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Glyphosate preparation and method for preparing same

A glyphosate and preparation technology, which is applied in the field of glyphosate preparations and its preparation, can solve the problem that glyphosate cannot be directly obtained from glyphosate preparations, and achieves reduction of equipment and personnel investment, reduction of waste water generation, and reduction of environmental protection. effect of stress

Active Publication Date: 2006-11-22
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In order to solve the problem that the preparation of glyphosate by oxidizing diglyphosate by catalytic oxidation method cannot directly obtain glyphosate preparations which can be directly applied in the prior art, the present invention provides a kind of method which can directly oxidize diglyphosate by catalytic oxidation method. Glyphosate preparation obtained by the prepared glyphosate and preparation method thereof

Method used

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  • Glyphosate preparation and method for preparing same
  • Glyphosate preparation and method for preparing same

Examples

Experimental program
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Effect test

Embodiment 1

[0036] Embodiment 1: the preparation of glyphosate preparation

[0037] step:

[0038] (a) Get 224g (content 24%) of the IDA reaction solution that catalytic dehydrogenation makes in the four-neck flask with stirring, add phosphorous acid 45g; Heat up, dropwise add 30% formaldehyde solution 50g and reflux for three hours.

[0039] (b) Add 110 g of water, 0.5 g of sodium tungstate, and 65 g of hydrogen peroxide (content 28%) to the diglyphosate obtained in step (a). Stir and heat up. Control the temperature within the range of 50°C to 90°C and keep it warm for 60 minutes; after the heat preservation is over, cool the temperature to 25°C to 55°C and keep it warm for 40 minutes. After the heat preservation was completed, 11 g of 10% ferrous sulfate aqueous solution was added dropwise when it was cooled to below 30° C. After the dropwise addition, 100 g of dehydration under reduced pressure was carried out, and then 35 g of isopropylamine was added dropwise. After the dropwise ...

Embodiment 2

[0040] Embodiment 2: the preparation of glyphosate preparation:

[0041] step:

[0042] 60 g of water, 0.1 g of sodium tungstate, and 70 g of hydrogen peroxide (content 28%) were added to the reaction mixture obtained in step (a) of Example 1. Stir and heat up. Control the temperature within the range of 50°C to 90°C and keep it warm for 80 minutes; after the heat preservation is over, cool the temperature to 25°C to 55°C and keep it warm for 40 minutes. When cooling below 30°C after the heat preservation, 17g of 10% ferrous sulfate aqueous solution was added dropwise, and 55g of dehydration under reduced pressure was carried out after the dropwise addition, and then ammonia gas was passed into the reactor. Until the pH value of the mixed liquid in the reactor reaches the range of 5-7. Add 10 g of a mixture of alkyl glucoside and coconut oil betaine with a mass ratio of 1:1 and stir evenly. After sampling analysis, its active ingredient content is 30.8%.

Embodiment 3

[0043] Embodiment 3: the preparation of glyphosate preparation:

[0044] step:

[0045]110 g of water, 0.3 g of sodium tungstate, and 55 g of hydrogen peroxide (content 28%) were added to the reaction mixture obtained in step (a) of Example 1. Stir and heat up. Control the temperature within the range of 65°C to 90°C and keep it warm for 90 minutes; after the heat preservation is over, cool the temperature to 25°C to 55°C and keep it warm for 50 minutes. After the heat preservation was completed, 25 g of 10% ferrous sulfate aqueous solution was added dropwise when cooling below 30° C., and 95 g of dehydration under reduced pressure was carried out after the dropwise addition, and 40 g of isopropylamine was then added dropwise. After the dropwise addition, the pH value of the mixed solution in the reactor was about 5. Add tallow amine ethylate 20g and stir evenly. Through sampling analysis, its active ingredient content is 30.3%.

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Abstract

The invention provides a glyphosate preparation and a preparation method thereof. The glyphosate is a glyphosate mixed liquid obtained after oxidation of diglyphosate, after being dehydrated, an alkali is added to convert the glyphosate into a salt, and then Add a surfactant to the mixture of the obtained salt as an auxiliary agent, and the surfactant is a mixture of one or more of nonionic surfactants or amphoteric surfactants or silicone surfactants, and mix well Obtain the glyphosate preparation. In the glyphosate preparation process of the present invention, there is no need to separate the original glyphosate in advance, and the synthesized glyphosate original drug is directly prepared for glyphosate preparation, which greatly reduces the input of equipment and personnel in production; at the same time There is basically no discharge of glyphosate mother liquor, fully utilizing the synthesized glyphosate technical material, and also reducing the generation of waste water in the production process, greatly reducing the pressure on environmental protection.

Description

(1) Technical field [0001] The invention relates to a glyphosate preparation and a preparation method thereof. (2) Background technology [0002] It is well known that glyphosate salts are widely used as no-residue or low-residue broad-spectrum herbicides. [0003] Glyphosate is most commonly prepared by the oxidation of diglyphosate. can be passed through concentrated H 2 SO 4 Oxidation method (Israeli patent 41842), H 2 o 2 and concentrated H 2 SO 4 Oxidation method (Israeli patent 42393) and electrolytic oxidation method (US patent 3859183) oxidize diglyphosate to prepare glyphosate. Diglyphosate can also be oxidized with oxygen or an oxygen-containing gas in the presence of a catalyst (US Patent 3969398). Compared with the above methods, the advantage of the catalytic oxidation method is that it does not require expensive chemicals and special equipment, and it is easy to obtain pure glyphosate. [0004] Although glyphosate itself is a very effective phytotoxic ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38A01N57/10
Inventor 王伟任不凡周曙光邵振威王萍秦龙李丽娟马梅红
Owner ZHEJIANG XINAN CHEM INDAL GROUP