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Modified lignin polyol and preparation method thereof

A polyol and lignin technology, applied in the field of modified lignin polyester polyol and its preparation, can solve the problems of catalyst toxicity, easy residue, and low material performance, and achieve low price, simple preparation, and high catalytic activity Effect

Pending Publication Date: 2022-04-15
NANJING ADVANCED BIOLOGICAL MATERIALS & PROCESS EQUIP INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Purpose of the invention: The technical problem to be solved by the present invention is the defects of lignin-based materials: after physical blending, the performance of the obtained material is low; the performance of the material obtained by catalyzing lignin grafted with caprolactone through tin compounds is improved, but there is a catalyst Defects such as toxicity and easy residue

Method used

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  • Modified lignin polyol and preparation method thereof
  • Modified lignin polyol and preparation method thereof
  • Modified lignin polyol and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0058] The first step: mix the caprolactone monomer with calcium hydride, stir overnight to remove residual moisture, and purify by distillation under reduced pressure; place the lignin in a vacuum oven overnight to remove water; place the catalyst in a vacuum oven for use; react The required organic solvent is dewatered through a solvent redistillation device.

[0059] Step 2: Weigh caprolactone (1.80g), alkali lignin (0.20g) and dissolve in N,N-dimethylformamide (10mL) to obtain a homogeneous solution, add To the reaction flask, weigh o-vanillin Schiff base Ni (Ⅲ) catalyst (0.01g) and add to the reaction flask. Stir (500rpm) at 120°C for 3h. After the end, expose the reaction mixture to the air and let it stand for 30min. After the volatile matter is removed, the quenching is completed. Take a small part for 1 H NMR analysis (CDCl 3 as a deuterated reagent). The remaining part was dissolved in 15 mL of dichloromethane and centrifuged (3000 rpm for 3 min). The supernatant...

Embodiment 2

[0061] The first step: mix the caprolactone monomer with calcium hydride, stir overnight to remove residual moisture, and purify by distillation under reduced pressure; place the lignin in a vacuum oven overnight to remove water; place the catalyst in a vacuum oven for use; react The required organic solvent is dewatered through a solvent redistillation device.

[0062] Step 2: Weigh caprolactone (1.90g), alkali lignin (0.10g) and dissolve in N,N-dimethylformamide (10mL) to obtain a homogeneous solution. Into the reaction flask, weigh o-vanillin Schiff base Ni (Ⅲ) catalyst (0.02g) and add to the reaction flask. React at 120°C with a stirring rate of 500rpm for 1h. After the end, expose the reaction mixture to the air and let it stand for 30min. After removing the volatile matter, the quenching is completed. Take a small part for further analysis. 1 H NMR analysis (CDCl 3 as a deuterated reagent). The remaining part was dissolved in 15 mL of dichloromethane and centrifuged (...

Embodiment 3

[0064] The first step: mix the caprolactone monomer with calcium hydride, stir overnight to remove residual moisture, and purify by distillation under reduced pressure; place the lignin in a vacuum oven overnight to remove water; place the catalyst in a vacuum oven for use; react The required organic solvent is dewatered through a solvent redistillation device.

[0065] Step 2: Weigh caprolactone (1.70g), alkali lignin (0.30g) and tetrahydrofuran (10mL) and mix them, add them to the reaction bottle in sequence with a magnetic stirrer under nitrogen protection, and weigh o-vanillin mat Ni(Ⅲ) catalyst (0.01g) was added to the reaction flask and stirred (500rpm) at 100°C for 6h. After the end, the reaction mixture was exposed to the air and left for 30min. After the volatile matter was removed, the quenching was completed. Take a small in part 1 H NMR analysis (CDCl 3 is a deuterated reagent). The remaining part was dissolved in 15 mL of dichloromethane and centrifuged (3000 r...

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Abstract

The preparation method comprises the following steps: taking cyclic ester, lignin, a metal (III) salen catalyst and an organic solvent as raw materials, and reacting under the protection of inert gas to obtain the lignin-containing polyol. The obtained lignin-containing polyol has a higher hydroxyl value and a lower acid value. Compared with the prior art, the catalyst used in the invention keeps higher catalytic activity compared with other metal catalysts, and the reaction time is shortened in the preparation process; the catalyst is derived from bio-based o-vanillin, is simple to prepare and easy to obtain, and is more environment-friendly; in addition, the catalyst exhibits low loading tolerance in the reaction. Meanwhile, the polyol is prepared by a one-pot method, activation or acylation of lignin is not needed, dissolvability of lignin before and after reaction is greatly different, separation of products is facilitated, and the polyol can replace petrochemical polyol to be applied to preparation of polyurethane materials.

Description

technical field [0001] The invention belongs to the field of polymer compounds, and in particular relates to a modified lignin polyester polyol and a preparation method thereof. Background technique [0002] As a natural biopolymer second only to cellulose in reserves, lignin has a highly three-dimensional branched structure with different functional groups, including aliphatic and phenolic hydroxyl groups, carboxyl groups, carbonyl groups, and methoxyl groups. Its biocompatibility, biodegradability, and cheap cost have shown functionality as an alternative to organic materials in various applications. Efficient and rational use of lignin is conducive to reducing the consumption of fossil energy and reducing environmental pollution. [0003] As we all know, polyester polyol is one of the main raw materials of polyester polyurethane, and ring-opening polymerization (ROP) has been proved to be one of the important methods for the synthesis of sustainable aliphatic polyester. ...

Claims

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Application Information

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IPC IPC(8): C08G63/664C08G63/82
Inventor 李玉光黄桂翔沈磊季栋胡玉静朱宁胡欣刘一寰方正乔凯张锴李亚军郭凯
Owner NANJING ADVANCED BIOLOGICAL MATERIALS & PROCESS EQUIP INST CO LTD
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