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Method for treating wastewater produced by methylation reaction in metribuzin synthesis

A technology of methylation and mezotrione is applied in the field of treating wastewater generated by methylation reaction in the synthesis of methitrione, can solve problems such as no literature reports on wastewater treatment, achieve good practical value, reduce environmental pollution, The effect of reducing production costs

Inactive Publication Date: 2009-06-03
JIANGSU HUAYI GARMENT CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] So far, no literature reports have been found on the treatment of wastewater generated by the methylation reaction during the synthesis of mecitrione

Method used

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  • Method for treating wastewater produced by methylation reaction in metribuzin synthesis

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Experimental program
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Effect test

Embodiment 1

[0012] The method for treating the wastewater produced by the methylation reaction in the synthesis of mecitrione in this embodiment has the following steps:

[0013] ①The 500ml three-necked bottle is equipped with a return tube, and a gas absorption device is connected to the outlet of the return tube. The gas absorbing device comprises a glass tube and an inverted funnel connected in sequence, and also includes a beaker, which is filled with a 10wt% NaOH solution. Add 350 g of waste water produced by the methylation reaction in the synthesis of mecitrione into the three-necked flask, add 4 mL of sulfuric acid with a concentration of 98 wt % under stirring, and then raise the temperature to 105° C. for reflux to deodorize and decolorize. The gas generated and volatilized by the waste water during heating passes through the return pipe, then passes through the glass tube and funnel, and is absorbed by the NaOH solution in the beaker to remove the odor.

[0014] Continue to re...

Embodiment 2～ Embodiment 4

[0020] The processing method of each embodiment is basically the same as that of Embodiment 1, and the differences are shown in Table 1.

Embodiment 5

[0022] The treatment method of the present embodiment is basically the same as that of Example 1, the difference being that: in step 1., during reflux for 1.5 hours, the color of the waste water in the there-necked bottle gradually changes from brown to lavender, and then gradually becomes almost colorless, Then this step does not need to add activated carbon, and directly proceed to step ②. In step ②, directly remove the return pipe on the three-necked bottle, then install the packed tower, and then recover the methanol in the waste water by batch rectification. See Table 1 for other differences.

[0023] Table 1

[0024]

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Abstract

The invention discloses a method for treating wastewater produced by methylation reaction in metribuzin synthesis. In the method, the wastewater produced by the methylation reaction in the metribuzin synthesis is added with an acidic treating agent, and the obtained mixture is heated to 90 DEG C-120 DEG C and refluxed for deodorization and decolorization; and volatile gas in the wastewater and gas produced in the reflux are absorbed by alkaline solution for deodorization. Methanol in the wastewater is recovered by a batch distillation method. Residual liquid is heated to 100 DEG C-150 DEG C for evaporation, and then the residual liquid is naturally cooled by stirring until sodium bromide crystal is separated out. Filtrate is oxidized by an oxidant at the oxidation temperature of 50 DEG C-80 DEG C. A system is cooled to 10 DEG C-40 DEG C, and bromine in the system is extracted by an organic extractant, thus obtaining organic phase extracting solution with the bromine. The method helps solve the problem of treating methylated wastewater in metribuzin production, and reduce environmental pollution and production cost, the recovery rate of the bromine reaches more than 93%, and the method has good use value, and is simple and feasible.

Description

technical field [0001] The invention relates to a method for treating waste water, in particular to a method for treating waste water produced by methylation reaction in metrizone synthesis. Background technique [0002] Mecitrione is a highly effective herbicide. The final step of its synthesis is methylation reaction. The waste water produced by this reaction has a dark color and strong odor, which contains more methanol and sodium bromide. Due to the heavy odor of wastewater, the methanol in it cannot be distilled and recovered; and if the wastewater is directly treated in a harmless manner by biological methods, the sodium bromide in it will have a great impact on the life of fungi; direct discharge of wastewater will pollute the environment and cause Great waste of raw materials. Therefore, effectively removing the odor of the wastewater can not only recover methanol and bromine resources with higher value to reduce production costs, but also have a positive effect on ...

Claims

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Application Information

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IPC IPC(8): C02F9/10C02F1/04C02F1/72C02F1/26C01D3/10C01B7/09C02F103/36
Inventor 郑纯智张国华文颖频张春勇赵德建
Owner JIANGSU HUAYI GARMENT CO LTD
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