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Method for synthesis of 1, 3-propanediol

A technology of propylene glycol and acetoxy propanol alcohol, applied in chemical instruments and methods, preparation of organic compounds, preparation of alcoholysis, etc., can solve the problems of low yield and selectivity of propylene glycol, and achieve the improvement of activity and stability. Effect

Active Publication Date: 2016-04-27
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is the problem of low yield and selectivity of 1,3-propanediol, and a new method for synthesizing 1,3-propanediol is provided, which has the advantages of high 1,3-propanediol yield and Features of high selectivity

Method used

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  • Method for synthesis of 1, 3-propanediol
  • Method for synthesis of 1, 3-propanediol
  • Method for synthesis of 1, 3-propanediol

Examples

Experimental program
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Effect test

Embodiment 1

[0027] The preparation of hydroformylation catalyst: the RhCl that contains 6.50gRh, contains 2.00gSr and contains 3.30gSb 3 ·3H 2 O, Sr(OA C ) 2 0.5H 2 O and Cl 3 Sb is fully mixed and dissolved in an aqueous hydrochloric acid solution with a concentration of 8wt%, to obtain 400ml of impregnation solution, and the specific surface of 1.0L is 168m 2 / g, spherical SiO with a pore volume of 0.94 and a diameter of 5.6 mm 2 The carrier was immersed in the above impregnating solution, left to stand for 3 hours and dried at 100° C. to obtain the catalyst. The Rh content of the catalyst was determined by ICP to be 6.50 g / L, the Sr content to be 2.00 g / L, and the Sb content to be 3.30 g / L.

[0028] Synthesis of 1,3-propanediol:

[0029]Step (1): Add 2.50 mol of toluene, 0.02 mol of hydroformylation main catalyst, 0.20 mol of triphenylphosphine and 1.65 mol of vinyl acetate into a 1L titanium reactor. 1.0MPa, then feed carbon monoxide and hydrogen until the pressure is 4.5MPa, ...

Embodiment 2

[0035] The preparation of hydroformylation catalyst: the RhCl that contains 6.50gRh, contains 2.00gSr and contains 3.30gHf 3 ·3H 2 O, Sr(OA C ) 2 0.5H 2 O and hafnium oxychloride (HfOCl 2 ·8H 2 O) fully mix and dissolve in water to obtain 400ml of impregnation solution, and the specific surface of 1.0L is 168m 2 / g, spherical SiO with a pore volume of 0.94 and a diameter of 5.6mm 2 The carrier was immersed in the above impregnating solution, left to stand for 3 hours and dried at 100° C. to obtain the catalyst. The Rh content of the catalyst measured by ICP is 6.50 g / L, the Sr content is 2.00 g / L, and the Hf content is 3.30 g / L.

[0036] Synthesis of 1,3-propanediol:

[0037] Step (1): Add 2.50 mol of toluene, 0.02 mol of hydroformylation main catalyst, 0.20 mol of triphenylphosphine and 1.65 mol of vinyl acetate into a 1L titanium reactor. 1.0MPa, then feed carbon monoxide and hydrogen until the pressure is 4.5MPa, increase the stirring speed to 800rpm, stir and heat...

Embodiment 3

[0053] The preparation of hydroformylation catalyst: the Rh(OAc) that contains 6.50gRh, contains 2.00gMg and contains 3.30gSb 3 , MgSO 4 and Sb 2 o 3 Fully mix and dissolve in an aqueous nitric acid solution with a concentration of 8wt%, to obtain 400ml of impregnation solution, and make 1.0L specific surface to 200m 2 / g, spherical Al with a pore volume of 1.00 and a diameter of 5.6mm 2 o 3 The carrier was immersed in the above impregnating solution, left to stand for 3 hours and dried at 80° C. to obtain the catalyst. The Rh content of the catalyst was determined by ICP to be 6.50g / L, the Mg content to be 2.00g / L, and the Sb content to be 3.30g / L.

[0054] Synthesis of 1,3-propanediol:

[0055] Step (1): Add 2.50 mol of toluene, 0.02 mol of hydroformylation main catalyst, 0.20 mol of triphenylphosphine and 1.65 mol of vinyl acetate into a 1L titanium reactor. 1.0MPa, then feed carbon monoxide and hydrogen until the pressure is 4.5MPa, increase the stirring speed to 80...

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Abstract

The invention relates to a method for synthesis of 1, 3-propanediol. The method mainly solves the problem that a 1, 3-propanediol catalyst obtained by the prior art has low activity and low selectivity. The method comprises vinyl acetate hydroformylation for 3-acetoxypropanal preparation, 3-acetoxypropanal hydrogenation for 3-acetoxypropanol preparation and 3-acetoxypropanol alcoholysis for 1, 3-propanediol preparation. The hydroformylation catalyst utilizes SiO2, Al2O3 or their mixture as a carrier and active ingredients comprise rhodium, an alkaline earth metal and at least one of VA and IVB metals. The method well solves the problem and can be used for 1, 3-propanediol industrial production.

Description

technical field [0001] The present invention relates to a process for the synthesis of 1,3-propanediol. Background technique [0002] 1,3-Propanediol (1.3-PDO) is an important chemical raw material, mainly used in the synthesis of plasticizers, detergents, preservatives, emulsifiers, and also used in food, cosmetics and pharmaceutical industries. Because it is an important polyester fiber monomer, its main use is as a monomer and terephthalic acid to synthesize a new type of polyester material, polytrimethylene terephthalate (PTT). [0003] The preparation methods of 1,3-propanediol include ethylene oxide one-step method, ethylene oxide two-step method, acrolein hydration method, acetaldehyde-formaldehyde condensation method, acrylate method, biological method, vinyl acetate hydroformylation, etc. At present, the industrialized production method of 1.3-PDO is chemical synthesis, and the international market is mainly monopolized by Degussa Company of Germany, Shell Company ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/128C07C31/20C07C67/293C07C69/14B01J23/644B01J23/58
Inventor 查晓钟杨运信
Owner CHINA PETROLEUM & CHEM CORP
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