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Lignin modified thermoplastic phenolic resin and preparation method thereof

A technology of phenolic resin and lignin, which is applied in the field of thermoplastic phenolic resin, can solve the problems of low phenol substitution rate and low chemical activity, and achieve the effects of improving reactivity, increasing the number of total hydroxyl groups, and increasing substitution rate

Active Publication Date: 2013-01-16
SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For this reason, the purpose of the present invention is to overcome the defects of low chemical activity of lignin and low substitution rate of lignin to phenol in the lignin modification process of phenolic resin existing in the prior art, thereby providing a method for preparing thermoplastic Phenolic resin method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Preparation of rare earth metal oxide / activated carbon catalyst

[0049] 0.1135kg Ce(NO 3 ) 3 ·6H 2 O was dissolved in 500ml of 1mol / L dilute nitric acid, and then 0.3kg of activated carbon was added, fully stirred at room temperature, impregnated for 5 hours, and then vacuum-dried at 30, 70, and 120°C for 6 hours respectively. Before the catalytic reaction, the catalyst Activation at 200 and 350 °C for 1 hour under the protection of nitrogen flow in a tubular resistance furnace, respectively, to obtain CeO with a loading capacity of 15% by weight of the carrier 2 / C Catalyst.

[0050] (2) Preparation of lignin-modified thermoplastic phenolic resin

[0051] Mix the extracted 10kg catechol with 2kg sulfuric acid lignin (Shandong Huatai Paper Co., Ltd.), and then add 0.1kg CeO 2 / C catalyst, stir evenly, then slowly heat the mixture to 160°C, and activate the reaction at 160°C for 0.5 hours; after the activation reaction is completed, add 10kg of ethanol to the m...

Embodiment 2

[0054] (1) Preparation of rare earth metal oxide / activated carbon catalyst

[0055] 0.0378kg Ce(NO 3 ) 3 ·6H 2 O was dissolved in 500ml of 1mol / L dilute nitric acid, and then 0.3kg of activated carbon was added, fully stirred at room temperature, impregnated for 5 hours, and then vacuum-dried at 30, 70, and 120°C for 6 hours respectively. Before the catalytic reaction, the catalyst Activation at 200 and 350 °C for 1 hour under the protection of nitrogen flow in a tube resistance furnace, respectively, to obtain CeO with a loading capacity of 5% by weight of the carrier 2 / C Catalyst.

[0056] (2) Preparation of lignin-modified thermoplastic phenolic resin

[0057] Mix the extracted 10kg phenol with 5kg enzymatic lignin (Shandong Longli Biotechnology Co., Ltd.), and then add 1kg CeO 2 / C catalyst, stir evenly, then slowly heat the mixture to 120°C, and activate the reaction at 120°C for 3 hours; , filter with filter paper to remove insoluble matter and recover the filtrat...

Embodiment 3

[0060] (1) Preparation of rare earth metal oxide / activated carbon catalyst

[0061] 0.06375kg La(NO 3 ) 3 ·6H 2 O was dissolved in 500ml of 1mol / L dilute nitric acid, and then 0.3kg of activated carbon was added, fully stirred at room temperature, impregnated for 5 hours, and then vacuum-dried at 30, 70, and 120°C for 6 hours respectively. Before the catalytic reaction, the catalyst Activation at 200 and 350 °C for 1 hour under the protection of nitrogen flow in a tubular resistance furnace, respectively, to obtain La with a loading capacity of 8% by weight of the carrier. 2 o 3 / C Catalyst.

[0062] (2) Preparation of lignin-modified thermoplastic phenolic resin

[0063] Mix the extracted 10kg phenol with the high boiling alcohol lignin (Jiang Tingda, Lignin, Chemical Industry Press, 2008, 12:98) of 3kg corn stalks, and then add 0.2kg La 2 o 3 / C catalyst, stir evenly, then slowly heat the mixture to 100°C, and activate the reaction at 90°C for 5 hours; after the activ...

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Abstract

The invention relates to lignin modified thermoplastic phenolic resin which is characterized in that the thermoplastic phenolic resin is prepared by a component A and a component B through polycondensation. The component A is a product obtained through an activating reaction on lignin by using a phenolic compound and rare-earth oxide / an activated carbon catalyst, and the component B is an acid catalyst and an aldehydes compound. A carrier of the rare-earth oxide / the activated carbon catalyst is activated carbon, and active component loaded on the activated carbon is the rare-earth oxide. The invention further relates to a method for preparing the lignin modified thermoplastic phenolic resin. The method is that the rare-earth oxide / the activated carbon catalyst is added to increase absolute quantity of phenolic hydroxyl groups and alcoholic hydroxyl groups of the lignin, increase of phenolic hydroxyl group quantity can substantially improve reactivity of the lignin, and a substitution rate of the lignin on phenol is improved.

Description

technical field [0001] The invention relates to the field of thermoplastic phenolic resins, in particular to a method for preparing lignin-modified thermoplastic phenolic resins. Background technique [0002] Thermoplastic phenolic resin is produced by reacting phenol and formaldehyde with a molar ratio of less than 1 under the action of an acidic catalyst. Thermoplastic phenolic resin (or called two-step phenolic resin), is a light-colored to dark brown brittle solid, soluble in ethanol, acetone and other solvents, and has long-term solubility. Thermoplastic phenolic resin can be used to manufacture various friction materials such as disc plates, drum plates, friction blocks, clutch faces, brake bands, and train brake shoes. However, phenol is a chemical raw material obtained from petroleum and other resources. With the gradual reduction of petroleum resources and the rise of petroleum prices, the price of phenol continues to rise. Therefore, it is extremely urgent to find...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28C08L61/14C08H7/00
Inventor 唐一林江成真焦峰李枝芳姜广锋邢介名董岳
Owner SHANDONG SHENGQUAN NEW MATERIALS CO LTD
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