Preparation method of furfural-modified lignin-based phenolic resin adhesive

A phenolic resin glue, lignin-based technology, applied in the direction of adhesives, aldehyde/ketone condensation polymer adhesives, adhesive types, etc., can solve the problems of decreased bonding strength of adhesives and inability to achieve high proportion replacement, etc. To achieve the effect of improving the bonding strength, improving the product purity and increasing the bonding strength

Active Publication Date: 2017-11-10
JILIN UNIV
13 Cites 18 Cited by

AI-Extracted Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a preparation method of a furfural-modified lignin phenolic resin adhesive, which solves the problems in...
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Abstract

The invention discloses a preparation method of a furfural-modified lignin-based phenolic resin adhesive and belongs to the technical field of the biomass energy chemical industry. According to the method, a xylose solution is prepared from biomass hemicellulose through hydrolysis under catalysis of diluted acid, furfural is prepared through dehydration of xylose under catalysis of concentrated acid, lignin is extracted under catalysis of alkali, and an alkali lignin solution is obtained; alkali lignin is subjected to phenolation modification with phenol as a phenolation reagent and alkali as a catalyst, phenol is replaced with the modified lignin in different proportions, formaldehyde is replaced with furfural in different proportions, and the lignin-based phenolic resin adhesive is prepared through collaborative copolymerization of lignin, furfural, phenol and formaldehyde. The product furfural prepared through hydrolysis and dehydration of hemicellulose is taken as a crosslinking agent, the industrial application problem that the glue strength of the adhesive is reduced due to the fact that the proportion of lignin replacing phenol is increased in the prior art is solved, and the total replacement rate of chemical products from biomass for phenol and formaldehyde from fossil resources is increased.

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Technology Topic

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  • Preparation method of furfural-modified lignin-based phenolic resin adhesive
  • Preparation method of furfural-modified lignin-based phenolic resin adhesive

Examples

  • Experimental program(18)
  • Comparison scheme(4)

Example Embodiment

[0041] Example 1
[0042] Step 1: Preparation of xylose solution
[0043] ① Mix the biomass with a sulfuric acid solution with a concentration of 2wt% at a solid-to-liquid ratio of 1Kg:10L, heat and reflux for 2h-4h, cool down and filter to obtain a hydrolyzate and hydrolyzed residue with a xylose concentration of 6.5wt%;
[0044] ②Adjust the sulfuric acid concentration in the hydrolyzed solution with a concentration of 3wt% to 2wt% in ①, add biomass according to the solid-to-liquid ratio of 1Kg:10L, heat and reflux for 3h, cool down and filter to obtain a xylose concentration of 10wt% Hydrolysis solution and hydrolysis residue;
[0045] ③Use a sulfuric acid solution with a concentration of 3wt% to adjust the sulfuric acid concentration in the hydrolysate in ② to 2wt%, add biomass according to the solid-to-liquid ratio of 1Kg:10L, heat and reflux for 2h-4h, cool and filter to obtain the xylose concentration of the hydrolysate 15.6wt% xylose solution and hydrolysis residue;
[0046] Step 2: Preparation of aqueous furfural solution
[0047] Add the sulfuric acid catalyst solution with a molar concentration of 2mol/L to the reactor, heat it to the reflux of the catalyst solution, add the promoter sodium chloride to saturation, stir to form a rotating liquid surface with a fixed concentration of catalyst and promoter, and then Step 1 Hydrolyzed to obtain a 15.6% by weight xylose solution sprayed into the reactor at a certain speed, heated to a constant temperature reaction, dehydrated xylose on the liquid surface layer to produce furfural vapor, the concentration of 7.33wt% furfural solution prepared by condensation , The yield reaches 75wt%;

Example Embodiment

[0048] Example 2
[0049] ① Collect the hydrolyzed residue in step 1 of Example 1, wash it to neutrality, and mix it with a sodium hydroxide solution with a concentration of 5wt% according to the solid-to-liquid ratio of 1Kg:8L, heat and reflux for 4h, reduce to room temperature, filter, Obtain alkali lignin solution and crude cellulose;
[0050] ②Add the alkali lignin solution, phenol and alkali catalyst obtained in ① into the reaction device, heat up to 80℃~100℃, and reflux for 0.5h~2h to obtain a phenolic modified alkali lignin solution;
[0051] The mass of lignin in the alkali lignin solution accounts for 40% of the total mass of lignin and phenol, the alkali catalyst is sodium hydroxide solution, and the mass of active ingredients in the alkali catalyst is 5% of the total mass of lignin and phenol;
[0052] ③Add 37% formaldehyde solution in batches to the phenolic modified alkali lignin solution obtained in ②, add 80% of the total formaldehyde solution in the first batch, adjust the system temperature to 65°C, and add the reaction for 1.0h , Then the temperature is raised to 80°C, the furfural solution obtained in step 2 and the remaining formaldehyde solution are added, react at a constant temperature for 1.0h, cool down to 70°C, and distill under reduced pressure until the viscosity of the solution is 600mPa·s, then discharge to obtain lignin-based phenolic aldehyde Resin adhesive, denoted as LPF4005.
[0053] The mass of furfural in the furfural solution accounts for 5% of the total mass of furfural and formaldehyde, and the remaining formaldehyde is 15%.

Example Embodiment

[0054] Example 3
[0055] The mass of lignin accounts for 40% of the total mass of lignin and phenol, and the mass of furfural accounts for 10% of the total mass of furfural and formaldehyde. Other conditions are the same as in Example 2, to obtain a lignin-based phenolic resin adhesive LPF4010.
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