Caprolactone-tung oil copolymerized polyol polymer and synthesis method thereof

A technology of copolyol and tung oil polyol, which is applied in the field of new caprolactone-tung oil copolyol polymer and its synthesis, to achieve good gloss and dry properties, weather resistance and aging resistance.

Inactive Publication Date: 2014-12-10
HIGH & NEW TECH RES CENT OF HENAN ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the previous research work of the applicant (Chinese patent 2009100653473), the applicant modified tung oil and obtained the aminolysis tung oil polyol, which made the application of tung oil more extensive and also provided good opportunities for the application of vegetable oil in polymers. Based on the research, PCL is modified by aminolysis of tung oil polyol in order to obtain new polycaprolactone materials with specific functional requirements, but there is no relevant literature report so far

Method used

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  • Caprolactone-tung oil copolymerized polyol polymer and synthesis method thereof
  • Caprolactone-tung oil copolymerized polyol polymer and synthesis method thereof
  • Caprolactone-tung oil copolymerized polyol polymer and synthesis method thereof

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Embodiment 1

[0028] Equipped with electric stirrer, thermometer, N 2 Add aminolysis tung oil polyol (hydroxyl value 289mgKOH / g) 6.17g, caprolactone (CL) 40.16g and account for 0.1% catalyst stannous octoate of total reactant weight in the four-neck flask of import port, reflux condenser, Start stirring and pass N continuously 2 Air for 30 minutes, heat the oil bath to 150-155°C, keep at this temperature for polymerization for 7 hours, then vacuumize at this temperature to remove unreacted caprolactone, then cool down to 100°C, and obtain caprolactone after cooling - Tung oil copolyol. The hydroxyl value determined by end group titration: OH=33 mgKOH / g, the corresponding number average molecular weight M n =3400. Figure 4 It is the infrared spectrogram of the caprolactone-tung oil copolyol polyol synthesized in the present embodiment.

[0029] attached by Figure 1-5 It can be seen that there is a significant difference between aminolysis tung oil polyol, caprolactone, polycaprolacton...

Embodiment 2

[0031] In the reaction device described in example 1, add aminolysis tung oil polyol (hydroxyl value 324mgKOH / g) 4.16g, caprolactone (CL) 61.18g and account for the catalyst stannous octoate of 0.23% of reactant gross weight, start stirring And continuously pass N 2 Air for 30 minutes, then heat up to 155-170°C with an oil bath, keep at this temperature for polymerization for 7 hours, then vacuumize at this temperature to remove unreacted caprolactone, then cool down to 100°C and discharge, after cooling A caprolactone-tung oil copolyol polymer is obtained. The hydroxyl value determined by end group titration: OH=18.92 mgKOH / g, the corresponding number average molecular weight M n =5930.

Embodiment 3

[0033] Add aminolysis tung oil polyol (hydroxyl value 325mgKOH / g) 3.46g in the reaction device described in example 1, caprolactone (CL) 60.56g and account for the catalyzer stannous octoate of 0.12% of reactant gross weight, start stirring And continuously pass N 2 Gas for 30 minutes, then heat up to 150-160°C with an oil bath, keep the polymerization reaction at this temperature for 7 hours, and then vacuumize at this temperature to remove unreacted caprolactone, then cool down to 100°C and discharge, after cooling A caprolactone-tung oil copolyol polymer is obtained. The hydroxyl value determined by end group titration: OH=17.53mgKOH / g, the corresponding number average molecular weight M n =6400.

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Abstract

The invention discloses a caprolactone-tung oil copolymerized polyol polymer and a synthesis method thereof, and belongs to the field of macromolecular synthesis. According to the method, a mass polymerization one-step method is adopted, low molecular weight tung oil polyol prepared from diethanol amine and tung oil by aminolysis reaction and caprolactone are used as polymerizing monomers, and stannous octoate is used as a polymerization catalyst, and the caprolactone-tung oil copolymerized polyol polymer of which the molecular weight is 0.2*10<4> to 1.1*10<4> is synthesized by changing the molar ratio of the caprolactone to the tung oil under protection of an inert gas (N2) at the temperature of 150-170 DEG C. The caprolactone-tung oil copolymerized polyol polymer can be used as a novel polyester to be widely applied to preparation of polymers and copolymers.

Description

technical field [0001] The invention relates to a novel caprolactone-tung oil copolyol polymer and a synthesis method thereof, belonging to the field of macromolecule chemical synthesis. Background technique [0002] Polycaprolactone (PCL, polycaprolactone) is a polymer with excellent performance. It has attracted extensive attention because of its superior biodegradability and memory, and its related research has also developed rapidly. PCL is a semi-crystalline polymer with a melting point of 59-64°C and a glass transition temperature of -60°C. Such a structure makes PCL have good flexibility and processability, and the product with the original shape can be restored to the original shape after being deformed and fixed by means of external stimulus such as heating. On the other hand, the product of PCL degradation is CO 2 and H 2 O, non-toxic to the human body, has excellent drug passage and mechanical properties, and can be used as biomedical materials (such as in vivo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/685C08G63/78C08G18/68
Inventor 郭晓战任志勇姜垒付阳郑果尚玉俊
Owner HIGH & NEW TECH RES CENT OF HENAN ACAD OF SCI
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