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Self-crosslinked fluorosilicate acrylic resin and preparation method thereof

A technology of acrylic resin and perfluoroalkyl ethyl acrylate, applied in the field of self-crosslinking fluorosilicon modified acrylic resin and its preparation, can solve the problem of unsatisfactory heat resistance, poor substrate adhesion and poor mechanical properties and other problems, to achieve the effects of excellent mechanical properties, strong water and oil resistance, and low surface energy

Active Publication Date: 2011-11-23
JINZHOU DPF TH CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The rapid development of acrylic resin is due to its excellent comprehensive properties, such as durability, transparency, stability, gloss retention, and color retention, and also because it can be adjusted to obtain different hardness, flexibility, and compliance with requirements. However, its disadvantage is that its mechanical properties are poor. There are currently two types of improvement methods: one is to introduce a certain amount of fluorine-containing olefin in the synthesis process of acrylic resin to obtain a fluorine-containing resin. Due to the high electronegativity of the F atom, fluorine Carbon resin has excellent weather resistance, chemical resistance, and stain resistance; the other is to introduce a certain amount of silicone functional groups into acrylic resin to make acrylic silicone oligomer resin, so that the resin side chain or terminal Si-O bonds with higher dissociation energy improve the properties of the resin such as high temperature resistance, cold resistance, moisture resistance, weather resistance, stain resistance, chemical corrosion resistance, and electrical insulation
Although these two modification methods have outstanding advantages, they also have shortcomings in some aspects, such as the heat resistance of the former is not ideal; the film-forming performance of the latter is poor, the curing temperature is high, and the adhesion to the substrate is poor.

Method used

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  • Self-crosslinked fluorosilicate acrylic resin and preparation method thereof
  • Self-crosslinked fluorosilicate acrylic resin and preparation method thereof
  • Self-crosslinked fluorosilicate acrylic resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Raw material distribution table

[0022] raw material name Mass percentage (g) Xylene 45 acrylic acid 0.6 Methyl methacrylate 32.0 ethyl acrylate 16.0 Hydroxyethyl Acrylate 3.4 Vinyltrimethoxysilane coupling agent 1.5 perfluorooctyl ethyl acrylate 0.5 tert-butyl hydroperoxide 1.0

[0023] in N 2 react under protection

[0024] (1) Add xylene into the reaction vessel according to the raw material dosage table, and raise the temperature to 100°C;

[0025] (2) Mix acrylic acid, methyl methacrylate, ethyl acrylate, hydroxyethyl acrylate, vinyltrimethoxysilane coupling agent, perfluorobutyl ethyl acrylate and tert-butyl hydroperoxide evenly, drop add 2 hours;

[0026] (3) Keep warm for 3.5 hours;

[0027] (4) Then cool down to 40°C and discharge to obtain a self-crosslinking fluorosilicon-modified acrylic resin with a molecular weight of 79,000. The properties of the obtained self-crosslinking fluorosilicon-m...

Embodiment 2

[0030] Raw material distribution table

[0031] raw material name Mass percentage (g) Xylene 50 acrylic acid 0.4 Methyl methacrylate 27.4 ethyl acrylate 13.7 Hydroxyethyl Acrylate 2.1 Vinyltrimethoxysilane coupling agent 3.2 perfluorooctyl ethyl acrylate 2.5 tert-butyl hydroperoxide 0.7

[0032] in N 2 react under protection

[0033] (1) Add xylene into the reaction vessel according to the raw material dosage table, and raise the temperature to 95°C;

[0034] (2) Mix acrylic acid, methyl methacrylate, ethyl acrylate, hydroxyethyl acrylate, vinyltrimethoxysilane coupling agent, perfluorobutyl ethyl acrylate and tert-butyl hydroperoxide evenly, drop Add 2.5 hours;

[0035] (3) keep warm for 4 hours;

[0036] (4) Then cool down to 50°C and discharge to obtain a self-crosslinking fluorosilicon-modified acrylic resin with a molecular weight of 70,000. The properties of the obtained self-crosslinking fluorosilicon-mo...

Embodiment 3

[0039] Raw material distribution table

[0040] raw material name Mass percentage (g) Xylene 55 acrylic acid 0.3 Methyl methacrylate 22.5 ethyl acrylate 11.3 Hydroxyethyl Acrylate 0.9 Vinyltrimethoxysilane coupling agent 5.0 perfluorooctyl ethyl acrylate 4.5 tert-butyl hydroperoxide 0.5

[0041] in N 2 react under protection

[0042] (1) Add xylene into the reaction vessel according to the raw material dosage table, and raise the temperature to 90°C;

[0043] (2) Mix acrylic acid, methyl methacrylate, ethyl acrylate, hydroxyethyl acrylate, vinyltrimethoxysilane coupling agent, perfluorobutyl ethyl acrylate and tert-butyl hydroperoxide evenly, drop add 3 hours;

[0044] (3) keep warm for 3 hours;

[0045] (4) Then cool down to 60°C and discharge to obtain a self-crosslinking fluorosilicon-modified acrylic resin with a molecular weight of 62,000. The properties of the obtained self-crosslinking fluorosilicon-modi...

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Abstract

The invention discloses self-crosslinked fluorosilicate acrylic resin and a preparation method thereof. The self-crosslinked fluorosilicate modified acrylic resin has the structural formula shown in the specifications, wherein n=4, 6 and 8, and the molecular weight is 60,000-80,000; X refers to a (meth)acryloxy functional group or an alkenyl-containing silane coupling agent; and X has the structural formula shown in the specifications, wherein R is -CH3 or -CH2CH3. The preparation method comprises the following steps of: adding a solvent into a reaction container, and heating to the temperature of between 90 and 100DEG C; uniformly mixing methyl methacrylate, acrylic acid, ethyl acrylate, hydroxyethyl acrylate, a silane coupling agent, perfluoroalkylethyl acrylate and tert-butyl hydroperoxide, and dripping for 2 to 3 hours; keeping the temperature for 3 to 4 hours; and reducing the temperature to 40-60DEG C and discharging. The prepared resin has high weatherability, high chemical resistance, high-temperature resistance, good mechanical properties and glossiness, and high insulativity; and the preparation method has simple process steps and is easy to implement.

Description

technical field [0001] The invention relates to a self-crosslinking fluorosilicon modified acrylic resin and a preparation method thereof. Background technique [0002] The rapid development of acrylic resin is due to its excellent comprehensive properties, such as durability, transparency, stability, gloss retention, and color retention, and also because it can be adjusted to obtain different hardness, flexibility, and compliance with requirements. However, its disadvantage is that its mechanical properties are poor. There are currently two types of improvement methods: one is to introduce a certain amount of fluorine-containing olefin in the synthesis process of acrylic resin to obtain a fluorine-containing resin. Due to the high electronegativity of the F atom, fluorine Carbon resin has excellent weather resistance, chemical resistance, and stain resistance; the other is to introduce a certain amount of silicone functional groups into acrylic resin to make acrylic silicon...

Claims

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Application Information

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IPC IPC(8): C08F220/14C08F220/06C08F220/18C08F220/28C08F220/24C08F230/08C09D133/12
Inventor 魏奇王富春魏潇
Owner JINZHOU DPF TH CHEM CO LTD
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