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Issue 02/2018

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from Science and research A big step toward 100% biobased By: YanBo Long, Director R&D JinHui Zhaolong Shanxi province, China Biobased materials are currently attracting much positive attention across an increasing number of industries. As a leading company in the biodegradable plastics industry, JinHui ZhaoLong, based in Shanxi province, China and a manufacturer of 20,000 tonnes of PBAT per year, has actively worked to promote the development of biodegradable plastic materials. The company’s biodegradable resins, marketed under the brand names Ecoworld ® and Ecowill ® have been well received in the market, with positive reports from satisfied users. On that basis, JinHui ZhaoLong completed the laboratory development of 20 % and 40 % good quality biobased and fully biodegradable resins in their Ecoworld series products and successfully started pilot production of 500 tonnes/year. Now, they are actively preparing to scale up production. Recently, the company achieved a further breakthrough in the research on increasing the biobased content in its biodegradable resin. The company has successfully synthesized a 100 % biobased and biodegradable PBSF resin with higher molecular weight using 1,4 butanediol (BDO), succinic acid (SA) and 2,5-furandicarboxylic acid (FDCA). The research and development results are presented in the following: Experimental material Biobased 2,5 furandicarboxylic acid, biobased succinic acid, biobased butanediol, biobased glycerol, selfsynthetisized hydrolysis-resistant titanium catalyst A, selfsynthesized compound organic titanium catalyst B. Synthetic method In this experiment, PBSF was synthesized by melting polycondensation. The overall reaction process is mainly divided into two steps: Esterification reaction Due to the poor thermal stability of FDCA, thermal decomposition occurs at about 190 °C. Succinic acid tends to sublime above 190 °C, owing to its low melting point. Therefore, the reaction temperature need to be controlled at 160-170 °C. The molar ratio of alcohol to acid is 1.4-1.6:1; self-synthetic catalyst A is added according to the total mass of the ester 200-400ppm, and FDCA and SA react with BDO respectively, yielding the esterification reaction, which requires a fractionating tower to dehydrate the generated moisture. The recommended pressure within the tower is 70-80kpa, which is more conducive to the forward reaction. Table 1 shows the results of the esterification reaction with different molar ratios of FDCA, SA and BDO under different esterification reaction times. The results show that the higher the FDCA content, the more difficult the esterification reaction. It should be noted that the acidic property in furandicarboxylic acid is strong, PKa = 2.28. It is not readily soluble in BDO. If the furandicarboxylic acid content is high, it is easy to catalyze BDO. However, some side effects Table 1: results of the esterification reaction Test No. Molar ratios of FDCA to SA Ratio of alcohol to acid Esterification temperature Esterification time Esterification rate 1 1:4 1.4 165°C 6h 95.3% 2 1:4 1.4 165°C 5h 94.1% 3 1:1.5 1.4 165°C 5h 90.6% 4 4:1 1.6 165°C 6h 85.1% Table 2: The results show that all the polymer molecular weight distribution is ideal and the degree of polymerization is ideal if the polymer’s molar ratio of FDCA to SA is 1: 4, as it then basically meets the requirements of blow molding or spinning. As the FDCA content rises, the more difficult polymerization becomes, and the longer it takes to reach the end of the aggregation. Sample Serial Molar ratio of FDCA to SA Mn·10 4 (g/mol) Mw·10 4 (g/mol) PDI 1 1:4 8.03 12.01 1.47 2 1:1.5 5.61 8.22 1.59 3 1.5:1 5.91 8.79 1.51 4 4:1 4.01 5.63 1.67 36 bioplastics MAGAZINE [02/18] Vol. 13

from Science and research and biodegradable polyesters may occur and a large amount of tetrahydrofuran can be generated. The polycondensation reaction can be carried out at an esterification rate is at least 95 %. Polycondensation In vacuum conditions

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