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In-situ hybridization photoreaction system of mercaptan-alkene/siloxane catalyzed by photoacid/photobase

A technology of alkali-catalyzed thiol and siloxane compounds, applied in the field of in-situ hybrid photoreaction system, can solve the problems of reducing polymerization volume shrinkage and the like, and achieve the effects of high glass transition temperature and high storage modulus

Inactive Publication Date: 2019-08-13
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the photopolymerization of thiol-ene, the chain growth and chain transfer are in a state of competition, so that the polymer has a large polymerization shrinkage, but the chain transfer reaction between the thiol and the double bond reduces the shrinkage of the polymerization volume

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1) Add 11.63mg of TBD·HBPh 4 and 5.82 mg of ITX, and injected with 0.1 ml of dimethyl sulfoxide (DMSO).

[0021] 2) Sonicate the above mixed system for 5 minutes at room temperature to completely dissolve it to form a uniform and transparent solution.

[0022] 3) Add 199.4 mg of triallyl isocyanurate to step 2).

[0023] 4) Add 146.6 mg of pentaerythritol tetrakis(3-mercaptopropionate) and 235.6 mg of 3-mercaptopropyltrimethoxysilane to step 2).

[0024] 5) Mix the solution obtained in step 4) evenly and introduce it into the prepared light-transmitting container.

[0025] 6) Put the light-transmitting container filled with samples in step 5) under the ultraviolet lamp (320-500nm) for reaction, the air humidity is 10%, the reaction time of the mixed solution in the light-transmitting container is 20min, and mix in the light-transmitting container The liquid reacts until a solid spline is formed.

[0026] 7) Take out the solid sample formed in step 6) and place it in...

Embodiment 2

[0028] Concrete experimental procedure is identical with embodiment 1, only changes following formula content:

[0029] TBD·HBPh 4 10.92 mg;

[0030] ITX 5.46mg;

[0031] Tetrakis(3-mercaptopropionic acid) pentaerythritol ester 205.22mg;

[0032] 3-Mercaptopropyltrimethoxysilane 141.35mg;

[0033] The properties of the obtained material at room temperature 25°C are shown in Table 1.

Embodiment 3

[0035] Concrete experimental procedure is identical with embodiment 1, only changes following formula content:

[0036] TBD·HBPh 4 12.34 mg;

[0037] ITX 6.17mg;

[0038] Tetrakis(3-mercaptopropionic acid) pentaerythritol ester 87.95mg;

[0039] 3-Mercaptopropyltrimethoxysilane 329.8mg;

[0040] The properties of the obtained material at room temperature 25°C are shown in Table 1.

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Abstract

The invention relates to an in-situ hybridization photoreaction system of mercaptan-alkene / siloxane catalyzed by photoacid / photobase. Specifically, a mercapto compound, a polyfunctional siloxane compound with mercapto groups, a double-bond compound, photoacid / photobase and other photosensitizers and a solvent are mixed in a certain ratio and subjected to ultrasonic dissolution, a mercapto-double bond polymerization reaction and a hydrolytic condensation reaction of siloxane are carried out under ultraviolet light irradiation in air with a certain humidity, and then a uniform organic / inorganichybrid network structure can be produced with a one-step method. According to the photoreaction system, the chain transfer reaction between double bonds and mercapto groups reduces the volume shrinkage of a polymer; oxygen inhibition is avoided; gelation is retarded; the crosslinking degree and reaction velocity can be controlled by adjusting different mercapto compound proportions and double-bondcompound types; the hydrolytic condensation process between siloxane functional groups can increase the glass transition temperature of the reaction system and improve the crosslinking density.

Description

technical field [0001] The invention relates to an in-situ hybrid photoreaction system of thiol-ene / siloxane catalyzed by photoacid generation / photobase generation. Specifically, mercapto compounds, multifunctional siloxane compounds with mercapto groups, double bond compounds, photoacid / base and other photosensitizers, solvents are mixed and ultrasonically dissolved, and then in a certain humidity of air, under the irradiation of ultraviolet lamps The mercapto-double bond polymerization reaction and the hydrolysis condensation reaction of siloxane can be used to prepare a uniform organic / inorganic hybrid network structure in one step. Background technique [0002] China is in a period of rapid development of the national economy, and the pressure of environmental protection has also increased sharply. It has become an inevitable trend to reduce the use of volatile organic solvents in coatings, inks, and adhesives. It is one of the best measures to solve this problem. Compa...

Claims

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Application Information

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IPC IPC(8): C08G75/045C08K3/36
CPCC08G75/045C08K3/36
Inventor 何勇邱桂仙聂俊
Owner BEIJING UNIV OF CHEM TECH
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