Method for producing dichloropropanol
A technology of dichloropropanol and derivatives, which is applied in the field of preparation of dichloropropanol and epichlorohydrin intermediates, can solve the problem of reducing the quality of waste acid, affecting product yield, and unavoidable dichloropropanol product belts. Sour water and other problems, to overcome the effect of product pollution
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Embodiment 1
[0024] Heat and stir the mixture of 657kg glycerin and 27kg phosphorous acid at 120°C, then blow anhydrous hydrogen chloride into the mixture at 4.1kmol / h for 2h, 3.2kmol / h for 4h, 2.1kmol / h for 4h, and finally 1.2kmol / h continued for 2 hours, a total of 31.8 kmol of hydrogen chloride was introduced, and the water and dichlorohydrin generated by the reaction were continuously removed during the process, and the conversion rate of glycerin was 99.2%. The total yield of dichloropropanol (1,3-dichloropropanol and 1,2-dichloropropanol) is 93.5%. The phosphorous acid content in the distillate is <0.001%.
Embodiment 2
[0026] Heat and stir the mixture of 709kg glycerin, 22kg phosphorous acid and 14kg adipic acid at 130°C, then blow anhydrous hydrogen chloride into the mixture, 3.8kmol / h for 2h, 3.6kmol / h for 4h, 2.8kmol / h for 2h 4h, the last 1.4kmol / h continued for 2h, a total of 36.0kmol hydrogen chloride was introduced, and the water and dichloropropanol produced by the reaction were continuously removed during the process, and the conversion rate of glycerin was 99.3%. The total yield of dichloropropanol (1,3-dichloropropanol and 1,2-dichloropropanol) is 93.3%. The phosphorous acid content in the distillate is <0.001%.
Embodiment 3
[0028] Heat and stir the mixture of 596kg of glycerin and 25kg of phosphorous acid at 100°C, then add 50kg of 25% hydrochloric acid dropwise, and then raise the temperature to 130°C, then blow anhydrous hydrogen chloride into the mixture at 3.2kmol / h for 2h, 3.0 kmol / h continued for 4h, 2.8kmol / h continued for 4h, and finally 1.4kmol / h continued for 2h. A total of 32.74kmol hydrogen chloride was introduced, and the water and dichloropropanol produced by the reaction were continuously removed during the process. The conversion rate of glycerol was 99.3%. The total yield of dichloropropanol (1,3-dichloropropanol and 1,2-dichloropropanol) is 93.7%. The phosphorous acid content in the distillate is <0001%.
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