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Modified lignin based carburizing agent and preparation method thereof

A lignin-based and lignin-based technology, which is applied in the field of lignin-based carbon formers and their preparation, can solve the problems of complex post-processing, numerous steps, and reduced lignin utilization efficiency, so as to achieve difficult migration, realize industrialized production, and simplify reformation. The effect of sexual steps

Inactive Publication Date: 2015-07-08
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reported modification methods usually use a three-step method to introduce the flame retardant element - phosphorus into lignin. There are many steps and complicated post-treatment, which indirectly reduces the utilization efficiency of lignin.
However, the introduction of phosphorus into lignin, especially soft lignin, by one-step method has not been reported yet.

Method used

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  • Modified lignin based carburizing agent and preparation method thereof
  • Modified lignin based carburizing agent and preparation method thereof
  • Modified lignin based carburizing agent and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] A preparation method of a modified lignin-based carbon forming agent, the preparation method comprising the steps of:

[0027] 1) Add soft lignin (SKL) (about 0.01 mole) into a three-necked flask filled with tetrahydrofuran (THF), and stir to make SKL evenly dispersed;

[0028] 2) Add 0.011 moles of triethylamine and mix well;

[0029] 3) Add 0.01 mole of THF solution of diphenoxyphosphoryl chloride dropwise at room temperature, and finish adding dropwise in 1.0 hr;

[0030] 4) Slowly increase the temperature to 67 o C, heat preservation reaction 8 hr;

[0031] 5) After the reaction, the mixture was rotated to remove part of the solvent, then added to methanol for precipitation, and the precipitate was washed with methanol several times;

[0032] 6) The target product is obtained after drying the obtained precipitate.

[0033] The infrared spectrogram of gained modified lignin-based carbon forming agent is shown in figure 1 , by comparing with the spectrum befo...

Embodiment 2

[0037] 1) Add alkali lignin (about 0.005 mol) into a three-necked flask filled with tetrahydrofuran (THF), and stir to disperse the alkali lignin evenly;

[0038] 2) Add 0.020 moles of triethylamine and mix well;

[0039] 3) Add 0.015 moles of diphenoxyphosphoryl chloride THF solution dropwise at room temperature, and finish adding dropwise in 1.5 hr;

[0040] 4) Slowly increase the temperature to 67 o C, heat preservation reaction 12 hr;

[0041] 5) After the reaction, the mixture was rotated to remove part of the solvent, then added to methanol for precipitation, and the precipitate was washed with methanol several times;

[0042] 6) The target product is obtained after drying the obtained precipitate.

[0043] Figure 4 Muffle furnace 500 before and after alkali lignin modification o In the digital photo of C residual charcoal, it can be clearly seen from the picture that the charring effect of alkali lignin after modification has been significantly improved, and the r...

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Abstract

The invention provides a modified lignin based carburizing agent and a preparation method thereof and belongs to the technical field of materials. The carburizing agent has a structure as shown in a formula I; the major raw materials of the carburizing agent are easily available, cheap and reproducible; the carburizing agent is prepared by use of a one-step method, and the preparation process is simple, feasible and low in cost. The modified lignin based carburizing agent is prepared by use of the one-step method; the inflaming retarding element phosphorus is introduced to the lignin molecules so that the carburization capability of the lignin and the compatibility of the lignin with the polymer can be improved; the formula I is as shown in the description, wherein R can be a phenyl or a phenoxyl.

Description

technical field [0001] The invention relates to a lignin-based carbon forming agent and a preparation method thereof, belonging to the field of technical materials. Background technique [0002] In recent years, intumescent flame retardants have been hailed as one of the most promising flame retardants because of their high efficiency, halogen-free, and environmental friendliness, and have attracted widespread attention. The intumescent flame retardant is mainly composed of acid source, carbon source and gas source, among which the char forming agent is particularly important, which directly affects the formation and quality of the carbon layer of polymer materials. In order to overcome the problems of low melting point, high water solubility, poor compatibility with matrix resin and easy leakage during material processing or use of traditional low-molecular-weight char-forming agents, high-molecular-weight char-forming agents have increasingly become one of the research hot...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00
Inventor 宋艳李锦春张鑫蒋明访
Owner CHANGZHOU UNIV
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