Progress Report Li Wei 2013.10.11. Synthesis of DMC MN synthesis: DMC synthesis: side reactions: MN DMC.

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Presentation transcript:

Progress Report Li Wei

Synthesis of DMC MN synthesis: DMC synthesis: side reactions: MN DMC

PdCl 2 -CuCl 2 /AC preparation 0.05g PdCl 2 and ?g CuCl 2 24~25ml 5mol/L HCl Heat-dissolving 3g AC Rotary Steaming at 85 ℃ Dry at 120 ℃ for 4 h Then calcination at 200 ℃ for 4h PdCl 2 -CuCl 2 /AC Pd:1wt% Cu:Pd=?:1 (mole ratio) Immerse 85 ℃ 4h Excessive impregnation Cu/Pd (mole ratio) 1:1 、 1.2:1 、 1.6:1 、 2:1 、 etc

GHSV=8000 h -1 T=110 ℃ ， P=0.1MPa(Gauge pressure) CO/MN=1:6 （ MN=20% ）， N 2 （ HCl ） Experiment

GHSV=8000 h -1 T=110 ℃ ， P=0.1MPa(Gauge pressure) CO/MN=1:6 （ MN=20% ）， N 2 （ HCl ） Experiment

GHSV=8000 h -1 T=110 ℃ ， P=0.1MPa(Gauge pressure) CO/MN=1:6 （ MN=20% ）， N 2 （ HCl ） Cu:Pd=1.2:1

GHSV=4000 h -1 T=110 ℃ ， P=0.1MPa(Gauge pressure) CO/MN=1:6 （ MN=20% ）， N 2 （ HCl ）

Cu:Pd=1.2:1 GHSV=3000 h -1 T=110 ℃ ， P=0.1MPa(Gauge pressure) CO/MN=1:6 （ MN=20% ）， N 2 （ HCl ）

Cu:Pd=1.2:1 CO:MN=1:6/1:4/1:2 GHSV=4000 h -1 T=110 ℃ ， P=0.1MPa(Gauge pressure) CO/MN=1:6/1:4/1:2 （ MN=20% ）， N 2 （ HCl ）

GHSV=4000 h -1 T=110 ℃ ， P=0.1MPa(Gauge pressure) CO/MN=1:6/1:4/1:2 （ MN=20% ）， N 2 （ HCl ） Cu:Pd=1.2:1 CO:MN=1:6/1:4/1:2

GHSV=4000 h -1 T=110 ℃ ， P=0.1MPa(Gauge pressure) CO/MN=1:6/1:4/1:2 （ MN=20% ）， N 2 （ HCl ）

Work plan 1. Optimization of process conditions 1.1 CO/MN （ Volume ratio ）： 1:6 、 1:4 、 1:2 （ MN=20% ） GHSV=3000 h -1 ， T=110 ℃ ， P=0.1MPa(Gauge pressure) ， N 2 （ HCl ） 1.2 T （℃）： 100 、 110 、 120 GHSV=3000 h -1 ， P=0.1MPa(Gauge pressure) ， CO/MN=1:6 （ MN=20% ）， N 2 （ HCl ） 1.3 P （ MPa ， Gauge pressure ）： 0.1 、 0.2 、 0.3 GHSV=3000 h -1 ， T=110 ℃ ， CO/MN=1:6 （ MN=20% ）， N 2 （ HCl ）

Work plan 2. Preparation of Catalyst 2.1 Loading of active components 1.Solvent H 2 O 、 HCl 、 NH 3 ▪ H 2 O 、 CH 3 OH 2. Loading of active components Incipient impregnation 、 Excessive impregnation

Work plan 2.2 AC pretreatment Chemical treatments ⑴ Redox modification ① HNO 3 、 H 2 O 2 ② H 2 ⑵ Acid and alkali treatments ① HCl ② NaOH 、 KOH ③ NaOH+HCl 、 KOH+HCl Thermal treatments ① N 2 ： 600 ℃、 700 ℃、 900 ℃ ② H 2 ： 600 ℃、 700 ℃、 900 ℃

Thank you