Method for preparing 1,3-propylene glycol

A technology of propylene glycol and hydroxypropionaldehyde, which is applied in 1 field, can solve the problems of extremely toxic and highly irritating, flammable acrolein, and high price, and achieve the effects of reducing production costs, good safety, and increasing unit consumption

Inactive Publication Date: 2003-07-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The above route also has problems similar to those of the first route. The single-pass yield of 1,3-propanediol is low. In the two-step reaction of hydration and hydrogenation, it is necessary to control the concentration of products and reactants to make the use of the reactor more efficient. dramatically drop
In addition, acrolein is flammable, extremely toxic and highly irritating, and expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] This embodiment is the preparation of catalyst A.

[0025] (1) Put 20 grams of phosphorus (industrial pure) into the crucible, melt 80 grams of nickel (industrial pure) and pour it into the crucible containing phosphorus, nickel and phosphorus will alloy themselves, and Ni-P mother will be obtained after cooling alloy.

[0026] (2) Add 1 gram of molybdenum and 50 grams of aluminum (industrial pure) to 49 grams of Ni-P master alloy, then place it in a vacuum button furnace, and keep it for 20 minutes after melting, and the vacuum degree in the furnace is 10 -2 Torr, temperature 1200°C, filled with argon to normal pressure, to prepare Ni-Mo-P-Al alloy.

[0027] (3) Ni-Mo-P-Al alloy is obtained by quick quenching by vacuum quenching method, the quick quenching conditions are copper roll line speed 39 m / s, injection pressure 0.09MPa, injection temperature 1260°C;

[0028] (4) The prepared product is pulverized in a ventilated environment until the maximum particle size is...

Embodiment 2

[0031] This embodiment is the preparation of catalyst B.

[0032] (1) Put 20 grams of phosphorus (industrial pure) into the crucible, melt 80 grams of nickel (industrial pure) and pour it into the crucible containing phosphorus, nickel and phosphorus will alloy themselves, and Ni-P mother will be obtained after cooling alloy.

[0033] (2) Add 2 grams of iron and 50 grams of aluminum (industrial pure) to 48 grams of Ni-P master alloy, then place it in a vacuum button furnace, and keep it for 20 minutes after melting, and the vacuum degree in the furnace is 10 -2 Torr, temperature 1200°C, filled with argon to normal pressure, to prepare Ni-Fe-P-Al alloy.

[0034] (3) Ni-Fe-P-Al alloy or Ni-Mo-P-Al alloy obtained by rapid quenching by vacuum quenching method, the rapid quenching conditions are copper roller line speed 39 m / s, injection pressure 0.09MPa, injection temperature 1260 ℃;

[0035] (4) The prepared product is pulverized in a ventilated environment until the maximum p...

Embodiment 3

[0038] Dissolve 1.0mol of paraformaldehyde (calculated as formaldehyde) with 100ml of isooctyl alcohol as solution A, use an equal amount of xylene to extract 1.06mol of acetaldehyde from acetaldehyde aqueous solution with a concentration of 40wt% as solution B, and add 100ml to a 1L three-necked bottle Isooctyl alcohol, 0.44gKOH, stir at 15±2°C under normal pressure, drop A and B into it at the same time, stir after dropping, and react for 2.5 hours. The reaction product is distilled under reduced pressure to obtain 3-hydroxypropane aldehyde.

[0039] Add 300ml of 23% 3-hydroxy propionaldehyde aqueous solution in an autoclave with a loading capacity of 0.5L, the catalyst B addition is 5 grams, and react under the conditions of 60±2°C, 6.9MPa, and a stirring speed of 1000rpm, and the obtained product After analysis, it can be seen that the yield of 1,3 propanediol is 90 mol%.

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PUM

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Abstract

A process for preparing 1,3-propanediol from formaldehyde and acetaldehyde includes such steps as under existance of alkali and organic solvent, reacting at 10-40 deg.C for 2-10 hr to obtain 3-hydroxypropanol, making the 3-hydroxypropanal in contact with catalyst, and hydrogenation reaction at 50-100 deg.c and 3-9 MPa. The said catalyst contains Ni (70-90 wt.%), Fe or Mo (0-9), P (1-5) and Al (rest). Its advantages are high output rate, high safety, and high activity and selectivity of said catalyst.

Description

technical field [0001] The present invention relates to the preparation method of 1,3-propanediol Background technique [0002] 1,3-propanediol is an important organic chemical raw material, mainly used in the production of polymers, such as thermoplastic polyurethane, poly(trimethylene terephthalate) (PTT), copolyester ether, etc., and can also be used as a solvent, Antifreeze and protectant. Among them, the performance of PTT prepared by using it instead of 1,4-butanediol and ethylene glycol is better than that of PBT (1,4-butylene terephthalate) and PET (polyethylene terephthalate). ester). [0003] In the prior art, the preparation method of 1,3-propanediol mainly contains the following two routes: [0004] (1) Use ethylene oxide as a raw material, undergo hydroformylation, and then hydrogenate to prepare 1,3-propanediol. For example, US 5689016 adopts the cobalt carbonyl promoted by rhodium carbonyl as the hydroformylation catalyst, and Ni, Co, Ru, Pt, Pd are the hy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185C07C29/14C07C31/20
Inventor 王海京段启伟杜泽学
Owner CHINA PETROLEUM & CHEM CORP
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