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Industrialized production method for continuous preparation of 2-chloro-5-methylpyridine

A methyl pyridine and solvent technology, applied in the production field of pesticide intermediates, can solve the problems of high equipment requirements, low industrial production capacity and high energy consumption, and achieve the effects of safe and reliable production, good product quality and simple process

Active Publication Date: 2017-06-09
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The other is the CMP chlorination route, with propionaldehyde and morpholine as starting materials, after six steps of reaction to synthesize CMP and then chlorination to generate CCMP; this route has six steps of reaction steps, the total yield of the product is 62%, and the energy consumption High; In addition, the morpholine-propionaldehyde CMP chlorination process uses a large excess of phosphorus oxychloride, which requires high equipment, and produces 10-15 tons of phosphorus-containing concentrated wastewater and 0.5t of solid waste per ton of CMP
[0006] Patent US5304651A discloses a method for synthesizing CMP by using propionaldehyde and benzylamine as raw materials through a three-step reaction. In the patent, this route has the advantages of fewer reaction steps, high product yield, less waste, and moderate technical difficulty. Potential for industrialization; the disadvantage is intermittent production, low industrial production capacity, and product quality is easily affected by the control level of production operators; it is difficult to implement industrialization

Method used

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  • Industrialized production method for continuous preparation of 2-chloro-5-methylpyridine
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  • Industrialized production method for continuous preparation of 2-chloro-5-methylpyridine

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0041] 1. Preparation

[0042] 1) Preparation of benzylamine triethylamine solution: turn on the stirring switch, open the nitrogen valve, and replace the air for 30 minutes, weigh 600 kg benzylamine and 800 kg triethylamine respectively at room temperature, and put them into the benzylamine triethylamine solution preparation kettle, stand-by

[0043] 2) Open the respective valves to form the first, second, third, fourth, and fifth stages in series in sequence, turn on their respective stirring, jacket general cooling and steam, and control the temperature of each kettle to the required level

[0044] 3) Add 100L triethylamine, 2.5 kg of 30% NaOH aqueous solution, and 100L triethylamine to the first, second, and fourth-stage reaction kettles respectively.

[0045] 4) The volumes of the first, second, third, fourth and fifth stages are 1000L, 1000L, 3000L, 3000L and 5000L respectively

[0046] 2. Feeding

[0047] 5) Start the benzylamine triethylamine and propionaldehyde fee...

example 2-5

[0053] In order to investigate the influence of the amount of triethylamine and the reaction temperature on the synthesis of benzyl propylimine, experiments were carried out in which different amounts of triethylamine and temperatures participated in the reaction, and all the other conditions were the same as in Example 1. The data is as follows:

[0054]

example 6

[0056] 1. Preparation

[0057] 10) Open the respective valves to form the A, B, C, D, and E kettles in series in sequence, turn on the respective stirring, jacket general cooling and steam, and control the temperature of each kettle to the requirement

[0058] 11) A, B, C, D, E tank volumes are 1000L, 3000L, 2000L, 2000L, 5000L respectively

[0059] 2. Feeding

[0060] 12) Turn on the benzylpropylimine and acetic anhydride feeding metering pumps respectively, and simultaneously pump the benzylpropylimine triethylamine solution and acetic anhydride into the kettle A, and the flow rates of the feeding pumps are 529kg / hr and 206kg respectively / hr

[0061] 13) After continuous feeding for about 1 hour, the material in kettle A overflows into kettle B

[0062] 14) After continuing to feed for about 3 hours, the material in tank B overflows into tank C, and part of the material is rapidly vaporized. Adjust the appropriate reflux ratio and continue to produce light components thr...

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Abstract

The invention discloses an industrialized production method for continuous preparation of 2-chloro-5-methylpyridine and relates to the technical field of production of pesticide intermediates. The industrialized production method for continuous preparation of the 2-chloro-5-methylpyridine includes the step of preparing the 2-chloro-5-methylpyridine with benzylamine as a main starting material and triphosgene or phosgene as a chlorinating agent in the presence of a catalyst in a tanks-in-series manner. The industrialized production method for continuous preparation of the 2-chloro-5-methylpyridine has the advantages that defects of small capacity of intermittent reaction equipment, unstable quality control and long-time preparation can be overcome; the preparation method is high in reaction yield and excellent in product quality, a total preparation yield is not less than 87.0%, and 2-chloro-5-methylpyridine content is not less than 99.5%.

Description

technical field [0001] The invention relates to the technical field of production of pesticide intermediates, in particular to a production method of imidacloprid intermediate 2-chloro-5-picoline (CMP). Background technique [0002] 2-Chloro-5-chloromethylpyridine (CCMP) is an important intermediate of the nicotinic insecticide imidacloprid, and its industrial manufacturing method mainly has two ways: direct synthesis and via 2-chloro-5-methylpyridine (CMP) Chlorination Preparation. The direct synthesis process route of consulting the data includes: picoline direct chlorination method (JP7-149726); nicotinic acid method (DE0373463); cyclopentadiene method; CMP chlorination preparation CCMP route has: 3-picoline oxychloride chemical method (DE3800179A1) and ring method. [0003] Due to the source of raw materials, production cost, difficulty in implementing industrialization and the constraints of the three wastes, there are currently two main synthetic routes adopted by ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 石苏洋马勇王秋萍孟先跃马捷杨震宇朱明星
Owner JIANGSU YANGNONG CHEM GROUP