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Fluorine-silicon double-block ultraviolet cured resin and preparation method thereof

A curing resin and double-block technology, which is applied in coatings, polyurea/polyurethane coatings, etc., can solve the problems of complete miscibility, poor high temperature resistance, phase separation instability, etc., and achieve no VOC emission problem, curing The effect of short time and high production efficiency

Inactive Publication Date: 2020-11-20
HARBIN INST OF TECH WUXI RES INST OF NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the added inorganic fillers have poor compatibility with the organic system of the paint, and it is difficult to achieve complete mutual solubility. Long-term storage will inevitably lead to an unstable state of separation, especially in the later storage and use process, due to the settlement of fillers. It will lead to stress concentration, damage to the internal structure at high temperature, affect subsequent use, and poor high temperature resistance

Method used

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  • Fluorine-silicon double-block ultraviolet cured resin and preparation method thereof
  • Fluorine-silicon double-block ultraviolet cured resin and preparation method thereof
  • Fluorine-silicon double-block ultraviolet cured resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Weigh 25.3g (0.05mol) of organosilicon intermediate (number average molecular weight M n =500) and 17.1g (0.05mol) of bisphenol AF in a reactor, heated up to 100°C, dried and removed water for 4h, and after cooling down to normal temperature, slowly added 34.1g (0.2mol) of hexamethylene Diisocyanate, the feeding time is 0.5h, the temperature is raised to 70°C, the heating time is 0.5h, the measured NCO value is 11%, the reaction is kept at 70°C for 4h, the NCO value drops to 5%, the temperature is lowered to 60°C, and 23.5g is added slowly (0.2mol) hydroxyethyl acrylate and 0.01g triethylamine, the feeding time is 0.5h, the temperature is raised to 80°C and the reaction is completed until the NCO value is 0.2%.

[0043] The above-mentioned prepared fluorine-silicon double-block UV-curable resin was tested for UV-curable performance. Take 10g of the resin, add 0.5g of cracking photoinitiator 1-hydroxycyclohexyl phenyl ketone, and evenly coat it on the corona-treated On ...

Embodiment 2

[0046] Take by weighing 55.3g (0.011mol) of organosilicon intermediate (number average molecular weight M n =5000) and 13.6g (0.033mol) of 1,4-bis(2-hydroxyhexafluoroisopropyl)benzene in a reaction kettle, heated up to 150°C, dried to remove water for 2h, and after cooling down to normal temperature, in a nitrogen atmosphere Slowly add 19.6g (0.088mol) isophorone diisocyanate under low temperature, the feeding time is 2h, the temperature is raised to 80°C, the heating time is 1h, the measured NCO value is 4.2%, and the heat preservation reaction is carried out at 80°C for 1h, and the NCO value drops to 2.1 %, cool down to 70°C, slowly add 11.5g (0.088mol) hydroxyethyl methacrylate and 0.2g triethylenediamine, the addition time is 0.5h, heat up to 100°C until the NCO value is 0.2%, and then react Finish.

[0047] Carry out UV curing performance test on the fluorosilicone diblock UV-curable resin prepared above, take 10g resin, add 0.1g cracking photoinitiator 2-hydroxy-2-methy...

Embodiment 3

[0050] Take by weighing 43.5g (0.022mol) of organosilicon intermediate (number average molecular weight M n =2000) and 17.8g (0.044mol) of 1,4-bis(2-hydroxyhexafluoroisopropyl)benzene in a reaction kettle, heated up to 130°C, dried for 2.5h, and cooled to room temperature, under nitrogen Slowly add 21.7g (0.132mol) of 1,4-cyclohexane diisocyanate under the atmosphere, the feeding time is 2h, the temperature is raised to 75°C, the heating time is 1h, the measured NCO value is 6.7%, and the reaction is kept at 75°C for 1h, and the NCO value decreased to 3.3%, lowered the temperature to 65°C, slowly added 17g (0.132mol) hydroxypropyl acrylate and 0.05g dibutyltin dilaurate, the addition time was 1h, raised the temperature to 90°C until the NCO value was 0.2%, and reacted Finish.

[0051] The above-mentioned fluorine-silicon double-block UV-curable resin was tested for UV-curable performance. Take 10g of the resin, add 0.1g of cracking photoinitiator 1-hydroxycyclohexyl phenyl ke...

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Abstract

The invention discloses a fluorine-silicon double-block ultraviolet cured resin, which comprises an organic silicon chain segment, a polyurethane chain segment and a fluorine-containing aromatic hydrocarbon chain segment, and is subjected to an end capping treatment by using acrylate. According to the fluorine-silicon double-block ultraviolet cured resin, no volatile organic solvent is used in thewhole production process, the process is environmentally friendly and free of pollution, the VOC emission is avoided, and the low-carbon and environment-friendly requirements are met. The molecular structure of the fluorine-silicon double-block ultraviolet cured resin always contains a plurality of double bonds, the curing rate is high, the resin can be completely cured within 5-20 seconds, the energy consumption is low, the production period is short, the production efficiency is high, and the production cost is low. The process is simple, no complex production process is needed, and the reaction process is stable and safe.

Description

technical field [0001] The invention relates to the field of polyurethane synthesis, in particular to a fluorosilicon double-block ultraviolet curable resin and a preparation method thereof. Background technique [0002] With the development of large-scale automated continuous production and the improvement of environmental protection requirements, UV-curable materials have been widely used in coatings, adhesives, inks and other fields. Ultraviolet curing technology can not only achieve efficient and rapid curing, but also has low energy consumption and no pollution during the curing process, which is convenient for the assembly line production operation of the factory and meets the requirements of environmental protection. UV curing technology has gradually replaced traditional curing methods and has become a green technology that has attracted widespread attention. [0003] At present, UV-curable coating materials mainly rely on adding inorganic fillers to improve heat re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/75C08G18/73C08G18/67C08G18/10C08G18/65C08G18/12C08G18/61C08G18/58C08G18/32C09D175/14
CPCC08G18/12C08G18/3812C08G18/58C08G18/61C08G18/672C08G18/73C08G18/755C08G18/758C09D175/14C08G18/65
Inventor 白永平王一晶龙军李卫东岳利培崔玉涛
Owner HARBIN INST OF TECH WUXI RES INST OF NEW MATERIALS