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Macromolecule photoinitiator for gradient polymerization as well as synthesis method and application thereof

A technology of photoinitiators and macromolecules, applied in the field of macromolecular photoinitiators for gradient polymerization and its preparation, can solve the problems of photocuring surface oxygen inhibition and other problems

Inactive Publication Date: 2009-12-09
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Gradient polymerization is achieved by introducing organic silicon segments into the photoinitiator molecule, and at the same time, it effectively solves the problem of oxygen inhibition on the photocuring surface

Method used

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  • Macromolecule photoinitiator for gradient polymerization as well as synthesis method and application thereof
  • Macromolecule photoinitiator for gradient polymerization as well as synthesis method and application thereof
  • Macromolecule photoinitiator for gradient polymerization as well as synthesis method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Synthesis of 184-Tego2342 Silicone Macromolecular Photoinitiator

[0056] 7g (2.5mmol) of Tegomer 2342 (DEGUSSA company) whose molecular formula is Formula 1 and 1.133g (5.5mmol) of DCC (dicyclohexylcarbodiimide) were dissolved in 150mL of ethyl acetate, and stirred at room temperature for 30 Minutes, 1.02 g (5 mmol) Irgacure 184 (1-hydroxycyclohexyl phenyl ketone) was added dropwise, and the reaction was carried out at room temperature for 24 hours after the addition. After filtering, the filtrate was washed three times with 5% NaOH solution and deionized water, and finally the solvent was distilled under vacuum to obtain a liquid product with a molecular formula of Formula 2. The number-average molecular mass was determined to be 3001 by gel chromatography (GPC). In the infrared spectrum, 3300cm -1 The nearby hydroxyl absorption peak disappears at 1752cm -1 The characteristic absorption peak of ester group appeared.

[0057]

[0058] Formula 1

[0059] From th...

Embodiment 2

[0063] Synthesis of HBP-Tego2342 Silicone Macromolecular Photoinitiator

[0064] 7g (2.5mmol) of Tegomer 2342 (DEGUSSA company) whose molecular formula is Formula 1 and 1.133g (5.5mmol) of DCC (dicyclohexylcarbodiimide) were dissolved in 150mL of ethyl acetate, and stirred at room temperature for 30 Minutes, 0.99g (5mmol) of HBP (4-hydroxybenzophenone) was added dropwise, and the reaction was completed at room temperature for 24 hours. After filtering, the filtrate was washed three times with 5% NaOH solution and deionized water, and finally the solvent was distilled under vacuum to obtain a liquid product with a molecular formula of Formula 3. The number-average molecular mass was determined to be 2993 by gel chromatography (GPC). In the infrared spectrum, 3145cm -1 The nearby hydroxyl absorption peak disappears at 1704cm -1 The characteristic absorption peak of ester group appeared.

[0065]

[0066] Formula 3

Embodiment 3

[0068] Synthesis of 1173-Tego2342 Silicone Macromolecular Photoinitiator

[0069] 7g (2.5mmol) of Tegomer 2342 (DEGUSSA company) whose molecular formula is Formula 1 and 1.133g (5.5mmol) of DCC (dicyclohexylcarbodiimide) were dissolved in 150mL of ethyl acetate, and stirred at room temperature for 30 Minutes, 0.821g (5mmol) 1173 (2-hydroxy-2-methyl-1-phenyl-1-propanone) was added dropwise, and the reaction was completed at room temperature for 24 hours. After filtering, the filtrate was washed three times with 5% NaOH solution and deionized water, and finally the solvent was distilled under vacuum to obtain a liquid product with a molecular formula of Formula 4. The number-average molecular mass was determined to be 2956 by gel chromatography (GPC). In the infrared spectrum, 3300cm -1 The nearby hydroxyl absorption peak disappears at 1750cm -1 The characteristic absorption peak of ester group appeared.

[0070]

[0071] Formula 4

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Abstract

The invention discloses a macromolecule photoinitiator for gradient polymerization as well as performance research thereof, which is characterized in that organosilicon-polymer is adopted to react with reactive micromolecule photoinitiator to prepare organosilicon macromolecule photoinitiator; the photoinitiator is applied to gradient polymerization to obtain a polymer with the molecular weight varying in a gradient way by a primary polymerization; and the gradient variation along vertical direction is uniform and has no obvious component interface. In addition, the initiator not only overcomes the defects of easy yellowing, evaporation and migration, great toxicity, poor thermal resistance and the like, but also is endowed with capability of spontaneous ascending by characteristics of organosilicon surface energy and low surface tensile force, thus effectively avoiding oxygen inhibition.

Description

technical field [0001] The invention relates to a macromolecular photoinitiator for gradient polymerization and a preparation method thereof, belonging to the field of polymer material synthesis. Background technique [0002] Gradient polymer refers to a new type of material in which the elements (composition, structure) that make up the polymer change continuously from one side to the other in a certain direction, and the properties and functions of the material also change in a gradient. Molecular weight is a basic element of polymers, which has a great influence on the performance and processing properties of polymers. When the molecular weight of the polymer changes, the properties of the polymer such as mechanical properties (strength, etc.), optical properties (refractive index, etc.), thermal properties (glass transition temperature, etc.), electrical properties (electrical conductivity, etc.), processing properties (fluidity, etc.) denaturation, etc.) etc. will chan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/48C08G77/38C08G77/388C08G77/392
Inventor 孙芳聂俊
Owner BEIJING UNIV OF CHEM TECH
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