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Method for treating brominated and etherified waste liquid of pyraclostrobin

A technology for the treatment of ester brominated ethers and waste liquids, which is applied in chemical instruments and methods, bromine/hydrogen bromide, bromine, etc., can solve problems such as increased costs, many impurities in the water phase, and limited use of sodium bromide, and achieves Improve utilization rate and reduce waste

Active Publication Date: 2018-11-06
SICHUAN FOURSTAR BIOTECH RANDD CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims to solve the problem of separately adding alkali and acid to neutralize the waste liquid in the bromination and etherification stages, which increases the cost; at the same time, there are more impurities in the water phase in the etherification stage, and the sodium bromide recovered after the acidification treatment is used Issues with limited scope

Method used

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  • Method for treating brominated and etherified waste liquid of pyraclostrobin
  • Method for treating brominated and etherified waste liquid of pyraclostrobin

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Add 5kg of wastewater containing 6.1% hydrobromic acid in the bromination section to 15kg of etherification wastewater containing 20% ​​sodium bromide.

[0040] Centrifuge to remove the insoluble matter in the mixed wastewater to obtain a light yellow clear liquid with a pH<1.

[0041] Put the clarified liquid into a 50L reaction kettle, then slowly add 2.9 kg of 60% sulfuric acid into the reaction vessel, stir and raise the temperature to 60 degrees Celsius, then slowly add 2.3kg of hydrogen peroxide with a concentration of 27.5% dropwise, heat up to distillation, condense and use 10kg of dichloroethyl alkane solution to collect bromine and bromine vapor from exhaust gas.

[0042] After most of the bromine is evaporated, the temperature is lowered to 60 degrees Celsius, and then 5kg of dichloroethane is pumped in to azeotrope the remaining bromine in the reactor, and the orange red color in the reactor fades. The above bromine-containing dichloroethane solutions were ...

Embodiment 2

[0045] Add 10kg of wastewater containing 8.2% hydrobromic acid in the bromination section to 10kg of etherification wastewater containing 21.4% sodium bromide salt.

[0046] Centrifuge to remove the insoluble matter in the mixed wastewater to obtain a light yellow clear liquid with a pH<1.

[0047]Put the clarified liquid into a 50L reaction kettle, then slowly add 2.0 kg of 60% sulfuric acid into the reaction vessel, stir and heat up to 60 degrees Celsius, then slowly add 2.2 kg of hydrogen peroxide with a concentration of 27.5%, heat up to distillation, condense and use 10kg of dichloroethyl alkane solution to collect bromine and bromine vapor from exhaust gas.

[0048] After most of the bromine is evaporated, the temperature is lowered to 60 degrees Celsius, and then 5kg of dichloroethane is pumped in to azeotrope the remaining bromine in the reactor, and the orange red color in the reactor fades. The above bromine-containing dichloroethane solutions were combined, and the...

Embodiment 3

[0051] A method for treating pyraclostrobin brominated etherification waste liquid, comprising the following steps:

[0052] A. Bromination and etherification waste liquid mixing

[0053] The waste liquid from the bromination section and the waste liquid from the etherification section are combined to precipitate 0.1% to 2.5% of organic impurities, and the clarified liquid is obtained by centrifugal filtration; the centrifugal speed is 2000 to 3000r / min.

[0054] B. Acidification of waste liquid

[0055] Add 50% to 65% sulfuric acid to the clarified liquid to obtain acidic waste liquid; the pH of the acidic solution is ≤2;

[0056] C. Hydrogen peroxide reaction

[0057] Add hydrogen peroxide to the acidic waste liquid in step B to obtain a reaction solution;

[0058] D. Absorbing bromine and tail gas for the first time

[0059] Heating the reaction solution in step C to 80-95° C. for distillation, condensing and absorbing bromine with a bromine absorption reagent to obtain...

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Abstract

The invention discloses a method for treating brominated and etherified waste liquid of pyraclostrobin, and belongs to the field of environmental protection and organic synthesis. In the prior art, brominated wastewater and etherified wastewater are separately treated, therefore, alkali and acid are respectively required to be added to neutralize the wastewater, then sodium bromide contained in the wastewater is concentrated and extracted, and since more impurities are contained in an aqueous phase of an etherification section, the recycled sodium bromide can only be used as a by-product of agricultural grade sodium bromide. Additional addition of acid and alkali causes the increase of the production cost of a company, and additional sodium bromide by-products are produced at the same time. Therefore, according to the invention, the brominated wastewater is used to mix with the etherified wastewater, and then hydrogen peroxide is used to oxidize and extract bromine therein, so that thegeneration of bromine-containing solid waste is avoided, and the recovered bromine can be further applied to the next batch of bromination reactions.

Description

technical field [0001] The invention relates to the field of environmental protection and organic synthesis, based on the post-treatment method of pyraclostrobin bromination and etherification waste liquid and the recovery of raw material bromine, and specifically relates to the post-treatment of pyraclostrobin three wastes and the recovery process of raw materials. Background technique [0002] Pyraclostrobin, also known as pyraclostrobin, is a methyl methoxyacrylate broad-spectrum fungicide with a pyrazole structure discovered by BASF in 1993. The drug has broad-spectrum bactericidal activity and is suitable for a wide range of crops. The main crop markets are soybeans, grains, corn, grapes, and fruits and vegetables. It can prevent and control plant diseases caused by almost all types of fungal pathogens such as Ascomycetes, Basidiomycetes, Deuteromycetes and Oomycetes, and it is also a hormone-type fungicide. It has the characteristics of low toxicity, safety to non-tar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D5/00C01B7/09C07C201/12C07C205/11C07D231/22
CPCC01B7/096C01D5/00C07C201/12C07D231/22C07C205/11
Inventor 朱槽刘虎李舟王文
Owner SICHUAN FOURSTAR BIOTECH RANDD CORP