公开(公告)号：EP4023633A1

公开(公告)日：2022-07-06

申请号：EP20913378.4

申请日：2020-12-11

申请人： Zhejiang University ,  Zhejiang University ,  Zhejiang NHU Special Materials Co., Ltd.

发明人： CHEN, Zhirong ,  WU, Wenbin ,  ZHOU, Guiyang ,  FENG, Ming ,  SHI, Xingxing ,  MA, Tao ,  FENG, Zhichao ,  ZHANG, Xiongwei ,  SUN, Qing ,  XU, Yong

IPC分类号： C07C253/10 ,  C07C255/04

摘要： Provided are a method and device for preparing adiponitrile. The method of the present disclosure comprises the steps of a first hydrocyanation reaction, an isomerization reaction and a second hydrocyanation reaction, wherein online Raman spectroscopy is used for detecting the content of a specific component in the system; and the reaction conditions are regulated based on the detection results, so as to achieve precise control of the materials in each step of the reaction system. The method of the present disclosure can reduce an amount of butadiene, thereby reducing the subsequent energy consumption needed for recycling butadiene and equipment investment after reaction; by monitoring the content of hydrocyanic acid in real time, the residue of hydrocyanic acid is reduced to a lower level, and the operation safety and the stability of a catalyst during reaction are improved; and the loss of the catalyst is reduced.

公开(公告)号：EP4190769A1

公开(公告)日：2023-06-07

申请号：EP22750655.7

申请日：2022-06-21

申请人： Zhejiang University ,  Zhejiang NHU Company Ltd. ,  Zhejiang NHU Special Materials Co., Ltd. ,  ZHEJIANG NHU NYLON MATERIALS CO., LTD.

发明人： CHEN, Zhirong ,  WU, Wenbin ,  YIN, Hong ,  ZHA, Zengshi ,  WANG, Keyan ,  MA, Li ,  HUANG, Guodong ,  ZHOU, Guiyang ,  XU, Yong

IPC分类号： C07C255/04 ,  C07C253/10 ,  B01J31/24 ,  C07F9/6571

摘要： The present disclosure relates to a use of a multidentate phosphite ligand in the catalytic synthesis of adiponitrile. The ligand is represented by the following general formula (I). The method of catalytic synthesis of adiponitrile comprises primary hydrocyanation, isomerization, and secondary hydrocyanation reactions, wherein the catalyst adopted each comprises a phosphite ligand-nickel complex composed of a nickel precursor and a multidentate phosphite ligand. The ligand molecule has a higher electron cloud density, and the phosphorus content capable of participating in coordination in the ligand molecule per unit mass is higher, so that the catalytic activity of the catalyst is improved, and the amount of the catalyst is reduced. Meanwhile, the steric and spatial configuration of the phosphite ligand-nickel complex may be adjusted by designing and optimizing the framework structure of the ligand, and the chemical environment and the steric effect around a metal center may be changed by the designing and optimizing mentioned above combine with flexibly regulating the electronic effect and the steric hindrance effect of a substituent on the molecular structure of the ligand, so that the selectivity of a linear product adiponitrile is improved.

公开(公告)号：EP4289855A1

公开(公告)日：2023-12-13

申请号：EP22755062.1

申请日：2022-06-29

申请人： Zhejiang NHU Company Ltd. ,  Zhejiang University ,  Zhejiang NHU Special Materials Co., Ltd. ,  ZHEJIANG NHU NYLON MATERIALS CO., LTD.

发明人： ZHA, Zengshi ,  CHEN, Zhirong ,  WU, Wenbin ,  ZHANG, Tinglan ,  YIN, Hong ,  WANG, Keyan ,  ZHOU, Litao ,  LI, Haoran ,  HUANG, Guodong ,  XU, Yong

IPC分类号： C07F9/141 ,  C07F9/145 ,  C07F9/572 ,  C07F9/6506 ,  C07F9/6584 ,  B01J31/02 ,  B01J31/06 ,  B01J35/08

摘要： A method for preparing a phosphorus-containing ligand is provided, which includes: mixing a phosphorus chloride compound, polypyridine ionic liquid-loaded porous microspheres with a first organic solvent to obtain a first mixture, and mixing a compound in Formula (2) with a second organic solvent to obtain a second mixture,

wherein Z is a multivalent aliphatic hydrocarbon group or a multivalent aromatic hydrocarbon group comprising at least one substituent group, wherein the substituent group is selected from hydrogen atom, halogen atom, C 1 -C 10 alkyl group, C 1 -C 10 alkoxy group, C 1 -C 10 alkanoyl group, aryl group, heteroaryl group, cyano group, or nitro group, and n is an integer from 1 to 8; and mixing the first mixture with the second mixture to make the first mixture react with the second mixture to obtain a reaction mixture, removing generated HCl, filtrating to obtain a filter liquor, and treating the filter liquor to obtain the phosphorus-containing ligand.