Continuous preparation method of herbicide intermediate 2, 4-dichlorphenoxyacetic acid
A technology of sodium dichlorophenoxyacetate and intermediates, which is applied in the field of herbicide intermediates 2, can solve the problems of difficult production management, many side reactions, and high labor intensity, so as to improve the production site environment and controllable production safety , the effect of reducing labor intensity
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example 1
[0012] 2,4-dichlorophenol and chloroacetic acid with a molar ratio of 1:1.2 are configured into an aqueous solution with a concentration of 35% and a concentration of 45%, and at a temperature of 80°C, successive reactions occur through three-stage condensation reaction towers, And the pH of the reaction is controlled to be 8 by adding a sodium hydroxide aqueous solution with a concentration of 30%. The content of the material analysis is: 2,4-dichlorophenol sodium: 0.1%, chloroacetic acid: 0.5%, sodium salt: 32.03%; Finally, the temperature of the reacted liquid material was lowered to 35° C. by reusing water, and suction filtration was performed to obtain the sodium 2,4-dichlorophenoxyacetate with a yield of 96.13%.
Embodiment 2
[0014] 2,4-dichlorophenol and chloroacetic acid with a molar ratio of 1:1.4 are configured into an aqueous solution with a concentration of 35% and a concentration of 45%, and at a temperature of 100°C, successively react through 4 stages of condensation reaction towers, And by adding the sodium carbonate aqueous solution that concentration is 30%, the mode control reaction pH is 10, gets material analysis content: 2,4-sodium dichlorophenolate: 0.1%, chloroacetic acid: 0.5%, sodium salt: 33.82%; Finally The liquid material after the reaction was cooled to 40° C. by reusing water and suction-filtered to obtain the sodium 2,4-dichlorophenoxyacetate with a yield of 98.00%.
Embodiment 3
[0016] 2,4-dichlorophenol and chloroacetic acid with a molar ratio of 1:1.5 are configured into aqueous solutions with a concentration of 35% and a concentration of 45%, and at a temperature of 110°C, successively react through five stages of condensation reaction towers, And the pH of the reaction is controlled to be 12 by adding a potassium hydroxide aqueous solution with a concentration of 30%. The content of the material analysis is: 2,4-dichlorophenol sodium: 0.1%, chloroacetic acid: 0.1%, sodium salt: 30.17%; Finally, the reacted liquid material was cooled to 45° C. by reusing water and filtered with suction to obtain the sodium 2,4-dichlorophenoxyacetate with a yield of 95.07%.
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