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Polysiloxane with side chain containing vinyl and quaternary ammonium salt, synthesis method of polysiloxane and application thereof in preparation of antibacterial silicone rubber

A technology of polysiloxane and quaternary ammonium salt, applied in the field of organic silicon polymer materials, can solve the problems of difficulty in preparing high molecular weight polysiloxane containing quaternary ammonium salt, low product yield, difficult industrialization, etc., and achieve high yield High, long-lasting antibacterial performance, molecular weight controllable effect

Inactive Publication Date: 2019-06-18
SHANDONG JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Many of the above methods are to synthesize polysiloxane first, and then introduce quaternary ammonium salt groups on the polysiloxane chain, which has low product yield and difficult operation, especially for the preparation of high molecular weight polysiloxane containing quaternary ammonium salt. Alkanes are particularly difficult and difficult to industrialize

Method used

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  • Polysiloxane with side chain containing vinyl and quaternary ammonium salt, synthesis method of polysiloxane and application thereof in preparation of antibacterial silicone rubber
  • Polysiloxane with side chain containing vinyl and quaternary ammonium salt, synthesis method of polysiloxane and application thereof in preparation of antibacterial silicone rubber
  • Polysiloxane with side chain containing vinyl and quaternary ammonium salt, synthesis method of polysiloxane and application thereof in preparation of antibacterial silicone rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] In a single-necked flask equipped with a spherical condenser and a magnet, add 4.22g of chloropropylmethyldiethoxysilane, 3.15g of N,N-dimethyl n-octylamine and 6ml of ethanol in sequence, and stir to make them evenly mixed. Nitrogen protection, reflux at 80°C, react for 48 hours, after the reaction, distill off the low boilers under reduced pressure to obtain a yellow transparent oily liquid, wash the product with petroleum ether three times, and dry it in vacuum for 24 hours, which is methyldiethoxysilane quaternary Ammonium salt monomer (i), yield 97%.

[0039] In a three-necked flask equipped with a spherical condenser, thermometer, and stirrer, add 2.00g of methyldiethoxysilane quaternary ammonium salt monomer (i), 0.48g of vinylmethyldiethoxysilane, 20.10g Hydroxy-terminated polydimethylsiloxane, 0.08g octamethyltrisiloxane and 0.23g tetramethylammonium hydroxide silicon alkoxide, stir to mix evenly, nitrogen protection, slowly raise the temperature to 70°C and keep...

Embodiment 2

[0041] In a single-necked flask equipped with a spherical condenser and a magnet, add 3.09g of chloromethylmethyldimethoxysilane, 3.15g of N,N-dimethyl n-octylamine and 6ml of ethanol in sequence, and stir to make them evenly mixed. Nitrogen protection, reflux at 80°C, and react for 48 hours. After the reaction, remove the low boilers by distillation under reduced pressure to obtain a yellow transparent oily liquid, wash the product with petroleum ether three times, and dry it in vacuum for 24 hours, which is methyldimethoxysilane quaternary Ammonium salt monomer (ii), yield 99%.

[0042] In a three-necked flask equipped with a spherical condenser, thermometer, and stirrer, add 3.00g of methyldimethoxysilane quaternary ammonium salt monomer (ii), 0.32g of vinylmethyldimethoxysilane, 25.12g Hydroxyl-terminated polydimethylsiloxane, 0.13g octamethyltrisiloxane and 0.28g tetramethylammonium hydroxide silicon alkoxide, stir to mix evenly, nitrogen protection, slowly raise the temp...

Embodiment 3

[0044] As described in Example 1, the difference is that the N,N-dimethyl n-octylamine used in the quaternization reaction was changed to imidazole.

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Abstract

The invention discloses a polysiloxane with a side chain containing vinyl and quaternary ammonium salt and a synthesis method of the polysiloxane. The polysiloxane with the side chain containing the vinyl and the quaternary ammonium salt is prepared by carrying out quaternization reaction on a halohydrocarbylalkoxysilane monomer and a tertiary amine compound to obtain a quaternary ammonium salt-containing alkoxysilane monomer; and then carrying out equilibrium polymerization on the quaternary ammonium salt-containing alkoxysilane monomer, vinyl alkoxysilane monomer and hydroxyl-terminated polydimethylsiloxane. The invention also discloses application of the polysiloxane with the side chain containing the vinyl and the quaternary ammonium salt as raw rubber to prepare antibacterial siliconerubber through hydrosilylation reaction, quaternary ammonium salt antibacterial group is introduced into the molecular structure of the raw rubber of the silicone rubber, so that an antibacterial agent is uniformly distributed in a matrix, and the obtained silicone rubber is durable in antibacterial property and high in safety. A new field is developed for the application of the organosilicon polymer quaternary ammonium salt, and a brand-new idea is provided for a new preparation technology of antibacterial materials.

Description

technical field [0001] The present invention relates to a kind of polysiloxane and its synthesis and the preparation method of antibacterial silicone rubber, especially relate to a kind of quaternary ammonium salt-containing polysiloxane and its synthesis method and its application in the preparation of antibacterial silicone rubber, that is, the side chain contains The invention relates to the synthesis of vinyl and quaternary ammonium polysiloxane and the method for preparing antibacterial silicone rubber by hydrosilylation addition, belonging to the field of organosilicon polymer materials. Background technique [0002] Silicone rubber has excellent aging resistance, heat resistance, cold resistance, good elasticity, special surface properties, good biological inertia and chemical stability, etc. It is an ideal antibacterial polymer material and is widely used in vitro Medical supplies and long-term implanted repair and replacement materials, such as machine tool equipmen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/44C08G77/08C08L83/10C08L83/05C08K3/36
Inventor 董福营唐新德王勤马丽霞李帅杰刘阳匡芮郝家文
Owner SHANDONG JIAOTONG UNIV
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