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Preparation method of 1,3-propylene glycol

A technology of propylene glycol and acetoxypropanol, which is applied in the field of preparation of 1,3-propanediol, can solve the problems of low yield and selectivity of propylene glycol, and achieve the effect of improving activity and stability

Active Publication Date: 2016-05-18
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 preparation method of 1,3-propanediol is provided, which has the advantages of high yield and low selectivity of 1,3-propanediol Sexual characteristics

Method used

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  • Preparation method of 1,3-propylene glycol
  • Preparation method of 1,3-propylene glycol
  • Preparation method of 1,3-propylene glycol

Examples

Experimental program
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Effect test

Embodiment 1

[0028] The preparation of hydroformylation catalyst: the RhCl that contains 6.50gRh, contains 2.20gSm and contains 3.20gSn 3 ·3H 2 O, SmCl 3 ·6H 2 O and stannous oxalate (SnC 2 o 4 ) is fully mixed and dissolved in an aqueous hydrochloric acid solution with a concentration of 8wt%, to obtain 400ml of soaking 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 was determined by ICP to be 6.50 g / L, the Sm content was 2.20 g / L, and the Sn content was 3.20 g / L.

[0029] Synthesis of 1,3-propanediol:

[0030]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....

Embodiment 2

[0036] The preparation of hydroformylation catalyst: the RhCl that contains 6.50gRh, contains 2.20gSm and contains 3.20gCr 3 ·3H 2 O, SmCl 3 ·6H 2 O and CrCl 3 ·6H 2 O is fully mixed and dissolved in pure 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 was measured by ICP to be 6.50 g / L, the Sm content was 2.20 g / L, and the Cr content was 3.20 g / L.

[0037] Synthesis of 1,3-propanediol:

[0038] 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 5.6MPa, increase the stirring speed to 800rpm, stir and heat up to the...

Embodiment 3

[0054] The preparation of hydroformylation catalyst: the Rh(OAc) that contains 6.50gRh, contains 2.20gCe and contains 3.20gGe 3 、Ce(OAc) 3 ·6H 2 O and GeCl 4 Fully mix and dissolve in an aqueous hydrochloric acid solution with a concentration of 8wt%y to obtain 400ml of impregnating solution, and make 1.0L of specific surface 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 measured by ICP to be 6.50 g / L, the Ce content was 2.20 g / L, and the Ge content was 3.20 g / L.

[0055] Synthesis of 1,3-propanediol:

[0056] 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 5.6MPa, increase the stirring ...

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Abstract

The invention relates to a preparation method of 1,3-propylene glycol and mainly solves the problem of low activity and selectivity of a 1,3-propylene glycol catalyst in the prior art. The preparation method includes the following steps: 1) performing hydroformylation to vinyl acetate to prepare 3-acetoxylpropyl aldehyde; 2) hydrogenating the 3-acetoxylpropyl aldehyde to prepare 3-acetoxylpropyl alcohol; and 3) hydrolyzing the 3-acetoxylpropyl alcohol to obtain the 1,3-propylene glycol. A catalyst for the hydroformylation is prepared with SiO2, Al2O3 or a mixture thereof as a carrier with active components including rhodium, lanthanum-series metals, and at least one metal element selected from the groups of IVA and VIB. The method solves the technical problem well and is used for industrial production of the 1,3-propylene glycol.

Description

technical field [0001] The invention relates to a preparation method 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 of the United S...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/09C07C69/14C07C67/293B01J31/34B01J31/28B01J23/62B01J23/652
Inventor 查晓钟杨运信
Owner CHINA PETROLEUM & CHEM CORP
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