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Preparation method of surface hydrophilic silicon rubber

A silicone rubber and hydrophilic technology, applied in the field of surface hydrophilic silicone rubber preparation, can solve the problems of poor oil resistance, solvent resistance, acid and alkali resistance, uneven surface grafted polymer layer, difficult vulcanization, etc.

Inactive Publication Date: 2014-01-08
CHANGZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the medical field, silicone rubber is widely used, but due to the limitations of silicone rubber itself, there are some disadvantages: such as low strength, poor oil resistance, solvent resistance, acid and alkali resistance, and difficult vulcanization
[0005] The current methods for modifying silicone rubber include: corona discharge treatment, plasma treatment, ozone-activated grafting, hydrosilylation method, radiation grafted polymer method, photochemically induced grafted polymer method, but through these methods in The polymer layer grafted on the surface is uneven. Xiao’s research group used polyacrylamide chemical modification initiated by free radicals, so that the hydrophilicity of the modified silicone rubber can be maintained for about 1 month, and the irreversible adsorption of enzymes is compared with The adsorption of the original silicone rubber is significantly reduced, but the hydrophilicity is not yet permanently maintained

Method used

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  • Preparation method of surface hydrophilic silicon rubber
  • Preparation method of surface hydrophilic silicon rubber
  • Preparation method of surface hydrophilic silicon rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Step (1) Add hydroxyl-terminated polydimethylsiloxane to a three-necked flask equipped with an electric stirrer, vacuum dehydrate at 80°C for 1 hour, add 7% methyl tributylketoxime silane, pass N 2 After stirring for 0.5h, add 0.1% dibutyltin dilaurate, pass N 2 Stir and react for 15 minutes, vacuum degassing, pour into a 2mm thick mold, and cure at room temperature for 7 days.

[0033] Step (2) Add the room temperature vulcanized silicone rubber prepared in step (1) into the reaction bottle, and add 50mL of 10% hydrochloric acid. Stir at room temperature for 4 h, and after the reaction, ultrasonically wash and dry under vacuum at 50°C.

[0034] Step (3) Add the surface-activated silicone rubber sheet in step (2) to a dry reaction bottle, add 30mL ethyl acetate, 1.3mL triethylamine and stir in an ice bath, add dropwise 1mL α-bromoisobutyryl A mixed solution of bromine and 10 mL of ethyl acetate was removed from the ice bath after 0.5 h of dripping. The reaction was c...

Embodiment 2

[0041] Step (1) Add hydroxyl-terminated polydimethylsiloxane to a three-necked flask equipped with an electric stirrer, vacuum dehydrate at 80°C for 3 hours, add 5% methyl tributylketoximosilane, pass N 2 After stirring for 0.5h, add 0.1% dibutyltin dilaurate, pass N 2 Stir and react for 20 minutes, vacuum degassing, pour into a mold with a thickness of 2 mm, and cure at room temperature for 10 days.

[0042] Step (2) Add the room temperature vulcanized silicone rubber prepared in step (1) into the reactor, and add 50mL of 10% hydrochloric acid. Stir at room temperature for 6 h, and after the reaction is completed, ultrasonically wash and dry under vacuum at 50°C.

[0043] Step (3) Add the surface-activated silicone rubber sheet in step (2) into a dry single-necked flask, add 30 mL of toluene, 1.3 mL of triethylamine and stir in an ice bath, add dropwise 1 mL of α-bromoisobutyryl bromide and 10mL of toluene mixed solution, after 0.5h drop, remove the ice bath. The reaction ...

Embodiment 3

[0046] Step (1) Add hydroxyl-terminated polydimethylsiloxane to a three-necked flask equipped with an electric stirrer, vacuum dehydrate at 100°C for 1 hour, add 7% methyl tributylketoximosilane, pass N 2 After stirring for 0.5h, add 0.05% dibutyltin dilaurate, pass N 2 Stir the reaction for 15 minutes, then vacuum degass it and inject it into a mold with a thickness of 2 mm, and cure it at room temperature for 7 days.

[0047] Step (2) The room temperature vulcanized silicone rubber prepared in step (1) was irradiated with ultraviolet light for 10 minutes to activate the surface of the silicone rubber.

[0048] Step (3) Add the surface-activated silicone rubber sheet in step (2) into a dry single-necked flask, add 30 mL of acetone, 1.3 mL of triethylamine and stir in an ice bath, dropwise add 1 mL of α-bromoisobutyryl bromide and 10mL of acetone mixed solution, after 0.5h drop, remove the ice bath. The reaction was carried out under magnetic stirring at room temperature for...

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Abstract

The invention relates to a preparation method of surface hydrophilic silicon rubber. The preparation method comprises the following steps of: (1) adding surface activated silicon rubber plates into a dry reaction bulb, adding a non-polar organic solvent and an acid-binding agent into the reaction bulb, stirring in an ice bath, dropping a mixed solution of an initiating agent and a non-polar solvent, then removing the ice bath, performing stirring reaction at the room temperature for 0.5 to 1 hour, performing ultrasonic washing after the reaction, and performing vacuum drying to obtain surface initiator-modified silicon rubber; and (2) adding the silicon rubber plates with a surface initiator, CuCl and 2,2'-bipyridyl into a vacuumized reaction bulb with nitrogen, then adding a hydrophilic monomer, adding an acetone and water mixed solvent, reacting for 4 to 24 hours at 40 to 60 DEG C, and performing ultrasonic washing and vacuum drying after the reaction to obtain silicon rubber of a surface grafting hydrophilic polymer. By the preparation method, the surface hydrophilic silicon rubber with uniform surface grafting and excellent hydrophilic performance can be prepared.

Description

technical field [0001] The invention belongs to the field of organosilicon materials, and relates to a method for preparing surface hydrophilic silicone rubber. Its main application fields include biomedicine, analysis and separation, and the like. technical background [0002] Due to its structure and other characteristics, silicone rubber has the advantages of high oxygen permeability, good mechanical properties, excellent heat resistance, electrical insulation, ozone resistance, weather resistance, chemical corrosion resistance, cold resistance, physiological inertia, etc. It is used more and more The more widely, among which it can be used in medicine as impression material, complete denture repair material, frame for repairing large area of ​​tracheal wall defect, injected silicone rubber facial filling prosthesis, nasal prosthesis, balloon silicone rubber lung prosthesis , Anti-noise earplugs, gastric tube, cochlear electrodes, implants, nickel-titanium memory alloy si...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/442
Inventor 姜彦史红岩蔡敏张洪文许胜张义
Owner CHANGZHOU UNIV
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