Method and system for continuously preparing 5-hydroxymethylfurfural and derivative thereof

A technology of hydroxymethyl furfural and alkoxymethyl furfural, applied in chemical instruments and methods, separation methods, chemical/physical processes and other directions, can solve the problems affecting the high yield generation of target products and the like

Active Publication Date: 2017-12-22
CHINA AGRI UNIV
View PDF9 Cites 13 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] There are active structures such as aldehyde groups, cyclic ethers, and dienes in the molecular structure of 5-HMF and alkoxymethylfurfural, which are aromatic, and can undergo hydration and polymerization at high temperatures or in the presence of catalysts (such as acids, alkalis, etc.) Side reactions such as levulinic acid and humins (humins) are generated, which seriously affects the high yield generation of the target product
In summary, there is also a lack of 5-hydroxymethylfurfural (5-HMF) and derivative 5-alkoxymethylfurfural (5-alkoxymethylfurfural) and its derivatives 5-hydroxymethylfurfural (5-HMF) that can be continuous, low-cost, and have commercial application prospects. AMF) preparation technology

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method and system for continuously preparing 5-hydroxymethylfurfural and derivative thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0101] 5-HMF was prepared by using fructose as raw material and HCl as catalyst.

[0102] An acid and alkali-resistant steel pipe with outer diameter OD=15.8mm, pipe wall thickness d=1.25mm, and pipe volume V=20ml is selected as the reaction device. The polar reaction phase consisted of 28ml water + 12ml DMSO. The non-polar extract phase consisted of 24ml methyl isobutyl ketone + 16ml 2-butanol. The concentration of fructose in the polar reaction phase was 5 wt.%. The concentration of HCl in the polar reaction phase is 0.2mol / L. The flow rate of the reaction solution was 10 ml / min (empty time = 2 min). The reaction temperature is 170° C., the reaction time is 30 minutes, and the reaction column pressure is 0.1 Mpa. The polar reaction liquid undergoes a full cycle reaction in the reaction device and the extraction device. After the reaction, the conversion rate of fructose was detected by high performance liquid chromatography to be 99%, and the selectivity of 5-HMF was 93...

Embodiment 2

[0104] 5-HMF was prepared with fructose as raw material and H3PO4 as catalyst.

[0105] Choose the same reaction device and reaction conditions as in Example 1. Change the catalyst to 0.2mol / L H3PO4. After the reaction, the conversion rate of fructose was detected by high performance liquid chromatography to be 98%, and the selectivity of 5-HMF was 91%.

Embodiment 3

[0107] 5-HMF was prepared with fructose as raw material and phosphotungstic acid as catalyst.

[0108] Choose the same reaction device and reaction conditions as in Example 1. Change the catalyst to 0.2mol / L phosphotungstic acid. After the reaction, the conversion rate of fructose was detected by high performance liquid chromatography to be 100%, and the selectivity of 5-HMF was 86%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention relates to a method and a system for continuously preparing 5-hydroxymethylfurfural (5-HMF) and a derivative 5-alkoxymethylfurfural (5-AMF) thereof with hexose or hexose-containing biomass as a material. The method takes the characteristic of thermal instability in a target product into full consideration and utilizes the characteristic of distinct polarity difference between the product and the material, a reaction unit and an extraction unit are separated in the process of preparing the 5-HMF and the 5-AMF, the biomass material reacts along with a polar reaction phase under high temperature and existence of a catalyst, the produced product flows out of reaction environment in time, and after being cooled, the product is extracted and retained by a non-polar extraction phase under normal temperature and pressure. The insufficiently reacting material or a polar intermediate product is retained in the polar reaction phase, and enters the reaction unit again to form circulation until the reaction is sufficient. In order to increase the distribution ratio and extraction efficiency of the product, a certain amount of inorganic salt can be added into a polar solvent. The method and the device effectively increase the selectivity and yield of the target product, and remarkably reduce the energy consumption of the whole preparation process. Material resources applicable to the method and the system are wide, including soluble monosaccharide, insoluble lignocellulose and the like. Pickiness about catalysts is avoided, and homogenous and heterogeneous catalysts which are commonly used in such reaction are all applicable to the method and the system.

Description

technical field [0001] The invention relates to the fields of chemistry and chemical industry, in particular to a continuous preparation of platform compound 5-hydroxymethylfurfural (5-HMF) and its derivative 5-alkoxymethanol using hexose or biomass containing hexose as raw material A method and apparatus for furfural (5-AMF). Background technique [0002] 5-Hydroxymethylfurfural (5-HMF) is an important biomass-based platform compound, which can replace the current petrochemical raw materials for the preparation of high-quality fuel oil, polymer monomers, pharmaceutical intermediates, etc. It has important application potential in production. 5-HMF can be produced from hexose or carbohydrates containing hexose through hydrolysis, isomerization, dehydration and other reactions. Carbohydrates containing hexose sugars, such as cellulose, inulin, starch, etc., are widely found in nature, and the annual renewable amount is huge. 5-HMF and low-carbon alcohols, such as methanol,...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/46B01J8/00B01J3/04B01J8/06B01D3/00B01D3/10B01D11/04
CPCB01D3/009B01D3/10B01D11/04B01J3/04B01J8/006B01J8/0085B01J8/025B01J8/06C07D307/46
Inventor 王洪亮朱万斌崔宗均王小芬袁旭峰程序
Owner CHINA AGRI UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products