Water-insoluble phosphonium salt bactericidal agent and its preparation method

A water-insoluble, quaternary phosphonium salt technology, applied in the field of preparation of water-insoluble quaternary phosphonium salt fungicides, water-insoluble quaternary phosphonium salt fungicides, to achieve the effect of extensive sources and excellent fungicidal activity

Inactive Publication Date: 2008-11-19
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, it has excellent bactericidal activity, not only has the long-acting, high-efficiency, fast, and broad-spectrum bactericidal effects of quaternary phosphonium salt-type bactericidal polymers based on resins, but also overcomes the susceptibil

Method used

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  • Water-insoluble phosphonium salt bactericidal agent and its preparation method
  • Water-insoluble phosphonium salt bactericidal agent and its preparation method
  • Water-insoluble phosphonium salt bactericidal agent and its preparation method

Examples

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Example Embodiment

[0046] Example 1

[0047] Mix 21g (0.08mol) of triphenylphosphine, 20.2g (0.1mol) of 1,3-dibromopropane, add 100ml of xylene as the solvent, stir and heat to reflux at 100°C for 16h, the reaction is carried out under the protection of nitrogen, cooling, It is filtered, washed with 50ml of ether, and dried under vacuum below 100°C to obtain the crude product of 3-bromopropyltriphenyl quaternary phosphonium salt. The reaction yield is about 90%. The reaction product was purified by ethanol recrystallization and dried in vacuum at 100°C. The structural formula is Br(CH 2 ) 3 P + Ph 3 ·Br - .

Example Embodiment

[0048] Example 2

[0049] Add about 15ml KH550 (γ-aminopropyltriethoxysilane), Na 2 CO 3 About 2.3g, 40ml of absolute ethanol. The 3-bromopropyltriphenyl quaternary phosphonium salt Br(CH 2 ) 3 P + Ph 3 ·Br - 10g was pre-dissolved in hot ethanol solution, added dropwise under stirring and refluxing, dripping for about 6h, then refluxing and stirring for 4h, after the reaction was completed, the inorganic salt was filtered off while hot, the solvent was removed by rotary distillation, and a large amount of ether was added to the residue , A white solid separated out, filtered to obtain a crude white solid. Product with CH 2 Cl 2 Recrystallize and purify with ether, filter, wash twice with ether, and finally vacuum dry to obtain quaternary phosphonium salt type amine propylated triethoxysilane, the structural formula is: (C 2 H 5 O) 3 Si(CH 2 ) 3 NH(CH 2 ) 3 P + Ph 3 ·Br - .

Example Embodiment

[0050] Example 3

[0051] Take about 20g of 30-100 mesh coarse-pored microsphere silica gel in 100ml of 5% methanesulfonic acid aqueous solution, stir and activate at 102℃ for 4h, filter, wash with distilled water to make neutral, and then filter at 100℃ below Vacuum drying.

[0052] Mix 1g of the activated coarse-pored microsphere silica gel with 2.58g of the quaternary phosphonium salt type amine propylated triethoxysilane prepared in Example 2. Use ethanol and water as solvents, stir and heat to reflux for 24 hours, and react under nitrogen protection. The product Extracted with ethanol for 6 hours and dried in vacuum below 60°C to obtain a water-insoluble amino-quaternary phosphonium salt type bactericide with silica gel as a carrier.

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Abstract

The invention relates to a water-insoluble quaternary ammonium salt bactericide and the preparation method thereof. The germicide is prepared by adopting silica gel inorganic material as a carrier and grafting amino-quaternary ammonium salt or quaternary ammonium-quaternary ammonium salt functional groups on the surface. The water-insoluble quaternary ammonium salt bactericide has excellent antibacterial activity, and has the advantages that the bactericide has a persistent effect of quaternary ammonium salt antibacterial polymer and also has a high-efficiency, quick and broad-spectrum antibacterial effect; the raw material is widely accessible; the cost is low; the synthetic process is simple. The bactericide is water-insoluble, and can be activated, regenerated and reutilized after the antibacterial rate is reduced, and is widely applicable to the sterilization of the fluid media such as various industrial and domestic waters, etc. and the preparation of antibacterial materials.

Description

technical field [0001] The invention relates to a bactericide, more precisely a water-insoluble quaternary phosphonium salt bactericide with silica gel inorganic materials as carriers. The invention also relates to a preparation method of the water-insoluble quaternary phosphonium salt fungicide. Background technique [0002] In order to overcome the shortcomings of water-soluble fungicides such as high toxicity, easy foaming, irritation, and residual toxicity after being discharged with sewage, people began to study water-insoluble fungicide polymers. [0003] US 6,261,538 synthesized a class of water-insoluble polyquaternary phosphonium salt fungicides, which were prepared by using resins capable of chloromethylation as carriers, immobilized amino-quaternary phosphonium salts, quaternary ammonium-quaternary phosphonium salts and other fungicidal active components. . The above-mentioned bactericide has rapid and efficient bactericidal activity, can be used repeatedly, and...

Claims

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Application Information

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IPC IPC(8): A01N57/18A01P1/00
Inventor 金栋吕效平王慧盈沈旋林陵
Owner NANJING UNIV OF TECH
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