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A kind of preparation method of phosphorus nitrogen modified lignin base expansion flame retardant

An intumescent flame retardant and lignin-based technology, which is applied in the field of preparation of phosphorus-nitrogen modified lignin-based intumescent flame retardant, can solve problems such as economic loss, flammability, and complex reaction of modified lignin. Achieve good flame retardant effect and simple synthesis process

Inactive Publication Date: 2021-04-02
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Polymer materials have excellent comprehensive properties and are favored by people and are widely used in various fields. However, due to the structure of polymer materials, most of the polymer materials we use in our daily life are flammable and will be accompanied by Generation of copious amounts of hot and toxic gases
The generation of a large amount of heat and toxic gases will easily cause casualties in the fire, and the fire caused by polymer materials will cause a lot of economic losses
[0003] All flame retardants have certain flame retardant properties, but there are also obvious deficiencies. For example, the reaction of modified lignin is more complicated and the cost is higher, while the compound system will have problems such as uneven dispersion in the matrix, resulting in flame retardancy. Poor combustion performance, LOI, etc.

Method used

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  • A kind of preparation method of phosphorus nitrogen modified lignin base expansion flame retardant
  • A kind of preparation method of phosphorus nitrogen modified lignin base expansion flame retardant
  • A kind of preparation method of phosphorus nitrogen modified lignin base expansion flame retardant

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 1) Add enzymatic lignin to deionized water adjusted to a pH of 10 with sodium hydroxide, then add 5 g of enzymatic lignin, 10 g of formaldehyde, and 10 g of PEI (600 molecular weight, McLean), and react at 60° C. for 5 h. After the reaction, adjust the pH to 4 with hydrochloric acid, centrifuge, wash and dry after obtaining the precipitate, and obtain the modified lignin grafted with PEI;

[0030] 2) Disperse 5 g of the modified lignin obtained above in a three-necked flask filled with deionized water, add phosphoric acid dropwise to adjust the pH to 3, and heat to 90° C. for 30 min. Then with 5g polyphosphoric acid (model P815555 (P2O5)% ≥ 85%), in the beaker that the deionized water of 20ml is housed, disperse evenly, add it dropwise in the there-necked bottle with constant pressure funnel, after dropwise Continue to react for 6h. After the reaction, the product was centrifuged, washed, and freeze-dried until constant weight;

[0031] The product obtained above is g...

Embodiment 2

[0035] The epoxy resin in Step 3) of Example 1 was replaced with PLA (3052D, Natureworks, USA) of the same quality, and the rest of the conditions were the same as in Example 1.

[0036] The resulting splines are unrated in the UL-94 test.

Embodiment 3

[0038] The epoxy resin of step 3) of embodiment 1 is replaced with PBS of the same quality, all the other conditions are identical with embodiment 1.

[0039] The resulting splines are rated V-2 in the UL-94 test.

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Abstract

The invention discloses a preparation method of a phosphorus-nitrogen modified lignin-based intumescent flame retardant. The preparation method comprises the steps of adding purified lignin into water, adding formaldehyde and polyethyleneimine, reacting at the temperature of 50-70 DEG C, filtering, washing with deionized water for several times, and freeze-drying to obtain modified lignin; addingwater into the modified lignin, dropwise adding phosphoric acid to adjust the pH value to be 3-4, heating and stirring, dropwise adding polyphosphoric acid into a lignin solution, and keeping stirring, condensing, refluxing, centrifuging, washing and drying to obtain a modified lignin-based flame retardant; and adding the modified lignin-based flame retardant into epoxy resin to obtain epoxy resinwith a flame retardant property. The lignin-based flame retardant grafted with phosphorus and nitrogen elements is prepared by a simple, convenient and environment-friendly method, does not contain halogen, and is natural and nontoxic, and harmful substances are not generated.

Description

technical field [0001] The invention belongs to the technical field of flame retardant preparation, and in particular relates to a preparation method of a phosphorus-nitrogen modified lignin-based expansive flame retardant. Background technique [0002] In recent years, my country's economy has shown a rapid upward trend, people's living standards have also been continuously improved, and polymer materials are also playing an increasingly indispensable role in life. Polymer materials have excellent comprehensive properties and are favored by people and are widely used in various fields. However, due to the structure of polymer materials, most of the polymer materials we use in our daily life are flammable and will be accompanied by Generation of copious amounts of hot and toxic gases. The generation of a large amount of heat and toxic gas will easily cause casualties in the fire, and the fire caused by the polymer material will cause a large amount of economic losses. [0...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/00C08L63/00C08L87/00
Inventor 何明陶然亢玉年罗振扬
Owner NANJING FORESTRY UNIV