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 hydro

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0041] Example 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 well and let stand for 12h, dry at 110℃ for 12h, and roast in muffle furnace at 350℃ 3h, get the silicotungstic acid carrier (STA / SiO 2 ); Then the copper nitrate (Cu(NO 3 ) 2 ·6H 2 O, 10.5g) and 35ml of water to make an aqueous solution, the STA / SiO 2 Add the above aqueous solution, immerse for 12h, and calcinate at 350℃ for 6h to prepare the catalyst Cu / STA / SiO 2 .

[0043] Weigh 8 g of the above catalyst and place it in a continuous-flow fixed-bed reactor. First, the catalyst was reduced at 300°C in a hydrogen-containing atmosphere for 6 hours, and the temperature was reduced to 190°C. Then, glycerin vapor diluted with hydrogen (hydrogen / glycerol molar ratio was 140) was introduced, and the glycerol mass space velocity was 0.1h -1 , The glycerin raw material contains 5wt% water, the reaction pressure is 0.36MPa, the...

Example Embodiment

[0044] Example 2

[0045] Weigh 8 g of the catalyst in Example 1 above and place it in a continuous-flow fixed-bed reactor. First, the catalyst was reduced at 300°C in a hydrogen-containing atmosphere for 6 hours, and then cooled to 210°C. Then, hydrogen-diluted glycerin vapor (hydrogen / glycerol molar ratio at 140) was introduced, and the glycerol mass space velocity was 0.08h -1 , The glycerin raw material contains 15wt% water, the reaction pressure is 0.36MPa, the glycerol conversion rate is 91.4%, the 1,3-propanediol selectivity is 23.8%, and the 1,2-propanediol selectivity is 18.9%.

Example Embodiment

[0046] Example 3

[0047] First, weigh 30gZrO 2 Powder (homemade, specific surface 56m 2 / g), add ammonium metatungstate aqueous solution (6.3g+40ml water), keep stirring at 40℃ water area for 8h, then stand for 4h, filter off the supernatant, dry at 110℃ for 12h, and heat it in a muffle furnace at 420℃ Calcined for 3h to obtain a carrier with tungstic acid (WO 3 / ZrO 2 ); Then the copper nitrate (Cu(NO 3 ) 2 ·6H 2 O, 7.6g) mixed with 15ml water to form an aqueous solution, and WO 3 / ZrO 2 Add the above aqueous solution, immerse for 12h, calcine at 420℃ for 6h to prepare the catalyst Cu / WO 3 / ZrO 2 , Forming into 20-40 mesh before use.

[0048] The reaction conditions were the same as in Example 1. The reaction results: the conversion rate of glycerol was 32.1%, the selectivity of 1,3-propanediol was 12.8%, and the selectivity of 1,2-propanediol was 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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