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Preparation method of chloramine phos

A technology of chloramidophos and chloral, which is applied in botany equipment and methods, chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, etc., can solve the problem of increasing production costs and not allowing methamidophos , highly toxic and other issues, to achieve the effects of reduced production costs, increased content, and reduced amounts of impurities and waste disposal

Inactive Publication Date: 2006-01-11
JIANGXI HEYI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The preparation method of chloramidophos invented by ZL97112828.6 patent is determined to use methamidophos as an intermediate or raw material to prepare chloramidophos. Methamidophos is an insecticidal compound with a production history of 30 years. This method is used to prepare chloramidophos There are two main defects: 1. Methamidophos is a highly toxic insecticide. After 2007, China will completely ban the application of methamidophos as an insecticide, and will not allow the derivatives of methamidophos to be used as insecticides. When the insecticide is used, the residual content of methamidophos exceeds the strict standard. According to the production process formulated by the original preparation method, in order to reach this standard, it is necessary to increase the process steps, thereby increasing the production cost and increasing the cost of chloramidophos production. Pollutants
2. For decades, the raw material content of methamidophos products produced in China has been below 75%, and the raw drugs of methamidophos products contain a large amount of impurities. As countries around the world pay more and more attention to environmental protection, the The quality requirements of pesticide commodities are also getting higher and higher. To prepare chloramidophos with 75% methamidophos as raw material, in order to meet the requirement of content ≥ 90%, it is necessary to configure corresponding unit chemical processes such as separation and treatment, which not only increases production The cost increases the source of pollution

Method used

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  • Preparation method of chloramine phos
  • Preparation method of chloramine phos
  • Preparation method of chloramine phos

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0026] step one

[0027] Weight ratio: spermine A: chloral = 1: 1.13

[0028] Put 100g of 95% spermine A and 50ml of toluene into a 500ml reaction bottle at one time, start stirring, control the temperature below 30°C and not lower than 5°C, start to slowly add 97% trichloroacetaldehyde dropwise, and add trichloroacetaldehyde dropwise Acetaldehyde 113g, drop in about 1 hour, after dropping, start to keep warm at 29°C and analyze with liquid chromatography until the spermine content in the reaction solution is ≤0.5%, the reaction is the end point, and keep warm for about 5 hours , settled and crystallized at 5°C, a large amount of white solids were produced, filtered and dried, the obtained solid was intermediate C, the weight of the obtained solid was 116g, the melting point was 68°C, and the content was ≥98%. The mother liquor is used as a toluene solvent substitute for the next synthesis reaction, and the C intermediate produced by using the mother liquor has a yield of 187...

example 2

[0033] step one

[0034] Weight ratio: 98% spermine: Chloral = 1:3

[0035] Put 300g of 98% chloral into a 500ml reaction bottle at one time, start stirring, control the temperature below 30°C, not lower than 5°C, start to slowly add 95% spermine dropwise, a total of 100g, after dripping, at 40°C Heat preservation reaction for 3 hours, then raise the temperature to 60°C, continue heat preservation reaction for 2 hours, which is the end point of the reaction, then evaporate excess chloral under high vacuum, cool down to normal temperature, add 100g of n-hexane, stir evenly, measure Among them, the C intermediate content is about 60%.

[0036] step two

[0037] Weight ratio: C: dimethyl carbonate = 1: 0.2

[0038] Put 20g of dimethyl carbonate and 100g of petroleum ether into a 500ml reaction bottle at one time, control the temperature at 40-50°C, and slowly add the C-n-hexane solution generated in the above step 1 dropwise. As the end point of the reaction, crystallize at a...

example 3

[0040] step one

[0041] Weight ratio: spermine: chloral = 1: 2.5

[0042] Put 250g of 98% chloral into a 500ml reaction bottle at one time, start stirring, control the temperature at about 38°C, slowly add 98% spermine dropwise, a total of 100g, after dropping, continue to stir and react at about 15°C for 32 hours, A large amount of solids precipitated, and then the temperature was lowered by 5°C, crystallized, filtered, and dried to obtain intermediate C, with a solid weight of 189 g and a content of 98%. The filtered mother liquor can be recycled.

[0043] Step 2: Same as Step 2 in Example 1 above.

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Abstract

A process for preparing thiophosphamide from O, O-dimethyl thiophosphamide and trichloroacetaldehyde through preparing the intermediate C, exchanging the sites of O and S in the intermediate by use of dimethyl sulfate (or carbonate), and preparing O, S-dimethyl (2, 2, 2-trichloro-1-hydroxy-ethyl) thio phosphamide. Its advantages are low cost and high purity.

Description

technical field [0001] The present invention relates to a preparation method of chloramidophos, in particular to a method for preparing chloramidophos by changing the original production method of chloramidophos with methamidophos as an intermediate or raw material and synthesizing a new intermediate compound Methods. Background technique [0002] Chloramidophos is an innovative insecticidal compound and a new derivative of methamidophos. It has obtained the patent authorization from the State Intellectual Property Office of the People's Republic of China in 2000. The patent number: ZL97112828.6, the main classification of international patents No.: ADIN57 / 28. And in 2005, it has obtained the registration license from the Ministry of Agriculture of China, and will soon enter the stage of large-scale industrialization and commercialization. [0003] The chemical name of chloramidophos: O, S--dimethyl (2,2,2-trichloro-1-hydroxy-ethyl) thiophosphoramid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/22A01N57/28
Inventor 李坚巨修练陈呈新
Owner JIANGXI HEYI CHEM
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