Preparation method of chlorophenoxycarboxylic acid substance
A technology for chlorophenoxycarboxylic acids and substances is applied in the field of preparation of chlorophenoxycarboxylic acids, and can solve the problems of complex process, high consumption of sodium chlorocarboxylate, complex process flow and the like
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[0025] The invention provides a method for preparing chlorinated phenoxycarboxylic acids, comprising: S1) mixing and reacting phenoxy fatty alcohol shown in formula (I), an oxidizing agent, an oxidation catalyst and an alkaline substance, and filtering to obtain Reaction solution; S2) Mix and react the reaction solution, catalyst A, catalyst B and chlorinating agent to obtain chlorophenoxycarboxylic acid substances shown in formula (II); the catalyst A is a Lewis acid; the Catalyst B is one or more of C5-C22 sulfides, thiazoles, substituted thiazoles, isothiazoles, substituted isothiazoles, thiophenes and substituted thiophenes; the substituted thiazoles, substituted isothiazoles and substituted The substituents in thiophene are independently selected from one or more of C1-C5 alkyl groups and halogens;
[0026]
[0027] Wherein, R is H or C1~C4 alkyl, preferably H or C1~C3 alkyl, more preferably H or C1~C2 alkyl; R 1 It is H or C1-C5 alkyl, preferably H or C1-C4 alkyl, mo...
Embodiment 1
[0039] Mix 139.6g (1mol) of phenoxyethanol, 300g (1mol) of water, 40.5g (1mol) of sodium hydroxide and 3.1g of cobalt acetate, add 350g of 10% hydrogen peroxide, raise the temperature to about 80°C and keep it for 12 hours. After passing the conversion, lower the temperature to room temperature and filter to remove the molecular sieve catalyst, directly add 0.28g ferric chloride and 0.3g dimethyl sulfide to the filtrate, and pass in chlorine gas, and keep the pH at about 10 during the process. After the chlorination is completed, see hydrochloric acid to adjust the pH to about 1, filtered and dried to obtain 214.1 g of the product with a purity of 98.2% and a yield of 95.1%.
[0040] Utilize high-performance liquid chromatography to analyze the product that obtains, obtain the liquid phase chromatogram such as figure 1 As shown, the obtained liquid chromatography results are shown in Table 1.
[0041] Table 1 Liquid Chromatography Results
[0042] peak number
Embodiment 2
[0044] Mix 139.6g (1mol) of phenoxyethanol, 300g (1mol) of water, 40.5g (1mol) of sodium hydroxide and 1.6g of manganese chloride, add 350g of 10% hydrogen peroxide, raise the temperature to about 160°C and keep it for 12 hours. After unqualified transfer, reduce to room temperature and filter to remove the manganese chloride catalyst, directly add 0.28g magnesium chloride and 0.31g dimethyl phenyl sulfide to the filtrate, pass into chlorine gas, keep the pH at about 10 during the process, after the chlorination ends, see Adjust the pH to about 1 with hydrochloric acid, filter, and dry to obtain 216.1 g of the product, with a purity of 98.2% and a yield of 96.2%.
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