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Catalyst/initiator system

A technology of initiation system and initiator, which is applied in the field of catalytic initiation system for the synthesis of polyester polymer materials, can solve the problems of low reaction conversion rate, high catalyst dosage, low product molecular weight, etc., and achieves high activity, wide operating space, Strong controllable effect

Active Publication Date: 2012-10-10
HUIZHOU HUAYANG MEDICAL EQUIP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0023] In order to solve at least one of the technical problems such as high catalyst consumption, low reaction conversion rate, low product molecular weight, poor thermal stability, and poor material uniformity used in the synthesis process of polyester polymer materials in the prior art, the present invention provides a Catalytic initiation system, the catalytic initiation system includes three components of main catalyst, initiator and co-initiator

Method used

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  • Catalyst/initiator system

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0132] Embodiment 1: Preparation of 90 / 10 glycolide / L-lactide copolymer

[0133] Catalyst preparation: the molar ratio of stannous octoate / benzyl alcohol / tri-p-hydroxyphenylphosphine is 1 / 15.0 / 1.5, with stannous octoate as the nominal name and toluene as the solvent to prepare a catalyst solution with a concentration of 0.012 moles / liter .

[0134] Accurately weigh 2088 grams of glycolide with a melting range of 82.0 to 82.5°C and 288 grams of L-lactide with a melting range of 95.5 to 96.1°C, add them to the reaction vessel, and then add 8.33ml of the prepared catalyst solution, that is, single The molar ratio of body / catalyst was 200,000.

[0135] At room temperature, absolute vacuum pressure ≤ 0.1mmHg, vacuumize for 24 hours to remove toluene solvent. Fill with high-purity nitrogen (99.999%) to keep the pressure at 0.035-0.050MPa. Raise the temperature to 98.0-105°C, stir for 1 hour, then raise the temperature to 205°C at a heating rate of 13-15°C / 10 minutes, and react fo...

Embodiment 2

[0153] Embodiment two: preparation 90 / 10 glycolide / L-lactide copolymer

[0154] Catalyst preparation: The molar ratio of triethylaluminum / dodecyl alcohol / 2,4,6-collidine is 1 / 10.0 / 2.5, with triethylaluminum as the nominal, toluene as the solvent, and the prepared concentration 0.0048 mol / L catalyst solution.

[0155] Accurately weigh 1044 grams of glycolide (melting range: 82.0-82.5°C) and 144 grams of L-lactide (melting range: 95.5-96.1°C) into the reaction vessel, then add 20.83ml of the prepared catalyst solution, The monomer / catalyst molar ratio was 100,000. At room temperature, absolute vacuum pressure ≤ 0.1mmHg, vacuumize for 24 hours to remove toluene solvent. Fill with high-purity nitrogen (99.999%) to keep the pressure at 0.035-0.050MPa. Raise the temperature to 98.0-105°C, stir for 1 hour, then raise the temperature to 185°C at 13-15°C / 10 minutes, and react for 12 hours. Stop the reaction, cool to room temperature, take out the material, crush it, and put the cru...

Embodiment 3

[0163] Embodiment three: prepare the copolymer of 15 / 85 glycolide / DL-lactide

[0164] Catalyst preparation: according to the molar ratio of lanthanum isopropoxide / benzyl alcohol / triisobutylphosphine as 1.0 / 15.0 / 1.0, with lanthanum isopropoxide as the nominal and toluene as the solvent, prepare a catalyst solution with a concentration of 0.01 mol / liter .

[0165] Accurately weigh 52.2 grams of glycolide (melting range: 82.0-82.5°C) and 367.2 grams of DL-lactide (melting range: 123.4-124.1°C) into the reaction vessel, then add 6.0ml of the prepared catalyst solution, The monomer / catalyst molar ratio was 50,000. At room temperature, absolute vacuum pressure ≤ 0.1mmHg, vacuumize for 24 hours to remove toluene solvent. Fill with high-purity nitrogen (99.999%) to keep the pressure at 0.035-0.050MPa. Raise the temperature to 128.0-135.0°C, stir for 1 hour, then raise the temperature to 165°C at 13-15°C / 10 minutes, and react for 15 hours. Stop the reaction, cool to room temperatur...

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Abstract

The invention provides a catalyst / initiator system, which comprise a primary catalyst, an initiator and a coinitiator, wherein the primary catalyst is at least one organic metal compound MeXn, wherein Me may be aluminum (Al), gallium (Ga), stannum (Sn), lead (Pb), zinc (Zn), cadmium (Cd) or one transition element; and X may be alkyl, alkoxy, cycloalkyl, cycloalkyloxy, aryl, aryloxy, carboxyl, alkoxycarbonyl, cycloalkyloxycarbonyl or aryloxycarbonyl. The initiator may be at least one matter containing active hydroxyl. The coinitiator may be one or more of a nitrogen-containing ligand matter, asulfur-containing ligand matter, a phosphorus-containing ligand matter, arsenic triphenyl (Ph3As), antimony trioxide (Ph3Sb) and triphenylbismuth (Ph3Bi). The catalyst / initiator system of the invention can be used for synthesizing polyester polymer materials, has high activity and effectiveness and improves the controllability of a reaction.

Description

[0001] This application is a divisional application of the Chinese invention patent application with the application number 200710030498.6, the application date of September 19, 2007, and the title of the invention "a preparation method of polylactide". technical field [0002] The invention relates to a catalytic initiation system, in particular to a catalytic initiation system for synthesizing polyester polymer materials. Background technique [0003] Polyglycolide, which is prepared by ring-opening copolymerization of glycolide and lactide (L-lactide or / and DL-lactide) monomers, not only has good biodegradability, biocompatibility, It is widely used in the field of biomedical materials such as surgical sutures, internal fixation of fractures, tissue repair, plastic surgery, anti-tissue adhesion, drug sustained release, tissue engineering, etc. [0004] There are currently two ways for the copolymerization of polylactide, one is to use glycolic acid (glycolic acid), lactic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/85C08G63/08
Inventor 潘高峰孟永刚
Owner HUIZHOU HUAYANG MEDICAL EQUIP