A kind of green treatment process of chlorophenyl glycerol dephenolization

Abstract

A green treatment process for dephenolization of chlorophenyl glycerol, the crude product of chlorophenyl glycerol is dissolved in a hot alkaline solution with a mass of 3 to 5 times, the temperature is 60 to 80 DEG C, the stirring speed is 100 to 300 r / min, and the mixture is stirred with The liquid level height ratio is 0.3 to 1, and the cooling time is 2 to 5 hours. When the temperature of the material drops to room temperature, the product is precipitated. The constant precipitation temperature is 25 ℃ for 1 to 3 hours, and it is allowed to stand for 0.5 hours. Pressure vacuum filtration, using 1 to 3 times the amount of filter cake to deionize at room temperature, so that the treatment is completed, the phenolic content of the product is below 100ppm, the product is processed again according to the above steps, the phenolic content of the product can be achieved. The loss rate does not exceed 3%. The invention simplifies the treatment process for removing phenol from the chlorophenyl glycerol product, improves the efficiency of removing phenol, is green and safe, the waste liquid is easy to treat, reduces the treatment cost, and creates conditions for its industrial application. The process realizes high dephenolization efficiency, green safety, no flammable, non-toxic solvent, low energy consumption, less waste liquid, and easy disposal.

Description

technical field [0001] The invention belongs to the technical field of preparation of antifungal and bacteriostatic agents, relates to the dephenolization treatment of a product of the antifungal and bacteriostatic agent chlorophenidyl ether, and in particular relates to a green treatment process for the dephenolization of chlorophenidyl ether. Background technique [0002] Chlorphenesin is a kind of excellent performance, anti-mold and bacteriostatic agent, it has good inhibitory effect on various bacteria, especially anti-fungal, bacteria, vaginal mold, Trichomonas disease. Its current synthesis method has about nine process routes. The process raw materials mainly use p-chlorophenol and 3-chloro-1,2-propylene glycol or 3-chloro-propylene oxide. Its preparation is the classic Williamson ether-forming reaction between p-chlorophenol sodium salt and halohydrin. This reaction is a SN2 bimolecular nucleophilic reaction to generate the main product, and a small amount of p-chl...

AI Technical Summary

Problems solved by technology

[0003] For the removal of p-chlorophenol in chlorphenesin products, the organic solvent crystallization process and multiple washing processes are widely used at home and abroad. Most of these solvents are toxic, harmful, flammable, and explosive, such as methanol, chloroform, etc. Moreover, the production implementation time is long, the requirements are high, and it has the disadvantages of high risk level.

In addition, for the adsorption analysis or elution process, the adsorption analysis process, the chlorphenesin product is solid, the main content is more than 90%, and the content of phenol is almost undetectable, which seriously exceeds the adsorption and desorption capacity of the adsorption column. restricted

In addition, the elution process often requires a large amount of eluent, and many times, but if p-chlorophenol is wrapped in the product, this method is almost ineffective

[0004] The above reflects that there are many problems such as large amount of solvent, flammability, toxicity, long time, high energy consumption and great harm in the process of dephenolization of chlorophenesin, which seriously restrict the sustainable and healthy development of enterprises.

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