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A kind of unsaturated polyether, photocurable resin and preparation method thereof

An unsaturated and polyether technology, applied in the field of unsaturated polyether, photocurable resin and its preparation, can solve the problem of long curing time, and achieve the effect of fast photocuring speed, excellent adhesion performance and simple synthesis

Active Publication Date: 2019-11-26
SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The polyurethane acrylate synthesized by this method has the advantages of high functionality, strong polarity, high strength and low viscosity, but its curing time is long, and its curing time is 70-110s when tested by finger dry method

Method used

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  • A kind of unsaturated polyether, photocurable resin and preparation method thereof
  • A kind of unsaturated polyether, photocurable resin and preparation method thereof
  • A kind of unsaturated polyether, photocurable resin and preparation method thereof

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preparation example Construction

[0023] In this specific embodiment, a preparation method of unsaturated polyether is provided, comprising the following steps: adding propylene glycol or butanediol as an initiator in a reaction vessel, adding an active metal cation catalyst, vacuum dehydration treatment, and passing in an inert gas , adding a chain extender to the reaction vessel, the chain extender is a glycidyl ether containing unsaturated bonds, a glycidyl ester containing unsaturated bonds, a photoactive glycidyl ether or a photoactive glycidol Esters; control the temperature of the reaction system at 0-140°C, and carry out ring-opening polymerization for 0.5-3 hours at a stirring speed of 300-500 rpm to prepare unsaturated polyether.

[0024] The chain extender is a mixture of one or more of glycidyl methacrylate, glycidyl acrylate, and allyl glycidyl ether.

[0025] The active metal cationic catalyst is sodium hydroxide, antimony pentachloride, tin tetrachloride, tin tetrachloride + trifluoroacetic acid...

Embodiment 1

[0041] Weigh 0.1 mol (7.609 g) of propylene glycol and 0.8529 g of potassium hydroxide (active cationic catalyst) and add them into the reaction vessel. Vacuum dehydration at 80°C for 30 min. Nitrogen gas was introduced to maintain a certain nitrogen flow rate. Slowly add 0.6 mol (85.29 g) of glycidyl acrylate dropwise into the reaction vessel, and the dropping time is controlled within 30-60 minutes. After the glycidyl acrylate was added dropwise, the reaction was continued for 1 h. Stop heating, and neutralize the system with 0.1mol / L phosphoric acid aqueous solution until the pH of the system is neutral. Add 20ml of deionized water, stir at room temperature for 30min, distill under reduced pressure to remove the water in the system, wash the system with petroleum ether, and distill under reduced pressure to remove the petroleum ether in the system to obtain a hydroxyl-terminated unsaturated polyether.

[0042] Such as figure 1 Shown is the NMR spectrum of the prepared h...

Embodiment 2

[0047] Weigh 0.17mol (12.94g) of propylene glycol into the reaction vessel, and vacuum dehydrate at 80°C for 30min. Nitrogen gas was introduced to maintain a certain nitrogen flow rate. Cool down to 65°C, add 1.135ml of cocatalyst trifluoroacetic acid into the reaction vessel, add 0.800ml of catalyst anhydrous tin tetrachloride into the reaction vessel, slowly add 1.02mol (145g) glycidyl acrylate dropwise into the reaction vessel For ester, the dropping time is controlled within 30-60min. After the glycidyl acrylate was added dropwise, the reaction was continued for 4h. Stop heating, add 150ml of dichloroethane, and let stand overnight (stand for about 24h). Filter to remove the lower layer liquid. Wash three times with methanol aqueous solution of disodium ethylenediamine tetraacetate, distill under reduced pressure, remove dichloroethane and water in the system, and obtain unsaturated polyether with terminal hydroxyl groups.

[0048] The hydroxyl-terminated unsaturated p...

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Abstract

The invention discloses an unsaturated polyether, a light-cured resin and a preparation method of the unsaturated polyether. The preparation method of the unsaturated polyether comprises the steps of adding diol or polyol, used as an initiator, into a reaction container, adding an active metal cationic catalyst, vacuum dehydrating, introducing an inert gas, and adding a chain extender into the reaction container, wherein the chain extender is glycidyl ether containing unsaturated bonds, glycidyl ester containing unsaturated bonds, glycidyl ether with optical activity or glycidyl ester with optical activity; and controlling a temperature of a reaction system at 0-140 DEG C, and performing ring-opening polymerization for 0.5-3 hours at a stirring speed of 300-500rpm, so as to prepare the unsaturated polyether. The unsaturated polyether prepared by the method can effectively shorten the curing time of the prepared UV-cured resin, improves the cross-linking density of the light-cured resin, and improves the performance of the light-cured resin.

Description

【Technical field】 [0001] The invention relates to an unsaturated polyether, a photocurable resin and a preparation method thereof. 【Background technique】 [0002] UV curing is a material surface treatment technology that appeared in the 1960s. It refers to the crosslinking of liquids with photocurable activity under ultraviolet light to form solid materials. UV curing technology has many advantages. For example, compared with other technologies, UV curing technology has a particularly fast curing speed. The curing time of UV curing technology is generally about tens of seconds, which is difficult for other curing technologies to achieve. The earliest industrialization of UV curing was in 1968, when Bayer of Germany developed a UV curing coating whose main components were unsaturated polyester and styrene. Now the application range of UV curing technology is expanding, including coatings, inks, adhesives and so on. [0003] UV curing products are composed of oligomers, reac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/28C08F2/48
CPCC08F2/48C08G65/002C08G65/2606
Inventor 唐国翌朱亚丽董运生姚有为陈丽杰
Owner SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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