Rapid synthesis method of biomass-based aromatic alcohol

A technology based on aromatic alcohols and synthesis methods, which is applied in the field of rapid synthesis of biomass-based aromatic alcohols, can solve problems such as environmental pollution, and achieve the effects of improving safety and economy, high alkali content, hydrophobicity, and good divergence

Pending Publication Date: 2022-07-29
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these calcium sources are usually thrown away as waste, causing environmental pollution

Method used

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  • Rapid synthesis method of biomass-based aromatic alcohol
  • Rapid synthesis method of biomass-based aromatic alcohol
  • Rapid synthesis method of biomass-based aromatic alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: Rapid synthesis method of biomass-based veratrol

[0034]Veratroaldehyde (0.5 mmol), eggshell-derived catalyst (1.8 mol %), solvent DMSO (2 mL), hydrogen source diphenylsilane (1.1 equivalents of H - ) and naphthalene (0.015 g) as an internal standard were added to a 15 ml pressure-resistant tube, the reactor was sealed and placed in an oil bath that had been raised to a specified temperature, and the reaction time was set. After the reaction stopped, 1 mL of water was added to quench the reaction. The liquid mixture was filtered with a filter membrane (pore size: 0.22 μm) before qualitative and quantitative analysis and was diluted by adding 3 mL of DMSO-free, and then identified by gas chromatography-mass spectrometry (Agilent 6890 nitrogen gas chromatography / 5973 mass spectrometry), and all products were identified by gas chromatography (Agilent 7890B) Analysis was performed using an HP-5 column (30 m x 0.320 mm x 0.25 micron) equipped with a flame ioniza...

Embodiment 2

[0035] Example 2: Preparation of Waste-Derived Calcium-Based Catalysts

[0036] Collect discarded egg shells, shells or bones, and wash them with deionized water for 3 to 5 times to remove the attached dust and impurities; manually remove the shell membrane, and use distilled water to wash some viscous organic substances on the inner surface again; Dry in an oven at ~100 °C for 8 ~ 10 h; then in a muffle furnace at a temperature of 400 ~ 1000 °C in air for 1 ~ 3 h to prepare a CaO catalyst. A mixture of CaO, glycerol and methanol with a molar ratio of 1:9:80 was added to a round-bottomed flask equipped with a magnetron, a thermometer and a reflux condenser, and the mixture was heated to 60-100 °C and stirred for 6-10 h. The obtained precipitate was centrifuged and washed with methanol and then dried to obtain a waste-derived calcium-based catalyst.

Embodiment 3

[0037] Embodiment 3: the rapid synthetic method of biomass-based veratrol

[0038] The catalyst was replaced with a bone-derived catalyst (1.8 mol%), and the others were the same as in Example 1. The conversion rate of veratrol (97.4%) was determined, and the yield of veratrol was 95.4%.

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Abstract

The invention discloses a rapid synthesis method of biomass-based aromatic alcohol, which comprises the following steps: by taking a biomass-based aromatic aldehyde compound as a substrate, dimethyl sulfoxide (DMSO) as a solvent and silane as a hydrogen source, reacting the biomass-based aromatic aldehyde compound with silane under the action of a waste-derived calcium-based catalyst (an egg shell-derived catalyst, a bone-derived catalyst or a shell-derived catalyst) to obtain the biomass-based aromatic alcohol. The biomass-based aromatic aldehyde compound is hydrogenated into a corresponding alcohol compound with high selectivity. The catalyst used in the system reaction is a waste derived catalyst, the reaction time is greatly shortened, the temperature is mild, the target product selectivity is remarkably improved, the conversion rate of veratraldehyde in representative reaction can reach 99.8%, and the veratryl alcohol yield can reach 99.6%.

Description

technical field [0001] The present invention relates to a kind of synthetic method of aromatic alcohol, in particular to a kind of fast synthesis method of biomass-based aromatic alcohol. Background technique [0002] With the over-exploitation and utilization of non-renewable fossil fuels in the traditional chemical industry, the accompanying problems such as energy depletion and environmental pollution have prompted mankind to explore and develop renewable energy. As the most abundant organic carbon resource, biomass shows considerable potential in the manufacture of biofuels and valuable chemicals. It has been reported that lignin peroxidase secreted by decay fungi can effectively degrade most endocrine disruptors that typically cause environmental pollution. As one of lignin derivatives, veratrol is a small metabolic molecule produced by many white rot fungi, which can significantly increase the activity of lignin peroxidase. In addition, furfuryl alcohol is a very imp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/14C07C41/26C07D213/30C07D307/42C07D307/44C07D333/16B01J31/26B01J31/02B01J23/02C07C43/23C07C33/32C07C33/22
CPCC07C41/26C07D307/44C07C29/14C07D307/42C07D333/16C07D213/30B01J23/02B01J31/26B01J31/0202B01J2231/643C07C43/23C07C33/32C07C33/22
Inventor 李虎简玉梅
Owner GUIZHOU UNIV
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