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Method of taking microalgae as raw material to prepare 5-hydroxymethyl furfural

A technology of hydroxymethylfurfural and microalgae, applied in the direction of organic chemistry, can solve the problems of difficult separation, recycling and reuse of inorganic acids, high cost of preparation of ionic liquids, low cost and greenness, etc., to achieve easy cultivation, solidification The effect of high carbon efficiency and easy localization

Active Publication Date: 2015-11-25
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are many problems in the above-mentioned researches, such as the difficulty of separation and recycling of inorganic acids, serious corrosion of reaction equipment, environmental pollution, high preparation costs of ionic liquids, and the harmfulness of free chromium salts to the environment, etc., thus limiting its use. Further industrial application; at the same time, the reaction raw materials are pure carbohydrates or terrestrial primary biomass, and there are relatively few studies on the preparation of HMF from aquatic biomass (such as algae)
[0004] Chinese patent (CN103508985A) discloses a method for producing furfural and / or HMF using red algae biomass as raw material. Red Antelope, Gracilaria and Eucheuma, but their raw materials need to be cleaned and crushed pretreatment, the catalyst is an inorganic acid and a certain amount of ionic liquid is used as a reaction solvent, which cannot meet the requirements of low cost and greenness

Method used

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  • Method of taking microalgae as raw material to prepare 5-hydroxymethyl furfural
  • Method of taking microalgae as raw material to prepare 5-hydroxymethyl furfural

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The experiments were carried out in a Parr autoclave with a volume of 100 ml. First add 0.5g Scenedesmus and 50mL deionized water in the reaction kettle, the solid-to-liquid ratio is 1g:100mL, wherein, the carbohydrate content of Scenedesmus is 65.00% (mass percentage), and the N content is 0.5% (mass percentage), The S content is 0% (mass percentage). After adding 0.2g of SAPO-34 catalyst, the reactor was sealed, and high-purity nitrogen was introduced to replace the air in the reactor, and the initial relative partial pressure of nitrogen was set to 1MPa, and the stirring speed was controlled at 600r / min. After the heating started, the temperature rose to 160°C at a rate of 15K / min, and the reaction lasted for 480min, then the heating was stopped and cooled to room temperature. After the reaction solution was centrifuged, the solid residue was dried overnight in an oven at 100° C., and the centrifuged supernatant was passed through a 0.22 μm microfilter for HPLC quan...

Embodiment 2

[0039] The specific implementation process is the same as in Example 1, except that the raw material added is chlorella, the carbohydrate content of chlorella is 50.24wt%, the N content is 0.3wt%, and the S content is 0.2wt%. Add 2.5g of Chlorella and 50mL of reaction solvent (composed of water and methyl isobutyl ketone, the volume ratio is 4:6), the solid-to-liquid ratio is 5g:100mL, and 2g of HZSM-5 catalyst is added at the same time; the reaction temperature is stabilized at 180°C , the reaction time was shortened to 360min, and the initial partial pressure of nitrogen was set at 1.4MPa. After the reaction is finished, the hydrothermal conversion rate of the chlorella reaches 75.3%, and the HMF yield reaches 26.7%.

Embodiment 3

[0041] The specific implementation process is the same as in Example 1, except that the added raw material is salina, the carbohydrate content of salina is 40.00wt%, the N content is 0.18wt%, and the S content is 0.35wt%. The quality of the salt algae added is 5g, the reaction solvent is 50mL (composed of water and toluene, the volume ratio is 3:7), the solid-liquid ratio is 10g:100mL, and the mass of 3g of Hβ catalyst is added at the same time, the temperature of the system is raised to 200 ° C, and the reaction time The time was shortened to 240min, and the initial partial pressure of nitrogen was set at 1.6MPa. After the reaction is finished, the hydrothermal conversion rate of the salina reaches 92.8%, and the HMF yield reaches 38.6%.

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Abstract

The invention provides a method of taking microalgae as a raw material to prepare 5-hydroxymethyl furfural. The method includes the following steps: taking microalgae as the raw material; allowing hydrolysis dehydration under action of reaction solvent and solid acid catalyst to generate 5-hydroxymethyl furfural. 5-hydroxymethyl furfural which is a platform compound and has high added value is obtained by utilizing microalgae which is an environment-friendly renewable biomass resource, so that efficient biological fixation and catalytic conversion of CO2 through microalgae are realized, hydrolysis dehydration is mild in condition, process is simple, the raw material is high in conversion rate and high in selectivity to 5-hydroxymethyl furfural which is a target product, and the catalyst is renewable and reusable after simple solid-liquid separation.

Description

technical field [0001] The invention relates to a method for preparing 5-hydroxymethylfurfural, in particular to a method for preparing 5-hydroxymethylfurfural by directly hydrolyzing and dehydrating microalgae as raw materials. Background technique [0002] With the increasingly prominent contradiction between supply and demand of global petrochemical resources, finding and developing resources and methods that can replace petroleum has become a common problem faced by the scientific and technological circles and industrial circles. Biomass resources have become one of the preferred materials to replace petrochemical resources due to their huge amount, renewability and high energy content. In the conversion process of biomass resources, 5-hydroxymethylfurfural (HMF) is an important platform compound, an important raw material and a key intermediate for the preparation of petrochemical products such as fuels, polyesters, and polyamide plastics. Therefore, the efficient conv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/46
CPCC07D307/46
Inventor 孙予罕王健健孔令照魏伟苗改朱春春汪靓李晋平孙志强王东飞
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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