Method for preparing chloraniliprole from Wille D as raw material

Abstract

The invention relates to a method for preparing chloraniliprole from Uille silk D. The method comprises the following steps: stirring and dissolving a Uille silk D raw material or a mixed raw material of Uille silk D, hydroquinone and p-aminophenol in any proportion into a mixed liquid of a specific inorganic acid solution and a specific organic solvent, then introducing chlorine while stirring, carrying out a chlorination reaction at 60-110 DEG C, and separating the chloraniliprole from the chloraniliprole silk D to obtain chloraniliprole silk D, when the melting point of the target product chloraniliprole is detected to be greater than or equal to 292 DEG C and is maintained for more than 10 minutes and the melting point is not continuously increased, stopping introducing chlorine to obtain a chloraniliprole crystal, and filtering, washing and drying to obtain a chloraniliprole finished product; cooling, filtering and decolorizing ammonium chloride generated in the reaction to obtain an ammonium chloride finished product; hydrogen chloride gas generated by the reaction is absorbed by washing water to form a hydrochloric acid finished product; excessive chlorine in the reaction process is absorbed by liquid caustic soda to form a sodium hypochlorite finished product; and the filtered and recycled mother liquor can be infinitely used, so that zero emission is realized.

Description

technical field [0001] The technical scheme of the present invention belongs to the field of organic chemistry, and specifically takes Ursi D as a raw material to directly synthesize chloranil. Background technique [0002] Chloran is a yellow powder with a melting point above 292°C. It is used in the production of pharmaceutical intermediates and antioxidants, and is also one of the main raw materials for the production of permanent violet pigments (partly for export). Beginning in the 1980s, foreign countries began to limit the content of dioxins in chloran products and formulate relevant standards. Since the late 1990s, my country has generally adopted the hydroquinone method instead of the phenol method to produce chloran products to meet the requirements. The requirements of medium and high-end users for dioxin indicators. However, due to the high price of hydroquinone in recent years, this process has been basically eliminated in China. At present, the production proc...

AI Technical Summary

Problems solved by technology

Present domestic basically is to adopt the production technology that takes p-aminophenol as raw material to synthesize chlorinated, but because this technology fails to solve the influence that produces ammonium chloride in the reaction process to mother liquor, makes the mother liquor used in production can't be continuously recycled, Not only the processing cost of the mother liquor is high, but also new pollution and solid waste may be generated. In addition, the price of p-aminophenol is also rising sharply, so this production process is difficult to meet the needs of current production enterprises.

[0003] In addition, in recent years, there have been patents for re-using phenol as raw material to produce chlorine, but due to dangerous and heavily polluting processes such as nitrification and the use of concentrated flow acid, as well as problems such as low product content and high dioxin content, there is no such patent yet. Reports on mass production, etc.