction of halogen preparation, etc., can solve the problems such as easy volatilization of catalyst organic acid, and achieve the effects of easy acquisition, large market application value and high yield
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[0015] Quaternary ammonium salt type Preparation of acidic ionic liquids (reference [1] Xiao Feng, Wang Guannan, Wu Youting, etc. Synthesis and characterization of quaternary ammonium salt ionic liquids with low melting point and low viscosity [J]. Journal of Nanjing University, 2010, 46(2): 179-185.): Take a 250mL three-necked flask, add 50mL of ethanol as a solvent, then add 27.9mL (0.2mol) of triethylamine and 23.7mL (0.22mol) of bromo-n-butane into the flask in turn, under nitrogen protection , heated to 80°C and stirred for 24h, then cooled to room temperature with stirring to obtain a yellow oily liquid. The solvent ethanol was removed by rotary evaporation, and the obtained solid was washed three times with ethyl acetate, and placed in a vacuum oven at 70°C for 24 hours to obtain an off-white solid [N 2224 ] Br ionic liquid intermediate. Take another 23.8g (0.1mol) [N 2224 ]Br and 12.1g (0.11mol) NaHSO 4 Add it to a 250mL one-necked flask, add 100mL of ethanol as a...
Embodiment 1
[0018] Place a 100mL four-neck flask equipped with a magnetic stirrer in an oil bath, and after installing a reflux condenser and a thermometer device, add 50g of glycerin therein, stir and heat. When the temperature reaches 110° C., weigh 0.03 mol of the ionic liquid catalyst, add it into a four-necked flask, and stir to disperse it evenly. Then, hydrogen chloride gas was introduced to carry out bubbling reaction, and the flow rate was adjusted to 50mL min -1 . The tail gas was passed through the NaOH solution and then passed into the atmosphere. After 20 hours of reaction, the reaction was stopped, and the product was quantitatively analyzed by gas chromatography. The influence of different ionic liquids on the glycerol chlorination process is shown in Table 1:
[0019] Table 1: Effects of different ionic liquids on the chlorination process of glycerol
[0020]
[0021] Note: 2-MCPD is 2-chloro-1,3-propanediol, 3-MCPD is 3-chloro-1,2-propanediol, 1,3-DCP is 1,3-dichlor...
Embodiment 2
[0024] in [N 2224 ] HSO 4 As a catalyst, the reaction temperature was changed to 90°C, 100°C, and 120°C, and the influence of different reaction temperatures on the chlorination process of glycerol was investigated. The results are shown in Table 2: the rest of the content is the same as in Example 1.
[0025] Table 2: Effects of different reaction temperatures on the chlorination process of glycerol
[0026]
[0027] As can be seen from Table 2, as the reaction temperature increases, the reaction rate is accelerated. When the reaction temperature is 120° C., the total yield of dichloropropanol is 89.66% after 20 hours of reaction.
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