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Preparation method of aliphatic polycarbonate polyol

A polycarbonate, aliphatic technology, applied in the field of high molecular polymers, can solve the problem of low carbonate content

Inactive Publication Date: 2012-10-17
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Aiming at the problem of low carbonate content in the structure, the Chinese patent application publication number CN102149746A discloses a method for synthesizing aliphatic polycarbonate polyols using Schiff base complexes to catalyze carbon dioxide and epoxides, which can prepare high carbonic acid Polycarbonate polyol with ester content, but the polymerization by-product, cyclic carbonate, has a high content of about 5%

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  • Preparation method of aliphatic polycarbonate polyol
  • Preparation method of aliphatic polycarbonate polyol
  • Preparation method of aliphatic polycarbonate polyol

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[0026] The embodiment of the present invention discloses a kind of preparation method of aliphatic polycarbonate polyol, comprising the following steps:

[0027] Copolymerize carbon dioxide and propylene oxide under the action of metal porphyrin complexes and chain transfer agents to obtain aliphatic polycarbonate polyols;

[0028] The metalloporphyrin complex is shown in formula (I) or formula (II):

[0029]

[0030] Wherein, M is cobalt, chromium, aluminum, titanium, zinc, magnesium, manganese or iron;

[0031] X is halogen, -NO 3 、CH 3 COO-, CCl 3 COO-, CF 3 COO-, ClO 4 -, BF 4 -, BPh 4 -, -CN, -N 3 Or a group with a structure of formula (1)~(12), preferably chlorine;

[0032]

[0033] R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 , R 10 , R 11 , R 12 , R 13 , R 14 , R 15 , R 16 , R 17 , R 18 , R 19 and R 20each independently selected from hydrogen, halogen, hydrocarbyl, heterohydrocarbyl, aryl, heteroaryl or a substituent represente...

Embodiment 1

[0067] After dissolving 3.23g of p-bromomethylbenzaldehyde in 1800ml of chloroform, 1.088g of pyrrole was added. Add 0.6721ml boron trifluoride-ether complex (BF 3 / OEt 2 ) After reacting for 1 hour, 2.76 g of dichlorodicyanobenzoquinone was quickly added, and the reaction was continued for 1 hour. The solvent was removed under reduced pressure, and the obtained solid was washed with methanol until the filtrate was colorless, and the intermediate product 1 was obtained with a yield of about 51%.

[0068] Dissolve 1.4g of γ-chloropropylmethyldimethoxysilane (TBD) and 0.96g of sodium hydride in 30ml of tetrahydrofuran at room temperature, slowly add 30ml of tetrahydrofuran solution containing 7.89g of the intermediate product 1, dropwise After reacting for 48 hours, it was filtered, and the filtrate was vacuum-dried, and the resulting solid was separated by silica gel column chromatography to obtain 6.04 g of purple solid, with a yield of about 62%. High-resolution electrospray...

Embodiment 2

[0072] After dissolving 3.23g of p-bromomethylbenzaldehyde in 1800ml of chloroform, 1.088g of pyrrole was added. Add 0.6721ml boron trifluoride-ether complex (BF 3 / OEt 2 ) After reacting for 1 hour, 2.76 g of dichlorodicyanobenzoquinone was quickly added, and the reaction was continued for 1 hour. The solvent was removed under reduced pressure, and the obtained solid was washed with methanol until the filtrate was colorless, and an intermediate product was obtained with a yield of about 51%.

[0073] Dissolve 1.4g of γ-chloropropylmethyldimethoxysilane (TBD) and 0.96g of sodium hydride in 30ml of tetrahydrofuran at room temperature, slowly add 30ml of tetrahydrofuran solution containing 7.89g of the intermediate product, after the dropwise addition After reacting for 48 hours, it was filtered, and the filtrate was vacuum-dried. The resulting solid was separated by silica gel column chromatography to obtain 6.04 g of purple solid, with a yield of about 62%. High-resolution el...

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Abstract

The invention provides a preparation method of aliphatic polycarbonate polyol. The preparation method comprises the following steps: carrying out copolymerization on carbon dioxide and an epoxy compound in the presence of a metalloporphyrin complex and a chain transfer agent to obtain aliphatic polycarbonate polyol, wherein the metalloporphyrin complex is as shown in a formula (I) or a formula (II), the quaternary ammonium salt, the quaternary phosphorus salt or the organic base group with great steric hindrance of the metalloporphyrin complex ensure that an electronic environment of ligand is more conducive to the stabilization of a metal active center, and after the metalloporphyrin complex and the chain transfer agent jointly act on the copolymerization, the content of the obtained by-product cyclic carbonate is low. Experimental results show that the content of the cyclic carbonate in the aliphatic polycarbonate polyol prepared by the preparation method is lower than 3%; and in addition, the content of carbonate in polycarbonate polyol prepared by the preparation method is as high as 85%-98%.

Description

technical field [0001] The invention relates to the field of high molecular polymers, in particular to a preparation method of aliphatic polycarbonate polyols. Background technique [0002] Aliphatic polycarbonate polyol refers to a class of polymers that contain repeated carbonate groups and aliphatic alkylene groups in the main chain of the molecule, and the ends of the molecular chain are hydroxyl groups. It is similar to aliphatic polyester polyols and polyether polyols, and is widely used in the fields of synthetic leather, adhesives and coatings. Its important downstream products, polyurethane materials, have excellent performance and various varieties, and are widely used in construction, chemical industry, electromechanical, metallurgy, medical and health fields. Compared with polyurethanes synthesized from polyester polyols and polyether polyols, polycarbonate polyurethanes prepared from polycarbonate polyols have better heat resistance, water resistance, antibacte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/34C08G64/02C08G18/44
Inventor 秦玉升付双滨王献红王佛松
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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