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Preparation of diethylene glycol monomethyl ether monolaurate catalyzed by active carbon supported KF/CaO.

Lou S, Jia L, Guo X, Wu P, Gao L, Wang J - Springerplus (2015)

Bottom Line: Diethylene glycol monomethyl ether monolaurate (DGMEML) was synthesized via the reaction of diethylene glycol monomethyl ether (DGME) with methyl laurate (ML) by a new solid base catalyst of KF/CaO/AC, which was prepared by impregnation method using active carbon as carrier.The catalysts were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), nitrogen physisorption-desorption and Hammett indicator methods; the effect of the mole ratio of KF to CaO, DGME to ML molar ratio, amount of catalyst, reaction time and temperature on the yield of DGMEML were studied; and the relationship between the structure of the catalyst and the yield of DGMEML was investigated.The formed KCaF3 and K2O were acting as the main active components in the catalytic transesterification; the highest yield of 96.3 % was obtained as KF-to-CaO molar ratio of 2.0, DGME to ML molar ratio of 4.0, catalyst amount of 5 wt%, and reaction time of 30 min at 75 °C; and the catalyst displayed good stability in the transesterification.

View Article: PubMed Central - PubMed

Affiliation: College of Chemistry and Chemical Engineering, Key Laboratory of Fine Chemicals of College of Heilongjiang Province, Qiqihar University, Qiqihaer, 161006 China.

ABSTRACT
Diethylene glycol monomethyl ether monolaurate (DGMEML) was synthesized via the reaction of diethylene glycol monomethyl ether (DGME) with methyl laurate (ML) by a new solid base catalyst of KF/CaO/AC, which was prepared by impregnation method using active carbon as carrier. The catalysts were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), nitrogen physisorption-desorption and Hammett indicator methods; the effect of the mole ratio of KF to CaO, DGME to ML molar ratio, amount of catalyst, reaction time and temperature on the yield of DGMEML were studied; and the relationship between the structure of the catalyst and the yield of DGMEML was investigated. The formed KCaF3 and K2O were acting as the main active components in the catalytic transesterification; the highest yield of 96.3 % was obtained as KF-to-CaO molar ratio of 2.0, DGME to ML molar ratio of 4.0, catalyst amount of 5 wt%, and reaction time of 30 min at 75 °C; and the catalyst displayed good stability in the transesterification.

No MeSH data available.


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FT-IR (A) and XRD (B) patterns of fresh catalyst (a), catalyst used and unwashed (b) and catalyst used and washed (c)
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Fig5: FT-IR (A) and XRD (B) patterns of fresh catalyst (a), catalyst used and unwashed (b) and catalyst used and washed (c)

Mentions: After transesterification under the optimal conditions, centrifugation and decantation was successively used to separate the catalyst from the mixture, and the catalyst was kept in the flask and directly used in the next round of reactions. It is noted that DGMEML yield of 80 % were obtained as the KCC-2.0 used in the next reaction. While KCC-2.0 used once and washed by acetone, the yield of DGMEML was 89 %. It can be found from Fig. 5A, all the characteristic absorption bands of the used catalyst are the same with that of fresh catalyst. However, unwashed catalyst appeared three new bands, the new peaks at 2850 and 2920 cm−1 attributed to the present of C-H stretching vibrations(Li et al. 2015), and absorption peak at 1740 cm−1 belongs to the C=O stretching vibration. After the catalyst washed by acetone, the absorption peaks at 2920, 2860 and 1740 cm−1 disappeared. It indicates the surface of the used catalyst was covered by the organic oligomer produced in the reaction process, which resulted in the decrease of the activity of the used KCC-2.0. XRD patterns of used KCC catalysts are shown in Fig. 5B. It can be seen that the intensity of KCaF3 characteristic peaks decreased when the catalyst used and washed by acetone. The characteristic peak of K2O was disappeared. So, the decrease of catalytic activity may due to the loss of the active compound on the surface, which may run off during the recycle process.Fig. 5


Preparation of diethylene glycol monomethyl ether monolaurate catalyzed by active carbon supported KF/CaO.

Lou S, Jia L, Guo X, Wu P, Gao L, Wang J - Springerplus (2015)

FT-IR (A) and XRD (B) patterns of fresh catalyst (a), catalyst used and unwashed (b) and catalyst used and washed (c)
© Copyright Policy - OpenAccess
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC4641147&req=5

Fig5: FT-IR (A) and XRD (B) patterns of fresh catalyst (a), catalyst used and unwashed (b) and catalyst used and washed (c)
Mentions: After transesterification under the optimal conditions, centrifugation and decantation was successively used to separate the catalyst from the mixture, and the catalyst was kept in the flask and directly used in the next round of reactions. It is noted that DGMEML yield of 80 % were obtained as the KCC-2.0 used in the next reaction. While KCC-2.0 used once and washed by acetone, the yield of DGMEML was 89 %. It can be found from Fig. 5A, all the characteristic absorption bands of the used catalyst are the same with that of fresh catalyst. However, unwashed catalyst appeared three new bands, the new peaks at 2850 and 2920 cm−1 attributed to the present of C-H stretching vibrations(Li et al. 2015), and absorption peak at 1740 cm−1 belongs to the C=O stretching vibration. After the catalyst washed by acetone, the absorption peaks at 2920, 2860 and 1740 cm−1 disappeared. It indicates the surface of the used catalyst was covered by the organic oligomer produced in the reaction process, which resulted in the decrease of the activity of the used KCC-2.0. XRD patterns of used KCC catalysts are shown in Fig. 5B. It can be seen that the intensity of KCaF3 characteristic peaks decreased when the catalyst used and washed by acetone. The characteristic peak of K2O was disappeared. So, the decrease of catalytic activity may due to the loss of the active compound on the surface, which may run off during the recycle process.Fig. 5

Bottom Line: Diethylene glycol monomethyl ether monolaurate (DGMEML) was synthesized via the reaction of diethylene glycol monomethyl ether (DGME) with methyl laurate (ML) by a new solid base catalyst of KF/CaO/AC, which was prepared by impregnation method using active carbon as carrier.The catalysts were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), nitrogen physisorption-desorption and Hammett indicator methods; the effect of the mole ratio of KF to CaO, DGME to ML molar ratio, amount of catalyst, reaction time and temperature on the yield of DGMEML were studied; and the relationship between the structure of the catalyst and the yield of DGMEML was investigated.The formed KCaF3 and K2O were acting as the main active components in the catalytic transesterification; the highest yield of 96.3 % was obtained as KF-to-CaO molar ratio of 2.0, DGME to ML molar ratio of 4.0, catalyst amount of 5 wt%, and reaction time of 30 min at 75 °C; and the catalyst displayed good stability in the transesterification.

View Article: PubMed Central - PubMed

Affiliation: College of Chemistry and Chemical Engineering, Key Laboratory of Fine Chemicals of College of Heilongjiang Province, Qiqihar University, Qiqihaer, 161006 China.

ABSTRACT
Diethylene glycol monomethyl ether monolaurate (DGMEML) was synthesized via the reaction of diethylene glycol monomethyl ether (DGME) with methyl laurate (ML) by a new solid base catalyst of KF/CaO/AC, which was prepared by impregnation method using active carbon as carrier. The catalysts were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), nitrogen physisorption-desorption and Hammett indicator methods; the effect of the mole ratio of KF to CaO, DGME to ML molar ratio, amount of catalyst, reaction time and temperature on the yield of DGMEML were studied; and the relationship between the structure of the catalyst and the yield of DGMEML was investigated. The formed KCaF3 and K2O were acting as the main active components in the catalytic transesterification; the highest yield of 96.3 % was obtained as KF-to-CaO molar ratio of 2.0, DGME to ML molar ratio of 4.0, catalyst amount of 5 wt%, and reaction time of 30 min at 75 °C; and the catalyst displayed good stability in the transesterification.

No MeSH data available.


Related in: MedlinePlus