Catalyst residue reduction and resource utilization method

Abstract

The invention discloses a catalyst residue reduction and resource utilization method. The method comprises the following steps that firstly, pressure-reduced drying is carried out on filter cakes obtained by pressure filtration after desolventizing of p-trifluoromethylaniline synthetic liquid, and p-trifluoromethylaniline and p-trifluoromethyl chlorobenzene are recycled by dried condensate through rectification; and secondly, the dried filter cakes are crushed and are heated to 280-350 DEG C, and the filter cakes are condensed and crystallized again to be separated out after ammonium chloride is decomposed. According to the scheme, p-trifluoromethylaniline catalyst residues are dried through a conventional industrial method, main components in the dried condensate are p-trifluoromethyl chlorobenzene and p-trifluoromethylaniline, the dried condensate can be merged into a rectification raw material of a p-trifluoromethylaniline production system, p-trifluoromethylaniline and p-trifluoromethyl chlorobenzene are separated through rectification, p-trifluoromethylaniline serves as a finished product, and p-trifluoromethyl chlorobenzene serves as the raw material. After treatment of the scheme, a small amount of acidic wastewater is generated, and solid waste can be reduced by more than 65%.

Description

technical field [0001] The invention relates to the technical field of residue utilization methods, in particular to a catalyst residue reduction and resource utilization method. Background technique [0002] p-Trifluoromethylaniline is an important chemical raw material, especially widely used in pesticides and medicines. It is used in the pharmaceutical industry to synthesize new immunosuppressant drugs such as leflunomide and teriflunomide. In terms of pesticides, it can synthesize fipronil (fipronil), fluvalinate, flufenazuron, herbicides butadiene, butadiene, etc.; in addition, it can also synthesize fluorine-containing liquid crystal materials, etc., with the green With the continuous deepening of chemical technology and new drug research, new uses have been continuously developed, and it has become an important chemical product with development prospects. [0003] In the current synthesis of p-trifluoromethylaniline, the commonly used technique is to use p-chlorobenz...

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Problems solved by technology

[0003] In the current synthesis of p-trifluoromethylaniline, the commonly used technique is to use p-chlorobenzotrifluoride as raw material, with cuprous chloride and potassium fluoride as catalysts, amination in ethanol, water or other solvents, and then After desolvation and rectification, p-trifluoromethylaniline is obtained. After the synthesis of p-trifluoromethylaniline, the separated catalyst residue loses its activity and cannot be used mechanically. It can only be treated as solid waste. Aspects have increased the amount of solid waste; in the production of p-trifluoromethylaniline, the amount of catalyst used is larger, and the price is higher, especially cuprous chloride. Therefore, catalyst consumption is an important factor for the cost of trifluoromethylaniline raw materials component