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Wastewater treatment method in metribuzin synthesis process

A synthesis process and wastewater treatment technology, which can be used in neutralization water/sewage treatment, multi-stage water treatment, natural water treatment, etc., which can solve problems such as cost waste and achieve the effect of reducing environmental pollution.

Inactive Publication Date: 2017-05-10
江苏恒隆作物保护有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Mecitrione is a high-efficiency herbicide. During its reaction, waste water will be produced. The waste water contains a lot of sodium bromide and methanol. cause a great waste of cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: a kind of waste water treatment method in the synthesis technique of metrizone, comprises the steps:

[0017] A: Add concentrated sulfuric acid with a concentration of 98% to 100L waste water, adjust the pH to 2, stir for half an hour, add sodium hydroxide solution, adjust the pH to 5, heat to above 105 degrees, reflux for one hour, and carry out intermittent distillation of the filtrate, get methanol;

[0018] B: Choose 40ml tri(octyl-decyl)alkyl tertiary amine and 60ml carbon tetrachloride to make complexing agent, add in the raffinate in the above steps, stir and extract for half an hour, stand and separate the lower aqueous phase after clarification, put The water phase is further distilled to obtain methanol; the oil phase is neutralized by adding sodium hydroxide to a pH of 7, and then further heated and evaporated, the evaporated gas is absorbed by sodium hydroxide solution, and sodium bromide crystals are precipitated after cooling; the above raffi...

Embodiment 2

[0019] Embodiment 2: a kind of waste water treatment method in the synthesis process of metrizone, comprises the following steps:

[0020] A: Add concentrated sulfuric acid with a concentration of 98% to 100L waste water, adjust the pH to 2, stir for half an hour, add sodium hydroxide solution, adjust the pH to 5, heat to 105 degrees, reflux for one hour, and carry out intermittent distillation of the filtrate to obtain Methanol;

[0021] B: Select 50ml of tri(octyl-decyl)alkyl tertiary amine and 50ml of carbon tetrachloride to make complexing agent, add in the raffinate in the above steps, stir and extract for half an hour, stand and separate the lower aqueous phase after clarification, and The water phase is further distilled to obtain methanol; the oil phase is neutralized by adding sodium hydroxide to a pH of 7, and then further heated and evaporated, the evaporated gas is absorbed by sodium hydroxide solution, and sodium bromide crystals are precipitated after cooling; th...

Embodiment 3

[0022] Embodiment 3: a method for treating waste water in the synthesis process of mecitrione, comprising the following steps: A: adding concentrated sulfuric acid with a concentration of 98% to 100L waste water, adjusting the pH to 2, stirring for half an hour and adding sodium hydroxide solution, Adjust the pH to 5, heat to above 105 degrees, reflux for one hour, and carry out intermittent distillation of the filtrate to obtain methanol;

[0023] B: Choose 40ml tri(octyl-decyl)alkyl tertiary amine and 60ml carbon tetrachloride to make complexing agent, add in the raffinate in the above steps, stir and extract for half an hour, stand and separate the lower aqueous phase after clarification, put The water phase is further distilled to obtain methanol; the oil phase is neutralized by adding sodium hydroxide to a pH of 7, and then further heated and evaporated, the evaporated gas is absorbed by sodium hydroxide solution, and sodium bromide crystals are precipitated after cooling;...

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PUM

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Abstract

The invention discloses a wastewater treatment method in a metribuzin synthesis process. The wastewater treatment method comprises the following steps of (A) adding concentrated sulfuric acid to wastewater, adjusting the pH value to be smaller than 3, stirring for half an hour, adding a sodium hydroxide solution, adjusting the pH value to be 4-5, heating the concentrated sulfuric acid to above 100 DEG C, refluxing for an hour, and carrying out intermittent distillation on filtrate to obtain methanol; and (B) preparing a complexing agent, adding the complexing agent to the residual liquid in the step (A), stirring and extracting for half an hour, clarifying a lower layer of water phase, carrying out standing and separating, further distilling the water phase to obtain methanol, adding an oil phase to sodium hydroxide for neutralizing until the pH value is 6-8, carrying gout heating and evaporating, absorbing the evaporated gas by using the sodium hydroxide solution, separating out sodium bromide crystal after cooling, introducing the residual liquid into a strengthened aerobic biochemical pool for treatment for 40-80 hours, carrying out oxidization treatment through ozone for 20 hours, and treating the wastewater which is subjected to oxidization treatment through the ozone again through the strengthened aerobic biochemical pool for 10 hours, thereby completing the whole treatment process. According to the wastewater treatment method, purification treatment can be carried out on the wastewater; and bromine and methanol in the wastewater can be recycled and the treated wastewater can be directly discharged, so that the environmental pollution is reduced.

Description

technical field [0001] The invention specifically relates to a wastewater treatment method in the synthesis process of mecitrione. Background technique [0002] Mecitrione is a high-efficiency herbicide, and waste water will be generated during its reaction. The waste water contains a lot of sodium bromide and methanol, and the waste water smells very strong. If the serious pollution of the environment is excluded, the methanol content in the waste water is better. If it is discharged Cause a lot of cost waste. Contents of the invention [0003] Aiming at the deficiencies in the prior art, the present invention provides a wastewater treatment method in the synthesis process of mecitrione. [0004] A method for treating waste water in a metrizone synthesis process, characterized in that it comprises [0005] Follow the steps below: [0006] A: Add concentrated sulfuric acid with a concentration of 98% to a certain amount of waste water, adjust the pH to less than 3, stir...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/14C01D3/10C07C29/80C07C31/04C02F103/36
CPCC02F9/00C01D3/10C02F1/04C02F1/26C02F1/66C02F2103/36C02F2301/08C07C29/80C07C31/04
Inventor 李华苏复刘利平郭金冬
Owner 江苏恒隆作物保护有限公司
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