Hyperbranched polyphosphate amide ester as well as preparation method and application thereof

A technology of polyphosphoramidate and branching degree, which is applied in the field of preparation of hyperbranched polyphosphoramidate and high-efficiency flame-retardant degradable polyester, which can solve the problems of large addition amount and non-degradable flame retardant, and achieve low viscosity , good rheological properties, and the effect of maintaining biodegradability

Inactive Publication Date: 2015-06-17
SHANGHAI JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the fact that the existing expansive flame retardant flame retardant polyester material has a large amount of addition and the flame retardant cannot be degraded, a degradable hyperbranched polyphosphoramide ester (HBPE) high-efficiency flame retardant is synthesized, and the hyperbranched Polyphosphoramidate Flame Retardants for Flame Retardant Biodegradable Polyester Materials

Method used

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  • Hyperbranched polyphosphate amide ester as well as preparation method and application thereof
  • Hyperbranched polyphosphate amide ester as well as preparation method and application thereof
  • Hyperbranched polyphosphate amide ester as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The redistilled POCl 3 Add 0.28mol into 170mL of dry acetonitrile, and then pour them into a 500ml three-necked flask. Nitrogen gas is introduced into the system to maintain anhydrous state. Slowly add dropwise to the reaction system, and the dropping time is 1h~1.5h. After the dropwise addition, control the reaction temperature at 40°C for 24h. Then keep the system at 82°C for 24 hours. After the reaction was completed, acetonitrile was evaporated by rotary evaporation, dissolved by adding DMSO, filtered, and then this operation was repeated once.

[0035] Then add ether, filter, and take the filter cake. The filter cake is the desired product.

[0036]Preparation of polylactic acid and the synthesized hyperbranched polyphosphoramidate blend system Take 50g of PLA, bake at 80°C for 24 hours, then add 50g of PLA, antioxidant 1010 (0.2wt%), and add 0.5-5g of the above-mentioned hyperbranched For polyphosphoramidate, in a torque rheometer, the controlled temperature ...

Embodiment 2

[0039] The redistilled POCl 3 Add 0.28 mol to 170mL of dry acetonitrile, and then pour them into a 500ml three-necked flask. Nitrogen gas is passed through the system to maintain anhydrous state. The temperature of the reaction system is controlled at 0-2°C and stirred rapidly. Alcohol amine is slowly added dropwise to the reaction system, and the dropping time is 1h~1.5h. After the dropwise addition is completed, the reaction temperature is controlled at 40°C for 24h. After the reaction is completed, a mixture of 40mL acetonitrile and 80g pyridine is added dropwise. After completion, keep the system at 82°C for 24 hours. After the reaction was completed, acetonitrile was first spun off, and after the reaction was completed, the acetonitrile was spun off, DMSO was added to dissolve, filtered, and this operation was repeated once. Then add ether, filter, and take the filter cake. The filter cake is the desired product, then add ether, filter, and take the filter cake. T...

Embodiment 3

[0043] The redistilled POCl 3 Add 0.28 mol to 170mL of dry acetonitrile, and then pour them into a 500ml three-neck flask. Nitrogen gas is introduced into the system to maintain anhydrous state. Slowly add it dropwise to the reaction system, the dropping time is 1h~1.5h, after the dropwise addition is completed, control the reaction temperature at 40°C for 24h, after the reaction is completed, add 40mL acetonitrile and 70g diisopropylethylamine dropwise After dropping the mixture, keep the system at 82°C for 24 hours. After the reaction is completed, acetonitrile is first spun off, and then DMSO is added to dissolve. After the reaction is completed, acetonitrile is spun off, DMSO is added to dissolve, and the operation is repeated once. Then add ether, filter, and take the filter cake. The filter cake is the desired product. Then add ether, filter, and take the filter cake. The filter cake is the desired product.

[0044] Preparation of polylactic acid and the synthe...

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Abstract

The invention discloses a hyperbranched polyphosphate amide ester and a preparation method of flame-retardant biodegradable polyester thereof. The hyperbranched polyphosphate amide ester is prepared in the following steps: firstly reacting such A3 monomers as phosphorus oxychloride with such BB' monomers as methanolamine, ethanolamine and propanolamine under the protection of nitrogen, and then, adding a catalyst and an acid binding agent to perform a polycondensation reaction to generate the hyperbranched polyphosphate amide ester through one-pot method. The molecular structure of the prepared hyperbranched polyphosphate amide ester simultaneously contains a phosphate bond and a phosphamide bond, and the prepared hyperbranched polyphosphate amide ester is biodegradable, so that when 2wt% of the synthesized hyperbranched polyphosphate amide ester is added in biodegradable polyester, the oxygen index reaches 30-35%, and UL-94 passes V-0 level. The prepared flame-retardant biodegradable polyester prepared by the invention keeps the biodegradability of the whole system, and the fire-retardant biodegradable polyester has better nucleation property. The flame-retardant biodegradable polyester can be used as fiber, engineering film and injection shaped piece.

Description

technical field [0001] The present invention relates to the field of degradable flame retardants. Specifically, it relates to a preparation method of hyperbranched polyphosphoramidate and high-efficiency flame-retardant degradable polyester. Background technique [0002] Hyperbranched polymers have a special topology, and their special spherical topology makes them have good solubility, low viscosity and low molecular entanglement. In the polymer blend system, this structure also makes the hyperbranched polymer rarely entangle with the blended polymer and becomes a good plasticizer, reducing the processing viscosity of the polymer. At the same time, the functional groups on the spherical surface and the controllability of the functional groups make it possible to produce special forces when blended with other polymers. This force is beneficial to the compatibility of the blend system. Phosphorus-containing hyperbranched polyphosphates and hyperbranched polyphosphoramidate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G79/04C07F9/24C08L67/00C08L67/04C08L67/02C08L85/02C08K5/5399
Inventor 韦平李志闫永刚钱勇
Owner SHANGHAI JIAOTONG UNIV
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