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Preparation method of aquacide dichloride

A technology for diquat and chloride salts, applied in the field of preparation of diquat dichloride salts, can solve the problems of unobtainable raw materials, low product purity and high cost, and achieves overcoming high production costs, obvious economic benefits, and low production costs Effect

Inactive Publication Date: 2016-12-14
NANJING REDSUN BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (2) Patent US2823987 obtains diquat dichloride by adding freshly prepared AgCl to the aqueous solution of diquat dibromide, and obtains diquat dichloride through halogen ion exchange reaction; this method uses expensive silver chloride, and the cost is high, and the reaction Long time, not suitable for industrial production
The raw material of this method is not easy to obtain, and it is difficult to react thoroughly, and the product purity is low, so it is not suitable for industrialized production

Method used

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  • Preparation method of aquacide dichloride

Examples

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Effect test

Embodiment 1

[0023] In a 2000ml four-neck flask equipped with a mechanical stirrer, a thermometer and a distillation device, add 640g (1.86mol) diquat dibromide salt, add water to prepare a diquat dibromide salt solution with a mass concentration of 40%, and start stirring , raise the temperature to 80°C, adjust the chlorine gas feed rate, and maintain the reaction temperature at 85°C for the reaction. The bromine produced during the reaction is captured by the condensation device, and the tail gas is absorbed by adding lye. When the reaction temperature dropped to 80°C, the reaction was over, the chlorine flow was stopped, and the residual bromine and chlorine gas in the solution were purged with air, detected by KI-starch test paper, and 185 g (2.6 mol) of chlorine gas was consumed in total for the electronic scale metering reaction to obtain the product Diquat dichloride 470g (1.85mol), molar yield 99.5%, the captured crude bromine was dewatered and dried with phosphorus pentoxide to fin...

Embodiment 2

[0025] In a 2000ml four-neck flask equipped with a mechanical stirrer, a thermometer and a reflux device, add 640g (1.86mol) diquat dibromide salt, add water to prepare a diquat dibromide salt solution with a mass concentration of 40%, and start stirring , the temperature was raised to 45°C, and the chlorine gas feeding rate was adjusted to maintain the reaction temperature at 50°C. When the reaction temperature dropped to 45°C, the reaction was over, and the bromine was distilled and separated by heating. After the distillation is finished, the residual bromine and chlorine in the solution are flushed with nitrogen, and detected by KI-starch test paper. Electronic weighing reaction consumes 156.2g (2.2mol) of chlorine gas in total, and obtains 468.6g (1.84mol) of diquat dichloride, a molar yield of 99.1%, and the collected crude bromine is dried by removing water and phosphorus pentoxide , finally got bromine 286.8g, bromine yield 96.3%.

Embodiment 3

[0027] In a 2000ml four-necked flask equipped with a mechanical stirrer, a thermometer and a distillation device, add 320g (0.93mol) diquat dibromide salt, add water to prepare a diquat dibromide salt solution with a mass concentration of 20%, and start stirring , raise the temperature to 80°C, adjust the chlorine gas feed rate, and maintain the reaction temperature at 83°C for the reaction. The bromine produced during the reaction is captured by the condensation device, and the tail gas is absorbed by adding lye. When the reaction temperature dropped to 80°C, the reaction was over, the chlorine flow was stopped, and the residual bromine and chlorine in the solution were purged by air, and detected by KI-starch test paper. The metering reaction of the electronic scale consumes 79g (1.1mol) of chlorine gas in total, and 235.7g (0.928mol) of the product diquat dichloride is obtained, and the molar yield is 99.8%. Finally, 143.4 g of bromine was obtained, and the yield of bromine...

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Abstract

The invention discloses a preparation method of aquacide dichloride. Bromide ions are oxidized by taking an aquacide dibromo salt aqueous solution as a raw material and taking chlorine as an oxidant to generate bromine and aquacide dichloride, wherein bromine is recycled by distillation and condensation; residual bromine and chlorine are purged by introducing air, oxygen, water vapor or inert gas to obtain aquacide dichloride. According to preparation of the aquacide dichloride, the aquacide dichloride is obtained by taking the aquacide dibromo salt aqueous solution as the raw material and by oxidizing by cheap chlorine, so that the preparation method of aquacide dichloride has the advantages of low production cost, simple reaction and high product yield, and is suitable for industrialized production. More importantly, expensive bromine is obtained by replacement, and bromine is a chemical raw material applied widely, can serve as a product to be sold directly and can also be circularly used for preparation of aquacide dichloride, so that the problem that existing herbicide aquacide has high production cost is solved and significant economic benefit is achieved.

Description

technical field [0001] The invention belongs to the fields of chemical industry and pesticides, and in particular relates to a preparation method of diquat dichloride. Background technique [0002] Diquat is a kind of herbicide with excellent performance. It can also be used to dry the stems and leaves of potatoes and sweet potatoes. Diquat in the usual sense refers to diquat dibromide, which is composed of 2,2 '-Bipyridyl and dibromoethane ring closure reaction. As the third largest herbicide in the world after glyphosate and diquat, the market demand for diquat has increased rapidly in recent years. However, due to the high bromine content in the dibromide salt of diquat and the high price of bromine itself, the production cost of diquat is too high, which limits the wide application of diquat to a certain extent. [0003] The herbicidal effect of diquat dibromide is its cationic part, which has nothing to do with the anion bromine. Since the relative atomic mass of chl...

Claims

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Application Information

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IPC IPC(8): C07D471/14
CPCC07D471/14
Inventor 陈洪龙王文魁陈新春蒋剑华薛谊
Owner NANJING REDSUN BIOCHEM CO LTD
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