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Preparation method of polycondensation macromolecular photoinitiator and prepared photoinitiator

A technology of photoinitiators and macromolecules, which is applied in the field of polycondensation macromolecular photoinitiators and its preparation, and can solve problems such as large pollution

Active Publication Date: 2021-05-07
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional mercury lamp light source is gradually banned due to high pollution, and replaced by LED light source. The preparation technology of short-wavelength LED light source is limited by packaging technology and materials. Trends in Aggregation Technology Development

Method used

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  • Preparation method of polycondensation macromolecular photoinitiator and prepared photoinitiator
  • Preparation method of polycondensation macromolecular photoinitiator and prepared photoinitiator
  • Preparation method of polycondensation macromolecular photoinitiator and prepared photoinitiator

Examples

Experimental program
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Effect test

Embodiment 1

[0035] A preparation method for polycondensation macromolecular photoinitiator, comprising the following steps:

[0036] (1) Weigh 1mol 2,5-formyl furan and 1mol cyclohexanone, dissolve them in 20mL of ethyl acetate, and mix them uniformly under stirring;

[0037] (2) Add 3-5 drops of 5% NaOH aqueous solution (0.5gNaOH, 9.5g water) to the mixed solution prepared in step (1), adjust the pH value to 13, react for 3h at 30°C, pass Enter nitrogen, use ice bath to continue reaction 3h, separate out light yellow crystal;

[0038] (3) The light yellow crystals in step (2) were washed with dichloromethane, and dried in vacuo to remove the solvent to obtain a pure light yellow product.

[0039] The test to the performance of the initiator prepared in the present embodiment is as follows: the product of embodiment 1 is with 1 * 10 -5 The molar concentration was dissolved in acetonitrile, and its UV absorption was tested.

[0040] Experimental results: Its absorption wavelength ranges...

Embodiment 2

[0042] A preparation method for polycondensation macromolecular photoinitiator, comprising the following steps:

[0043] (1) Weigh 1mol 2,5-formylfuran and 1mol cyclohexanone and dissolve them in 20mL of ethanol / ethyl acetate (volume ratio 20% / 80%), and mix evenly under stirring;

[0044] (2) Add 3-5 drops of 5% NaOH aqueous solution (0.5gNaOH, 9.5g water) to the mixed solution prepared in step (1), adjust the pH value to 13, react for 3h at 30°C, pass Enter nitrogen, use ice bath to continue reaction 3h, separate out light yellow crystal;

[0045] (3) The light yellow crystals obtained in step (2) were washed with dichloromethane, dried in vacuo to remove the solvent, and a pure light yellow product was obtained.

[0046] The test to the performance of the initiator prepared in the present embodiment is as follows: the product of embodiment 2 is with 1 * 10 -5 The molar concentration was dissolved in acetonitrile, and its UV absorption was tested.

[0047] Experimental res...

Embodiment 3

[0049] A preparation method for polycondensation macromolecular photoinitiator, comprising the following steps:

[0050](1) Weigh 1mol 2,5-formyl furan and 1mol cyclohexanone and dissolve in 20mL of chloroform, and mix evenly under stirring;

[0051] (2) Add 3-5 drops of 5% NaOH aqueous solution (0.5gNaOH, 9.5g water) to the mixed solution prepared in step (1), adjust the pH value to 13, react for 3h at 30°C, pass Enter nitrogen, use ice bath to continue reaction 3h, separate out light yellow crystal;

[0052] (3) The light yellow crystals obtained in step (2) were washed with chloroform, and dried in vacuo to remove the solvent to obtain a pure light yellow product.

[0053] The test to the performance of the initiator prepared in the present embodiment is as follows: the product of embodiment 3 is with 1 * 10 -5 The molar concentration was dissolved in acetonitrile, and its UV absorption was tested.

[0054] Experimental results: Its absorption wavelength ranges from 250n...

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Abstract

The invention discloses a preparation method of a polycondensation macromolecular photoinitiator, relates to the technical field of synthesis of photoinitiators in the field of photopolymerization, and comprises the following steps: combining a polyaldehyde without α-H with a ketone containing α-H or a ketone containing Mix acetyl compounds, add solvent, add alkali solution with a mass fraction of 1%-25%, pass nitrogen gas to react, react at 20-50°C for 1-24h, ice-bath for 1-10h to precipitate crystals, use organic solvent After washing and removing the solvent, the product is obtained, and the present invention also provides the polycondensation macromolecular photoinitiator prepared by the above preparation method. The beneficial effects of the present invention are: the preparation method is simple, the reaction is mild, and the product is easy to purify; the prepared photoinitiator and polyethylene glycol monomer have a relatively high reaction rate without adding a co-initiator. The double bond conversion rate can reach about 90% within 300s.

Description

technical field [0001] The invention relates to the technical field of synthesis of photoinitiators in the field of photopolymerization, in particular to a polycondensation macromolecular photoinitiator and a preparation method thereof. Background technique [0002] In the photocuring system, after the photoinitiator absorbs appropriate light energy, it undergoes a photophysical process to a certain excited state. If the energy at this time is greater than the energy required for bond breaking, it can generate primary active species, such as free radicals or ions, thereby initiating the polymerization reaction. As a photoinitiator, it usually needs to meet the following conditions: (1) the quantum efficiency of initiation is high; (2) the range of absorption spectrum matches the irradiation light source; (3) good thermal stability, no dark reaction; (4) and monomer It has good compatibility with prepolymer. [0003] The traditional mercury lamp light source is gradually ba...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G6/02C08G65/02C08F2/48
CPCC08F2/48C08G6/02C08G65/02
Inventor 朱晓群钟美娟聂俊
Owner BEIJING UNIV OF CHEM TECH