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Alkoxy aluminum complex, and preparation and application thereof

A technology of aluminum alkoxide and complex, applied in the field of aluminum alkoxide complex and its preparation and application

Active Publication Date: 2014-12-24
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction of the direct polycondensation method is an equilibrium reaction. A small amount of water in the later stage of the polycondensation reaction is difficult to completely remove, and oligomers are often obtained, so it is rarely used (Xie Deliang, Jiang Biao, Yang Changzheng. Hydroxy acid triggers ε-caprolactone Research on ring-opening polymerization [J]. Acta Polymer Sinica, 2000(5): 532-537)

Method used

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  • Alkoxy aluminum complex, and preparation and application thereof
  • Alkoxy aluminum complex, and preparation and application thereof
  • Alkoxy aluminum complex, and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Compounds with general formula III (R 1 = R 2 = Ph; R 3 =Me) synthesis:

[0025] At room temperature, in the toluene or n-hexane solution containing (0.64g, 2.0mmol) compound [(2-N, N-dimethylamino-5-methylphenyl) benzhydrylmethanol with nitrogen protection, Slowly add AlMe with a syringe 3 1.5 mL (2M) of n-hexane solution. Stir and heat to reflux for 1.5h (room temperature: 6h). After cooling, the volatiles were removed under reduced pressure to obtain a white crystalline solid. Add 25mL of n-hexane, dissolve with slight heat, and then crystallize at 0°C to obtain 0.70g (95%) of colorless crystals; melting point: 182-184°C; elemental analysis (EA) measured value (theoretical value): C 77.22 (77.18 ); H 7.52(7.56); N 3.71(3.75). 1 H NMR (300.13MHz, CDCl 3 ): δ-0.18(s, 6H, AlMe 2 ), 2.05(s, 3H, ArMe), 2.33(s, 6H, NMe 2 , 6.87-7.87 (m, 13H, Ar-H).

Embodiment 2

[0027] Compounds with general formula III (R 1 = R 2 = Ph; R 3 = Synthesis of Et):

[0028] At room temperature, to the toluene or n-hexane solution containing (0.64g, 2.0mmol) compound [(2-N, N-dimethylamino)-5-methylphenyl] benzhydryl alcohol with nitrogen protection , slowly add Et with a syringe 3 Al in n-hexane solution 1.5mL (1.75M). Stir and heat to reflux for 1.5h (room temperature: 6h). After cooling, it was dried with a vacuum pump to obtain a white crystalline solid. Add 30 mL of n-hexane, dissolve with slight heat, and crystallize at 0°C to obtain 0.73 g (91%) of colorless crystals; melting point: 184-186°C. Elemental analysis (EA) found (calculated): C 77.80 (77.77); H 8.00 (8.03); N 3.52 (3.49). 1 H NMR (300.13MHz, CDCl 3 ): δ-0.02(q, 4H, 3 J H-H = 7.1Hz, CH 2Me), 1.12(t, 6H, 3 J H-H = 7.1Hz, CH 2 Me), 2.28(s, 3H, Ar-Me), 2.71(s, 6H, NMe 2 ), 6.77-7.37 (m, 13H, Ar-H). 13 C NMR (300.13MHz, C 6 D. 6 ): -1.1 (-CH 2 ), 9.63(Me), 21.1(Ar-Me), 42.7(N...

Embodiment 3

[0030] Pentacoordinate aluminum alkoxide complexes with general formula I (R=OCH 2 Ph; R 1 =R 2 =Ph) synthesis:

[0031] The toluene solution (11wt.% solution, 1.98mmol) of the benzyl alcohol of 1.94 grams is added dropwise under stirring to the compound (R 1 =R 2 = Ph; R 3 =Et) (0.40 g, 0.99 mmol) in 20 ml of toluene at -78°C (cooled with ethanol and liquid nitrogen). After reacting for one hour, remove the low-temperature bath, allow the reaction solution to rise to room temperature naturally, remove all volatile substances under reduced pressure, and recrystallize the residue with toluene to obtain 0.22 g (60%) of colorless crystals. Mp. > 285 ° C ( break down). 1 H NMR (600MHz, CDCl 3 ): δ (ppm) 2.24 (s, 3H, C-CH 3 ), 2.36(s, 3H, N-CH 3 ), 2.40 (s, 3H, N-CH 3 ), 4.50(d, 3 J H-H =14Hz, 1H, OCH 2 C 6 h 5 ), 4.76(d, 3 J H-H =14Hz, 1H, OCH 2 C 6 h 5 ), 7.00-7.50 (m, 31H, aromatic C-H). Elemental analysis (EA) found (calculated): C 79.61 (79.87); H 6.92 (6.7...

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Abstract

The invention relates to an alkoxy aluminum complex, and preparation and application thereof. The alkoxy aluminum complex has the structure disclosed as a general formula I. The preparation method comprises the following steps: thoroughly mixing a compound disclosed as a structural formula III with twice moles of alcohol, and reacting at a temperature between -78 to 25 DEG C for 10-120 minutes; and after the reaction finishes, concentrating and recrystallizing the mixture to obtain the alkoxy aluminum complex. The complex can be used as a catalyst to catalyze the ring-opening polymerization of lactone in an organic solvent to generate a poly-lactone resin; the lactone is epsilon-caprolactone or gamma-butyrolactone; the mol ratio of the catalyst to the lactone is 1:(1-5000), the reaction temperature is 25-108 DEG C, and the reaction time is 10-600 minutes; the conversion rate can reach more than 95%; and the molecular weight distribution can be controlled within 1.40.

Description

technical field [0001] The invention relates to a five-coordination alkoxy aluminum complex and its preparation and application in polylactone synthesis. Background technique [0002] Polyfatty lactones are an important class of thermoplastics and have important applications in medical materials. Especially polyε-caprolactone and polyγ-butyrolactone can also be mixed into many other plastics to modify them (X.Zhang, U.P.Wyss, D.Pichora, M.F.A.Goosen, J.Macromol R.G.Sinclair, J.Macromol.Sci.Pure Appl.Chem.A33(1996)585; A.Duda, A.Kowalski, S.Penczek, H.Uyama, S. Kobayashi. Macromolecules 35 (2002) 4266). Polyε-caprolactone (PCL) obtained by ring-opening polymerization of ε-caprolactone (ε-CL) is an example. It has high crystallinity (up to 69%) and good thermal stability, and its decomposition temperature is as high as 350 ℃. At the same time, polyε-caprolactone is easily decomposed by microorganisms or enzymes under natural conditions, and finally produces carbon dioxide ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/06C08G63/08C08G63/84
Inventor 义建军朱百春郝海军陈商涛毛静周曼溪肖勇
Owner PETROCHINA CO LTD