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A kind of UV-curable low-oxygen polymerization-inhibiting nano-hybrid filler and preparation method thereof

A technology of ultraviolet light and oxygen inhibition, used in epoxy resin coatings, coatings, etc., can solve the problems of less addition, poor particle dispersion, slow curing speed, etc., to achieve easy control, improve dispersion, and alleviate oxygen resistance. poly effect

Inactive Publication Date: 2017-12-26
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] All in all, nano-SiO used in the existing UV technology field 2 The modification of fillers is mainly the surface treatment of silane coupling agent and the loading of photoinitiator, which has certain effects on improving the performance of UV coatings, but there are still defects such as small amount of addition, slow curing speed, and poor particle dispersion.

Method used

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  • A kind of UV-curable low-oxygen polymerization-inhibiting nano-hybrid filler and preparation method thereof
  • A kind of UV-curable low-oxygen polymerization-inhibiting nano-hybrid filler and preparation method thereof
  • A kind of UV-curable low-oxygen polymerization-inhibiting nano-hybrid filler and preparation method thereof

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Effect test

Embodiment 1

[0033] The preparation method of the UV-curable low-oxygen polymerization-inhibiting nano-hybrid filler provided in this embodiment includes the following steps:

[0034] In a four-necked flask equipped with a stirrer, a thermometer, a constant pressure funnel, and a reflux condenser, 10 parts (unit mol, amount of substance) of γ-aminopropyltriethoxysilane were added under nitrogen protection, and then 20 Parts (unit mol, amount of substance) of glycidyl acrylate are added dropwise to the flask, and the rate of addition is controlled to keep the temperature in the bottle basically constant. Until the N-H peak of the target product of the first step disappears on the infrared spectrum, the target product of the first step is generated and sealed and stored.

[0035] In a four-neck flask equipped with a stirrer, a thermometer, a constant pressure funnel, and a reflux condenser, the first step target product is charged under nitrogen protection, and 20 parts (unit mol, amount of ...

Embodiment 2

[0040] The preparation method of the UV-curable low-oxygen polymerization-inhibiting nano-hybrid filler provided in this embodiment includes the following steps:

[0041] In a four-necked flask equipped with a stirrer, a thermometer, a constant pressure funnel, and a reflux condenser, add 10 parts (unit mol, amount of substance) of aminoethylaminoethylaminopropyltriethoxysilane under nitrogen protection , then add 10 parts (unit mol, amount of substance) glycidyl acrylate dropwise into the flask, control the drop rate to keep the temperature in the bottle basically constant, after the dropwise addition, raise it to about 70°C (water bath), stir React until the N-H peak of the target product of the first step disappears on the infrared spectrum, and the target product of the first step is generated and sealed and stored.

[0042] In a four-necked flask equipped with a stirrer, a thermometer, a constant pressure funnel, and a reflux condenser, the first step target product is ch...

Embodiment 3

[0047] The preparation method of the UV-curable low-oxygen polymerization-inhibiting nano-hybrid filler provided in this embodiment includes the following steps:

[0048] In a four-necked flask equipped with a stirrer, a thermometer, a constant pressure funnel, and a reflux condenser, add 10 parts (unit mol, amount of substance) N-β-aminoethyl-γ-aminopropyl trimethyl Oxysilane, and then drop 30 parts (unit mol, amount of substance) glycidyl methacrylate into the flask, control the dropping speed to keep the temperature in the bottle basically constant, after the dropping is completed, it rises to about 40°C (water bath), stir the reaction until the N-H peak of the target product in the first step disappears on the infrared spectrum, and generate the target product of the first step for sealed preservation.

[0049] In a four-necked flask equipped with a stirrer, a thermometer, a constant pressure funnel, and a reflux condenser, the first step target product is charged under ni...

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Abstract

The invention discloses a preparation method of UV (ultraviolet)-curable low-oxygen-polymerization-inhibition nano hybrid filler. The method comprises steps as follows: an aminosilane coupling agent and multifunctional acrylic glycidol are taken, the temperature is adjusted to range from 40 DEG C to 70 DEG C for a reaction, a first-step target product is obtained, multifunctional isocyanate, a polymerization inhibitor and a catalyst are added to the first-step target product, the temperature is adjusted to range from 50 DEG C to 80 DEG C for a continuous reaction, a second-step target product is obtained, a polymerization inhibitor, a catalyst and a photoinitiator are added to the second-step target product, the temperature is adjusted to range from 80 DEG C to 100 DEG C for a continuous reaction, a third-step target product is obtained, a mixed solvent containing functional silane is added to the third-step target product, the temperature is adjusted to range from 25 DEG C to 60 DEG C for hydrolysis under the slightly alkaline condition and under the ultrasonic effect, a product after hydrolysis is dried, and the UV-curable low-oxygen-polymerization-inhibition nano hybrid filler is obtained. The method adopts the simple technology and is easy to control, and the prepared product can relieve oxygen polymerization inhibition and increase the UV-curing speed.

Description

technical field [0001] The invention belongs to the technical field of ultraviolet-curable nano-hybrid fillers, and in particular relates to an ultraviolet-curable low-oxygen polymerization-inhibiting nano-hybrid filler and a preparation method thereof. Background technique [0002] Nano-silica is an inorganic filler with wide sources and low cost, which is widely used in nanocomposite materials. However, due to its high specific surface area and hydrophilic properties, it is not easy to disperse in nanocomposites, and the agglomeration phenomenon is relatively serious. Curing properties, etc., have a more significant impact on the preparation of nanocomposites based on rapid photopolymerization technology. [0003] In general, the addition of inorganic nano-fillers will reduce the photocuring speed and affect the hardness and scratch resistance of the composite material. How to ensure uniform and stable dispersion of nano-fillers and not significantly slow down the polyme...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/67C08K9/06C08K9/04C08K3/36C09D163/10C09D7/12
CPCC08G18/674C08G18/6765C08K3/36C08K9/06C08K9/08C08K2201/011C09D7/62C09D163/10
Inventor 廖正福芦璐何维霖林绍雄汪慧
Owner GUANGDONG UNIV OF TECH