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Method for preparing methyl levulinate from acidified montmorillonite catalyzed biomass sugar

A technology of methyl levulinate and biomass sugar, which is applied in the field of organic synthesis, can solve the problems of complex preparation, harsh conditions, and expensive raw materials, and achieve the effects of simple preparation, mild reaction conditions, and easy-to-obtain raw materials

Inactive Publication Date: 2016-04-06
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although some solid acid catalysts have high catalytic activity, the raw materials are expensive, the preparation is complicated, and the conditions are harsh.

Method used

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  • Method for preparing methyl levulinate from acidified montmorillonite catalyzed biomass sugar
  • Method for preparing methyl levulinate from acidified montmorillonite catalyzed biomass sugar
  • Method for preparing methyl levulinate from acidified montmorillonite catalyzed biomass sugar

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The preparation method of the hydrogen-type montmorillonite is as follows: 1g of K10-montmorillonite is added to 50ml of sulfuric acid solution (the mass concentration of the sulfuric acid solution is 20%), heated to 100°C and stirred for 0.5 to 2 hours, then stop heating and continue Stir for 0.5-1 hour. The obtained mud was filtered, washed several times with deionized water to remove sulfuric acid, and then dried at 120°C for a day and night to obtain H-MMT. The final gray powder was named 20-H-MMT.

[0024] The sulfuric acid solution concentration of 20% was replaced by 5%, 10% or 30%, and the finally obtained gray powder was named 5-H-MMT, 10-H-MMT or 30-H-MMT respectively. And all of them can be used as catalysts to catalyze the preparation of methyl levulinate from biomass sugar.

Embodiment 2

[0026] The preparation method of the sulfated montmorillonite is as follows: 1g of K10-montmorillonite is added to 50ml of sulfuric acid solution (the mass concentration of sulfuric acid solution is 20%), heated to 100°C, stirred and reacted for 0.5 to 2 hours, and the heating is stopped Stirring was continued for 0.5-1 hour. The obtained mud was filtered and then calcined at 500 °C for 5 h to obtain SO 4 2- / MMT. The final powder was named 20-SO 4 2- / MMT (wherein 20 represents that the mass concentration of the sulfuric acid solution used is 20%), can be used as a catalyst to catalyze the preparation of methyl levulinate from biomass sugar.

[0027] image 3 Give the 20-SO that this embodiment makes 4 2- / MMT catalyst XRD patterns.

[0028] Replace 20% of the mass concentration of sulfuric acid with 5%, 10% or 30%, and the final powders are named 5-SO 4 2- / MMT, 10-SO 4 2- / MMT or 30-SO 4 2- / MMT. And all of them can be used as catalysts to catalyze the prepar...

Embodiment 3

[0030] 0.18g (1mmol) glucose and 20-SO4 roasted at 500°C for 5h 4 2- / MMT catalyst 0.15g and anhydrous methanol 20ml were placed in a 30mL autoclave, sealed the autoclave, and reacted at 200°C for 4 hours, and filtered to obtain the methyl levulinate solution after the autoclave was cooled, and added the internal standard Naphthalene (16mg), to be tested.

[0031] figure 1 The gas chromatogram of the product methyl levulinate is given and compared with the gas chromatogram of the methyl levulinate standard. figure 2 The mass spectrum of the product methyl levulinate is given, and compared with the mass spectrum of the methyl levulinate standard.

[0032] The obtained solution was detected by gas chromatography-mass spectrometry (GC-MS model is TRACEDSQ). According to the concentration-peak area standard curve and the product peak area, the molar yield of methyl levulinate in the product of Example 3 can be calculated to be 48%.

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Abstract

The invention relates to a method for preparing methyl levulinate from biomass saccharide by using acidified montmorillonite as a catalyst, belonging to the technical field of organic synthesis. According to the method, biomass saccharide and methanol used as raw materials react in a reaction kettle at 160-220 DEG C for 2-5 hours by using sulfated montmorillonite or hydrogen-type montmorillonite as a solid acid catalyst to synthesize the methyl levulinate. The sulfated montmorillonite or hydrogen-type montmorillonite is prepared by the following steps: treating montmorillonite with sulfuric acid, filtering, washing with water, and calcining. The invention provides a new solid acid catalyst and new reaction route for converting biomass saccharide into methyl levulinate, and the methyl levulinate can be prepared by using the simple catalyst under mild conditions. The methyl levulinate can be widely used as an important platform compound in the biomass conversion process, and can be used as a food additive, essence, gasoline additive, biofuel or the like.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for preparing methyl levulinate based on acidified montmorillonite catalyzed biomass sugar, which uses acidified montmorillonite as a solid acid catalyst to convert biomass under mild conditions Preparation of methyl levulinate from sugar. Background technique [0002] The quest to produce chemicals and fuels from renewable resources has received much attention over the past few decades due to a number of reasons including global warming, fluctuations in oil supply, increasing crude oil prices and existing regulations restricting the use of non-renewable resources. Among these renewable resources, the conversion of biomass sugars to more valuable products (such as levulinic acid or methyl levulinate) has attracted much attention due to the wide variety of sources and forms of biomass sugars. [0003] As an important platform compound in the process...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/716C07C67/00
CPCB01J21/16B01J27/02C07C67/00C07C69/716
Inventor 田戈徐兴良张显龙冯守华邹伟健
Owner JILIN UNIV
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