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A kind of preparation method of metrizone and the treatment method of waste liquid

A treatment method, the technology of mezatrione, is applied in chemical instruments and methods, purification/separation of hydrocarbons, organic chemistry, etc., which can solve the problems of impurity and low solvent recovery rate, and achieve high recovery rate, high purity, secondary The effect of less product

Active Publication Date: 2020-09-15
JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method produces a large amount of impure sodium sulfate and potassium sulfate mixed salt, uses a large amount of easily poisonous low-boiler solvent acetone, and the solvent recovery rate is low

Method used

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  • A kind of preparation method of metrizone and the treatment method of waste liquid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 540g p-xylene in a 2L four-necked bottle, add 8.5g of 98% concentrated sulfuric acid dropwise, add 180g of triazone with a content of 95% at one time under stirring, and add 59.5g of dimethyl sulfate dropwise when the temperature rises to 70°C, and control The dropping time is 0.5h. After the dropping is completed, the temperature is raised to 80°C and kept at this temperature for 8 hours. The gas phase qualitatively detects that the remaining content of triazone is 0.9%. When the ice-water bath cools down to 60°C, add water to the reaction solution 30g, then layered to obtain the p-xylene layer and the water layer, the p-xylene layer is washed with 5% liquid caustic soda of 20g to collect the alkali washing solution, and the p-xylene layer after the liquid caustic washing is washed with 20g water to collect the water washing solution, The p-xylene layer washed with water was distilled at 85°C under reduced pressure, transferred to a vacuum drying oven for 8 hours at...

Embodiment 2

[0039] Add 505g of p-xylene in a 2L four-necked bottle, add 8.5g of 98% concentrated sulfuric acid dropwise, add 180g of triazone with a content of 95% at one time under stirring, and add 61.5g of dimethyl sulfate dropwise when the temperature rises to 70°C. The dropping time is 0.5h. After the dropping is completed, the temperature is raised to 75°C and kept at this temperature for 6 hours. The remaining content of triazone is detected to be 1.2% in gas phase sampling. Continue to keep warm for 4 hours and re-sample the remaining content of triazone 0.8%, when ice-water bath is cooled to 55 ℃, add water 30g in the reaction solution, carry out layering then and obtain p-xylene layer and water layer, p-xylene layer is washed with 5% liquid caustic soda of 22g and collects alkali washing liquid, through The p-xylene layer washed with liquid caustic soda was washed with 20 g of water to collect the washing liquid, the p-xylene layer after water washing was distilled under reduced ...

Embodiment 3

[0043]Add 530g of p-xylene into a 2L four-necked bottle, add 8.6g of 98% concentrated sulfuric acid dropwise, add 180g of triazone with a content of 95% at one time under stirring, and add 60.4g of dimethyl sulfate dropwise when the temperature rises to 70°C, and control The dropping time is 0.5h. After the dropping, the temperature is raised to 80°C and kept at this temperature for 7 hours. The gas phase qualitatively detects that the remaining content of triazone is 0.85%. When the ice-water bath cools down to 58°C, add water to the reaction solution 30g, then layered to obtain the p-xylene layer and the water layer, the p-xylene layer is washed with 5% liquid caustic soda of 20g to collect the alkali washing solution, and the p-xylene layer after the liquid caustic washing is washed with 20g water to collect the water washing solution, The p-xylene layer washed with water was distilled at 85°C under reduced pressure, transferred to a vacuum drying oven for 8 hours at 60°C, a...

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Abstract

The invention relates to a preparation method of metribuzin and a treatment method of waste liquid. The preparation method comprises the following steps: carrying out heat-insulation reaction on triazinone and dimethyl sulfate at 75 to 80 DEG C in the presence of p-xylene and concentrated sulfuric acid; after the reaction is finished, cooling to 60 DEG C or below; adding water and quenching the reaction; washing a p-xylene layer, distillating under the reduced pressure and drying to obtain the metribuzin. According to the preparation method provided by the invention, the triazinone, which is convenient to purchase in the market, is used as a raw material, the p-xylene is used as a solvent and the concentrated sulfuric acid is used as a catalyst; the metribuzin is prepared through a methodof dropwise adding the dimethyl sulfate; in the reaction process, few byproducts are produced and the treatment method is simple. In a wastewater treatment link, the p-xylene and water can be recycledand utilized and unreacted triazinone is easy to recycle and reutilize. The method provided by the invention has the advantages of high recycling rate, low cost and short production period and the prepared metribuzin has high purity and meets safety and environment protection requirements.

Description

technical field [0001] The invention specifically relates to a method for preparing metrizone and a method for treating waste liquid. Background technique [0002] Metribuzin, English common name: metribuzin, chemical name: 4‐amino‐6‐(1,1‐dimethylethyl)‐3‐methylthio‐1,2,4‐triazine‐5‐tetrahydro Ketone, a systemic selective herbicide, exerts its herbicidal activity mainly by inhibiting the photosynthesis of sensitive plants. After spraying, the germination of seedlings of sensitive weeds is not affected. After emergence, the leaves chlorotic, and finally die of nutrient depletion. It has a good control effect on annual broad-leaved weeds and some grass weeds, but is ineffective on perennial weeds. The efficacy of mecitrione is greatly affected by soil type, organic matter content, humidity and temperature, and the conditions for use are relatively strict. If used improperly, it may be ineffective or even cause phytotoxicity. [0003] Most of the commonly used synthetic metho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D253/075C07C7/00C07C15/08
CPCC07C7/005C07C15/08C07D253/075
Inventor 纪雷姜宇华蔡军义周斌吕宜飞
Owner JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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