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Material formula of polyurethane of enzymolysis lignin, and preparation method

A technology for enzymatically decomposing lignin and polyurethane, which is applied in the field of comprehensive utilization of biomass resources and polyurethane manufacturing, can solve the problems of polyurethane manufacturing cost impact, low yield of propoxylated lignin, structural changes, etc., and achieve improved tensile strength Strength and elongation at break, increased swelling resistance, improved tensile strength effect

Inactive Publication Date: 2007-05-09
FUZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] In the previous research report on the preparation of lignin polyurethane, there was a precedent of using lignosulfonate as raw material, but lignosulfonate was extracted from the traditional papermaking "black liquor", which not only contained high impurities, but also Natural lignin in plant raw materials undergoes major structural changes after being cooked by alkali and sulfite. Lignosulfonate has low chemical activity and cannot directly react with isocyanate. It must first react with propylene oxide to form propoxylated lignin After being primed, it can react with isocyanate to form polyurethane
The yield of propoxylated lignin is low, and organic solvents are also used, which will have an adverse impact on environmental protection and the manufacturing cost of polyurethane
In addition, there are also studies on a new method of preparing polyurethane from high-boiling alcohol lignin prepared by high-boiling alcohol solvent method. The preparation of polyurethane from high-boiling alcohol lignin has many improvements compared to using lignin sulfonate as raw material, but the high-boiling alcohol solvent method prepares polyurethane. Lignin needs to use higher-priced high-boiling alcohol, and the recovery of high-boiling alcohol solvent needs to consume more energy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 5.5g of enzymatic lignin and 3.1g of toluene diisocyanate (TDI) and dissolve in 20ml of tetrahydrofuran, stir and heat to 60°C for 1 hour, then add 14.5g of polyether diol (PEG220) and 4.2g of toluene Diisocyanate (TDI), the temperature of the system was raised to 100°C and maintained for 2 hours. Then add 0.2 g of chain-extending cross-linking agent dichlorodiaminodiphenylmethane (MOCA), continue the reaction for 1 hour, and distill off the brown solid obtained from the solvent under reduced pressure (pressure range 5-20mmHg, time 1 hour, temperature 80°C) , washed with water and dried (drying conditions: temperature 90° C., time 1 hour) to obtain 22.3 g of enzymatic lignin polyurethane.

Embodiment 2

[0025] Weigh 15.5g of enzymatic lignin and dissolve it in 100g of 3% sodium hydroxide aqueous solution, pour it into a 500ml three-neck flask, add 25g of formaldehyde solution and heat and stir, react at 90°C for 1.5 hours, add 10ml of 35% hydrochloric acid to neutralize and The pH value of the solution was 2-3, and the lignin hydroxymethylated derivatives were precipitated out, washed with water for 3 times, and then dried at 80° C. for 2.0 hours to obtain 21.5 g of lignin hydroxymethylated derivatives.

[0026] Weigh 8.5g of lignin hydroxymethylated derivatives and 4.2g of diphenylmethane diisocyanate (MDI) and dissolve them in 50g of diethylene glycol and polyester polyol produced by adipic acid, heat at 125-130°C and maintain vacuum for 1.5 hours Dehydration, then lower the temperature to 80°C, add 0.1g of antioxidant 1010, pour into a mold, vulcanize in an oven at 120°C for 3 hours, and then release the mold to obtain enzymatic lignin polyurethane.

Embodiment 3

[0028] Add 180g of castor oil and 10g of pentaerythritol into a 500ml three-necked flask, heat to 120°C under the protection of carbon dioxide gas, add 0.3g of calcium naphthenate catalyst, heat up to 230°C for alcoholysis, add 10g of pentaerythritol within 30 minutes, and continue to keep warm until Stop the reaction after being transparent, cool to 100°C and filter to obtain castor oil-pentaerythritol prepolymer (polymer polyol).

[0029] Weigh 5.5g of enzymatic lignin and 3.1g of toluene diisocyanate (TDI) and dissolve in 20ml of tetrahydrofuran, stir and heat to 60°C for 1 hour, then add 20g of castor oil-pentaerythritol prepolymer and 4.8g of toluene diisocyanate , the temperature was raised to 90° C. and maintained for 2.0 hours to obtain an enzymatic lignin polyurethane liquid.

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Abstract

This invention provides a method for preparing cellulolytic enzyme lignin polyurethane and its raw materials. The raw materials comprise: cellulolytic enzyme lignin or its derivative, polyisocyanate, polyol oligomer, chain extension and crosslinking agent, organic solvent and additive. The method comprises: (1) dissolving cellulolytic enzyme lignin or its derivative in the organic solvent, mixing with polyol or a mixture of polyol and organic solvent, and heating or stirring to mix uniformly; (2) adding polyisocyanate, heating, adding conventional additives or fillers, heating to react completely, and vacuum-distilling to obtain brown solid; (3) washing the solid with water, and drying to obtain cellulolytic enzyme lignin polyurethane. The cellulolytic enzyme lignin is a natural polymeric material extracted from wood, bamboo and straw, thus can effectively utilize biomass resources and replace petrochemical raw materials. The method largely improves the process for preparing cellulolytic enzyme lignin polyurethane, which has a better modification effect than traditional sulfonated lignin, and lower cost than high-boiling-point alcohol lignin.

Description

Technical field: [0001] The invention relates to the comprehensive utilization of biomass resources and the polyurethane manufacturing industry, in particular to the process and formula of using enzymatically decomposed lignin and its derivatives as the main raw material of lignin polyurethane. Background technique: [0002] In the previous research report on the preparation of lignin polyurethane, there was a precedent of using lignosulfonate as raw material, but lignosulfonate was extracted from the traditional papermaking "black liquor", which not only contained high impurities, but also Natural lignin in plant raw materials undergoes major structural changes after being cooked by alkali and sulfite. Lignosulfonate has low chemical activity and cannot directly react with isocyanate. It must first react with propylene oxide to form propoxylated lignin After being primed, it can react with isocyanate to form polyurethane. The yield of propoxylated lignin is low, and organi...

Claims

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Application Information

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IPC IPC(8): C08G18/64C08G18/72C08G18/42C08G18/48C08L75/04
Inventor 程贤甦
Owner FUZHOU UNIVERSITY
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