Nanocellulose whisker modified bifunctional photoinitiator and preparation method thereof

A nanocellulose and photoinitiator technology, applied in coatings, polyurea/polyurethane coatings, etc., can solve the problems of reducing the internal stress of the coating, low volatility, and inability to fully exert cellulose properties, and achieve enhanced mechanical The effect of good performance, tensile resistance and good application prospects

Active Publication Date: 2017-05-31
CARPOLY CHEM GRP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] Chinese patent CN 104356153 A relates to a method for preparing a macromolecular photoinitiator by using epichlorohydrin, polyethylene glycol, photoinitiator, etc. Odor, low volatility, good compatibility with resin, etc., and because of the polyglycol chain segment contained in the photoinitiator molecule, the internal stress of the coating is reduced, thereby effectively reducing the occurrence of coating shrinkage. But the preparation process of this method is complicated, and the raw materials used have certain toxicit

Method used

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  • Nanocellulose whisker modified bifunctional photoinitiator and preparation method thereof
  • Nanocellulose whisker modified bifunctional photoinitiator and preparation method thereof
  • Nanocellulose whisker modified bifunctional photoinitiator and preparation method thereof

Examples

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Example Embodiment

[0047] The preparation method of water-dispersed nano cellulose whiskers: take absorbent cotton as raw material, add 64% sulfuric acid, hydrolyze in 60℃ water bath for 3 hours, add appropriate amount of deionized water to terminate the reaction, reduce to room temperature, add NaOH / Na 2 CO 3 Buffer solution, neutralized to pH 7, centrifuged to filter the neutralized solution, washed with deionized water several times, and then dispersed on a sonicator ultrasonically, placed in a dialysis bag for dialysis for about 10 days to obtain a solid mass content of 1.4% Suspension.

[0048] The preparation method of acetone-dispersed nano-cellulose whiskers: the water-dispersed nano-cellulose whiskers are vacuum freeze-dried at a vacuum of 100 Pa and a temperature of -45°C for 48 hours to obtain dry and fluffy nano-cellulose whiskers. Acetone was added for ultrasonic dispersion for 30 minutes to obtain an acetone-dispersed nanocellulose whisker suspension. Detected by transmission electron...

Example Embodiment

[0052] Example 1

[0053] In this embodiment, the diisocyanate is isophorone diisocyanate (IPDI), the photoinitiator is Darocur 1173, the catalyst is dibutyl tin dilaurate, the mass ratio of nanocellulose whiskers to IPDI is 1:5, and IPDI to Darocur 1173 moles The ratio is 1:1.5.

[0054] Synthesis of nano-cellulose whiskers and diisocyanate semi-adducts: 9.49g IPDI and 1.89g freeze-dried nano-cellulose whiskers (dispersed with 25g acetone ultrasonically) were added to the four necks with stirring, exhausting and condenser tubes In the flask, 0.0572 g of catalyst was added dropwise, and nitrogen gas was blown for 10 minutes to remove oxygen in the reaction environment. Stir and react for 3 hours at 60-65°C to obtain nano-cellulose whisker-IPDI semi-adduct.

[0055] The photoinitiator was modified: 10.51g of Darocur 1173 was dropped into a four-necked flask and allowed to react with another NCO group of the diisocyanate for 4 hours. The reaction product was centrifuged to remove th...

Example Embodiment

[0058] Example 2

[0059] In this embodiment, the diisocyanate is isophorone diisocyanate (IPDI), the photoinitiator is Irgacure 184, the catalyst is dibutyltin dilaurate, the mass ratio of nanocellulose whiskers to IPDI is 1:5, and IPDI to Irgacure The molar ratio of 184 is 1:1.5.

[0060] Synthesis of nano-cellulose whiskers and diisocyanate semi-adducts: 9.49g IPDI and 1.89g freeze-dried nano-cellulose whiskers (dispersed with 25g acetone ultrasonically) were put into a four-necked flask with stirring, exhausting and condenser tubes In the process, 0.0572 g of catalyst was added dropwise, and nitrogen gas was blown for 10 minutes to remove oxygen in the reaction environment. Stir and react for 3.5 hours at 60-65°C to obtain nano-cellulose whisker-IPDI semi-adduct.

[0061] The photoinitiator was modified: 13.07g Irgacure 184 was dropped into a four-neck flask, and it was allowed to react with another -NCO group of IPDI for 4.5 hours. The reaction product was centrifuged to remo...

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Abstract

The invention relates to a nanocellulose whisker modified bifunctional photoinitiator and a preparation method thereof. The preparation method comprises the following steps: preparation of nanocellulose whisker and diisocyanate semi-adduct: a catalyst is added dropwise to a nanocellulose whisker and diisocyanate mixture, and the nanocellulose whisker and diisocyanate semi-adduct is obtained after a reaction; modification of a photoinitiator: the photoinitiator is added dropwise to the nanocellulose whisker and diisocyanate semi-adduct, and the nanocellulose whisker modified photoinitiator is obtained after a reaction. The nanocellulose whiskers are grafted to polymer chains of a paint film through photolysis and photopolymerization. The modified photoinitiator prepared with the preparation method has double effects of the photoinitiator and a material reinforcer, is not prone to migration and is high in photo-initiation efficiency, and a photocured material has the advantages of good mechanical property, tensile property and the like and has good application prospect.

Description

technical field [0001] The invention relates to the technical field of photoinitiators, in particular to a nano-cellulose whisker-modified bifunctional photoinitiator and a preparation method thereof. Background technique [0002] Photoinitiators are key components of photocurable coatings. The photoinitiator (PI) receives light energy from the ground state to the excited state (PI * ), and then decomposed into free radicals (R). The free radical combines with the carbon-carbon double bond of the monomer (M), and on this basis, the chain grows to make the carbon-carbon double bond polymerize. Which is accompanied by the transfer and termination of free radicals on the growth chain. The process of photoinitiated free radical polymerization is as follows: [0003] chain triggers: [0004] [0005] R 1 ·+M→R 1 -M· [0006] Chain growth: [0007] [0008] Chain transfer: [0009] R 1 -M n ·+R 3 -H→R 1 -M n -H+R 3 · [0010] R 3 ·+M→R 3 -M· [0011] Chai...

Claims

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Application Information

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IPC IPC(8): C08B15/06C08F2/48C09D175/14
CPCC08B15/06C08F2/48C09D175/14
Inventor 叶代勇方丽冯钦
Owner CARPOLY CHEM GRP
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