Polycarbonate polyol with phosphorus-containing side chain as well as preparation method and application of polycarbonate polyol

A polycarbonate and polyol technology, applied in the field of polycarbonate polyol and its preparation, can solve the problems of narrow molecular weight distribution, main chain phosphate is not resistant to hydrolysis, etc., and achieve narrow molecular weight distribution, excellent mechanical properties, and transparent color Odor free effect

Active Publication Date: 2022-04-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The polycarbonate polyol side chain containing phosphorus in the polycarbonate polyol proposed by the present invention not only realizes halogen-free flame retardancy but also can solve the problem that the main chain phosphate structure is not resistant to hydrolysis, and also has a relatively narrow molecular weight distribution, and the polyurethane prepared by it has Good mechanical properties and flame retardant properties

Method used

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  • Polycarbonate polyol with phosphorus-containing side chain as well as preparation method and application of polycarbonate polyol
  • Polycarbonate polyol with phosphorus-containing side chain as well as preparation method and application of polycarbonate polyol
  • Polycarbonate polyol with phosphorus-containing side chain as well as preparation method and application of polycarbonate polyol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Add 232g of 9,10-dihydro-9-heterooxo-10-phosphophenanthrene-10-oxide (DOPO) and 72g of glycolaldehyde into a 5L reaction kettle, add 2200g of ethanol, heat up to 70°C, reflux conditions , stirred and reacted for 10 h, cooled and discharged, filtered, washed with ethanol, and dried at 100°C under nitrogen atmosphere to obtain intermediate A.

[0045] 13CNMR (CDCl 3 ,100MHz), δppm, 58.6, 81.1, 119.9, 121.1, 121.2, 121.8, 122.0, 125.0, 127.7, 129.0, 132.8, 136.4, 136.6, 150.2.

[0046](2) Under the protection of nitrogen, 72.7g of intermediate A, 279.7g of 1,6-hexanediol, 0.41g of tetraethyl titanate, and 181.2g of dimethyl carbonate were sent into a reaction kettle with a rectification tower, and the reaction The temperature of the kettle was gradually raised to 160°C, and the transesterification reaction was carried out at atmospheric pressure for 10 hours. At the same time, the rectification temperature at the top of the tower was controlled at 64°C, and by-product...

Embodiment 2

[0049] Add 232g of 9,10-dihydro-9-heterooxo-10-phosphinephenanthrene-10-oxide (DOPO) and 88g of 3-hydroxypropionaldehyde into a 5L reactor, add 2500g of toluene, heat up to 100°C, and reflux conditions , stirred and reacted for 8h, cooled and discharged, filtered, washed with toluene, and dried at 120°C under nitrogen atmosphere to obtain intermediate A.

[0050] Under the protection of nitrogen, 87.9g of intermediate A, 253.8g of 1,5-pentanediol, 0.45g of tetrapropyl carbonate, and 261.9g of diethyl carbonate were sent into the reaction kettle with a rectification tower, and the temperature of the reaction kettle was gradually raised to 170°C, transesterification reaction at normal pressure for 9 hours, while controlling the rectification temperature at the top of the tower to 78.3°C, and extract by-products at the top of the tower. After the transesterification reaction reached the end point, the pressure was reduced to 2.4kPa, vacuum polycondensation was carried out for 42 ...

Embodiment 3

[0052] Add 232g of 9,10-dihydro-9-heterooxo-10-phosphinephenanthrene-10-oxide (DOPO) and 105g of 4-hydroxybutyraldehyde into a 5L reactor, add 2300g of xylene, heat up to 130°C, and reflux Under the conditions, the reaction was stirred for 6 hours, cooled and discharged, filtered, washed with ethanol, and dried at 100°C under nitrogen atmosphere to obtain intermediate A.

[0053] Under the protection of nitrogen, 92.9g of intermediate A, 133.2g of 1,6-hexanediol, 117.4g of 1,5-pentanediol, 0.48g of dibutyltin dilaurate, and 314.5g of dipropyl carbonate were sent to the belt rectification In the reaction kettle of the tower, the temperature of the reaction kettle was gradually raised to 180°C, and the transesterification reaction was carried out at normal pressure for 8 hours. At the same time, the rectification temperature at the top of the tower was controlled at 97.2°C, and by-products were extracted from the top of the tower. After the transesterification reaction reaches t...

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Abstract

The invention discloses polycarbonate polyol with a phosphorus-containing side chain as well as a preparation method and application of the polycarbonate polyol. The polycarbonate polyol has a structural expression shown in the specification. The preparation method of the polycarbonate polyol comprises the following steps: firstly, preparing a reaction product intermediate A of DOPO and a hydroxy aldehyde compound, and then sequentially carrying out transesterification and vacuum polycondensation reaction on the intermediate A, micromolecular polyol and diester carbonate under the action of a catalyst to obtain the polycarbonate polyol. The side chain of polycarbonate polyol contains phosphorus, halogen-free flame retardance is achieved, the problem that a main chain phosphate structure is not resistant to hydrolysis can be solved, meanwhile, the polycarbonate polyol has relatively narrow molecular weight distribution, and polyurethane prepared from the polycarbonate polyol has good mechanical performance and flame retardance.

Description

technical field [0001] The invention relates to a polycarbonate polyol, in particular to a side chain phosphorus-containing polycarbonate polyol and a preparation method and application thereof. Background technique [0002] Polycarbonate polyol is a polymer with hydroxyl groups (-OH) at both ends of the molecular chain, and the main chain of the molecule contains alkylene and carbonate group (-OCOO-) repeating units. It is widely used in synthetic leather, TPU, Adhesives, coatings and other fields. [0003] The synthesis methods of polycarbonate polyols mainly include phosgene method, cyclic carbonate ring-opening polymerization method, carbon dioxide epoxide regulated copolymerization method and transesterification method. The most common craft. However, the preparation of polycarbonate polyols by transesterification has the problems of high content of low-molecular polyols and wide molecular weight distribution in the product. This broad distribution is generally undes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/30C08G64/02C08G18/46
Inventor 崔通通刘洋秦承群张明峰
Owner WANHUA CHEM GRP CO LTD
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