Preparation process of polyester carbonate with high molecular weight whole alternant structure

A polycarbonate, alternating structure technology, applied in the field of polymer materials, can solve the problems of long reaction time, low carbonate units, low catalyst activity, etc., and achieve high selectivity of polymerization products, mild reaction conditions, and high catalyst activity. Effect

Inactive Publication Date: 2005-01-05
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Japanese published patents JP 02142824 and JP 02575199 use expensive porphyrin complexes to catalyze carbon dioxide and alkylene oxides to synthesize polycarbonate, with a catalytic efficiency of 10 3 ~10 4 gram of polymer/mole of catalyst, but the molecular weight of the polymer is only about 5000, and the reaction time needs more than 10 days
Chinese patent application numbers CN 89100701.6 and CN 91109459.8 disclose a bimetallic catalyst system supported by polymers with anion coordination, and can also obtain 10 4 Catalytic efficiency in grams of polymer per mole of catalyst, but the support is difficult to separate from the resulting polycarbonate
In U.S. Patent US 6133402 and J.Am.Chem.Soc., (2002, 124, 14284), Coates

Method used

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  • Preparation process of polyester carbonate with high molecular weight whole alternant structure
  • Preparation process of polyester carbonate with high molecular weight whole alternant structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a stainless steel autoclave with an effective volume of 200ml, add in the following order at ambient temperature: 0.5×10 -3 mole SalenCoX(R 1 = R 2 =t-Bu,R 3 , R 4 Yes-(CH 2 ) 4 -, X is 2,4-dinitrophenol oxyanion), 0.5×10 -3Mole of tetra-n-butylammonium iodide, 1 mole of propylene oxide, and then pass through carbon dioxide gas and maintain a constant pressure of 2.0MPa. Control the temperature at 25°C, react under magnetic stirring for 4 hours, slowly release unreacted carbon dioxide in the autoclave, collect unreacted propylene oxide in a cold trap at -20°C under low pressure, and then add a certain amount of methanol / chloroform The mixture dissolves the polymer, and then a large amount of ether is added to precipitate polycarbonate. It was filtered, washed several times with ether, and dried in vacuo to constant weight to obtain 38 g of polypropylene carbonate as a white solid. The average molecular weight of this polymer measured by gel permeation chromat...

Embodiment 2

[0027] In the same apparatus as used in Example 1, under the same conditions, only tetra-n-butylammonium bromide was used instead of tetra-n-butylammonium iodide. After reacting at 25° C. for 4 hours, 41 grams of polypropylene carbonate was obtained with a molecular weight of 32,000 and a molecular weight distribution of 1.53, and the carbonate units in the polymer exceeded 99%.

Embodiment 3

[0029] In the same apparatus as used in Example 1, under the same conditions, only tetra-n-butylammonium chloride was used instead of tetra-n-butylammonium iodide. After reacting at 25° C. for 4 hours, 34 g of polypropylene carbonate was obtained, the molecular weight was 32300, the molecular weight distribution was 1.55, and the carbonate units in the polymer exceeded 99%.

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PUM

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Abstract

The invention is a method of preparing high-molecular weight fully alternative structural polycarbonate, providing a method of preparing high-molecular weight, highly alternative structural plycarbonate by using two-component catalyst to selectively catalyze epoxy alkane and carbon dioxide to react at low pressure or medium pressure. The two-component catalyst is composed of a primary catalyst tetradentate Schiff alkali metal complex (R1)(R2)SalenMX and an aid-catalyst R1R23YX1 salt, where R1 and R2 in (R1)(R2)SalenMX are -H, C1-C6 alkyls, C1-C6 alkoxys, -Cl,-Br or -NO2; M is trivalent metallic cation; X is monovalent anion; R1 and R2 in the salt are alkyls, Y is family-five element and X1 is monovalent anion. The molar ration of the primary catalyst to the aid-catalyst is 0.2-5 : 1. The catalytic efficiency reaches 10 to the power 5 g polymer/mol catalyst, the molecular weight of the polymer is over 30000, the molecular weight distribution is less than 2, the alternative structure is over 99%. The method has moderate reacting conditions, and simple operation; the used catalyst is simple to synthesize, low-cost, high-activity, and suitable for industrialized application.

Description

technical field [0001] The invention belongs to the technical field of polymer materials. The invention relates to a method for preparing high-molecular-weight polycarbonate with complete alternating structure, which is efficient, simple and has relatively mild reaction conditions. Background technique [0002] Carbon dioxide is the main gas that causes the greenhouse effect, and it is also one of the most abundant carbon sources on earth. The chemical fixation of carbon dioxide is an important research field of green chemistry. Among them, a main direction of utilizing carbon dioxide is to prepare polycarbonate by copolymerizing it with alkylene oxide under the action of a catalyst. The high polymer can be photodegraded and biodegraded; meanwhile, it has excellent performance of blocking oxygen and water. Therefore, polycarbonate can be used as engineering plastics, biodegradable non-polluting materials, disposable medical and food packaging materials, adhesives, and com...

Claims

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Application Information

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IPC IPC(8): C08G64/34
Inventor 吕小兵王翌
Owner DALIAN UNIV OF TECH
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