A kind of anti-hardening cotton wool preparation method

An anti-hardening, aqueous solution technology, applied in the direction of organic chemistry, can solve the problems of easy agglomeration, crystal structure, regulation density and safety impact, and does not give cotton length, etc., to achieve the effect of high fluidity

Active Publication Date: 2018-05-22
浙江大鹏药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is mainly to solve the impact of residual carbon disulfide on the crystal structure, density and safety of the product, but it does not give how to solve the problem of easy agglomeration of cotton long

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 1000g of carbon disulfide into the three-necked flask, and then add 100mL of potassium permanganate solution with a mass concentration of 2% dropwise. After the dropwise addition, continue to stir and wash for 50 minutes, then let it stand for 30 minutes, separate layers, remove the water phase, and collect the washed The final carbon disulfide solution was used for the next reaction.

[0022] Then, in another new clean there-necked flask, add 700g monomethylamine aqueous solution, wherein, the mass concentration of monomethylamine aqueous solution is 35% (equivalent to 245g methylamine (7.9mol)), control temperature at<30 ℃ , add 300g (3.9mol) of the above-mentioned carbon disulfide solution dropwise, after the dropwise addition, continue the heat preservation reaction for 2 hours, after the reaction is completed, let stand for 30 minutes, separate layers, and remove the excess carbon disulfide in the lower layer (can be applied to the next batch) , collecting the ...

Embodiment 2

[0025] Add 1000g of carbon disulfide into the there-necked flask, then add 100mL of sodium permanganate solution with a mass concentration of 3% dropwise, continue stirring and washing for 50min after the dropwise addition, then let stand for 30min, separate layers, remove the water phase, collect the washed The final carbon disulfide solution was used for the next reaction. Certainly, the mass concentration of the above-mentioned sodium permanganate solution can also be any percentage within 2%-5%.

[0026] Then, add 700g monomethylamine aqueous solution in another new clean there-necked bottle, wherein, the mass concentration of monomethylamine aqueous solution is 40% (equivalent to 280g methylamine 9.0mol), control temperature at 20 ℃-25 ℃ 380g (equivalent to 5.0mol) of the above-mentioned carbon disulfide solution was added dropwise. After the dropwise addition, the insulation reaction was continued for 2.5 hours. batch), the aqueous solution containing N-methyldithiocarb...

Embodiment 3

[0029] The pretreatment of carbon disulfide in this embodiment is consistent with that of Embodiment 1, and will not be repeated here.

[0030] Add 700g of monomethylamine aqueous solution into a clean three-necked bottle, wherein the mass concentration of monomethylamine aqueous solution is 40% (equivalent to 280g of methylamine), control the temperature at about 25°C, and dropwise add the above-mentioned pretreated carbon disulfide solution 410g , after the dropwise addition, continue the insulation reaction for 2.5 hours. After the reaction is over, let it stand for 30 minutes, separate layers, and separate the excess carbon disulfide in the lower layer (which can be applied to the next batch). The aqueous solution of formic acid is directly used in the next step reaction; the consumption ratio of carbon disulfide and methylamine here can be adjusted as required, generally making the consumption of carbon disulfide relatively excessive;

[0031] In another reactor, adding 7...

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Abstract

The invention relates to a method for preparing anti-hardening cotton wool, which belongs to the technical field of pesticide synthesis. In order to solve the existing problem of short storage time and easy agglomeration, a method for preparing cotton wool that is resistant to hardening is provided. The method includes adding a permanganate aqueous solution to the carbon disulfide solution for pretreatment, layering, and collecting the pretreated Carbon disulfide solution; react the pretreated carbon disulfide solution with concentrated methylamine aqueous solution to obtain an aqueous solution containing N-methyldithiocarbamic acid; in the presence of phosphate, amphoteric surfactant and EDTA, react with formaldehyde to obtain The amount of phosphate added is 1.0%-1.5% of the mass of formaldehyde, and the mass ratio of phosphate: amphoteric surfactant: EDTA is 1:0.5-0.6:0.01-0.02. The invention can increase the uniformity and distribution concentration of the particles and increase the compaction resistance of the cotton wool particles, so as to have the effect of high fluidity.

Description

technical field [0001] The invention relates to a method for preparing anti-hardening cotton wool, which belongs to the technical field of pesticide synthesis. Background technique [0002] Methron is a low-toxicity broad-spectrum fumigation nematicide, which can also control soil fungi, underground pests and weeds. When applied in a moist soil environment, it can decompose and spread to the soil particles, effectively killing various nematodes, pathogenic bacteria and weed seeds in the soil, so as to achieve a cleaning effect and have a long-lasting medicinal effect. It is also suitable for controlling various nematodes on vegetables, strawberries, etc. Usually, cotton wool is processed into dosage forms such as powder and wettable powder. [0003] At present, the domestic and foreign production methods for damaron mainly use carbon disulfide, monomethylamine and formaldehyde as the main raw materials, which are formed through a two-step reaction, specifically: first, rea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D285/34
Inventor 徐学春徐大国王辉杜青峰王自田
Owner 浙江大鹏药业股份有限公司
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