Oligomeric quaternary ammonium salt bactericide and preparation method thereof

A technology of polyquaternary ammonium salt and fungicide, which is applied in the field of preparation of oligomeric quaternary ammonium salt, can solve problems such as insoluble in water, and achieve the effects of improving binding ability, accelerating leakage, good water solubility and surface activity

Inactive Publication Date: 2017-09-15
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The Chinese patent with the publication number of 103191671A discloses a trimerized quaternary ammonium salt type cationic surfactant, which is simple to prepare, has good thermal stability, and has a wide range of applications, but because its linking group is a benzene ring, its molecular structure determines its characteristics. It is difficult to dissolve in water, so it is mainly used in industry as a metal corrosion inhibitor and emulsifier, but less as a fungicide

Method used

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  • Oligomeric quaternary ammonium salt bactericide and preparation method thereof
  • Oligomeric quaternary ammonium salt bactericide and preparation method thereof
  • Oligomeric quaternary ammonium salt bactericide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1) see image 3 , Add the weighed 0.02mol of dodecyldimethyl tertiary amine into a 100mL three-necked flask filled with 10mL of isopropanol, heat to 50°C, and then drop 4.0mL of 2.5mol / L hydrochloric acid solution into it , Stir at 450r / min until uniform. Gradually add 0.01mol of epichlorohydrin to the system dropwise within 30 minutes, and adopt a temperature program at the same time. After 12 hours, the heating was stopped to obtain a crude product. The crude product was evaporated under reduced pressure at 85°C and 0.09MPa to remove the solvent, then dissolved in acetone at 60°C, recrystallized at room temperature, filtered with suction, and redissolved. After repeating three times, dry to obtain hydroxypropyl gemini quaternary ammonium salt (marked as: 12-3(OH)-12); the yield is 87.9%.

[0032] 2) Weigh 0.025 mol of 12-3(OH)-12 and 0.0625 mol of p-toluenesulfonyl chloride (TsCl), add them into a three-necked flask filled with chloroform, stir evenly, and add mass ...

Embodiment 2

[0035] 1) with embodiment 1.

[0036] 2) with embodiment 1.

[0037]3) Weigh 0.008 mol of 12-3(TsO)-12, 0.008 mol of guanidine hydrochloride and 0.008 mol of sodium ethoxide into a mixture of 20 mL of DMF and 20 mL of ethanol, stir and gradually raise the temperature from room temperature to 160°C within 30 minutes, and react for 12 hours. Stop heating to obtain the crude product, adjust the pH to weak acidity, remove excess water and ethanol by rotary evaporation under reduced pressure at 90°C and 0.09MPa, remove the precipitate of guanidine hydrochloride by filtration, and continue to remove DMF by rotary evaporation at 140°C and 0.09MPa under reduced pressure and p-toluenesulfonic acid, then add acetone, freeze and recrystallize to obtain a white needle-like powder solid that is the oligomeric quaternary ammonium fungicide, and the yield is 42.19%.

Embodiment 3

[0039] 1) with embodiment 1.

[0040] 2) with embodiment 1.

[0041] 3) Weigh 0.024 mol of 12-3(TsO)-12, 0.008 mol of guanidine hydrochloride and 0.008 mol of sodium ethoxide into a mixture of 100 mL of DMF and 20 mL of ethanol, stir and gradually raise the temperature from room temperature to 140°C within 30 minutes, and stop after 12 hours of reaction. Heating to obtain crude product, adjust the pH value to weak acidity (pH value is 5 ~ 6), at 90 ° C, 0.09 MPa under reduced pressure rotary evaporation to remove excess water and ethanol, filter to remove the guanidine hydrochloride precipitate, and continue at 140 ° C and DMF and p-toluenesulfonic acid were removed by rotary steaming at 0.09MPa under reduced pressure, then acetone was added, and then frozen and recrystallized to obtain a white needle-like powder solid which was the oligomeric quaternary ammonium fungicide with a yield of 73.72%.

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Abstract

The invention relates to an oligomeric quaternary ammonium salt bactericide and a preparation method thereof. Ester p-toluenesulfonate-based gemini quaternary ammonium salt, guanidine hydrochloride and sodium alkoxide are added into solvent, stirred and heated to 120 DEG C to 180 DEG C, heating is stopped after 10 to 48 hours of reaction, so that a crude product is obtained, and after post-treatment, the oligomeric quaternary ammonium salt bactericide is obtained; and the substance amount ratio of the ester p-toluenesulfonate-based gemini quaternary ammonium salt, the guanidine hydrochloride and the sodium alkoxide is (0.008 to 0.040):0.008:0.008. The gemini quaternary ammonium salt is introduced to a plurality of active sites, eight active sites are contained in the structure of the oligomeric quaternary ammonium salt bactericide, the oligomeric quaternary ammonium salt bactericide can show good water solubility and surface activity in aqueous solution, and an important role is played in the process of oligomeric quaternary ammonium salt preparation. A bacteria killing test on three types of bacteria, i.e. sulfate reducing bacteria, iron bacteria and saprophytic bacteria, indicates that the oligomeric quaternary ammonium salt bactericide has a good bactericidal effect.

Description

technical field [0001] The invention relates to a preparation method of oligomeric quaternary ammonium salt, in particular to a bactericide of oligomeric quaternary ammonium salt and a preparation method thereof. Background technique [0002] Quaternary ammonium salt surfactants, as an important kind of surfactants, have been extensively studied and applied. It plays an insoluble role in sterilization, road construction, papermaking, textile, paint, metal corrosion, leather, etc. [0003] However, the current research on it mainly stays on single active center surfactants and gemini surfactants, while the research on oligomers such as trimers and tetramers is less. In the same molecular structure, multiple active centers are connected together through the linking group, which effectively inhibits the repulsion between the polar head groups of the surfactant, and the aggregation of lipophilic groups also promotes the increase of molecular distortion. The repulsion between t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A01N47/44A01P1/00C07C279/12C07C277/08
CPCA01N47/44C07C213/04C07C277/08C07C279/12C07C303/28C07C309/30C07C215/18
Inventor 郭睿李欢乐甄建斌李晓芳王超程敏杨江月刘爱玉
Owner SHAANXI UNIV OF SCI & TECH
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