Treatment method for CTC rectifying still residues

A treatment method and rectification still technology, which is applied in the field of CTC rectification still residue treatment, can solve the problems of incineration equipment corrosion, unfavorable environmental protection, and environmental secondary pollution, so as to reduce treatment costs, benefit environmental protection, Ease of incineration

Active Publication Date: 2017-06-30
内蒙古佳瑞米精细化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, at present, the residue of the still is generally incinerated as solid waste in China. However, since the residue of the CTC rectification is acidic and contains a large amount of chlorine atoms, a large amount of HCl is produced during the incineration process, which causes signif

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  • Treatment method for CTC rectifying still residues

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Experimental program
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Effect test

Embodiment 1

[0033] 1. In a 1000mL round bottom flask, add 200g of CTC distillation still residue and 500g of methanol, connect the condenser, stir and reflux for 30 minutes, then cool and suction filter to obtain 658.5g of filtrate;

[0034] 2. Return the filtrate to the 1000mL round bottom flask, connect the condenser, reflux under stirring conditions (reflux temperature 80°C), add solid sodium hydroxide to the reaction solution in three batches (the input amount of each batch is basically the same) 8g (0.2mol), gas chromatographic tracking reaction, when the total amount of chlorinated compounds in the reaction solution <2%, stop heating, continue to stir;

[0035] 3. When the temperature of the reaction solution drops to room temperature, add dropwise dilute hydrochloric acid with a concentration of 10-20wt.% to the reaction solution, adjust the pH to 5, continue stirring for 3 hours, then pour the reaction solution into water, wash with water three times, and let it stand Separate the...

Embodiment 2

[0037] The amount of methanol in step 1 in Example 1 is changed to 1000g, and other operating conditions include the same as in Example 1 after treatment steps. 107.3 g of the final residue was obtained, the total amount of chlorinated compounds was 0.7%, and the yield was about 93.2%.

Embodiment 3

[0039] The methyl alcohol of step 1 among the embodiment 1 is changed into ethanol, and other operation conditions comprise the uniform embodiment 1 same of aftertreatment step. 118.5 g of the final residue was obtained, the total amount of chlorinated compounds was 1.8%, and the yield was about 91.6%.

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Abstract

The invention discloses a treatment method for CTC rectifying still residues and belongs to the technical field of treatment of solid waste in chemical industry production processes. According to the method, a solvent is added into the rectifying still residues for an impurity removing technique at first; and then solid alkali is added into a mixed liquid subjected to impurity removing in batches, a temperature increasing refluxing reaction is conducted, high-content pyridine chlorides are converted into carbon, hydrogen, oxygen and nitrogen compounds, and incineration treatment is facilitated. The economic pressure of enterprises for treating the still residues is relieved, and the environment is protected.

Description

technical field [0001] The invention belongs to the technical field of solid waste treatment produced in the chemical production process, and in particular relates to a treatment method for CTC rectification still residue. Background technique [0002] CTC, the chemical name is 2-chloro-6-trichloromethylpyridine, the CAS number is 1929-82-4, and it is a white solid with a relative density of 1.58 (water is 1.0) at room temperature. CTC is an important pesticide and pharmaceutical intermediate, a digestive inhibitor, also known as a nitrogen fertilizer synergist. CTC is mainly produced by chlorination of 2-picoline in the presence of a catalyst and a solvent (US3420883, US4483993, US4487935, US4564681, JP2005255560, EP0557967). During the preparation of CTC, the chlorination reaction of 2-picoline is affected by many factors. During the reaction, other positions on the pyridine ring will undergo nucleophilic substitution to generate 2,3-dichloro-6-trichloromethylpyridine, 2 ...

Claims

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Application Information

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IPC IPC(8): A62D3/34A62D101/22
CPCA62D3/34A62D2101/22
Inventor 柯有胜王克勇王立家张树田
Owner 内蒙古佳瑞米精细化工有限公司
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