Method for preparing epoxy chloropropane
A technology of epichlorohydrin and calcium hydroxide, which is applied in the direction of alkali metal chloride, calcium/strontium/barium chloride, calcium/strontium/barium halide, etc., which can solve the problem of large amount of organic solvent, large environmental pollution, and raw material High cost and other problems, to achieve the effects of easy separation, low environmental pollution, and high yield of the product epichlorohydrin
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Embodiment 1
[0020] Take by weighing 29.5 g calcium hydroxide, 2 g sodium hydroxide and 70 g water and mix and stir to form soda-lime milk, for subsequent use;
[0021] Put 100 g of the crude glycerin chlorination product in an ice-water bath, under stirring, add milk of soda lime in batches to prevent the exothermic acid-base reaction. Slowly heat up to 20°C and keep it warm for 1 h. After the saponification reaction, let stand and cool to obtain reaction solution A; filter reaction solution A under reduced pressure, adjust the pH of the filtrate to neutral with hydrochloric acid, and then distill under reduced pressure to obtain Solution of epichlorohydrin and isolated solid;
[0022] The results show that the conversion rate of dichloropropanol is 99.2%, and the yield of epichlorohydrin is 97.4%;
[0023] Dissolve the separated solid in hot distilled water, filter while hot, cool the filtrate to crystallize, filter the cooled filtrate, and dry the crystal to obtain NaCl and CaCl 2 Mix...
Embodiment 2
[0025] Take by weighing 29.5 g calcium hydroxide, 5 g sodium hydroxide and 70 g water and mix and stir to form soda lime milk, for subsequent use;
[0026] Put 100 g of the crude glycerin chlorination product in an ice-water bath, add soda-lime milk in batches under stirring, to prevent the exothermic acid-base reaction, the temperature of the reaction solution suddenly rises, first keep it at 0-5 °C for 0.5 h, then Slowly heat up to 15°C and keep it warm for 2 hours. After the saponification reaction, let stand and cool to obtain reaction solution A; filter reaction solution A under reduced pressure, adjust the pH of the filtrate to neutral with hydrochloric acid, and then distill under reduced pressure to obtain Solution of epichlorohydrin and isolated solid;
[0027] The result shows that dichloropropanol conversion rate is 99.9%, and epichlorohydrin yield is 98.5%;
[0028] Dissolve the separated solid in hot distilled water, filter while hot, cool the filtrate to crystal...
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