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Method for extracting oxime compounds from cymoxanil mother liquor wastewater to synthesize cymoxanil

A technology of oxime compound and cyanurate cyanide is applied in the field of extracting oxime compound to synthesize cyanuric acid cyanamide, which can solve the problems of difficulty in direct treatment of wastewater, high operating cost, and high investment in treatment equipment, so as to increase efficiency and competitiveness, and reduce the cost of treatment. The effect of load and operation safety

Active Publication Date: 2012-09-12
利民化学有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is quite difficult to directly treat the wastewater, and the investment in the treatment device is high, and the operating cost is high

Method used

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  • Method for extracting oxime compounds from cymoxanil mother liquor wastewater to synthesize cymoxanil
  • Method for extracting oxime compounds from cymoxanil mother liquor wastewater to synthesize cymoxanil
  • Method for extracting oxime compounds from cymoxanil mother liquor wastewater to synthesize cymoxanil

Examples

Experimental program
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Embodiment 1

[0027] A method for synthesizing cymoxanil by extracting oximide from cymoxanil mother liquor wastewater, its specific operation steps are as follows:

[0028] Step 1. Pump the waste water from the mother liquor storage tank into the extraction reaction kettle, and add acid to the cymoxanil mother liquor while stirring. The acid used in this embodiment is concentrated sulfuric acid, and the pH value is adjusted to 0.5-1.5, and the oximide is gradually precipitated. After reacting for 12 minutes, discharge and suction filter to obtain an oximide filter cake;

[0029] Step 2. Mix the oximide obtained in Step 1 with water in a mass ratio of 1:3 and place it in the reactor. Under stirring, adjust the pH value to 7-8 with alkali. The alkali used in this example is 40% Liquid caustic soda completely dissolves the oximate;

[0030] Step 3. After stirring and heating to 35°C, add dimethyl sulfate dropwise. The molar ratio of the dropped dimethyl sulfate to oximate is 1.38:1; at the s...

Embodiment 2～6

[0035] A method for synthesizing cymoxanil by extracting oximate from cymoxanil mother liquor wastewater, the specific parameters in the operation process are shown in Table 1, and other operating steps and operating methods are the same as in Example 1.

[0036] Concrete parameters in the operation process among table 3 embodiment 2~6

[0037]

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Abstract

The invention provides a method for extracting oxime compounds from cymoxanil mother liquor wastewater to synthesize cymoxanil. The method comprises the following steps: stirring the cymoxanil mother liquor and adding acid to the cymoxanil mother liquor; regulating the pH value to 0.5-1.5, and after reacting for 10-15 minutes, carrying out sucking filtration to obtain an oxime compound filter cake; mixing the oxime compound filter cake with water, and regulating the pH value to 7-8 by caustic soda liquid in a stirring state so as to completely dissolve the oxime compounds; stirring and heating the dissolved oxime compounds to 30-35 DEG C, dropping dimethyl sulfate according to a molar ratio of 1.20-1.40 of the dimethyl sulfate to the oxime compounds; at the same time, dropping the causticsoda liquid so as to ensure that the pH value is kept to be 7-8 and the temperature is kept 33-38 DEG C and then continuing to stirring for 1-1.5 hours; standing still and cooling an obtained productto be below 25 DEG C, centrifuging and water washing the product and then drying the product to obtain the cymoxanil. The method has safe and convenient operation, solves the technical problem of extracting the oxime compounds from the cymoxanil mother liquor wastewater and directly synthesizing the cymoxanil by the oxime compounds and realizes the recovery and recycling of useful substances in the wastewater.

Description

technical field [0001] The invention relates to a synthesis method of cymoxanil, in particular to a method for synthesizing cymoxanil by extracting an oxime compound from cymoxanil mother liquor wastewater. Background technique [0002] During the synthesis of cymoxanil, a large amount of cymoxanil mother liquor wastewater will be produced. The synthesis process of cymoxanil is as follows: In the reaction kettle, add 1-cyanoacetyl-3-ethylurea, sodium nitrite, and methanol aqueous solution, stir and slowly raise the temperature to 30°C, add 30% hydrochloric acid dropwise, and control the reaction temperature Do not exceed 40°C, check the pH during the dropwise addition, keep the pH of the reaction solution at 5-6, continue to stir for 2 hours, and synthesize 1-cyanoacetyl-3-ethylurea oxime (abbreviated as "oximide"). Use 30% sodium hydroxide solution to adjust the pH to 7-8, and simultaneously add dimethyl sulfate dropwise. During the process of dropping lye and dimethyl sul...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C275/50C07C273/18
Inventor 孙敬权张荣全袁虎袁爱峰马凡敬
Owner 利民化学有限责任公司