Organic silicon cationic light-cured resin containing oxetane structure and preparation method of resin

A technology of light-curing resin and oxetane, which is applied in the field of ultraviolet light-curing silicon-containing resin preparation, can solve the problems of poor compatibility between silicone and resin, unsatisfactory comprehensive performance, etc., and achieve the effect of small volume shrinkage

Active Publication Date: 2016-12-07
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the cost is low, the compatibility between silicone and resin is poor, and the overall performance is not ideal

Method used

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  • Organic silicon cationic light-cured resin containing oxetane structure and preparation method of resin
  • Organic silicon cationic light-cured resin containing oxetane structure and preparation method of resin
  • Organic silicon cationic light-cured resin containing oxetane structure and preparation method of resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh 44.05g of 3-hydroxymethyloxetane, add it dropwise to 87.08g of toluene diisocyanate (TDI), and add 0.06g of dibutyltin dilaurate, maintain the temperature at 40°C for 2h, then raise the temperature Keep warm at 70°C, stop the reaction when the NCO content reaches the theoretical value, and obtain polyurethane semi-adduct A1.

[0033] Weigh 64.05g of dimethylol-terminated polysiloxane (hydroxyl value: 43.72mg KOH / g), add 13.11g of the prepared product A1 to it, and add 0.03g of dibutyltin dilaurate, react at 70°C , until the absorption peak of NCO in the infrared spectrum disappears, stop the reaction, and obtain the organosilicon cationic photocurable resin B1 containing the oxetane structure.

[0034] Prepared resin B1: viscosity is 1520mPa s (GB / T 9269-1988, 60°C); refractive index is 1.51; chromaticity is (APHA) 1G; elongation is 122%; Tg is -22°C; pencil hardness It is 2H; the volume shrinkage rate reaches 3%; the adhesion level is 0.

Embodiment 2

[0036] Weigh 22.03g of 3-hydroxymethyloxetane, add it dropwise to 62.56g of diphenylmethane diisocyanate (MDI), add 0.04g of dibutyltin dilaurate, and keep the temperature at 50°C for 1h Afterwards, the temperature was raised to 80° C. to keep the temperature, and the reaction was stopped when the NCO content reached the theoretical value, and the polyurethane semi-adduct A2 was obtained.

[0037] Weigh 65.45g of dihydroxypropyl-terminated polysiloxane (hydroxyl value 42.78mg KOH / g), add 16.92g of the prepared product A2 to it, and add 0.04g of dibutyltin dilaurate, and react at 80°C , until the absorption peak of NCO in the infrared spectrogram disappears, the reaction is stopped, and the organic silicon cationic photocurable resin B2 containing the oxetane structure is obtained.

[0038] Prepared resin B2: viscosity is 1610mPa s (GB / T 9269-1988, 60°C); refractive index is 1.52; chromaticity is (APHA) 1G; elongation is 108%; Tg is -20°C; pencil hardness It is 3H; the volume ...

Embodiment 3

[0040] Weigh 22.03g of 3-hydroxymethyloxetane, add it dropwise to 55.57g of isophorone diisocyanate (IPDI), and add 0.04g of dibutyltin dilaurate, and maintain the temperature at 45°C for 1.5 After one hour, the temperature was raised to 65°C to keep the temperature, and when the NCO content reached the theoretical value, the reaction was stopped to obtain the polyurethane semi-adduct A3.

[0041] Weigh 64.05g of dimethylol-terminated polysiloxane (hydroxyl value 43.72mg KOH / g), add 15.52g of the prepared product A3 to it, and add 0.04g of dibutyltin dilaurate, react at 65°C , until the absorption peak of NCO in the infrared spectrum disappears, stop the reaction, and obtain the organosilicon cationic photocurable resin B3 containing the oxetane structure.

[0042] Prepared resin B3: viscosity is 1589mPa s (GB / T 9269-1988, 60°C); refractive index is 1.47; chroma is (APHA) 25; elongation is 150%; Tg is -30°C; pencil hardness It is 1H; the volume shrinkage rate reaches 2%; the ...

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Abstract

The invention discloses organic silicon cationic light-cured resin containing an oxetane structure and a preparation method of the resin. The preparation method comprises the steps that 1, oxetane reacts with diisocyanate to prepare semi-additive polyurethane of which one end is of the oxetane structure, and the other end is of an isocyanato structure; 2, semi-additive polyurethane is modified with hydroxyl on organic siloxane molecular chains, and then the organic silicon cationic light-cured resin is obtained. The resin prepared through the method has the excellent properties that in the light curing process, the volume shrinkage rate is low, and the adhesive force to a base material is high; in addition, the light curing process is not inhibited by oxygen, and a curing reaction is not prone to be stopped.

Description

technical field [0001] The invention relates to an organic silicon cationic light-curable resin containing an oxetane structure, belonging to the field of preparation of ultraviolet light-curable silicon-containing resins. Background technique [0002] With the enhancement of people's awareness of environmental protection and the increasingly stringent environmental regulations of various countries, UV-curable materials are gradually replacing traditional solvent-based materials due to their advantages such as no solvent or low solvent, fast curing speed, low organic volatiles, and good coating performance. coating. Ultraviolet light curing includes two mechanisms: free radical light curing and cationic light curing. Among them, free radical light curing is widely used, but due to the poor adhesion of the cured film to the substrate, it has a strong oxygen inhibition effect and a unique Mucous membrane irritation, so its application is subject to certain restrictions. Comp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/388C08G77/38C08G77/16
CPCC08G77/16C08G77/38C08G77/388
Inventor 聂俊宋文迪朱晓群方大为
Owner BEIJING UNIV OF CHEM TECH
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