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Metallic alkoxy complex, catalyst composition and preparation method of poly-caprolactone or poly-lactide

A technology of metal alkoxy and complexes, applied in metal/metal oxide/metal hydroxide catalysts, preparation of organic compounds, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of polylactide Low molecular weight, wide molecular weight distribution, and uncontrollable molecular weight of polyε-caprolactone, etc., to achieve high catalytic activity, reduced dosage, and high catalytic efficiency

Active Publication Date: 2012-06-13
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the Chinese patent document with application number 01114244.8 discloses a method for preparing polyε-caprolactone using stannous octoate as a catalyst, but the molecular weight of polyε-caprolactone obtained by catalysis of stannous octoate is uncontrollable and the molecular weight distribution wide; application number is 200610016623.3 Chinese patent discloses a kind of preparation method and the application method of the Schiff base aluminum catalyst for lactide ring-opening polymerization, but the catalytic activity of Schiff base aluminum is low, the polylactide finally obtained lower molecular weight

Method used

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  • Metallic alkoxy complex, catalyst composition and preparation method of poly-caprolactone or poly-lactide
  • Metallic alkoxy complex, catalyst composition and preparation method of poly-caprolactone or poly-lactide
  • Metallic alkoxy complex, catalyst composition and preparation method of poly-caprolactone or poly-lactide

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preparation example Construction

[0061] The present invention also provides the preparation method of polyε-caprolactone and polylactide, comprising the following steps:

[0062] The ε-caprolactone monomer or lactide monomer reacts under the action of a catalyst to obtain poly ε-caprolactone or polylactide, and the catalyst is the metal alkoxy complex or A catalyst composition composed of a metal alkoxy complex and a compound containing a hydroxyl group.

[0063] The molar ratio of the metal alkoxy complex to the ε-caprolactone monomer or lactide monomer in the catalyst is 1:1-10000, preferably 1:1000-9000.

[0064] The polymerization reaction time of ε-caprolactone monomer or lactide monomer is preferably 0.03h~24h, more preferably 0.5h~20h, most preferably 3h~10h; ε-caprolactone monomer or lactide The temperature of monomer polymerization reaction is preferably 10°C to 130°C, more preferably 25°C to 100°C.

[0065] Since metal alkoxy complexes are sensitive to oxygen and water, the reaction is preferably ...

Embodiment 1

[0070] Embodiment 1 prepares metal alkoxy complexes A1~A9

[0071] Under anhydrous and oxygen-free conditions, slowly drop 10mL of toluene solution containing benzyl alcohol into the toluene solution containing calcium chloride, wherein the content of benzyl alcohol is 0.22g (2mmol), and the content of calcium chloride is 0.11g (1mmol); Add 0.017g elemental iodine, reflux reaction 24h, reaction formula is as follows:

[0072]

[0073] The reaction mixture was cooled and filtered to obtain 0.25 g of white solid complex A1 with a yield of 76%.

[0074] The complex A1 was subjected to elemental analysis, and its molecular formula was C 14 h 12 CaO 2 , molecular weight 252.32: C, 66.64; H, 4.79; Ca, 15.88; O, 12.68.

[0075] The preparation method of complexes A2~A9 is the same as that of A1, the difference is that methanol, ethanol, isopropanol, n-butanol, tert-butanol, phenol, diphenylmethanol and triphenylmethanol are reacted with calcium chloride in sequence , were obt...

Embodiment 2

[0084] Example 2 Preparation of metal alkoxy complexes A10-A18

[0085] Under anhydrous and oxygen-free conditions, 10 mL of toluene solution containing benzyl alcohol is slowly added dropwise to the toluene solution containing bistrimethylsilylamide magnesium, wherein the content of benzyl alcohol is 0.22 g (2 mmol), bistrimethylsilylamide The content of magnesium methylsilylamide is 0.11g (1mmol); 0.017g elemental iodine is added, and the reflux reaction is carried out for 24h. The reaction formula is as follows:

[0086]

[0087] The reaction mixture was cooled and filtered to obtain 0.38 g of white solid complex A10 with a yield of 90%.

[0088] The complex A10 was subjected to elemental analysis, and its molecular formula was C 14 h 12 MgO 2 , with a molecular weight of 236.5: C, 71.08; H, 5.11; Mg, 10.27; O, 13.53.

[0089] The preparation method of complexes A11~A18 is the same as that of A10, the difference is that methanol, ethanol, isopropanol, n-butanol, tert...

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Abstract

The invention provides a metallic alkoxy complex of which the molecular formula is disclosed as Formula (I). The invention also provides a catalyst composition which comprises the metallic alkoxy complex and a hydroxy compound, wherein the mol ratio of the metallic alkoxy complex to the hydroxy compound is 1:(0.1-1000). The preparation method of the poly-epsilon-caprolactone or poly-actide comprises the following steps: reacting an epsilon-caprolactone monomer or lactide monomer under the action of the metallic alkoxy complex or the catalyst composition to obtain poly-epsilon-caprolactone or poly-actide. The metallic alkoxy complex and the catalyst composition thereof can efficiently catalyze the synthesis of the poly-epsilon-caprolactone or poly-actide. The molecular weight of the poly-caprolactone or poly-actide can be controlled by the mol ratio of the metallic alkoxy complex to the hydroxy compound, and can be adjusted within the range of 1-600 thousand, and the molecular weight distribution ranges from 1.03 to 1.50.

Description

technical field [0001] The invention relates to the field of catalysts, in particular to a metal alkoxy complex, a catalyst composition and a preparation method of polycaprolactone or polylactide. Background technique [0002] Polyε-caprolactone (PCL) and polylactide (PLA) are polyester biodegradable materials with excellent biodegradability, so they are widely used to make disposable containers, tableware, films, fibers, clothing and auto parts, which is conducive to solving the environmental pollution problems caused by petrochemical resources. In addition, PCL and PLA also have the characteristics of good biocompatibility, non-toxicity and degradation adjustability, which meet the requirements of medical polymer materials. Controlled-release carrier materials and other aspects have application prospects. [0003] The synthesis of early polyester was mainly based on the condensation reaction of acids and alcohols, but the structure of the polymer synthesized by this reac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/70C07C33/22C07C31/28C07C33/24C07C39/235C07C37/66C08G63/87C08G63/83C08G63/84C08G63/08
CPCC08G63/823C07C33/22C07C33/24C07C29/70B01J21/00B01J23/00C08G63/82C08G63/08C07C31/28B01J31/0212B01J2231/14B01J2531/22C07C31/30C07F3/04C07F5/069C08G63/826C08G63/83C08G63/84C08G63/85
Inventor 崔冬梅王洋
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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