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Preparation method of hydrogen abstracting type photoinitiator based on higher fatty acid and product thereof

A technology of higher fatty acid and photoinitiator, applied in the direction of organic chemistry, etc., can solve the problems of odor toxicity, migration, etc., and achieve the effects of increasing molecular weight, easy operation and simple preparation method

Pending Publication Date: 2021-12-31
CHONGQING UNIV OF POSTS & TELECOMM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The currently reported ketene photoinitiators and most of the UV photoinitiators are small molecules. After the photocuring reaction, the residual ketene photoinitiators will also cause migration problems, resulting in odor and toxicity.

Method used

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  • Preparation method of hydrogen abstracting type photoinitiator based on higher fatty acid and product thereof
  • Preparation method of hydrogen abstracting type photoinitiator based on higher fatty acid and product thereof
  • Preparation method of hydrogen abstracting type photoinitiator based on higher fatty acid and product thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Prepare a hydrogen abstraction type photoinitiator based on higher fatty acids, the specific preparation method is as follows:

[0043] 1. Dissolve 28.2g (0.1mol) of oleic acid and 12.7g (0.1mol) of oxalyl chloride in N,N-dimethylformamide (DMF) solvent, and react at 140°C for 24 hours to obtain the acid chloride compound Finally (determined by pointing the plate), add 7.4g (0.1mol) of hydroxyacetone, add 0.635g of triethylamine as a catalyst, and use triethylamine to adjust the pH value of the system to neutral after reacting at 70°C for 5 hours. , point plate through the column purification, to obtain the intermediate product.

[0044] 2, the intermediate product of 16.6g (0.05mol) and the 2-pyrrole carboxaldehyde of 9.8g (0.1mol) are under ethanol solvent, add dropwise 3~5 drops of NaOH aqueous solution (0.5g NaOH and 9.5g solution formed by water configuration), adjust the pH value to 13, and react for 3 hours under the protection of nitrogen at 30°C, then use an i...

Embodiment 2

[0051] Prepare a hydrogen abstraction type photoinitiator based on higher fatty acids, the specific preparation method is as follows:

[0052] 1. Dissolve 28.4g (0.1mol) of octadecanoic acid and 10.2g (0.1mol) of 3-hydroxy-2-pentanone in acetonitrile solution, add 2mL of concentrated sulfuric acid as a catalyst, and react at 70°C for 2 hours , cooled to precipitate a solid, washed with water, and dried with anhydrous sodium sulfate to obtain an intermediate product.

[0053] 2. The furfuraldehyde of the intermediate product and 9.6g (0.1mol) is added in the ethanol solvent for dissolving, and 3-5 drops of a mass fraction of 5% NaOH aqueous solution (0.5g of NaOH and 9.5g of water are configured to obtain) are added dropwise to adjust The pH value was 13, reacted under the protection of nitrogen at 70°C for 3 hours, continued the reaction in an ice bath for 3 hours, and precipitated a pale yellow solid, washed with water, and dried over anhydrous sodium sulfate to obtain a hydr...

Embodiment 3

[0058] Prepare a hydrogen abstraction type photoinitiator based on higher fatty acids, the specific preparation method is as follows:

[0059] 1. Dissolve 56g (0.2mol) of linoleic acid and 11g (0.1mol) of 1.5-hydroxypentanone in acetonitrile solution, add concentrated sulfuric acid as a catalyst, react at 70°C for 2 hours, cool to precipitate solids, and water After washing, it was dried over anhydrous sodium sulfate to obtain an intermediate product.

[0060] 2. Add the intermediate product and 22.4 g (0.2 mol) of thiophene formaldehyde into the ethanol solvent, add dropwise 3 to 5 drops of 5% NaOH aqueous solution (0.5 g of NaOH and 9.5 g of water), and adjust the pH value After reacting for 3 hours under the protection of nitrogen at 70°C, use an ice bath to continue the reaction for 3 hours, and a light yellow solid precipitates out. The product is washed with water and dried over anhydrous sodium sulfate to obtain a hydrogen abstraction photoinitiator S-1 based on higher ...

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Abstract

The invention relates to a preparation method of a hydrogen abstracting type photoinitiator based on higher fatty acid and a product thereof, and belongs to the technical field of preparation of photoinitiators. According to the preparation method of the hydrogen abstracting type photoinitiator, a higher fatty acid long alkyl chain is introduced on the basis of the structure of the ketene hydrogen abstracting type photoinitiator, and the higher fatty acid long alkyl chain is introduced into the structure of the ketene photoinitiator, so that the polarity of the photoinitiator can be improved, and the compatibility of the photoinitiator and a prepolymer is improved; meanwhile, the molecular weight of the photoinitiator can also be increased, and the situation that after the photocuring reaction is finished, the residual photoinitiator is migrated out of a cured film, and toxicity and odor are caused is prevented. The long alkyl chain does not participate in conjugation of the photoinitiator, the maximum absorption wavelength of the photoinitiator is 350-450 nm, so that the photoinitiator can be matched with an ultraviolet blue light LED. The hydrogen abstracting type photoinitiator which is good in compatibility with a photocuring system and low in migration effect meets the requirements in the photocuring field.

Description

technical field [0001] The invention belongs to the technical field of photoinitiator preparation, and relates to a preparation method of a hydrogen abstraction type photoinitiator based on higher fatty acid and a product thereof. Background technique [0002] Photocuring technology is widely used in coatings, inks, adhesives, photoresists and other fields due to its advantages of fast curing speed, energy saving and environmental protection. Photocurable formulations generally include prepolymers, photoinitiators, and diluents. Photoinitiator, as a key component in the photocuring formulation, plays a role in determining the degree of polymerization of the prepolymer. Ketene photoinitiator is a kind of hydrogen abstraction type photoinitiator which is easy to prepare and cheap. It has rich scientific research value and has been proved to have good photoinitiation performance; Rigid structure, this structure may not only cause poor compatibility between the ketene photoini...

Claims

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Application Information

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IPC IPC(8): C07D207/333C07D307/46C07D333/22C08F2/48C08F120/20
CPCC07D207/333C07D307/46C07D333/22C08F2/48C08F120/20
Inventor 李经方周贤菊谢广新
Owner CHONGQING UNIV OF POSTS & TELECOMM
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