Method and composition for realizing mercapto-alkyne deep photopolymerization

Abstract

The invention relates to a method and composition for realizing mercapto-alkyne deep photopolymerization. The composition is prepared from, by mass, 20-80 parts of photopolymerizable mercapto monomers, 20-80 parts of photopolymerizable alkyne monomers, 0.5-8 parts of free radical photoinitiator and 0.1-5 parts of up-conversion material. The composition can have a light clicking chemical reaction under the direct radiation of near infrared rays. By means of the method, the maximum depth of photopolymerization of a mercapto-alkyne system can reach 8 cm or above, the problem that deep photopolymerization is difficult in a traditional mercapto-alkyne system is broken through, and the application field of a photopolymerization technology is expanded.

Description

technical field

[0001] The invention belongs to the technical field of photopolymerization materials, and in particular relates to a composition containing an up-conversion material capable of undergoing deep photopolymerization of mercapto-yne under the irradiation of near-infrared light. Background technique

[0002] Because mercapto-alkyne photopolymerization combines many advantages of traditional click chemistry and photoinitiation processes, it has attracted extensive attention from researchers. At the same time, mercapto-yne photopolymerization is not sensitive to water, the polymerization network structure is regular, and the shrinkage rate is low. Compared with the mercapto-ene system, the mercapto-yne system has a higher cross-linking density and a higher sulfur content, which can significantly Increase the optical transparency of polymeric materials, so it has a wide range of applications in the fields of optical materials, coatings, adhesives, molecular devices, ...

Examples

Embodiment 1

[0029] A composition for realizing deep layer photopolymerization of mercapto-yne, the components contained in the composition and the parts by mass of each component are:

[0030]

[0031] Mix the above composition evenly and add it into the test tube, place it vertically and use the emission wavelength 980nm, energy density 12mW / cm 2 The light source was irradiated from top to bottom on the top of the test tube, and solidified after 3 minutes to obtain a 1.92 cm column, and the triple bond conversion rate at the bottom was 40%.

Embodiment 2

[0033] A composition for realizing deep photopolymerization of mercapto-yne, the components contained in the composition and the mass parts of each component are the same as those in Example 1, the difference lies in changing the up-conversion material NaYF 4 The content is 0.9 parts, the length of the column obtained under the same light conditions is 2.35 cm, and the conversion rate of the triple bond at the bottom is 45%.

Embodiment 3

[0035] A composition for realizing deep photopolymerization of mercapto-yne, the components contained in the composition and the mass parts of each component are the same as those in Example 1, the difference lies in changing the up-conversion material NaYF 4 The content is 1.2 parts, the emission wavelength is 980nm, and the energy density is 20.3mW / cm 2 The light source is irradiated from top to bottom on the top of the test tube. After 3 minutes of curing, the length of the column reaches 4.6 cm, and the conversion rate of the triple bond at the bottom is 42%.

technical field

[0001] The invention belongs to the technical field of photopolymerization materials, and in particular relates to a composition containing an up-conversion material capable of undergoing deep photopolymerization of mercapto-yne under the irradiation of near-infrared light. Background technique

[0002] Because mercapto-alkyne photopolymerization combines many advantages of traditional click chemistry and photoinitiation processes, it has attracted extensive attention from researchers. At the same time, mercapto-yne photopolymerization is not sensitive to water, the polymerization network structure is regular, and the shrinkage rate is low. Compared with the mercapto-ene system, the mercapto-yne system has a higher cross-linking density and a higher sulfur content, which can significantly Increase the optical transparency of polymeric materials, so it has a wide range of applications in the fields of optical materials, coatings, adhesives, molecular devices, ...

Examples

Embodiment 1

[0029] A composition for realizing deep layer photopolymerization of mercapto-yne, the components contained in the composition and the parts by mass of each component are:

[0030]

[0031] Mix the above composition evenly and add it into the test tube, place it vertically and use the emission wavelength 980nm, energy density 12mW / cm 2 The light source was irradiated from top to bottom on the top of the test tube, and solidified after 3 minutes to obtain a 1.92 cm column, and the triple bond conversion rate at the bottom was 40%.

Embodiment 2

[0033] A composition for realizing deep photopolymerization of mercapto-yne, the components contained in the composition and the mass parts of each component are the same as those in Example 1, the difference lies in changing the up-conversion material NaYF 4 The content is 0.9 parts, the length of the column obtained under the same light conditions is 2.35 cm, and the conversion rate of the triple bond at the bottom is 45%.

Embodiment 3

[0035] A composition for realizing deep photopolymerization of mercapto-yne, the components contained in the composition and the mass parts of each component are the same as those in Example 1, the difference lies in changing the up-conversion material NaYF 4 The content is 1.2 parts, the emission wavelength is 980nm, and the energy density is 20.3mW / cm 2 The light source is irradiated from top to bottom on the top of the test tube. After 3 minutes of curing, the length of the column reaches 4.6 cm, and the conversion rate of the triple bond at the bottom is 42%.

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