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Method for preparing 3,4-dimethylpyrazole and phosphate and metal organic complex thereof

A technology of dimethylpyrazole and phosphoric acid, applied in the direction of 2/12 group organic compounds without C-metal bonds, zinc organic compounds, organic chemistry, etc., can solve the problem of inability to continuous production, complicated operation steps and low production efficiency and other problems, to achieve significant industrial application value, improve reaction efficiency, and reduce raw material costs.

Inactive Publication Date: 2019-04-19
SINOCHEM AGRI LINYI R&D CENT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The 3-methyl-3-buten-2-one in this method is easy to polymerize, not easy to preserve, and the operation steps are complicated, requiring a large amount of equipment such as reactors, the most important thing is that continuous production cannot be performed, and the production efficiency is low
[0004] Thereby, existing preparation 3,4-dimethylpyrazole, DMPP and the means that DMPP is modified still need to be improved

Method used

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  • Method for preparing 3,4-dimethylpyrazole and phosphate and metal organic complex thereof
  • Method for preparing 3,4-dimethylpyrazole and phosphate and metal organic complex thereof
  • Method for preparing 3,4-dimethylpyrazole and phosphate and metal organic complex thereof

Examples

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Effect test

Embodiment 1

[0092] (1) Synthesis of methyl isopropyl ketone

[0093] After vaporizing and mixing water and isoprene separately, preheat to 180°C, enter H 3 PO 4 -B / diatomaceous earth catalyst bed for hydration reaction. The phosphoric acid content of the catalyst is 65wt%, the boron content is 6wt%, the reaction temperature is 250°C, the molar ratio of water and isoprene is 6.0, and the space velocity LHSV is 0.5h -1 , the reaction pressure is 0.1MPa. The reaction pressure was regulated by a pressure controller at the outlet of the reactor. The conversion rate of isoprene was 93.4%, the selectivity was 95.7%, the yield was 89.4%, and the purity of the product determined by gas chromatography was 99.7%.

[0094] (2) Synthesis of 3,4-dimethylpyrazole

[0095] Add 150kg (3kmole) of hydrazine hydrate with a mass fraction of 80% into the reactor, then add a small amount of water, start stirring, and slowly add 300kg (3kmole) of sulfuric acid with a concentration of 98% dropwise after the t...

Embodiment 2

[0098] Synthesis of 3,4-Dimethylpyrazole Phosphate (DMPP)

[0099] Dissolve 145kg of 3,4-dimethylpyrazole in 174kg of ethanol and react with 174kg of phosphoric acid with a mass fraction of 85%. The reaction temperature is 50°C and the reaction time is 8h. After the reaction is completed, the temperature is lowered, crystallized, and filtered , dried to obtain about 279.5kg of white powdery solid product, the yield was 95.4%, and the purity of the product as determined by high performance liquid chromatography was 99.3%.

Embodiment 3

[0101] Synthesis of 3,4-Dimethylpyrazole Complex with Zinc

[0102] After dissolving 96kg (1kmole) of 3,4-dimethylpyrazole in 200kg of chloroform, 100kg of absolute ethanol containing 34kg (250mole) of zinc chloride was added dropwise. Stir at room temperature for 8 hours, filter after the reaction is completed, wash the filter cake with methanol for 1 to 2 times, and obtain about 115kg of white powdery solid product after drying, with a yield of about 88%. The purity of the product determined by high performance liquid chromatography is 95.4%. The rate is 64% to 67.7%.

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Abstract

The invention discloses a method for preparing 3,4-dimethylpyrazole and phosphate and metal organic complex thereof. The method for preparing the 3,4-dimethylpyrazole comprises the steps that (1) isoprene is in contact with water under the action of a catalyst to obtain methyl isopropyl ketone; (2) the methyl isopropyl ketone is in contact with hydrazine hydrate under the action of sulfuric acid and iodide to obtain the 3,4-dimethylpyrazole. The method for preparing the 3,4-dimethylpyrazole has the advantages that the isoprene is taken as a raw material, the preparation method is simple, and the yield and purity of the product are high.

Description

technical field [0001] The invention relates to the technical field of fertilizer additives, in particular, the invention relates to a method for preparing 3,4-dimethylpyrazole and its phosphate and metal-organic complexes. Background technique [0002] 3,4-Dimethylpyrazole phosphate (DMPP) is an efficient, safe, non-toxic and cheap nitrogen fertilizer nitrification inhibitor developed by BASF. Adding nitrification inhibitor DMPP to fertilizer can control the conversion of ammonium nitrogen to nitrification In order to realize the stable supply of nitrogen, reduce the leaching of nitrate nitrogen and the emission of nitrogen oxides, so as to achieve the purpose of improving the utilization rate of chemical fertilizers, protecting the environment and promoting agricultural development. For example, Entec compound fertilizer can use the strengthening effect of plants to absorb ammonium nitrogen and nitrate nitrogen to obtain synergistic yield-increasing benefits. While reducin...

Claims

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Application Information

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IPC IPC(8): C07D231/12C07F3/06C05G3/08C05G3/90
CPCC07D231/12C07F3/003C05G3/90
Inventor 魏延青刘晓波张西兴秦跃军
Owner SINOCHEM AGRI LINYI R&D CENT CO LTD
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