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Super-branching silicon-base macromolecule optical initiator and preparation method thereof

A hyperbranched silicon-based, photoinitiator technology, applied in the field of macromolecular photoinitiators, can solve the problems of easy migration, toxicity, poor heat resistance, etc., achieve good heat resistance, increase thermal decomposition temperature, and improve heat resistance. Effect

Inactive Publication Date: 2007-11-28
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to improve the toxicity, easy migration and poor heat resistance of small molecule photoinitiators, the present invention provides a macromolecular photoinitiator based on hyperbranched organosilicon polymers, when it is used to trigger When the compound is polymerized or cross-linked, it has good photoinitiating activity, and can endow the polymerized or cross-linked resin with excellent heat resistance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The hyperbranched silicon-based macromolecular photoinitiator formula includes: 34.5 grams of methylhydrogen dichlorosilane, 9.6 grams of magnesium powder, 30.6 grams of allyl chloride, 180 grams of tetrahydrofuran, 0.15 grams of chloroplatinic acid-tetramethyldivinyl Silane complex (Karstedt catalyst), 44.1 g of IHT-PI 185, 15.8 g of pyridine, 0.2 g of 4,4'-dimethylaminopyridine, 200 g of n-hexane, 300 g of acetonitrile. Its preparation method is:

[0031] (1) Heat the mixture of 9.6 grams of magnesium powder and 150 grams of tetrahydrofuran to 40 degrees, add dropwise 23 grams of methylhydrogen dichlorosilane and 30.6 grams of allyl chloride, and react at 40 degrees for 24 hours;

[0032] (2) Cool down to room temperature, filter the precipitate and evaporate the solvent, and distill under reduced pressure at -0.85 MPa and 47 degrees to obtain methylhydrogen diallylsilane;

[0033] (3) Add 10 grams of tetrahydrofuran and 0.1 gram of chloroplatinic acid-tetramethyldiv...

Embodiment 2

[0040] The hyperbranched silicon-based macromolecular photoinitiator formula includes: 34.5 grams of methylhydrogen dichlorosilane, 11.0 grams of magnesium powder, 35.2 grams of allyl chloride, 400 grams of tetrahydrofuran, 0.15 grams of chloroplatinic acid-tetramethyldivinyl Silane complex (Karstedt catalyst), 52.3 g of IHT-PI 1173, 23 g of triethylamine, 0.2 g of 4,4'-dimethylaminopyridine, 450 g of ethanol. Its preparation method is:

[0041] (1) The mixture of 11.0 grams of magnesium powder and 170 grams of tetrahydrofuran was heated to 65 degrees, and 23 grams of methylhydrogen dichlorosilane and 35.2 grams of allyl chloride were added dropwise, and reacted at 65 degrees for 12 hours;

[0042] (2) Cool down to room temperature, filter the precipitate and evaporate the solvent, and distill under reduced pressure at -0.85 MPa and 47 degrees to obtain methylhydrogen diallylsilane;

[0043] (3) Add 10 grams of tetrahydrofuran and 0.05 grams of chloroplatinic acid-tetramethyl...

Embodiment 3

[0050] The hyperbranched silicon-based macromolecular photoinitiator formula includes: 34.5 grams of methylhydrogen dichlorosilane, 10.6 grams of magnesium powder, 33.7 grams of allyl chloride, 200 grams of tetrahydrofuran, 0.13 grams of chloroplatinic acid-tetramethyldivinyl Silane complex (Karstedt catalyst), 46.3 g of IHT-PI 2959, 17 g of pyridine, 0.2 g of 4,4'-dimethylaminopyridine, 200 g of n-hexane, 360 g of methanol. Its preparation method is:

[0051] (1) The mixture of 10.6 grams of magnesium powder and 150 grams of tetrahydrofuran was heated to 55 degrees, 23 grams of methylhydrogen dichlorosilane and 33.7 grams of allyl chloride were added dropwise, and reacted at 55 degrees for 18 hours;

[0052] (2) Cool down to room temperature, filter the precipitate and evaporate the solvent, and distill under reduced pressure at -0.85 MPa and 47 degrees to obtain methylhydrogen diallylsilane;

[0053] (3) Add 20 grams of tetrahydrofuran and 0.08 grams of chloroplatinic acid-...

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PUM

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Abstract

The present invention discloses one kind of superbranched Si-base macromolecular photoinitiator and its preparation, and features that the superbranched Si-base macromolecular photoinitiator is prepared through the first Si-H addition reaction to prepare superbranched organosilicon polymer with excellent flowability, high solubility and excellent reaction performance, and the subsequent reaction of the organosilicon polymer and modified small molecular weight photoinitiator. The superbranched Si-base macromolecular photoinitiator can initiate the polymerization or cross-linking of compound containing acrylate or similar radical under the irradiation of ultraviolet ray. It is superior to small molecular weight photoinitiator, and has low mobility, low toxicity, high heat resistance and capacity of raising the heat resistance of the cured resin.

Description

technical field [0001] The invention relates to a macromolecular photoinitiator and belongs to the field of polymer material synthesis. Background technique [0002] Due to the advantages of high efficiency, energy saving, and environmental protection, photopolymerization and photocuring technology, especially in places that are sensitive to heat, have become scientific research hotspots and one of the fastest growing industrial technologies in recent years. Photoinitiator is an important part of photopolymerization or photocuring system, which not only affects the initiation rate, but also has an important influence on the properties of cured products (such as toxicity, mechanical properties, thermal properties, etc.). The existing small-molecule photoinitiators have disadvantages such as large odor, high volatility, poor migration resistance, high toxicity, and yellowing, which are difficult to meet the needs of further development of photopolymerization and photocuring te...

Claims

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Application Information

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IPC IPC(8): C08F2/50C08G77/60C08F20/00
Inventor 范晓东王生杰
Owner NORTHWESTERN POLYTECHNICAL UNIV
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