Ortho-coumaric acid-ltbh complex and its synthesis method
A synthesis method and technology of o-coumaric acid, applied in the field of o-coumaric acid-LTbH complex and its synthesis, can solve the problems of low content and rare analysis reports
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[0033] The synthetic method of above-mentioned o-coumaric acid-LTbH complex can comprise the following steps:
[0034] 1) Synthesis of Cl-LTbH:
[0035] Tb(NO 3 ) 3 ·6H 2 O, NaCl, and hexamethylenetetramine were dissolved in water to obtain an aqueous solution, wherein Tb(NO 3 ) 3 ·6H 2 The mol ratio of O, NaCl, hexamethylenetetramine is: 1: (10-15): (0.5-1.5); Preferably Tb (NO 3 ) 3 ·6H 2 O, NaCl, and hexamethylenetetramine are dissolved in degassed water. Degassed water refers to water that removes the dissolved gas in the water. It can be obtained by boiling distilled water for 10 minutes. The amount of degassed water is preferably 60-120mL / mmolTb (NO 3 ) 3 ·6H 2 O.
[0036] Nitrogen was passed into the above aqueous solution 2 , into N 2 The time is preferably 3-10min, and then the hydrothermal reaction is carried out, the preferred reaction temperature is 70-100°C; the preferred reaction time is 12-18h, after the reaction is completed, filter the obtained pr...
Embodiment 1
[0047] 0.453g (1mmol) Tb (NO 3 ) 3 ·6H 2 O, 0.585g (10mmol) NaCl, 0.07g (0.5mmol) hexamethylenetetramine were dissolved in 65mL degassed water to obtain an aqueous solution, which was transferred to the reaction kettle and passed into the aqueous solution with N 2 3min, then hydrothermal reaction at 70°C for 18 hours. After the reaction, the obtained product was filtered by suction, washed with deionized water and then filtered by suction, repeated twice, and then vacuum-dried at 40°C for 24 hours to obtain 0.210 g of white powder Cl-LTbH with a yield of 90 %.
[0048] 0.103 g (0.63 mmol) of o-coumaric acid and 0.025 g (0.63 mmol) of NaOH were added to 8 mL of deionized water, and ultrasonically dissolved the o-coumaric acid to obtain a clear aqueous solution of o-coumaric acid sodium salt.
[0049] Disperse 0.05g (0.21mmol) of Cl-LTbH in 70mL of deionized water, mix it with the above-prepared aqueous solution of sodium p-coumaric acid, transfer it to a reaction kettle, an...
Embodiment 2
[0051] 0.453g (1mmol) Tb (NO 3 ) 3 ·6H 2 O, 0.761g (13mmol) NaCl, 0.14g (1mmol) hexamethylenetetramine are dissolved in 80mL exhaust water, obtain aqueous solution, this aqueous solution is transferred in the reactor and feeds N into this aqueous solution 2 5min, then 90°C hydrothermal reaction for 14 hours. After the reaction, the obtained product was filtered with suction, washed with deionized water and then filtered with suction, repeated 3 times, and then vacuum-dried at 60°C for 20 hours to obtain 0.221g of white powder Cl-LTbH with a yield of 95%. .
[0052] Add 0.207g (1.26mmol) of o-coumaric acid and 0.040g (1.0mmol) of NaOH into 5mL of deionized water, and ultrasonically dissolve the o-coumaric acid to obtain a clear aqueous solution of o-coumaric acid sodium salt.
[0053] Disperse 0.075g (0.32mmol) of Cl-LTbH in 80mL of deionized water and mix it with the above-prepared aqueous solution of sodium o-coumaric acid salt, transfer it to a reaction kettle, and condu...
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