阅读说明：本技术 一种H-Beta催化玉米秸秆制备5-羟甲基糠醛的方法 (Method for preparing 5-hydroxymethylfurfural from corn straws under catalysis of H-Beta ) 是由 李晓云 梁敏 段冰瑜 于 2019-10-11 设计创作，主要内容包括：本发明属于生物质化工领域,特别涉及一种H-Beta催化玉米秸秆制备5-羟甲基糠醛的方法。该方法主要包括以下步骤：玉米秸秆、H-Beta和γ-戊内酯/水溶剂按照一定质量比加入反应釜中,在电加热130～190℃温度条件下,磁力搅拌反应1～8h,反应结束后,冷却至室温,通过离心进行固液分离即得。该方法使用H-Beta联合γ-戊内酯/水溶剂的反应方法,具有催化活性高、产物分离简单、催化剂和溶剂易回收,环境友好等优点,整个方法操作简单,易于操作,具有良好的应用前景。(The invention belongs to the field of biomass chemical industry, and particularly relates to a method for preparing 5-hydroxymethylfurfural by catalyzing corn straws with H-Beta. The method mainly comprises the following steps: adding corn straw, H-Beta and gamma-valerolactone/water solvent into a reaction kettle according to a certain mass ratio, reacting for 1-8H under the condition of electric heating at the temperature of 130-190 ℃, cooling to room temperature after the reaction is finished, and performing solid-liquid separation by centrifugation to obtain the corn stalk and gamma-valerolactone/water solvent. The method uses a reaction method combining H-Beta and gamma-valerolactone/water solvent, has the advantages of high catalytic activity, simple product separation, easy recovery of catalyst and solvent, environmental protection and the like, and has simple operation, easy operation and good application prospect.)

1. A method for preparing 5-hydroxymethylfurfural by catalyzing corn straws with H-Beta is characterized by comprising the following characteristic steps:

(1) mixing corn straws, H-Beta and gamma-valerolactone-water solution, putting the mixture into a reaction kettle, and stirring and reacting for 1-8 hours at the temperature of 130-190 ℃;

(2) after the reaction is finished, cooling to room temperature, and carrying out solid-liquid separation by centrifugation to obtain the catalyst.

2. The method for preparing 5-hydroxymethylfurfural from corn stalks under the catalysis of H-Beta according to claim 1, wherein the H-Beta molecular sieve is synthesized by adopting a mixed template agent.

3. The method for preparing 5-hydroxymethylfurfural from corn stalks under the catalysis of H-Beta according to claim 1, wherein the mass ratio of the corn stalks to the H-Beta is (0.2-20) to 1, the volume ratio of gamma-valerolactone to water is (1-30) to 1, and the feed-liquid ratio of the corn stalks to the gamma-valerolactone-water solution is (mass g: volume ml) is 1 to (40-120).

4. The method for preparing 5-hydroxymethylfurfural from corn stalks under the catalysis of H-Beta according to claim 1, wherein the magnetic stirring speed in the step (1) is 500-1000 rpm.

Technical Field

The invention relates to a method for preparing 5-hydroxymethylfurfural from corn straws under the catalysis of H-Beta, and belongs to the technical field of biomass chemical industry.

Background

The molecular formula of the 5-hydroxymethylfurfural is C₆H₆O₃The relative molecular weight of 126.1 is light yellow, and the compound contains a furan ring, a hydroxymethyl group and an aldehyde group in the molecule, so that the compound has good reactivity, can be used for preparing various derivatives such as 2, 5-dimethylfuran, levulinic acid, 2, 5-difurandicarboxylic acid and the like, and can also be used for synthesizing furan products such as furan resin, furan asphalt cement and the like. Therefore, 5-hydroxymethylfurfural is widely applied to the fields of fine chemical engineering, pharmacy and the like as an important fine compound.

The method for preparing 5-hydroxymethylfurfural mainly takes glucose, fructose, starch, cellulose and the like as raw materials and adopts concentrated sulfuric acid as a catalyst to prepare the 5-hydroxymethylfurfural. The preparation of 5-hydroxymethylfurfural by using concentrated sulfuric acid has the advantages of short time, high yield and the like, but has the problems of serious equipment corrosion, complex process, more byproducts, difficult catalyst recovery, environmental pollution and the like, the whole process flow has high requirements on the quality of equipment and generates a large amount of acidic waste liquid and sulfur-containing solid waste, and although the hydrolysis reaction can be normally and effectively carried out, the analysis on the environmental protection, the economy and the ecology of the whole production process is not suitable for large-scale production and does not meet the requirements of green chemical industry.

The gamma-valerolactone is a green solvent derived from biomass, has the characteristics of low melting point, high boiling point, good stability and the like, and can promote the conversion of the corn straws into the 5-hydroxymethylfurfural. In a gamma-valerolactone/water mixed solvent, the clean production of 5-hydroxymethylfurfural is realized by the self-catalysis of an acid site of an H-Beta molecular sieve, the generation of waste acid, waste water and waste gas is greatly reduced, and the separation of the catalyst from a target product and the separation of the target product from the solvent are simple and convenient to operate, easy to implement and strong in operability.

Disclosure of Invention

The invention aims to provide a method for preparing 5-hydroxymethylfurfural from corn straws under the catalysis of H-Beta.

The technical scheme of the invention is summarized as follows:

(1) mixing corn straws, H-Beta and gamma-valerolactone-water solution, putting the mixture into a reaction kettle, and stirring and reacting for 1-8 hours at the temperature of 120-200 ℃; (2) after the reaction is finished, cooling to room temperature in a water bath, and carrying out solid-liquid separation by centrifugation to obtain the catalyst.

The corn straw used in the step of preparing the 5-hydroxymethylfurfural is ensiled corn straw.

The catalyst H-Beta used in the preparation step of the 5-hydroxymethylfurfural is synthesized by adopting a mixed template method.

In the step of preparing the 5-hydroxymethylfurfural, the mass ratio of the corn straws to the H-Beta is (0.2-20) to 1, the volume ratio of the gamma-valerolactone to the water is (1-30) to 1, and the material-liquid ratio of the corn straws to the gamma-valerolactone/water mixed solvent is (mass g: volume ml) 1 to (40-120).

The stirring speed in the 5-hydroxymethylfurfural preparation step is 500-1000 rpm.

The invention has the following remarkable advantages:

the method for producing 5-hydroxymethylfurfural has low corrosion to equipment, can be implemented in a common hydrothermal reaction kettle, is simple to operate, has high catalyst stability, and can be recycled. The whole reaction condition is mild, the later-stage product is easy to separate from the catalyst, the yield of the 5-hydroxymethylfurfural is high, the solvent is easy to recover, the requirement of green chemistry can be met, and the method has a good application prospect.

Detailed Description

The present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited to these specific examples. Various substitutions and alterations can be made without departing from the technical idea of the invention as described above, according to the common technical knowledge and conventional means in the field, and the scope of the invention is covered.