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Novel method for preparing lignosulphonate epoxy resin

A technology of lignosulfonate and epoxy resin, which is applied in the field of biomass material manufacturing adhesive, can solve the problems of complex phenolization process and intermediate products, limited source of raw materials, harsh processing conditions, etc. Complex treatment, the effect of improving mechanical properties

Inactive Publication Date: 2011-08-31
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (2) The phenolization process and intermediate products are complex and have side reactions
[0007] (3) The pretreatment conditions of raw materials are harsh, and a large amount of alcohols are used as solvents, which are obtained after high-temperature and high-pressure cooking, and the source of raw materials is limited

Method used

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  • Novel method for preparing lignosulphonate epoxy resin
  • Novel method for preparing lignosulphonate epoxy resin
  • Novel method for preparing lignosulphonate epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Dissolve 16 grams of lignosulfonate in 160ml of water, filter and remove insoluble impurities to obtain lignosulfonate solution; measure 150ml of lignosulfonate solution, add to N 2 In the three-necked flask protected and reflux condensed, add 1.5ml of 50wt% hydrobromic acid and 0.6000g of cetyltributylphosphine bromide catalyst, the temperature is controlled at 60°C, react for 1 hour, use ethyl acetate to extract, water The solvent was removed by washing to obtain 25 g of the phenolated product, which was 2 Add 25g of epichlorohydrin to the obtained phenolated product under protective conditions, control the temperature at 60°C, add 2.5ml of 10wt% sodium hydroxide alkaline solution dropwise, and remove the solvent and unreacted epichlorohydrin after 2h. N 2 Under protective conditions, 20ml of toluene solvent was added to fully dissolve, and 2.5ml of 10wt% sodium hydroxide alkaline solution was added dropwise, and reacted at a temperature of 70° C. for 3 hours to obta...

Embodiment 2

[0026] Dissolve 16 grams of lignosulfonate in 160ml of water, filter and remove insoluble impurities to obtain lignosulfonate solution; measure 150ml of lignosulfonate solution, add to N 2 In the three-necked flask protected and reflux condensed, add 75ml of 50wt% hydrobromic acid and 0.6000g of cetyltrimethylammonium bromide catalyst, the temperature is controlled at 150°C, react for 12 hours, extract with ethyl acetate, wash with water method to remove the solvent to obtain 25g phenolated product, in N 2 Add 75g of epichlorohydrin to the obtained phenolated product under protective conditions, control the temperature at 80°C, add 20ml of 10wt% sodium hydroxide alkaline solution dropwise, and remove the solvent and unreacted epichlorohydrin after 3h. 2 Under protective conditions, 20ml of toluene solvent was added to fully dissolve, and 20ml of 10wt% sodium hydroxide alkaline solution was added dropwise, and reacted at a temperature of 70° C. for 3 hours to obtain a lignosulf...

Embodiment 3

[0028] Dissolve 16 grams of lignosulfonate in 160ml of water, filter and remove insoluble impurities to obtain lignosulfonate solution; measure 150ml of lignosulfonate solution, add to N 2 In the three-necked flask of protection and reflux condensation, add 35ml 45wt% hydroiodic acid and 0.6000g polyethylene glycol-600 catalyst, the temperature is controlled at 100°C, react for 6 hours, use ethyl acetate extraction, water washing method to remove solvent, Obtain 25g phenolated product, in N 2 Add 45g epichlorohydrin to the obtained phenolated product under protective conditions, control the temperature at 70°C, add dropwise 10ml of 10wt% potassium hydroxide alkaline solution, and after 3h, remove the solvent and unreacted epichlorohydrin, N 2 Under protective conditions, 20ml of toluene solvent was added to fully dissolve, and 10ml of 10wt% potassium hydroxide alkaline solution was added dropwise, and reacted at a temperature of 70° C. for 3 hours to obtain a lignosulfonate ep...

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Abstract

The invention discloses a novel method for preparing lignosulphonate epoxy resin, which comprises the following steps of: dissolving lignosulphonate in water to remove impurities, adding Lewis acid and catalyst, reacting at 60-150 DEG C, purifying the phenolate product by using the methods of extraction and washing, and synthesizing the epoxy resin by the lignin phenolate and the epoxy chloropropane under the alkaline condition. The preparation method has the advantages of wide material source, simple preparation process, low price and wide application range, and avoids using a large amount of alcohol solvents.

Description

technical field [0001] The invention belongs to the technical field of using biomass materials to manufacture adhesives, and in particular relates to a new method for preparing lignin epoxy resin by using lignosulfonate obtained from papermaking waste liquid as a raw material and undergoing phenolization modification. Background technique [0002] In nature, the reserve of lignin is second only to cellulose, and it is regenerated at a rate of 50 billion tons every year. The pulp and paper industry separates about 140 million tons of cellulose from plants every year, and at the same time obtains about 50 million tons of lignin by-products. But so far, the by-products of lignin are seldom used effectively, causing serious environmental pollution and waste of resources. Lignin is the only non-petroleum resource that can provide renewable aromatic compounds in nature. Its quantity is second only to cellulose, and it is the second largest natural polymer material. [0003] Epox...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/02C08H6/00C08H7/00
Inventor 郭红霞王群李春生
Owner BEIJING UNIV OF TECH
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