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Preparation method of multi-quaternary ammonium salt fungicide
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A multi-quaternary ammonium salt and fungicide technology, which is applied in the field of preparation of multi-quaternary ammonium salt fungicides, can solve problems such as complex preparation methods, and achieve the effects of simple preparation methods, wide sources of raw materials, and low prices
Inactive Publication Date: 2016-08-31
大连和田科技有限公司
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Problems solved by technology
At the same time, the preparation of polymerized quaternary ammonium salt needs to introduce a polymerization process, and its preparation method is relatively complicated.
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Embodiment 1
[0017] Halogenation of polyols: Mix 1 mole of glycerin and 3.2 moles of thionylchloride with an equal volume of toluene at room temperature, stir for 0.5 hours, heat up to toluenereflux temperature and stir for 4 hours, cool to room temperature, and oxidize with hydrogen Washing with sodium solution and liquid separation three times, recovering the organic layer, drying and distilling off toluene to obtain polyhalogenated alkanes;
[0018] Synthesis of polyquaternary ammonium salts: Mix N,N-dimethylbutylamine and ethanol in equal volumes, after N,N-dimethylbutylamine is completely dissolved, add polyhalogenated alkanes three times, heat to ethanolreflux temperature, and Under the condition of ethanolreflux, react for 6 hours, remove the reflux condensing device, distill the ethanol away, and obtain the polyquaternary ammonium salt fungicide.
Embodiment 2
[0020] Halogenation of polyols: Mix 1 mole of trimethylolpropane and 3.5 moles of hydrogenbromide with an equal volume of n-heptane at room temperature, stir for 0.5 hours, raise the temperature to the reflux temperature of n-heptane and stir for another 3 hours, Cool to room temperature, wash with potassiumhydroxide solution, separate liquid three times, recover the organic layer, dry and distill off n-heptane to obtain polyhalogenated alkanes;
[0021] Synthesis of polyquaternary ammonium salts: Mix N,N-dimethylpentylamine and ethanol in equal volumes. After N,N-dimethylbutylamine is completely dissolved, add polyhalogenated alkanes three times, heat to ethanol reflux temperature, and Under the condition of ethanol reflux, react for 3 hours, remove the reflux condensing device, and distill the ethanol away to obtain the polyquaternary ammonium salt fungicide.
Embodiment 3
[0023] Halogenation of polyols: Mix 1 mole of trimethylolpropane and 3.1 moles of hydrogenbromide with an equal volume of n-octane at room temperature, stir for 0.7 hours, raise the temperature to n-octane reflux temperature and stir for 3.5 hours, Cool to room temperature, wash with sodiumcarbonate solution, separate liquid three times, recover the organic layer, dry and distill off n-octane to obtain polyhalogenated alkanes;
[0024] Synthesis of polyquaternary ammonium salts: Mix N,N-dimethylhexylamine and ethanol in equal volumes. After N,N-dimethylbutylamine is completely dissolved, add polyhalogenated alkanes three times, heat to ethanol reflux temperature, and Under the condition of ethanol reflux, react for 4 hours, remove the reflux condensing device, and distill the ethanol away to obtain the polyquaternary ammonium salt fungicide.
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Abstract
The invention relates to a preparation method of a multi-quaternaryammonium salt fungicide. The preparation method comprises the following steps: halogenating polylol: mixing the polylol and a halogenating reagent in a solvent 1 at room temperature; after stirring for 0.5-1 hour, heating to a reflowing temperature of the solvent 1 and stirring for 3-4 hours; cooling to room temperature; washing with an alkali solution and separating the solution for three times; recycling an organic layer; drying and distilling to remove the solvent 1, so as to obtain polybasic haloalkane; synthesizing multi-quaternaryammonium salt: mixing tertiary amine and a solvent 2; after the tertiary amine is completely dissolved, adding the polybasic haloalkane by three times; heating to the reflowing temprature of the solvent 2 and reacting for 3-6 hours under the condition that the solvent 2 reflows; and removing a reflowing condensation device and distilling to remove the solvent 2 so as to obtain the multi-quaternaryammonium salt fungicide. The preparation method of the multi-quaternary ammonium salt fungicide has the advantages that the types of the quaternary ammonium salt fungicide are expanded so that the prepared product has good sterilization effect and a similar complicated synthesis process of polymerized quaternary ammonium salt is also avoided.
Description
technical field [0001] The invention relates to a bactericide, in particular to a preparation method of a polyquaternary ammonium salt bactericide. Background technique [0002] Quaternaryammonium compounds are a kind of fungicides with high antibacterial activity and good application effect. As early as the beginning of last century, there were related reports on the sterilization of quaternary ammonium salts. Its bactericidal effect is derived from the negative charge interaction between the nitrogen cation of the quaternary ammonium group in the molecule and the acidic phospholipid in the biological cell membrane. Once the two are combined, the hydrophobic tail group of the quaternary ammonium salt will be embedded in the interior of the bacterial hydrophobic membrane. Effectively penetrates the membrane surface of bacteria. When the quaternary ammonium salt concentration is high, the quaternary ammonium salt will destroy the structure of the bacterial cell membrane. ...
Claims
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