Technology for preparing micro-molecular phenolic compound through microwave reinforced continuous degradation of lignin in hydrogen donor

A technology of phenolic compounds and lignin, which is applied in the field of microwave-enhanced continuous degradation of lignin in a hydrogen donor to prepare small molecule phenolic compounds, can solve the problems of high reaction temperature, long reaction time, and large energy consumption, and achieve the goal of reaction Speed ​​increase, to solve the effect of discontinuous response

Inactive Publication Date: 2013-05-01
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the hydrogenolysis technology of solid acid and hydrogen donor can be used to degrade lignin to obtain higher yields of phenolic compounds, there are still problems such as high reaction temperature, long reaction time, discontinuous preparation process, and high energy consumption. There is still a considerable distance from large-scale industrialization

Method used

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  • Technology for preparing micro-molecular phenolic compound through microwave reinforced continuous degradation of lignin in hydrogen donor
  • Technology for preparing micro-molecular phenolic compound through microwave reinforced continuous degradation of lignin in hydrogen donor
  • Technology for preparing micro-molecular phenolic compound through microwave reinforced continuous degradation of lignin in hydrogen donor

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Effect test

Embodiment 1

[0031] Lignin is continuously added to the microwave-enhanced continuous degradation reactor by a pump through a solid feeding system, tetralin and p-toluenesulfonic acid, wherein the mass ratio of lignin, tetralin and p-toluenesulfonic acid is 30:60:1, Continuous degradation reaction at 180°C for 20 minutes; the degradation product is neutralized with NaOH aqueous solution in the neutralization tank of the degradation product separation device, and enters the primary settling tank and the secondary settling tank successively, and the primary settling tank and the lower layer of the secondary settling tank The products were combined, and the aqueous phase product was obtained by filtration, and then the pH was adjusted to 2~3 with hydrochloric acid in the acidification tank to obtain a small molecular phenolic compound. The product was analyzed by GC-FID, and the yield of the small molecular phenolic compound was calculated as 15.8%. The upper layer of the secondary settling t...

Embodiment 2

[0033] Lignin is continuously fed into the microwave-enhanced continuous degradation reactor through a solid feeding system, decahydronaphthalene and hydrochloric acid through a pump, wherein the mass ratio of lignin, decahydronaphthalene and hydrochloric acid is 30:30:1, and is continuously degraded at 150°C React for 40 min; the degradation product is neutralized with NaOH aqueous solution in the neutralization tank of the degradation product separation device, and enters the primary sedimentation tank and the secondary sedimentation tank successively, and the lower layer products of the primary sedimentation tank and the secondary sedimentation tank are combined and filtered to obtain The water phase product was then adjusted to pH 2~3 with hydrochloric acid in the acidification tank to obtain small molecular phenolic compounds. The product was analyzed by GC-FID, and the yield of small molecular phenolic compounds was calculated to be 2.9%. The upper layer of the secondary ...

Embodiment 3

[0035] Lignin is continuously fed into the microwave-enhanced continuous degradation reactor through a solid feeding system, dihydroanthracene and sulfuric acid through a pump, wherein the mass ratio of lignin, dihydroanthracene and sulfuric acid is 50:150:1, and it is continuously degraded at 160°C Reacted for 35 min; the degradation product was neutralized with NaOH aqueous solution in the neutralization tank of the degradation product separation device, and entered into the primary sedimentation tank and the secondary sedimentation tank successively, and the lower layer products of the primary sedimentation tank and the secondary sedimentation tank were combined, and obtained The water phase product was then adjusted to pH 2~3 with hydrochloric acid in the acidification tank to obtain small molecular phenolic compounds. The product was analyzed by GC-FID, and the yield of small molecular phenolic compounds was calculated to be 13.5%. The upper layer of the secondary settling...

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Abstract

The invention discloses a technology for preparing a micro-molecular phenolic compound through the microwave reinforced continuous degradation of lignin in a hydrogen donor. The technology comprises the following steps: 1, continuously adding lignin to a microwave reinforced screw rod continuous degradation reacting device through a solid charging system, continuously adding the hydrogen donor and a catalyst to the continuous degradation reacting device through pumps, and carrying out a continuous degradation reaction of lignin at 150-200DEG C for 10-40min; 2, neutralizing degradation products in a neutralization pool in a degradation product separation device with an aqueous solution of NaOH, allowing the neutralized degradation products to enter a primary settling pool and a secondary settling pool, mixing lower-layer products of the primary settling pool and the secondary settling pool, filtering to obtain a water-phase product, using hydrochloric acid in an acidifying pool to adjust the pH to 2-3 in order to obtain the micro-molecular phenolic compound; and 3, filtering a used hydrogen donor which is the upper-layer product of the secondary settling pool, and regenerating in a Pd / C catalytic fixed bed hydrogenation device to obtain a regenerated hydrogen donor for cycle use. The technology which adopts continuous operation enables the treatment amount to be large and is suitable for the large-scale industrial application.

Description

technical field [0001] The invention relates to a process for preparing small-molecular phenolic compounds through continuous degradation of microwave-enhanced lignin in a hydrogen-donating agent. Background technique [0002] Lignin is a precious resource endowed by nature to human beings. It is the third natural organic matter after cellulose and chitin. It is estimated that 150 billion tons of lignin can be produced by plant growth in the world every year. Lignin is an aromatic polymer compound composed of phenylpropane structural units connected by ether bonds and carbon-carbon bonds. The three basic phenylpropane structural units are guaiacylpropane, syringylpropane and p-hydroxybenzene propane, as shown in the molecular formula. Therefore, lignin is the only raw material from which renewable aromatic compounds can be obtained from natural resources. The effective utilization of lignin will achieve huge economic and social benefits in industries such as agriculture, f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/52C07C39/02C07C45/67C07C47/58C07C47/565C07C41/18C07C43/23
Inventor 傅杰潘晶莹李音吕秀阳
Owner ZHEJIANG UNIV
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