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Process for removing N-nitroso-pendimethalin from pendimethialin

A technology of nitroso pendimethalin and pendimethalin, applied in chemical instruments and methods, preparation of amino compounds from amines, preparation of amino compounds, etc., can solve the problems of reducing the content of nitrosamines and not being able to use them , to achieve the effects of lowering the denitration temperature, reducing the amount of removing agent, and lowering the reaction temperature

Inactive Publication Date: 2007-11-14
CNPC JILIN CHEM GROUP CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since pyrolysis produces not only the target product pendimethalin, but also a quinone substance structure with an equal amount of substance, the pyrolysis method can only be used to further reduce the content of nitrosamines in the product, but not in the production of nitrosamines. Use when amine content is high

Method used

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  • Process for removing N-nitroso-pendimethalin from pendimethialin
  • Process for removing N-nitroso-pendimethalin from pendimethialin
  • Process for removing N-nitroso-pendimethalin from pendimethialin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 6g (0.02mol) of pendimethalin containing a certain amount of N-nitroso pendimethalin (content 30%) detected by HPLC was dissolved in 30g (24ml) of 1,2-dichloroethane, stirred Place it in a three-necked flask with a condenser, a thermometer and a stirring heating device, then add 12g of concentrated hydrochloric acid (10ml), gradually raise the temperature to 75°C, and react for 1h; then add 1.2g of FeCl 2 4H 2 O (0.006mol), continue to maintain 75 ° C for 3h, and then stop stirring. Sampling was detected by HPLC, and the content of N-nitrosodimethalin was lower than 100ppm.

[0032] Liquid chromatography analysis conditions: C18 column (150mm×4mm), mobile phase: acetonitrile: water = 80:20 (v / v), flow rate 1.0mL / min, detection wavelength 254nm, pendimethalin retention time is 5.93min , The retention time of N-nitroso pendimethalin was 3.36min, and the area was normalized and quantified (the same below).

Embodiment 2

[0034] 6g (0.02mol) is dissolved in 6g (5ml) 1, in 2-dichloroethane, starts Stir and place it in a three-necked flask with a condenser, a thermometer and a stirring heating device, then add 3g (2.5ml) of concentrated hydrochloric acid, gradually raise the temperature to 75°C, and react for 1h; then add 0.3g of FeCl 2 4H 2 O (0.0015mol), continue to keep the reaction at 75°C for 3h and then stop stirring, take a sample and detect it by HPLC, the content of N-nitrosodimethalin is less than 100ppm. (analysis method is with embodiment 1).

Embodiment 3

[0036] 6g (0.02mol) of pendimethalin containing a certain amount of N-nitroso pendimethalin (content 30%) detected by HPLC was dissolved in 60g (47.7ml) of 1,2-dichloroethane, Start stirring and place it in a three-necked flask with a condenser, a thermometer and a stirring heating device, then add 15g (12.6ml) of concentrated hydrochloric acid, gradually raise the temperature to 75°C, and react for 1h; then add 6g of FeCl 2 4H 2 O (0.03mol), continue to maintain 75 ° C for 3h, and then stop stirring. Sampling was detected by HPLC, and the content of N-nitrodimethalin was lower than 100ppm. (analysis method is with embodiment 1).

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Abstract

This invention relates to method of removing N - nitroso Pendimethalin from herbicide Pendimethalin Ling. The invention takes FeCl2.4H2O as drawing off agent under concentrated hydrochloric acid presence. The process: dissolve Pendimethalin that containing certain amount of N - nitroso Pendimethalin in ethylene dichloride, then by whiping move the solution to three-necked bottle with condenser pipe, thermometer and whiping- heating arrangement. The weight ratio of crude Pendimethalin and ethylene dichloride is 1:1 to 10; add Concentrated hydrochloric acid, the weight ratio of Pendimethalin and Concentrated hydrochloric acid is 1:0.5 to 2.5, gradually heating-up to 75 deg and take reaction for 1 hour; then add FeCl2. 4H2O to the three-necked bottle, the weight ratio of FeCl2. 4H2O and crude Pendimethalin is 1:1 to 20, keep 75 deg for 3h. NN- NO compound content is less than 100ppm.

Description

[0001] technical field [0002] The invention relates to a method for removing part of N-nitroso pendimethalin from the original drug of herbicide pendimethalin and converting it into pendimethalin; FeCl 2 4H 2 O is a reagent for removing, and the content of N-nitroso pendimethalin is reduced to below 100ppm. Background technique [0003] Substituted anilines will produce N-nitroso compounds as by-products during the nitration process. Since N-nitroso compounds are carcinogenic to most mammals, the U.S. Environmental Protection Agency has made strict regulations on the content of N-nitroso compounds in various chemicals. The content of chemicals must be reduced to below the specified standard content before marketing, and the content of N-nitroso compounds in pendimethalin (N-nitroso pendimethalin, the same below) is limited to Below 135ppm. Therefore how to reduce the content of N-nitroso compounds in pendimethalin has become an extremely important problem. [0004] The...

Claims

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Application Information

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IPC IPC(8): C07C211/52C07C209/00C07C209/68
Inventor 张锁秦田晓金张新民霍凤华郑良玉李耀先
Owner CNPC JILIN CHEM GROUP CORP
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