Phenolic resin adhesive synthesized through in situ alkali lignin autocatalysis and preparation method of phenolic resin adhesive

A technology of alkali lignin and phenolic resin, applied in the field of phenolic resin adhesive and its preparation, can solve problems such as activity reduction, and achieve the effects of simplifying steps, reducing costs, and improving production efficiency

Inactive Publication Date: 2017-07-14
JIANGNAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to overcome the disadvantages of agglomeration and activity reduction caused by re-dissolving lignin solids after drying in the traditional method, and adopts the method of pretreatment to remove sugar substances and metal ions firstly, eliminating the need for acid-precipitated lignin And its re-drying process; overcome the complex process of adding catalysts in the traditional method of lig

Method used

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  • Phenolic resin adhesive synthesized through in situ alkali lignin autocatalysis and preparation method of phenolic resin adhesive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Mix 50g of crushed bamboo with 50g of 2.0% dilute sulfuric acid solution with a mass fraction of sulfuric acid, stir and heat at 70°C for 4h, then filter, wash with 6L deionized water until nearly neutral, and dry in an oven Obtain filter residue.

[0032] (2) Take 8 g of the above-mentioned bamboo residues treated with dilute sulfuric acid, add 72 g of 5.0 mol / L KOH to a 100 mL reactor, and react at 110° C. for 3 h. Then carry out suction filtration, and the filtrate is the alkali lignin stock solution.

[0033] (3) Blend 100 mL of the above-mentioned alkali lignin stock solution with 5 g of phenol, heat up to 90° C., and heat and stir for 0.5 h to obtain a phenolized modified alkali lignin solution;

[0034] (4) Add 2.0 g of formaldehyde solution to the above-mentioned phenolized modified alkali lignin solution, and perform in-situ polymerization at 90° C. for 3 hours;

[0035] (5) Add 0.4 g of urea to the above in-situ polymerization solution, react at 70° C. f...

Embodiment 2

[0038] (1) Mix 50 g of crushed rice straw with 250 g of dilute sulfuric acid solution with a sulfuric acid mass fraction of 7.0%, stir and heat at 85°C for 3 hours, then filter, wash with 6L deionized water until nearly neutral, and dry in an oven Obtain filter residue.

[0039](2) Take 8 g of the above-mentioned rice straw treated with dilute sulfuric acid, add 48 g of 6.0 mol / L NaOH to a 100 mL reactor, and react at 70° C. for 6 h. Then carry out suction filtration, and the filtrate is the alkali lignin stock solution.

[0040] (3) Blend 100 mL of the above-mentioned alkali lignin stock solution with 7.5 g of phenol, heat up to 70° C., heat and stir for 4.0 h, and obtain a phenolized modified alkali lignin solution;

[0041] (4) Add 2.4 g of formaldehyde solution to the above-mentioned phenolized modified alkali lignin solution, and perform in-situ polymerization at 80° C. for 0.5 h;

[0042] (5) Add 0.35g of urea to the above in-situ polymerization solution, react at 80°C...

Embodiment 3

[0045] (1) Mix 50 g of crushed rice husk with 400 g of dilute sulfuric acid solution with a sulfuric acid mass fraction of 6.0%, stir and heat at 95° C. for 2 h, then filter, wash with 6 L of deionized water until nearly neutral, and dry in an oven Dry to obtain a filter residue.

[0046] (2) Take 8g of the above-mentioned rice husks treated with dilute sulfuric acid, add 64g of 1.0mol / L Ca(OH) 2 In a 100mL reactor, react at 90°C for 9h. Then carry out suction filtration, and the filtrate is the alkali lignin stock solution.

[0047] (3) Take the above-mentioned 100mL alkali lignin stock solution and blend it with 6.0g phenol, raise the temperature to 80°C, heat and stir for 1.5h, and obtain a phenolized modified alkali lignin solution;

[0048] (4) Add 1.5 g of formaldehyde solution to the above-mentioned phenolized modified alkali lignin solution, and perform in-situ polymerization at 85° C. for 0.5 h;

[0049] (5) Add 0.3 g of urea to the above in-situ polymerization sol...

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Abstract

The invention discloses a phenolic resin adhesive synthesized through in situ alkali lignin autocatalysis. A preparation method of the phenolic resin adhesive comprises the following processes of (1) crushing a biomass material, pickling by using a sulfuric acid, filtering and drying to obtain a filter residue; (2) fully reacting an alkali liquor with the filter residue and then filtering to obtain an alkali lignin liquid; (3) directly adding phenol to the alkali lignin liquid, carrying out phenolic in situ modified reaction; (4) directly adding a formaldehyde solution to a phenolized lignin solution and carrying out molecular in situ polymerization; and (5) adding a little of formaldehyde capture agent urea, further reacting, dewatering and discharging to obtain the lignin-modified phenolic resin adhesive. The processes of alkali lignin molecular extraction and in situ modification and in situ synthesis of the phenolic resin adhesive are continuous and the efficiency is greatly improved. Meanwhile, a catalyst does not need to be added in the processes of in situ modification and synthesis of alkali lignin to form phenolic resin, so that autocatalytic reaction is achieved.

Description

technical field [0001] The invention relates to the fields of materials and chemical industry, in particular to a phenolic resin adhesive obtained by extraction of alkali lignin molecules, in-situ autocatalytic modification and autocatalytic synthesis and a preparation method thereof. Background technique [0002] In today's world, as a non-renewable resource, the price of petroleum continues to soar, which leads to higher and higher production costs of phenolic resin adhesives. As one of the important raw materials of phenolic resin adhesives, the price of phenol has remained high for a long time. In order to reduce the production cost of phenolic resin adhesives, finding other cheaper raw materials to replace phenol has become a very popular research topic at present. With the continuous development of society, green environmental protection is more required by all parties in the society. For this reason, it has become a trend to use more natural polymers instead of phenol...

Claims

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Application Information

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IPC IPC(8): C09J161/32C08G14/12C08H7/00
CPCC08G14/12C08H6/00C09J161/32
Inventor 石刚李赢白绘宇王大伟倪才华周雪映
Owner JIANGNAN UNIV
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