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Method for preparing lignin-based phenolic resin adhesive and co-producing quickly-composted fertilizer returned into field by utilizing fiber ethanol fermentation residues

A fermentation residue and cellulosic ethanol technology, applied in adhesives, aldehyde/ketone condensation polymer adhesives, adhesive types, etc., can solve the problems of long gelation time and short storage days of lignin-based phenolic resins, and achieve Effects of improving economic competitiveness, extending storage days, and shortening gel time

Active Publication Date: 2017-12-22
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Purpose of the invention: In order to solve the problems of long gelation time and short storage days of lignin-based phenolic resins, the present invention provides a method for preparing lignin-based phenolic resin adhesives from cellulosic ethanol fermentation residues and co-producing fast-rotten return-to-field fertilizers

Method used

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  • Method for preparing lignin-based phenolic resin adhesive and co-producing quickly-composted fertilizer returned into field by utilizing fiber ethanol fermentation residues
  • Method for preparing lignin-based phenolic resin adhesive and co-producing quickly-composted fertilizer returned into field by utilizing fiber ethanol fermentation residues

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Take 50 kg of corn stalk fiber ethanol fermentation residue, add 500 kg of 5 wt.% NaOH aqueous solution, and stir at 60° C. for 20 min to carry out alkali extraction of lignin.

[0026] After the reaction, the obtained solid-liquid mixture was put into a filter press for solid-liquid separation to obtain 540 kg of alkali extract and 10 kg of solid residue. Add 0.3 kg of HM straw decomposing agent to the solid residue for composting treatment, the decomposing temperature is normal temperature, and the decomposing time is 20 days, so as to realize the reuse of biomass in the field. The ultrafiltration membrane with a molecular weight cut-off of 10000Da is used to carry out ultrafiltration on the alkali extract, the ultrafiltration pressure is 0.6MPa, and the ultrafiltration stirring speed is 500rpm to obtain the retentate A1 and the permeate A2; the permeate A2 continues to use the molecular weight cut-off Perform ultrafiltration for a 5000Da ultrafiltration membrane to o...

Embodiment 2

[0029] Take 100 kg of corn straw fiber ethanol fermentation residue, add 700 kg of 4 wt.% NaOH aqueous solution, stir at 70° C. for 30 min to carry out alkali extraction of lignin.

[0030] After the reaction, the obtained solid-liquid mixture was put into a filter press for solid-liquid separation to obtain 785kg of alkali extract and 15kg of solid residue, and the solid residue was added with 0.4kg HM straw decomposing agent for composting. The decomposing temperature is normal temperature, and the decomposing time is 15 days, so as to realize the return and reuse of biomass. The ultrafiltration membrane with a molecular weight cut-off of 10000Da is used for ultrafiltration of the alkali extract, the ultrafiltration pressure is 0.4MPa, and the ultrafiltration stirring speed is 400rpm to obtain the retentate A1 and the permeate A2; the permeate A2 continues to use the molecular weight cut-off Perform ultrafiltration for a 5000Da ultrafiltration membrane to obtain the retentat...

Embodiment 3

[0033] Take 30 kg of lignin solution A with a molecular weight greater than 10,000 Da in Example 1 and add it to a glass reactor, then add 9 kg of molten phenol, set the stirring speed of the mechanical stirring tank to 650 rpm, and react at 90 ° C for 2 hours to obtain a phenolized modified lignin solution. Cool to 80°C, then add 13.7kg of 37wt.% formaldehyde aqueous solution, react at 80°C for 2h, then cool down to 65°C, add 0.9kg of urea and stir for 0.5h. Cool to 40°C and discharge to obtain a lignin-based phenolic resin adhesive.

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Abstract

The invention discloses a method for preparing a lignin-based phenolic resin adhesive and co-producing quickly-composted fertilizer returned into the field by utilizing fiber ethanol fermentation residues. The method comprises the following steps: firstly, carrying out alkali extraction on the fiber ethanol fermentation residues, and carrying out solid-liquid separation to obtain solid residues and an alkali extracting solution; secondly, adding a decomposition agent into the solid residues for carrying out composting and returning a compost into the field; thirdly, carrying out staged ultrafiltration concentration on the alkali extracting solution to obtain a lignin solution A, a lignin solution B, a lignin solution C and a lignin solution D; fourthly, adding molten phenol into the lignin solution for carrying out phenol reaction; fifthly, adding formaldehyde into a reaction liquid obtained in the fourth step for carrying out a condensation reaction. Compared with a phenolic resin adhesive prepared from ungraded lignin, the lignin-based phenolic resin adhesive prepared according to the method disclosed by the invention has the advantages that the gelation time is greatly shortened and the storage time of the phenolic resin adhesive is prolonged; the phenolic resin adhesive disclosed by the invention achieves the level of a commercial phenolic resin adhesive.

Description

technical field [0001] The invention relates to a preparation method of a phenolic resin, in particular to a method for preparing a lignin-based phenolic resin adhesive by using cellulosic ethanol fermentation residue and co-producing quick-rot and returning field fertilizer. Background technique [0002] At the beginning of this century, with the soaring international oil prices and the increasing demand for energy in countries around the world, the research and development of ethanol production technology using cellulosic raw materials has become the focus of research at home and abroad. In recent years, the industrialization research of cellulosic ethanol has achieved rapid development. In order to accelerate the realization of the development goals proposed in the "Advanced Energy Plan", the United States helps to achieve the goals proposed in its "Plan to Reduce Petroleum by 20% within 10 Years". The 2007 U.S. Energy Plan In the next 4 years, 385 million US dollars will...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J161/14C08G8/28C05F15/00
CPCC09J161/14C05F5/008C08G8/28C05F11/08
Inventor 应汉杰朱晨杰甘涛唐成伦陈彦君陈勇吴菁岚柳东牛欢青
Owner NANJING UNIV OF TECH
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