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Process used for the production of 1,3-propanediol

A technology of propylene glycol and hydroformylation catalyst, which can be applied in chemical instruments and methods, preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, etc., and can solve the problems of low yield and selectivity of propylene glycol.

Active Publication Date: 2018-01-09
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 producing 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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  • Process used for the production of 1,3-propanediol
  • Process used for the production of 1,3-propanediol
  • Process used for the production of 1,3-propanediol

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Preparation of hydroformylation main catalyst: RhCl containing 6.50gRh, containing 2.40gLa and containing 3.10gSb 3 ·3H 2 O, La(OAc) 3 ·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 measured by ICP to be 6.50 g / L, the La content was 2.40 g / L, and the Sb content was 3.10 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 5.3MPa, increase the...

Embodiment 2

[0035] Preparation of hydroformylation main catalyst: RhCl containing 6.50gRh, containing 2.40gLa and containing 3.10gNb 3 ·3H 2 O, La(OAc) 3 ·5H 2 O and NbCl 5 Fully mix and dissolve 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 La content was 2.40 g / L, and the Nb content was 3.10 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 5.3MPa, increase the sti...

Embodiment 3

[0053] The preparation of hydroformylation main catalyst: the Rh(OAc) that contains 6.50gRh, contains 2.40gCe and contains 3.10gSb 3 、Ce(OAc) 3 ·6H 2 O 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 6.50 g / L, the Ce content was 2.40 g / L, and the Sb content was 3.10 g / 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 5.3MPa, increase the stirr...

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Abstract

The invention relates to a method for producing 1.3-propanediol, which mainly solves the problem of low yield and selectivity of 1.3-propanediol when vinyl acetate is successively prepared through hydroformylation, hydrogenation and hydrolysis routes. By adopting the method used for the production of 1,3-propanediol: hydroformylation of vinyl acetate to give 3-acetoxypropionaldehyde; hydrogenation of 3-acetoxypropionaldehyde to give 3-acetoxypropanol; 3-acetoxypropanol Alcoholysis obtains 1.3 propanediol; Hydroformylation catalyst adopts SiO2, Al2O3 or its mixture is carrier, active component comprises the technical scheme of rhodium, lanthanide metal elements and at least one metal element selected from VA and VB, relatively The technical problem has been well solved, and it can be used in the industrial production of 1.3-propylene glycol.

Description

technical field [0001] The present invention relates to a process for the production 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 Patents(China)
IPC IPC(8): C07C31/20C07C29/09C07C69/14C07C67/293B01J31/36B01J31/28B01J23/644B01J23/648
Inventor 查晓钟杨运信
Owner CHINA PETROLEUM & CHEM CORP
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