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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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  • Summary
  • 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 toxicity
Chinese patent CN 104530682 A relates to the preparation of a nanocellulose / sulfonated polyaryletherketone composite membrane. The nanocellulose and sulfonated polyaryletherketone are mixed through a solution to obtain a composite membrane with good mechanical properties and low price, but Direct physical mixing will lead to problems such as poor compatibility and inability to give full play to the properties of cellulose
[0018] Currently, there is no report on the chemical compounding of nanocellulose whiskers with photoinitiators

Method used

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

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preparation example Construction

[0047] The preparation method of water-dispersed nano-cellulose whiskers: use absorbent cotton as raw material, add sulfuric acid with a mass concentration of 64%, hydrolyze in a water bath at 60°C for 3 hours, add an appropriate amount of deionized water to terminate the reaction, cool down to room temperature, add NaOH / Na 2 CO 3 Buffer solution, neutralized to a pH value of 7, centrifuged to filter the neutralized solution, washed several times with deionized water, then ultrasonically dispersed on an ultrasonic instrument, placed in a dialysis bag for dialysis for about 10 days, and obtained a solid mass content of 1.4% suspension.

[0048] The preparation method of acetone-dispersed nanocellulose whiskers: vacuum freeze-drying water-dispersed nanocellulose whiskers at a vacuum degree of 100 Pa and a temperature of -45°C for 48 hours to obtain dry and fluffy nanocellulose whiskers solids, and then Add acetone and ultrasonically disperse for 30 minutes to obtain acetone-dis...

Embodiment 1

[0053] In this embodiment, the diisocyanate is selected from isophorone diisocyanate (IPDI), the photoinitiator is selected from Darocur1173, the catalyst is dibutyltin dilaurate, the mass ratio of nanocellulose whiskers to IPDI is 1:5, and the molar ratio of IPDI to Darocur1173 The ratio is 1:1.5.

[0054] Synthesis of nanocellulose whiskers and diisocyanate semi-adducts: 9.49g IPDI and 1.89g freeze-dried nanocellulose whiskers (sonically dispersed with 25g acetone) were added to a four-neck tube with stirring, pumping and cooling tubes In the flask, 0.0572g of catalyst was added dropwise, followed by nitrogen gas for 10 minutes to remove the oxygen in the reaction environment. Stirring and reacting at 60-65°C for 3 hours to obtain nanocellulose whiskers-IPDI semi-adduct.

[0055] Modification of the photoinitiator: 10.51 g 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 w...

Embodiment 2

[0059] In the present embodiment, diisocyanate selects isophorone diisocyanate (IPDI) for use, photoinitiator selects Irgacure 184 for use, catalyzer is dibutyltin dilaurate, the mass ratio of nanocellulose whisker and IPDI is 1:5, IPDI and Irgacure 184 molar ratio is 1:1.5.

[0060] Synthesis of nanocellulose whiskers and diisocyanate semi-adducts: 9.49g IPDI and 1.89g freeze-dried nanocellulose whiskers (sonically dispersed with 25g acetone) were added to a four-neck flask with stirring, air extraction and condenser tubes In, 0.0572g catalyst was added dropwise, and nitrogen gas was passed for 10 minutes to remove oxygen in the reaction environment. Stirring and reacting at 60-65°C for 3.5 hours to obtain nanocellulose whiskers-IPDI semi-adduct.

[0061] Modification of the photoinitiator: 13.07g of Irgacure 184 was dropped into a four-necked flask to react with another -NCO group of IPDI for 4.5 hours. The reaction product was centrifuged to remove the supernatant; it was...

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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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