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 pro

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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
Comparison scheme
Effect test

Example Embodiment

[0028] [Example 1]

[0029] The preparation of the hydroformylation catalyst: the Co containing 8.60g Co, 1.80g Sr and 3.00g Sn 2 (CO) 8 , Sr(OA C ) 2 ·0.5H 2 O and triphenyltin chloride (C 18 H 15 ClSn) was thoroughly mixed and dissolved in an acetic acid aqueous solution with a concentration of 10wt% to obtain 400ml of immersion liquid, and 1.0L specific surface was 168m 2 / g, spherical SiO with a pore volume of 0.94 and a diameter of 5.6mm 2 The carrier is immersed in the above-mentioned impregnating solution, and left to stand for 3 hours to dry at 100°C to obtain the catalyst. The Co content of the catalyst determined by ICP is 8.60g / L, the Sr content is 1.80g / L, and the Sn content is 3.00g / L.

[0030] Synthesis of 1,3-propanediol:

[0031] Step (1): Add 2.50mol of toluene, 0.02mol of the main hydroformylation catalyst, 0.20mol of triphenylphosphorus and 1.65mol of vinyl acetate into a 1L titanium reactor, first use argon to exhaust the air in the kettle and press it to 2.0MPa,...

Example Embodiment

[0036] [Example 2]

[0037] The preparation of the hydroformylation catalyst: the Co containing 8.60g Co, 1.80g Sr and 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 mix and dissolve in an acetic acid aqueous solution with a concentration of 10wt% to obtain 400ml of immersion liquid, with 1.0L specific surface area of ​​168m 2 / g, spherical SiO with a pore volume of 0.94 and a diameter of 5.6mm 2 The carrier is immersed in the above-mentioned impregnating solution, and left to stand for 3 hours to dry at 100°C to obtain the catalyst. The Co content of the catalyst determined by ICP is 8.60g / L, the Sr content is 1.80g / L, and the Zn content is 3.00g / L.

[0038] Synthesis of 1,3-propanediol:

[0039] Step (1): Add 2.50mol of toluene, 0.02mol of the main hydroformylation catalyst, 0.20mol of triphenylphosphorus and 1.65mol of vinyl acetate into a 1L titanium reactor, first use argon to exhaust the air in the kettle and press it to 2.0MPa,...

Example Embodiment

[0054] [Example 3]

[0055] Preparation of hydroformylation catalyst: Co(OAc) containing 7.00g Co, 0.50gBe and 1.00g Sn 2 ·4H 2 O, BeCl 2 And SnCl 2 ·2H 2 O is thoroughly mixed and dissolved in an aqueous solution of hydrochloric acid with a concentration of 8wt% to obtain 400ml of immersion liquid. The 1.0L specific surface is 200m 2 / g, spherical Al with pore volume of 1.00 and diameter of 5.6mm 2 O 3 The carrier is immersed in the above-mentioned impregnating solution, and left to stand for 3 hours to dry at 80°C to obtain the catalyst. The Co content of the catalyst determined by ICP is 7.00g / L, the Be content is 0.50g / L, and the Sn content is 1.00g / L.

[0056] Synthesis of 1,3-propanediol:

[0057] Step (1): Add 2.50mol of toluene, 0.02mol of the main hydroformylation catalyst, 0.20mol of triphenylphosphorus and 1.65mol of vinyl acetate into a 1L titanium reactor, first use argon to exhaust the air in the kettle and press it to 2.0MPa, then feed carbon monoxide and hydrogen unt...

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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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