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Method for producing 1,3-propylene glycol from vinyl acetate

A technology of vinyl acetate and propylene glycol, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, organic chemistry, etc., can solve the problems of low yield and selectivity of propylene glycol, and achieve improved activity and stability sexual effect

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 production method of 1,3-propanediol is provided, which has the advantages of high yield and selectivity of 1,3-propanediol Sexual characteristics

Method used

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  • Method for producing 1,3-propylene glycol from vinyl acetate
  • Method for producing 1,3-propylene glycol from vinyl acetate
  • Method for producing 1,3-propylene glycol from vinyl acetate

Examples

Experimental program
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Effect test

Embodiment 1

[0029] The preparation of hydroformylation catalyst: the Co containing 8.60gCo, containing 1.80gSr and containing 3.00gSn 2 (CO) 8 , Sr(OA C ) 2 0.5H 2 O and triphenyltin chloride (C 18 h 15 ClSn) fully mixed and dissolved in the concentration of 10wt% acetic acid aqueous solution to obtain immersion liquid 400ml, 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 Co content of the catalyst was determined by ICP to be 8.60 g / L, the Sr content to be 1.80 g / L, and the Sn content to be 3.00 g / L.

[0030] Synthesis of 1,3-propanediol:

[0031] 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. 2.0MPa, then feed carbon monoxide and hydrogen until the pressure is 11.8M...

Embodiment 2

[0037] The preparation of hydroformylation catalyst: the Co containing 8.60gCo, containing 1.80gSr and containing 3.00gZn 2 (CO) 8 , Sr(OA C ) 2 0.5H 2 O and zinc citrate (Zn 3 (C 6 h 5 o 7 ) 2 2H 2 O) fully mixed and dissolved in the acetic acid aqueous solution with a concentration of 10wt%, to obtain 400ml of impregnation solution, and the specific surface of 1.0L was 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 Co content of the catalyst was determined by ICP to be 8.60 g / L, the Sr content to be 1.80 g / L, and the Zn content to be 3.00 g / L.

[0038] Synthesis of 1,3-propanediol:

[0039] 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. 2.0MPa, then feed carbon monoxide and hydr...

Embodiment 3

[0055] The preparation of hydroformylation catalyst: the Co(OAc) that contains 7.00gCo, contains 0.50gBe and contains 1.00gSn 2 4H 2 O, BeCl 2 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 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 Co content of the catalyst was determined by ICP to be 7.00 g / L, the Be content to be 0.50 g / L, and the Sn content to be 1.00 g / L.

[0056] Synthesis of 1,3-propanediol:

[0057] 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. 2.0MPa, then feed carbon monoxide and hydrogen until the pressure is 11.8MPa, incr...

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Abstract

The invention relates to a method for producing 1,3-propylene glycol from vinyl acetate to mainly solve the problems of relatively low catalyst activity and selectivity of 1,3-propylene glycol in the prior art. By adoption of the technical scheme that the preparation method of 1,3-propylene glycol comprises the following steps: carrying out hydroformylation on vinyl acetate to obtain 3-acetoxypropanal, carrying out hydrogenation on 3-acetoxypropanal to obtain 3-acetoxypropanol, and hydrolyzing 3-acetoxypropanol to obtain 1,3-propylene glycol, wherein a hydroformylation catalyst adopts SiO2, Al2O3 or a mixture thereof as a carrier, and the active components comprise at least one of iron series elements, an alkaline earth metal element, and at least one metal element selected from IVA and IIB, the technical problems are well solved, and the method can be used for industrial production of 1,3-propylene glycol.

Description

technical field [0001] The invention relates to a method for producing 1,3-propanediol from vinyl acetate. 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 Compa...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/09B01J23/835B01J23/80
Inventor 查晓钟杨运信
Owner CHINA PETROLEUM & CHEM CORP
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