US 12,234,214 B2
Method for continuously synthesizing 5-hydroxymethylfurfural by using micro-channel reactor
Kai Zhu, Nanjing (CN); Yiping Huang, Nanjing (CN); Meng Hu, Nanjing (CN); Changhai Yue, Nanjing (CN); Jingjing Huang, Nanjing (CN); Shuangtao Li, Nanjing (CN); Kai Guo, Nanjing (CN); and Zheng Fang, Nanjing (CN)
Assigned to CHINA CONSTRUCTION INDUSTRIAL & ENERGY ENGINEERING GROUP CO., LTD, Nanjing (CN)
Filed by CHINA CONSTRUCTION INDUSTRIAL & ENERGY ENGINEERING GROUP CO., LTD., Nanjing (CN)
Filed on Jul. 19, 2024, as Appl. No. 18/778,902.
Application 18/778,902 is a continuation of application No. PCT/CN2022/131016, filed on Nov. 10, 2022.
Claims priority of application No. 202211231876.8 (CN), filed on Sep. 30, 2022.
Prior Publication US 2024/0376064 A1, Nov. 14, 2024
Int. Cl. C07D 307/48 (2006.01); B01J 19/00 (2006.01)
CPC C07D 307/48 (2013.01) [B01J 19/0013 (2013.01); B01J 19/0093 (2013.01)] 5 Claims
OG exemplary drawing
 
1. A method for continuously synthesizing 5-hydroxymethylfurfural by using a micro-channel reactor, wherein the micro-channel reactor comprises a T-shaped micro-mixer and a capillary tube, a T-shaped channel inside the T-shaped micro-mixer communicates with three ports correspondingly, a port corresponding to one end of a vertical channel is connected with a syringe I, the syringe I is mounted on a syringe pump I, an aqueous glucose solution is conveyed into the T-shaped micro-mixer under an action of the syringe I and the syringe pump I, two ports corresponding to two ends of a horizontal channel are connected one-to-one with a syringe II and the capillary tube, respectively, the syringe II is mounted on a syringe pump II, and methyl butyl ketone is conveyed into the T-shaped micro-mixer under an action of the syringe II and the syringe pump II; another end of the capillary tube is provided with a back pressure valve;
wherein, specific steps for continuously synthesizing 5-hydroxymethylfurfural are as follows:
formulating an aqueous glucose solution containing FeCl3 and HCl, separately conveying the aqueous glucose solution and methyl butyl ketone to a T-shaped micro-mixer, then enabling a aqueous glucose solution phase and a methyl butyl ketone phase to flow in the capillary tube in a segmented flow manner while performing a 5-hydroxymethylfurfural synthesis reaction, and collecting a reaction product flowing out of the capillary tube, wherein 5-hydroxymethylfurfural generated by the reaction is present in an organic phase of the reaction product;
wherein, a volume ratio of the aqueous glucose solution to methyl butyl ketone conveyed into the T-shaped micro-mixer is 1:(3˜5); an inner diameter of the capillary tube is 200˜1000 μm;
wherein the 5-hydroxymethylfurfural synthesis reaction in the capillary tube is carried out at a temperature of 150˜170° C. for 12˜20 min under a pressure of 0.5˜1.2 MPa.