Preparation method of thermal-insulation lignin-base polyurethane foam

A polyurethane foam and lignin-based technology, which is applied in the field of preparation of thermal insulation lignin-based polyurethane foam, can solve problems such as difficulties, many side reactions, and increased preparation of lignin polyurethane foam, and achieve low cost and high addition of lignin The effect of low content and low price

Active Publication Date: 2015-04-29
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the harsh reaction conditions of high temperature and high pressure, coupled with many side reactions, have added great difficulties to the preparation of lignin polyurethane foam.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Use 40ml of 0.1mol / L NaOH solution to adjust the pH of 10g of enzymatic lignin to 12, stir evenly for 2 hours, filter out the insoluble substances to obtain lignin filtrate, adjust the pH of the filtrate to 2,60 with 0.5mol / L hydrochloric acid solution After heating at ℃ for 3 hours, filter the lignin solution, and then dry it in a vacuum oven at 60℃ to obtain the preliminarily purified lignin.

[0036] Take 5g of initially purified lignin, add 30ml of methanol, and stir evenly to obtain a methanol solution in which part of the lignin is dissolved. Pour it into 40ml of deionized water to precipitate lignin, and dry it in a vacuum oven at 60°C to obtain methanol organic solvent-based lignin. white.

[0037] Take 2g of methanol-organic solvent-type lignin obtained from the above purification, dissolve it completely with 20ml of 0.1mol / L NaOH solution, adjust the pH to 12, stir well, add 4ml diethanolamine, stir well, heat to 80°C, slowly add 3ml 37wt% formaldehyde aqueou...

Embodiment 2

[0041] Add 10mL (12.80g) of glycerol to 30mL of 0.1mol / L NaOH solution, adjust the pH to 12, stir well, add 0.35g of catechol, heat to 90°C, and slowly add 2.6ml (3.071g) of cyclic Oxychloropropane for 1 h, reflux for another 2 h, finally add 2 g of the lignin amino polyol obtained in Example 1, and react at 120° C. for 4 h. After the reaction, the pH of the reaction solution was adjusted to 2 with 0.5mol / L hydrochloric acid. After the lignin was completely precipitated, it was washed with deionized water until neutral, then centrifuged at 7000r / min for 10min, and finally placed at 60°C. Dry overnight in a vacuum oven to obtain lignin amino polyol-glycerin.

[0042] The obtained lignin amino polyol-glycerol has good compatibility with polyethylene glycol 200, the residue rate is less than 5%, good dispersibility, and the hydroxyl content is 304.71mgKOH / g.

Embodiment 3

[0044] Take 2 g of the methanolic organic solvent-type lignin purified in Example 1, dissolve it completely with 20 mL of 0.1 mol / L NaOH solution, adjust the pH to about 10, stir well, add 3 ml of diethylenetriamine, stir well, and heat To 50°C, slowly add 2ml of 37wt% formaldehyde aqueous solution dropwise for 1h, and then react for 2h. After the reaction is over, add an appropriate amount of isopropanol to the reaction solution. The volume ratio of the reaction solution to be added and isopropanol is 1:6. The lignin amine was obtained by washing with ionic water until neutral, and finally drying in a vacuum oven at 50°C overnight.

[0045] Add 15ml (19.2g) of glycerol to 40ml of 0.1mol / L NaOH solution, adjust the pH to 12, stir evenly, add 0.52g of catechol, heat to 90°C, slowly add 3.5ml (4.13g) of cyclic Oxychloropropane for 1 h, reflux for 2 h, finally add 3 g of ligninamine obtained in the above steps, and react at 100° C. for 4 h. After the reaction, the pH of the rea...

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Abstract

The invention discloses a preparation method of thermal-insulation lignin-base polyurethane foam, which comprises the following steps: uniformly mixing methanol organic solvent lignin with diethanolamine or diethylenetriamine under alkali solution conditions, slowly and dropwisely adding a formaldehyde water solution, reacting to obtain lignin amino polyalcohol or lignin amine, grafting epoxy chloropropane to glycerol by using catechol as a catalyst to obtain lignin amino polyalcohol-glycerol or lignin amine-glycerol; and mixing the lignin amino polyalcohol-glycerol or lignin amine-glycerol with an organic solvent polyalcohol, and carrying out foaming technique of polyurethane foam to obtain the thermal-insulation lignin-base polyurethane foam. The lignin-base polyalcohol subjected to chemical modification has higher hydroxy content and higher reaction activity, greatly enhances the compatibility between the lignin and organic solvent polyalcohol, has favorable dispersity, and can be used for preparing the safe, nontoxic, green and environment-friendly degradable polyurethane thermal-insulation foam material.

Description

technical field [0001] The invention belongs to the field of polymer materials and relates to a preparation method of heat-insulating lignin-based polyurethane foam. More specifically, it relates to a method of reacting lignin polyol with high hydroxyl content and isocyanate to form polyurethane foam. Background technique [0002] Due to its excellent physical and chemical properties, polyurethane foam has a wide range of applications in the fields of materials, chemicals, and medicine. However, with the aggravation of environmental pollution and resource shortage, green and degradable polyurethane foam has attracted more and more attention from the state and scientific researchers. Lignin is a natural polymer compound that is green, environmentally friendly, renewable, rich in sources, low in price, and second only to cellulose in content. If it is used, it can greatly reduce the cost of polyurethane foam and damage to the environment. However, the utilization of lignin i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/64C08H7/00C08J9/14C08G101/00
CPCC08G18/6492C08H6/00C08J9/144C08J2375/04
Inventor 应汉杰夏治停朱晨杰陈勇吴菁岚庄伟陈晓春
Owner NANJING UNIV OF TECH
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