Method for preparing single benzene ring phenolic compound from alkali lignin

A technology for monophenol and alkali lignin, which is applied in the field of catalytic conversion of lignin to prepare monophenol compounds, can solve the problems of inability to realize continuous flow reaction, increase the difficulty of catalyst recycling and product separation, etc. Low, mild reaction conditions, low energy consumption

Inactive Publication Date: 2012-03-14
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

The reaction between solid lignin and solid catalyst in a fixed-bed reactor is actually a batch reaction, which cannot achieve continuous flow reaction; and as the reaction time progresses, coking and polymerization will form carbon deposits on the catalyst bed, which increases catalyst recovery and utilization. The difficulty of product separation

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  • Method for preparing single benzene ring phenolic compound from alkali lignin

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Embodiment 1

[0018] Preparation of Au nanoparticle catalysts. Add 1 mL of 1% by weight HAuCl hydrate to 100 mL of water with constant stirring 4 ·3H 2 O. After 10 minutes, 1 ml of 1% by weight sodium citrate hydrate was added. After 10 minutes of addition, an additional 1 mL of 0.075% by weight NaBH was added 4 , the solution was stirred continuously for 5 minutes, and stored for future use.

[0019] Transfer the prepared catalyst into a 300 ml reaction kettle, add 5.0 grams of alkali lignin (kraft lignin) and 3.0 grams of potassium carbonate, feed hydrogen replacement three times, heat to 120 ° C, open the hydrogen inlet valve, and the pressure stabilization of the inlet The valve is adjusted to 6.0MPa. After reacting for 10 hours, stop the reaction, cool, adjust the pH value to 7, extract three times with ethyl acetate, 50 mL each time, after combining, use gas chromatography to analyze the product distribution, remove ethyl acetate with rotary evaporation, and weigh it as the total...

Embodiment 2

[0021] Preparation of Ni nanoparticle catalysts. (1) The preparation of hydrazine hydrate / NaOH solution is as follows: 1.0M NaOH solution is added dropwise to 100 mL of 85% hydrazine hydrate solution until the pH value is 13. (2) Mix 150mL of n-hexane, 30g of surfactant CTAB, and 40mL of n-hexanol, and add the hydrazine hydrate / NaOH solution dropwise under stirring until clear, forming a hydrazine hydrate microemulsion. (3) Preparation of 0.5M NiCl 2 Solution 100mL. (4) Mix 150mL n-hexane, 30g surfactant CTAB, and 30mL n-hexanol, and add 0.5M NiCl dropwise under stirring 2 solution until clear as NiCl 2 Microemulsion. (5) Put the NiCl2 microemulsion bottle into an oil bath with a temperature of 70° C., quickly add the hydrazine hydrate microemulsion, continue stirring for 1 hour, cool down, and set aside. Measure 100mL of catalyst solution, adopt the reaction method of Example 1. The reaction results are shown in Table 1.

Embodiment 3

[0023] Preparation of Ru nanoparticle catalysts. Weigh 1.8g of PVP K-30, dissolve it in 100ml of water, and stir for 15 minutes. Weigh RuCl 3 ·xH 2 O 120mg was dissolved in 4mL water, and mixed with PVP solution, the reaction temperature was 90°C, the reaction time was 12 hours, the hydrogen flow rate was 30mL / min, cooled, and set aside. Adopt the reaction method of embodiment 1. The reaction results are shown in Table 1.

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Abstract

A method for preparing single benzene ring phenolic compounds by catalytic conversion of alkali lignin. Hydrogen is added into water phase to degrade alkali lignin into single benzene ring phenolic compound, under a reaction temperature of 90-180 DEG C, a hydrogen pressure of 1.0-10.0MPa and under effect of a metal nanoparticle catalyst; and alkali compound is added into the reaction. The metal nanoparticle catalyst is one or more selected from Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag or Au in any ratio. The method has mild reaction conditions, low energy consumption, low costs, high operating safety and easily separated products.

Description

technical field [0001] The invention relates to a method for catalytically converting lignin to prepare monobenzene ring phenolic compounds. Background technique [0002] Biomass mainly includes agricultural straw and forest biomass. In nature, lignin is an important component of biomass (approximately 15-30% by weight, 40% of energy), which is regenerated at a rate of 50 billion tons per year. The pulp and paper industry of lignin separates about 140 million tons of cellulose from plants every year, and at the same time obtains about 50 million tons of lignin products, but so far, more than 95% of lignin is still discharged directly into the "black liquor" The rivers or rivers are burned after being concentrated, and are rarely used effectively, resulting in waste of resources and environmental pollution. Lignin is a polymer composed of monomers derived from phenylpropane, a complex phenolic polymer formed from four alcohol monomers (p-coumaryl alcohol, coniferyl alcohol,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/52C07C39/04C07C39/07C07C43/23C07C41/01
Inventor 王峰徐杰宋奇于维强
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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