Method for producing 1,3-propanediol
A technology of propylene glycol and glycerol, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems of harsh reaction conditions, low yield, and increased cost, etc. Achieve high conversion and selectivity, high catalyst activity, and mild reaction conditions
Examples
Embodiment 1
[0042] First, weigh 30g SiO 2 (Qingdao Ocean Chemical Factory, 20-40 mesh), add silicotungstic acid (STA) aqueous solution (5.3g+50ml water), stir evenly, let stand for 12h, dry at 110°C for 12h, then bake in a muffle furnace at 350°C 3h, the carrier (STA / SiO 2 ); then copper nitrate (Cu(NO 3 ) 2 ·6H 2 O, 10.5g) and 35ml water are made into an aqueous solution, and STA / SiO 2 Add the above aqueous solution, impregnate for 12h, and bake at 350°C for 6h to prepare the catalyst Cu / STA / SiO 2 .
[0043] Weigh 8 g of the above-mentioned catalyst and place it in a continuous-flow fixed-bed reactor. Firstly, the catalyst was reduced for 6 hours in a hydrogen-containing atmosphere at 300°C, cooled to 190°C, and then glycerin vapor diluted with hydrogen (hydrogen / glycerol molar ratio was 140), and the mass space velocity of glycerol was 0.1h -1 , the glycerol raw material contains 5 wt% of water, the reaction pressure is 0.36MPa, the conversion rate of glycerin is 56.9%, the selec...
Embodiment 2
[0045] Weigh 8 g of the catalyst in the above-mentioned Example 1 and place it in a continuous-flow fixed-bed reactor. Firstly, after the catalyst was reduced in a hydrogen-containing atmosphere at 300°C for 6h, the temperature was lowered to 210°C, and then hydrogen-diluted glycerol vapor (hydrogen / glycerin molar ratio was 140) was introduced, and the mass space velocity of glycerol was 0.08h. -1 , the glycerol raw material contains 15 wt% of water, the reaction pressure is 0.36MPa, the conversion rate of glycerin is 91.4%, the selectivity of 1,3-propanediol is 23.8%, and the selectivity of 1,2-propanediol is 18.9%.
Embodiment 3
[0047] First, weigh 30g of ZrO 2 Powder (self-made, specific surface 56m 2 / g), add it to ammonium metatungstate aqueous solution (6.3g+40ml water), keep stirring at 40°C for 8h, then let it stand for 4h, filter off the supernatant, dry at 110°C for 12h, then place it in a muffle furnace at 420°C Roasting 3h, obtains the carrier of loading tungstic acid (WO 3 / ZrO 2 ); then copper nitrate (Cu(NO 3 ) 2 ·6H 2 O, 7.6g) and 15ml water are made into aqueous solution, and WO 3 / ZrO 2 Add the above aqueous solution, impregnate for 12h, and bake at 420°C for 6h to prepare the catalyst Cu / WO 3 / ZrO 2 , Pressed to 20-40 mesh before use.
[0048] The reaction conditions are the same as those in Example 1, and the reaction results are as follows: glycerol conversion rate 32.1%, 1,3-propanediol selectivity 12.8%, 1,2-propanediol selectivity 32.2%.
PUM
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Description
Claims
Application Information
- IPC
- C07C31/20; C07C29/60; B01J23/888; B01J27/185
- Inventors
- 朱玉雷; 李永旺