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Method for preparation of phenolic compound by direct hydrogenolysis of lignin

A technology of phenolic compounds and lignin, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of harsh equipment requirements, low yield of phenols, high price, etc., and achieve mild equipment requirements, No need for high temperature and high pressure, easy to operate

Inactive Publication Date: 2015-01-14
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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AI Technical Summary

Problems solved by technology

[0005] Most of the above-mentioned hydrogenolysis of lignin requires an external hydrogen source, and it is carried out under high temperature and high pressure conditions. The requirements for equipment are relatively strict and energy consumption is large.
Although the reaction conditions are relatively mild in a few reports, the yield of phenols is low, or the presence of a high-boiling reaction medium is required, or tetrahydronaphthalene is used as a hydrogen donor, and the price of this hydrogen donor is relatively expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Weigh 1g of lignin and 0.05g of palladium chloride catalyst in an autoclave, add 10mL of methanol, ultrasonicate, and mix well. 200 ° C hydrogenolysis reaction 3h. After centrifugation and cyclohexane extraction to separate the supernatant, the product was analyzed by GC-MS, the conversion rate of lignin was 58%, and the selectivity of phenols was 89%. Phenols are mainly 4-propyl guaiacol, 4-propyl syringyl alcohol, 4-propyl phenol, propylene guaiacol, syringyl alcohol, propylene phenol phenolic compounds; other products are dimerization body compound.

[0013] Quantitative analysis of the internal standard: use durene as the internal standard, and its quality is constant. According to the ratio of the peak area of ​​the phenolic component to the peak area of ​​durene, the mass of the phenolic component in the product can be obtained, thereby obtaining the conversion rate of lignin. The selectivity of phenols is calculated by the following formula.

[0014] The form...

Embodiment 2

[0017] Weigh 1g of lignin and 0.1g of ammonium tungstate catalyst in an autoclave, add 10mL of methanol, ultrasonicate, and mix well. 200 ° C hydrogenolysis reaction 3h. Centrifuge, extract and separate the supernatant with cyclohexane, the product is analyzed by GC-MS, the conversion rate of lignin is 59%, and the selectivity of phenols is 92%. The lignin conversion rate and the selectivity of phenols are the same as in Example 1.

Embodiment 3

[0019] Weigh 1g of lignin and 0.1g of palladium chloride catalyst in an autoclave, add 10mL of ethylene glycol, ultrasonicate, and mix well. 200 ° C hydrogenolysis reaction 3h. Centrifuge, extract and separate the supernatant with cyclohexane, the product is analyzed by GC-MS, the conversion rate of lignin is 51%, and the selectivity of phenols is 87%. The lignin conversion rate and the selectivity of phenols are the same as in Example 1.

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Abstract

The invention relates to a method for preparation of a phenolic compound by lignin direct hydrogenolysis adopting hydrogen produced in situ by a solvent as a hydrogen donor under catalysis effects. The method comprises the following steps of adding lignin, catalysts and a solvent into a pressure-resistant container, carrying out a reaction process at a temperature of 150-350 DEG C for 1-20h and carrying out filtration and extraction separation. The method has a lignin conversion rate of more than 50% and phenol selectivity of more than 85% and can produce main products such as 4-propylguaiacol, 4-propylsyringol, 4-propylphenol, propenylguaiacol, syringol and allylphenol. The catalysts used by the method comprise palladium chloride, ruthenium chloride, cobaltous chloride, phospho-tungstic acid, nickel molybdate, barium molybdate, Pd / TiO2, Ru / TiO2 and Au / TiO2, a mass ratio of lignin to the catalysts is in a range of 1: 0.03 to 1: 1 and a mass ratio of lignin to the hydrogen donor is in a range of 1: 50 to 1: 150. The related lignin hydrogenolysis process has a simple technology and can be used for production of high-added value phenolic compounds by a biomass route.

Description

technical field [0001] The invention belongs to the field of biomass refining, and in particular relates to a method for preparing phenolic compounds through direct hydrogenolysis of lignin. Background technique [0002] With global warming and decreasing of chemicals and liquid fuels, energy and environmental issues have increasingly become the focus of attention of people from all walks of life. Fossil energy is non-renewable, and biomass as a renewable resource that can be converted into liquid fuels and chemicals will become a development trend. Lignin is one of the important components of biomass, and it is a natural organic matter second only to cellulose in stock. However, its utilization rate is quite low. More than 95% of lignin is produced in the form of papermaking by-products or waste products, and a small part is used for combustion to obtain heat energy, resulting in waste of resources and environmental pollution. Efficient use of lignin has become a hot topi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/23C07C41/18C07C39/06C07C39/19C07C37/52
CPCC07C37/52C07C41/18
Inventor 王峰张晓辰徐杰王业红王敏张超锋张哲
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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