Purification method for Xinjunan
A purification method, the technology of octoprodil, which is applied in the field of pesticides, can solve the problems of complicated process, many impurities in the finished product, and low purity, and achieve the effect of high purity of the finished product, less impurities, and simple and easy operation method
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Embodiment 1
[0022] The embodiment of the present invention provides a method for purifying caprolactin, which includes the following steps:
[0023] (1) Add the caprolactone mother liquor to the glacial acetic acid solution, and stir the resulting mixed solution for use;
[0024] (2) Refrigerate the mixed solution to form an ice-water mixture, take out the ice-water mixture and filter with suction, remove the filtrate and leave the frozen material;
[0025] (3) Melt the frozen material and extract with chloroform or a mixture of acetone and chloroform;
[0026] (4) After extraction, take the upper liquid and add xylene for extraction;
[0027] (5) Discard the xylene extract, add the aqueous ammonia solution to the lower layer solution and mix well, and then filter with suction to obtain the caprolactin solid.
[0028] among them,
[0029] In the step (1), the volume ratio of the caprolactone mother liquor and the glacial acetic acid solution is 1:8, and the concentration of the glacial acetic acid so...
Embodiment 2
[0035] The embodiment of the present invention provides a method for purifying caprolactin, which includes the following steps:
[0036] (1) Add the caprolactone mother liquor to the glacial acetic acid solution, and stir the resulting mixed solution for use;
[0037] (2) Refrigerate the mixed solution to form an ice-water mixture, take out the ice-water mixture and filter with suction, remove the filtrate and leave the frozen material;
[0038] (3) Melt the frozen material and extract with chloroform or a mixture of acetone and chloroform;
[0039] (4) After extraction, take the upper liquid and add xylene for extraction;
[0040] (5) Discard the xylene extract, add the aqueous ammonia solution to the lower layer solution and mix well, and then filter with suction to obtain the caprolactin solid.
[0041] among them,
[0042] In the step (1), the volume ratio of the caprolactone mother liquor and the glacial acetic acid solution is 1:5, and the concentration of the glacial acetic acid so...
Embodiment 3
[0048] The embodiment of the present invention provides a method for purifying caprolactin, which includes the following steps:
[0049] (1) Add the caprolactone mother liquor to the glacial acetic acid solution, and stir the resulting mixed solution for use;
[0050] (2) Refrigerate the mixed solution to form an ice-water mixture, take out the ice-water mixture and filter with suction, remove the filtrate and leave the frozen material;
[0051] (3) Melt the frozen material and extract with chloroform or a mixture of acetone and chloroform;
[0052] (4) After extraction, take the upper liquid and add xylene for extraction;
[0053] (5) Discard the xylene extract, add the aqueous ammonia solution to the lower layer solution and mix well, and then filter with suction to obtain the caprolactin solid.
[0054] among them,
[0055] In the step (1), the volume ratio of the caprolactone mother liquor and the glacial acetic acid solution is 1:10, and the concentration of the glacial acetic acid s...
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Abstract
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