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Method for extracting phenolic compounds from biological oil

A technology for phenolic substances and bio-oil, which is applied in chemical instruments and methods, preparation of organic compounds, and ether separation/purification, etc., can solve the problems of difficult extraction, inability to separate phenolic substances, and no public reports, etc. simple craftsmanship

Inactive Publication Date: 2012-07-25
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Bio-oil is rich in phenol, 2-methoxyphenol, 2-methoxy-4-methylphenol, 2-methoxy-4-ethylphenol and other phenolic substances, all of which are important chemical raw materials. , how to extract these phenolic substances with higher added value from bio-oil has always been a difficult problem, and there has been no public report so far
Chinese patent 201010113843.4 discloses a method for separating bio-oil polygeneration by dual-solvent extraction. This method uses ether and dichloromethane as extraction agents to separate lignin components in bio-oil, but cannot further extract phenolic substances. isolated from lignin

Method used

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  • Method for extracting phenolic compounds from biological oil
  • Method for extracting phenolic compounds from biological oil
  • Method for extracting phenolic compounds from biological oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The bio-oil prepared by rapid cracking of pine sawdust was distilled, and the distillate at 120-260° C. contained dozens of mixed substances, as shown in Table 1, wherein the content of phenolic substances was 24.17% (molar ratio). Take 100ml of bio-oil distillate, drop into calcium chloride solution containing 0.3mol calcium ions, drop into NaOH solution to adjust the pH value to 8.5, shake and stir evenly in a water bath at 25°C, a complex precipitate is formed, after vacuum filtration , after the precipitate was acidified and replaced by 2.5mol / L hydrochloric acid solution, 10ml of ethyl acetate was added dropwise for extraction, the upper layer solution was extracted, and the extractant was distilled to finally obtain 0.4g of phenolic substances.

[0035] The sample is injected into GC-MS, and the composition of the bio-oil extract obtained by analysis is shown in Table 2 and figure 2 shown.

[0036] Table 2

[0037] peak number

[0038] Note: CaCl 2 A...

Embodiment 2

[0040] Similar to Example 1, take 100ml of bio-oil distillate, drop into calcium chloride solution containing 0.3mol calcium ions, drop into NaOH solution to adjust the pH value to 8.5, oscillate and stir evenly in a 75°C water bath, and complexes precipitate After vacuum filtration, the precipitate was acidified and replaced by 2.5mol / L hydrochloric acid solution, extracted by dropping 10ml of ethyl acetate, and the upper layer solution was extracted. After distilling the extractant, 2.8g of phenolic substances were finally obtained, indicating that In the solution treated in a 75°C water bath, the extraction rate of phenolic substances is increased by 6-7 times. The sample is injected into GC-MS, and the composition of the bio-oil extract obtained by analysis is shown in Table 3 and image 3 shown.

[0041] table 3

[0042] peak number

[0043] Note: CaCl 2 As a precipitant, 75 ° C extraction temperature, ethyl acetate as an extractant.

Embodiment 3

[0045] Similar to Example 1, take 100ml of bio-oil distillate, drop into magnesium chloride solution containing 0.3mol of magnesium ions, drop into NaOH solution to adjust the pH value to 8, oscillate and stir evenly in a 75°C water bath, and a complex precipitate is formed. After vacuum filtration, the precipitate was hydrolyzed and replaced by 1.5 mol / L hydrochloric acid solution, then extracted with 10 ml of ethyl acetate dropwise, the upper layer solution was extracted, and the extractant was distilled to finally obtain 3.4 g of powdered phenolic substances. The sample was injected into GC-MS, and the composition of the obtained bio-oil extract was shown in Table 4.

[0046] Table 4

[0047] peak number

[0048] Note: MgCl 2 As a precipitant, 75 ° C extraction temperature, ethyl acetate as an extractant.

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Abstract

The invention discloses a method for extracting phenolic compounds from a biological oil, and relates to an extraction process of the biological oil. The method comprises the steps of preprocessing the biological oil, and extracting a distillate containing phenolic compounds; adding a soluble salt into the extracted distillate containing phenolic compounds to obtain a solution A; adjusting a pH value of the solution A to be more than 7 so as to obtain a solution B; placing the solution B in a water bath and heating to obtain a complexing precipitate; collecting the complexing precipitate, and performing vacuum filtration to prepare a filter cake; placing the filter cake into hydrochloric acid to perform replacement, extracting with an extractant, and performing vacuum drying on the extract liquor to extract the phenolic compounds. By use of a soluble metal salt as a precipitant and an acetic acid ester or dichloromethane solution as the extractant, the phenolic compounds can be extracted from a biomass pyrolysis oil. Compared with the prior art, the method disclosed by the invention is simple in process, and the purities of the extracted phenolic compounds can be up to more than 96%.

Description

technical field [0001] The invention relates to a bio-oil extraction process, in particular to a method for extracting phenolic substances from bio-oil. Background technique [0002] The development of biomass energy technology and the reduction of dependence on crude oil have become the key to the sustainable development of my country's energy applications. Biomass energy, as the only renewable energy that can be converted into liquid fuel, ranks fourth in the world's total energy consumption after coal, oil and natural gas, and occupies an important position in the entire energy system. Biomass refers to all organic substances formed directly or indirectly by photosynthesis of green plants, including plants, animals, microorganisms and their excretion and metabolites other than fossil fuels. Biomass pyrolysis is an important aspect of biomass energy application technology. It can convert biomass raw materials, such as straw, wood chips, and agricultural product processing...

Claims

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Application Information

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IPC IPC(8): C07C43/23C07C41/44C07C39/04C07C39/06C07C39/07C07C37/86
Inventor 王夺刘运权吕东灿袁亮
Owner XIAMEN UNIV
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