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Preparation method of silica gel immobilized quaternary phosphonium salt

A technology of quaternary phosphonium salt and silica gel, which is applied in the field of preparation of insoluble quaternary phosphonium salt and silica gel-loaded quaternary phosphonium salt, which can solve the problems of residual toxicity and difficult separation, and achieve the effect of easy separation and wide sources

Inactive Publication Date: 2018-04-17
浙江肯特催化材料科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its purpose is to overcome the defects of the prior art, solve the problem of difficult separation and residual toxicity of water-soluble quaternary phosphonium salt after sterilization, and prepare an insoluble quaternary phosphonium salt with good thermal stability and high mechanical strength

Method used

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  • Preparation method of silica gel immobilized quaternary phosphonium salt
  • Preparation method of silica gel immobilized quaternary phosphonium salt
  • Preparation method of silica gel immobilized quaternary phosphonium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of preparation method of silica gel immobilized quaternary phosphonium salt comprises the following two steps:

[0025] (1) Preparation of quaternary phosphonium salt type silane

[0026] Add 24.08g (0.1mol) of γ-chloropropyltriethoxysilane and 26.23g (0.1mol) of triphenylphosphine into 100ml of benzyl alcohol, mix well, and react under reflux at 125°C for 24h under nitrogen protection. At the end of the reaction, diethyl ether was added to precipitate a precipitate, which was collected by filtration, recrystallized from ethanol, and then dried in vacuum, and the product was quaternary phosphonium salt type silane.

[0027] (2) Preparation of silica gel immobilized quaternary phosphonium salt

[0028] Weigh 10g of 100-200 mesh column chromatography silica gel, place it in 60mL of methanesulfonic acid aqueous solution with a concentration of 5mg / ml, stir and activate it at about 102°C for 4h, filter, wash with distilled water to make it neutral, and put it at 100...

Embodiment 2

[0031] (1) Preparation of quaternary phosphonium salt type silane

[0032] Add 24.08g (0.1mol) of γ-chloropropyltriethoxysilane and 20.23g (0.1mol) of tributylphosphine into 100ml of N,N-dimethylamide and mix well. ℃ reflux reaction for 10h. At the end of the reaction, diethyl ether was added to precipitate a precipitate, which was collected by filtration, recrystallized from ethanol, and then vacuum-dried at 60°C, and the product was quaternary phosphonium salt-type silane.

[0033] (2) Preparation of silica gel immobilized quaternary phosphonium salt

[0034] Weigh 10g of 100-200 mesh column chromatography silica gel, put it in 60ml of methanesulfonic acid aqueous solution with a concentration of 5mg / ml, stir and activate it at about 102°C for 4h, filter, wash with distilled water to make it neutral, and put it at 100°C after suction filtration The following vacuum drying.

[0035] Mix 1g of activated column chromatography silica gel with 3g of the prepared quaternary pho...

Embodiment 3

[0037] The used silica gel immobilized quaternary phosphonium salt in Example 1 was filtered and separated from the system, washed with deionized water, and a mixed solution of concentrated salt and ethanol was added (V (concentrated hydrochloric acid): V (ethanol) = 1:8), Soak for 4 hours, filter, wash with deionized water until neutral, and filter to obtain a regenerated and activated quaternary phosphonium salt supported on silica gel.

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Abstract

The invention provides a preparation method of a silica gel immobilized quaternary phosphonium salt. A silica gel type inorganic material is taken as a carrier, and the surface of the carrier is grafted with a quaternary phosphonium salt type sterilization group so as to synthesize a water-insoluble quaternary phosphonium salt. The quaternary phosphonium salt has good sterilization performance, isinsoluble in water, is easy to separate after sterilization, does not have residual poisons, and can be reused after being treated by hydrochloric acid. Furthermore, because an inorganic material such as silica gel is taken as a microcarrier, the defect that an organic polymer serving as the carrier is easily affected can be overcome; the prepared quaternary phosphonium salt has the advantages ofrigid structure, wide carrier source, low cost and better thermal stability; and the prepared quaternary phosphonium salt can be widely applied to sterilization and disinfection of fluid mediums suchas various industrial and civil water as well as preparation of antibacterial materials.

Description

technical field [0001] The invention relates to a preparation method of a silica gel-loaded quaternary phosphonium salt, which belongs to the field of fungicides, in particular to an insoluble quaternary phosphonium salt. Background technique [0002] Quaternary phosphonium salt is a new type of cationic fungicide. Since phosphorus is a third-period element, it has a large ionic radius, strong polarization, and strong electropositivity, so quaternary phosphonium salt has good antibacterial properties, broad-spectrum, low toxicity, and stability. It has been widely used as a bactericide and algicide in industrial circulating water systems, a fungicide for oilfield water injection and an agricultural pesticide. Because of its low foam, strong slime stripping ability and wide pH range, it is used as a substitute for traditional quaternary ammonium fungicides in industrial circulating water and oilfield water injection systems. [0003] Water-soluble quaternary phosphonium salt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A01N25/08A01N57/22A01N57/20A01P1/00A01P3/00
CPCA01N25/08A01N57/20A01N57/22
Inventor 杨建锋洪钟强华超君杨龙张志明徐凯嘉徐青华兰欣蕾陈剑武金珍珍
Owner 浙江肯特催化材料科技有限公司
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