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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

Active Publication Date: 2010-06-23
SYNFUELS CHINA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although the above methods can obtain higher yields, these methods are all carried out in the liquid phase and require the use of a large amount of organic solvents, which not only increases the difficulty of subsequent separation, but also increases the cost and causes environmental pollution.
[0008] The present inventor has found through a large number of researches to adopt the gas-phase hydrogenolysis reaction process, using glycerol or glycerol aqueous solution as raw material, under mild reaction conditions, by using non-noble metal catalysts, 1,3-propanediol can be prepared in a higher yield, thereby overcoming the above-mentioned The patented catalyst is too expensive, the yield of 1,3-propanediol is low, a large amount of organic solvent is used, and the reaction conditions are harsh.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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%.

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Abstract

The invention relates to a method for producing 1,3-propanediol with glycerol as material by way of gas phase hydrogenolysis of glycerol, which includes the following step that: under the existence of metal-acid bifunctional catalyst, the glycerol receives gas phase hydrogenolysis, so that the 1,3-propanediol is prepared; and the invention also relates to the application of the metal-acid bifunctional catalyst in the reaction for preparing the 1,3-propanediol by way of gas phase hydrogenolysis of glycerol. The metal-acid bifunctional catalyst contains the following components loaded on carrier: (a) solid acidic active component, (b) metal component (one of copper, nickel or cobalt) with hydrogenation activity, and (c) optionally added metal addition agent component (one or more of iron, zinc, tin, manganese and chromium). The method can directly obtain the 1,3-propanediol by way of hydrogenolysis, as well as 1,2-propanediol. The method has the advantages of mild reaction conditions, simple technique and continuous operation.

Description

technical field [0001] The invention relates to a method for preparing 1,3-propanediol, in particular, the invention relates to a method for preparing 1,3-propanediol by direct gas-phase hydrogenolysis of glycerol. Background technique [0002] 1,3-propanediol is one of the important monomers for the synthesis of new polyester PTT. PTT has excellent performance due to its helical structure, which combines the softness of nylon, the bulkiness of acrylic fiber and the stain resistance of polyester, plus its inherent elasticity, moderate glass transition temperature and good processing performance. The excellent properties of the fiber are integrated, so the production of 1,3-propanediol has been widely concerned (Petrochemical Industry, 2006, 35, 597). In addition, 1,3-propanediol is also used in food, pharmaceutical, cosmetics, antifreeze and other industries. [0003] There are many processes for the production of 1,3-propanediol. At present, the processes widely used in ...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/60B01J23/888B01J27/185
Inventor 朱玉雷李永旺黄龙
Owner SYNFUELS CHINA TECH CO LTD
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