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A method for separating and recovering amiloride from waste residue of amiloride ammonium salt

A technology of amiloride ammonium salt and triclopyralid ammonium salt, which is applied in the field of separation and recovery of amiloride, can solve the problems of no relevant reports on the separation of substances containing pyridines with special structures, achieve qualified color, simple operation, The effect of avoiding pollution

Active Publication Date: 2019-04-30
HUNAN BIDE BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although the domestic and foreign literature and patents have studied the separation of some pyridine compounds, there is no relevant report on the separation of the pyridine compounds with special structure involved in the present invention.

Method used

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  • A method for separating and recovering amiloride from waste residue of amiloride ammonium salt
  • A method for separating and recovering amiloride from waste residue of amiloride ammonium salt
  • A method for separating and recovering amiloride from waste residue of amiloride ammonium salt

Examples

Experimental program
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Effect test

Embodiment 1

[0049] Add 2000L water, 150kg industrial hydrochloric acid, 150kgLaCl to the 3000L reactor in sequence 3 ·6H 2 O solid, 600kg raw material, stirring at room temperature for about 4h. During this period, the liquid phase is used to track the changes of the content of each substance in the reaction solution, and when the content of isomers drops below 1%, the next step operation is started.

[0050] Under the condition of normal temperature, turn on the condensing circulating water, slowly add 450kg of 30% NaOH solution, and the pH value of the solution is 9-10 at this time. After the pH of the reaction solution is stabilized, press filter with a plate and frame filter press to obtain filter cake II and filtrate I. Slowly add 230kg industrial hydrochloric acid in the filtrate I to adjust the pH value to be less than 2. After stirring for 20 minutes, filter to obtain filter cake III, wash it with 1000kg of water, and put it into an oven. After drying, the finished product of ...

Embodiment 2

[0053] The steps are the same as in Example 1, the difference is that the filter cake IV obtained in Example 1 is used instead of the transition metal compound to carry out the separation reaction. The white finished product of amiloride was obtained. The dry weight is 301.8kg, the content is 98.5%, and the yield is 61.9%. The pale yellow-white isomer of picloram was obtained. The dry weight is 170.6kg, the content is 93.3%, and the yield is 33.1%.

Embodiment 3

[0055] Its step is with embodiment 1, difference is: used FeSO 4 ·7H 2 O (552kg) was isolated as a transition metal compound. The off-white finished product of amiloride was obtained. The dry weight is 274.8kg, the content is 97.4%, and the yield is 55.8%. The pale yellow-white isomer of picloram was obtained. The dry weight is 196.1kg, the content is 85.2%, and the yield is 34.8%.

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Abstract

The present invention provides a method for separating and recovering picloram from picloram ammonium salt waste. According to the method, the ammonium salt waste produced during a picloram industrial production process is adopted as a raw material, and under the action of an acid and a transition metal compound, the high content picloram and the isomer 6-amino-3,4,5-Trichloropyridine carboxylic acid finished product are separated and recovered from the waste residue. With the method of the present invention, the effective utilization of the waste residue is achieved, and the environment pollution is reduced.

Description

technical field [0001] The invention belongs to the application field of green chemical industry, and mainly relates to a method for separating and recovering amiloride from waste residue of amiloride ammonium salt. Background technique [0002] The moisture content of the wet slag of the waste residue of amiloride ammonium salt is generally between 50% and 55%. The main components of the dry matrix of the waste residue of amiloride ammonium salt are: 4-amino-3, 5,6-triclopyridine carboxylate ammonium salt and 6-amino-3,4,5-triclopyridine carboxylate ammonium salt with a mass content of 10%-90%. The rest also contain a small amount of other isomers, such as ammonium salt of 3-amino-4,5,6-trichloroformate and ammonium salt of 5-amino-3,4,6-trichloropyridine carboxylate. unavoidable impurities. [0003] The structural formula of the main substance in the waste residue of amiloride ammonium salt is as follows: [0004] [0005] When R-NH 2 When it is located at the 4th p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/803C07D213/79
CPCC07D213/79C07D213/803
Inventor 付林薛晚霞王争龚红龙欧阳王宇李华轩
Owner HUNAN BIDE BIOTECH