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1,3-propanediol synthesis method

A synthesis method and technology of propylene glycol, which are applied in chemical instruments and methods, preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems of low yield and selectivity of propylene glycol, and improve the activity. and stability effects

Active Publication Date: 2016-05-18
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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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 synthesis 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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Embodiment 1

[0027] The preparation of hydroformylation catalyst: the RhCl that contains 6.50gRh, contains 1.50gLi and contains 3.50gSn 3 ·3H 2 O, LiCl, and SnCl 2 2H 2 O 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 5.6mm 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 Li content was 1.50 g / L, and the Sn content was 3.50 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 5.2MPa, increase the stir...

Embodiment 2

[0035] The preparation of hydroformylation catalyst: the RhCl that contains 6.50gRh, contains 1.50gLi and contains 3.50gTi 3 ·3H 2 O, LiCl, and TiCl 4 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 5.6mm 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, Li content 1.50g / L, Ti content 3.50g / 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 5.2MPa, increase the stirring speed to 800rpm, stir and heat up to...

Embodiment 3

[0053] The preparation of hydroformylation catalyst: the Rh(OAc) that contains 6.50gRh, contains 1.50gK and contains 3.50gGe 3 、K 2 SO 4 and GeCl 4 Fully mixed and dissolved in 10wt% acetic acid aqueous solution to obtain 400ml of impregnating solution, and the specific surface of 1.0L was 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 100° C. to obtain the catalyst. The Rh content of the catalyst was determined by ICP to be 6.50 g / L, the K content to be 1.50 g / L, and the Ge content to be 3.50 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 5.2MPa, increase the stirring speed to 800rpm, stir and heat ...

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Abstract

The invention relates to a 1,3-propanediol synthesis. The invention mainly aims at solving the problems of low activity and low selectivity of 1,3-propanediol catalyst in prior arts. The 1,3-propanediol synthesis method comprises the following steps: vinyl acetate is subjected to hydroformylation, such that 3-acetoxypropionaldehyde is obtained; 3-acetoxypropionaldehyde is hydrogenated, such that 3-acetoxypropanol is obtained; and 3-acetoxypropanol is is hydrolyzed, such that 1,3-propanediol is obtained. A hydroformylation catalyst adopts SiO2, Al2O3 or a mixture thereof as a carrier, and active components comprise rhodium, alkali metal and at least one metal element selected from IVA and IVB. With the above technical scheme, the technical problem is well solved. The method can be applied in 1,3-propanediol industrial production.

Description

technical field [0001] The invention relates to a synthesis 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 Sta...

Claims

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Application Information

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IPC IPC(8): C07C29/09C07C31/20C07C67/293C07C69/14B01J23/62B01J23/58
Inventor 查晓钟杨运信张丽斌
Owner CHINA PETROLEUM & CHEM CORP
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