Purification method of 1,1,3-trichloroacetone and application thereof
A technology of trichloroacetone and purification method, applied in the separation/purification of carbonyl compounds, organic chemistry and other directions, can solve problems such as potential safety hazards and potential quality risks of folic acid
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Embodiment 1
[0046] This example illustrates 1,1,3-trichloroacetone prepared by the purification method of the present invention.
[0047] The purification process is carried out in a 50-liter reactor with a filter sieve plate at the bottom.
[0048] First, mix 20Kg of 1,1,3-trichloroacetone with a purity of 65% by weight and 10Kg of water in a reactor, and stir at 24°C for 12 minutes, wherein the stirring rate is 200r / min. During the stirring process Water was added, and the water was added at a rate of 300 ml / min, then the mixture was allowed to stand for 10 minutes, and the lower oil layer was separated to remove high-chlorine impurities;
[0049] Next, lower the temperature of the layered upper layer solution to 5° C., and stir for 2 hours at a stirring rate of 100 r / min;
[0050] Then, use nitrogen pressure filtration, the pressure is 0.1Mpa, directly pass through the sieve plate at the bottom of the reactor to obtain solid crystals, and then spray and wash with 1Kg of cold water at ...
Embodiment 2
[0054] This example illustrates 1,1,3-trichloroacetone prepared by the purification method of the present invention.
[0055] The purification process is carried out in a 50-liter reactor with a filter sieve plate at the bottom.
[0056] First, mix 20Kg of 1,1,3-trichloroacetone with a purity of 50% and 4Kg of water in a reactor, and stir at 45°C for 15 minutes, wherein the stirring speed is 300r / min, and during the stirring process, add Water, the water was added at a rate of 300 ml / min, then the mixture was allowed to stand for 15 minutes, and the lower oil layer was separated to remove high-chlorine impurities;
[0057] Next, lower the temperature of the layered upper layer solution to 20° C., and stir for 0.5 hours at a stirring rate of 200 r / min;
[0058] Then, use nitrogen pressure filtration, the pressure is 0.2Mpa, directly pass through the sieve plate at the bottom of the reaction kettle to obtain solid crystals, and then spray and wash with 1Kg of cold water at 25°C...
Embodiment 3
[0062] This example illustrates 1,1,3-trichloroacetone prepared by the purification method of the present invention.
[0063] The purification process is carried out in a 50-liter reactor with a filter sieve plate at the bottom.
[0064] First, mix 20Kg of 1,1,3-trichloroacetone with a purity of 60% and 40Kg of water in a reactor, and stir at 15°C for 30 minutes, wherein the stirring speed is 100r / min, and during the stirring process, add Water, the water was added at a rate of 500 ml / min, then the mixture was allowed to stand for 30 minutes, and the lower oil layer was separated to remove high-chlorine impurities;
[0065] Next, lower the temperature of the upper layer solution after stratification to 10° C., and stir for 10 hours at a stirring rate of 100 r / min;
[0066] Then, use nitrogen pressure filtration, the pressure is 0.2Mpa, directly pass through the sieve plate at the bottom of the reaction kettle to obtain solid crystals, and then spray and wash with 1Kg of cold ...
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