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Phosphamide cross-linked chitosan bio-based flame retardant and preparation method thereof

A technology of cross-linked chitosan and phosphorylated chitosan, which is applied in the field of phosphoramide cross-linked chitosan bio-based flame retardant and its preparation, can solve the problems of reduced thermal stability and affecting the mechanical properties of matrix materials, etc. , to achieve the effects of increasing the char formation rate, improving the anti-droplet behavior, and increasing the flame retardant efficiency

Inactive Publication Date: 2021-12-31
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few related studies involving the design of the molecular structure of CS. They only focus on the introduction of phosphate groups into the CS molecule to form phosphorylated chitosan (PCS), but the thermal stability of the phosphorylated chitosan Reduced, and will affect the mechanical properties of the matrix material

Method used

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  • Phosphamide cross-linked chitosan bio-based flame retardant and preparation method thereof
  • Phosphamide cross-linked chitosan bio-based flame retardant and preparation method thereof
  • Phosphamide cross-linked chitosan bio-based flame retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0035]Adopt tetrahydrofuran solvent (100mL THF) to dilute 16.1g chitosan (deacetylation degree is 85%, structural unit is 0.1mol), join in the four-necked flask that has reflux condenser, stirrer and nitrogen protection device, add 0.4mol triethylamine is used as an acid-binding agent; 0.2mol phenylphosphoryl dichloride is dissolved in 100ml tetrahydrofuran and diluted; the molar ratio of chitosan unit to added aromatic phosphoryl dichloride is 1:2 (mol:mol) ;The phenylphosphoryl dichloride solution is gradually added dropwise to the chitosan dispersion through a constant pressure funnel, the temperature is maintained between -10-0°C, the titration time is 2h, and the stirrer speed is controlled at about 500rpm; after the titration is completed, the The temperature of the reaction solution was raised to 70°C, and the reaction was continued for 24 hours; a solution of triethylenetetramine (0.04mol) diluted with tetrahydrofuran (100ml) was added, and the reaction was continued fo...

Embodiment 2

[0037] Adopt 100mL tetrahydrofuran solvent (THF) to dilute 16.1g chitosan (deacetylation degree is 90%, structural unit is 0.1mol), join in the four-necked flask that has reflux condenser, stirrer and nitrogen protection device, add 1.0 mol triethylamine is used as acid binding agent; 0.3mol phenyl phosphoryl dichloride is dissolved in 100ml tetrahydrofuran; the mol ratio of chitosan structural unit and aromatic phosphoryl dichloride is 1:3 (mol:mol); The phenylphosphoryl dichloride solution is gradually added dropwise to the chitosan dispersion through a constant pressure funnel, the temperature is maintained between -5-0°C, the titration time is 2h, and the stirrer speed is 800rpm; after the titration is completed, the temperature of the reaction solution is raised To 70°C, continue to react for 24h; add tetraethylenepentamine solution (0.06mol) diluted with tetrahydrofuran (50ml), continue to react for 10h, after the reaction is completed, filter out the initial product, was...

Embodiment 3

[0039] Adopt dichloromethane solvent (100mL) to dilute 16.1g chitosan (deacetylation degree is 90%, structural unit, 0.1mol), join in the four-necked flask that has reflux condenser, stirrer and nitrogen protection device, add 0.6mol triethylamine is used as acid-binding agent; 0.25mol phenylphosphoryl dichloride is dissolved in 100ml methylene chloride; the mol ratio of chitosan structural unit to aromatic phosphoryl dichloride is 1:2.5 (mol:mol ); the phenylphosphoryl dichloride solution is gradually added dropwise to the chitosan dispersion through a constant pressure funnel, the temperature is maintained between -5-5°C, the titration time is 2h, and the stirrer speed is 500rpm; after the titration is completed, the reaction The temperature of the solution was raised to 60°C, and the reaction was continued for 24 hours; tetraethylenepentamine (0.06mol) solution diluted with tetrahydrofuran (100ml) was added to continue the reaction for 16 hours. Phosphoryl dichloride and ex...

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Abstract

The invention provides a phosphamide cross-linked chitosan bio-based flame retardant and a preparation method thereof. Amino and hydroxyl of chitosan are chemically modified through phosphorylation and amidation, and due to the fact that flame-retardant elements phosphorus and nitrogen are introduced into a molecular structure at the same time, the char yield and flame retarding efficiency of chitosan are increased. The flame retardant can play an efficient flame retardant role in polylactic acid. When the weight content of the added phosphorylated chitosan flame retardant is 3.0 wt%, the limit oxygen index of polylactic acid can be increased to 25% or above, the UL-94 combustion grade reaches V-0, and the influence on the mechanical property of the material is small. The phosphamide cross-linked chitosan disclosed by the invention is a bio-based degradable efficient environment-friendly flame retardant.

Description

technical field [0001] The invention relates to a chemically modified chitosan bio-based flame retardant, in particular to a phosphoramide cross-linked chitosan bio-based flame retardant applied to high-efficiency flame-retardant modification of polylactic acid and a preparation method thereof. Background technique [0002] Polylactic acid (PLA) is considered to be the biomaterial with the most development potential and the most extensive application prospects due to its excellent mechanical properties, biocompatibility and processing properties. It is currently mainly used in medical materials, fibers and other fields. As a renewable resource, PLA material is an ideal product that can replace petroleum resources. However, PLA materials have the disadvantage of being flammable. The LOI of pure PLA products is 19.0-20.0%, and there is a droplet phenomenon during the combustion process, which has a greater fire hazard. Therefore, it is necessary to carry out flame-retardant mo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08C08L67/04C08L5/08
CPCC08B37/003C08L67/04C08L2201/02C08L5/08
Inventor 吴宁晶马小兵刘鹏博
Owner QINGDAO UNIV OF SCI & TECH