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Method used for synthesizing 1,3-propanediol

A technology of propylene glycol and compound, applied in the field of synthesizing 1,3-propylene glycol, 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 method for synthesizing 1,3-propanediol is provided, which has a high yield of 1,3-propanediol and high selectivity

Method used

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  • Method used for synthesizing 1,3-propanediol
  • Method used for synthesizing 1,3-propanediol
  • Method used for synthesizing 1,3-propanediol

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Experimental program
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Embodiment 1

[0027] Preparation of hydroformylation catalyst support II: 0.80 L of ammonium fluorosilicate aqueous solution containing 2.50 gF and 1.0 L of spherical SiO with a diameter of 5.6 mm 2 Carriers were mixed and dried at 100° C. to obtain the catalyst carrier precursor I. Fully mix 0.60g of rubidium hydroxide powder with 5.0g of silica sol with a concentration of 35wt% to obtain a coating solution, and spray the coating solution evenly on 1.0L of catalyst carrier precursor I, dry at 100°C, and place in a muffle furnace at 500°C The catalyst support II is obtained after calcination. The carrier was analyzed by IC and ICP, and the F content was 2.45g / L, and the Rb content was 0.49g / L.

[0028] The preparation of hydroformylation main catalyst: the RhCl that will contain 6.50gRh 3 ·3H 2 O was dissolved in pure water to obtain 500ml of impregnating solution, and 1.0L of the catalyst carrier II was impregnated in the above impregnating solution, left to stand for 3h and dried at 10...

Embodiment 2

[0066] Preparation of hydroformylation catalyst support II: 0.80 L of ammonium fluoride aqueous solution containing 2.50 gF and 1.0 L of spherical SiO with a diameter of 5.6 mm 2Carriers were mixed and dried at 100° C. to obtain the catalyst carrier precursor I. Fully mix 1.07g of lithium oxide powder with 5.0g of silica sol with a concentration of 35wt% to obtain a coating solution, spray the coating solution evenly on 1.0L of catalyst carrier precursor I, dry at 100°C, and bake in a muffle furnace at 500°C Finally, the catalyst carrier II is obtained. The carrier was analyzed by IC and ICP, and the F content was 2.45g / L, and the Li content was 0.49g / L.

[0067] The preparation of hydroformylation main catalyst: the RhCl that will contain 6.50gRh 3 ·3H 2 O was dissolved in pure water to obtain 500ml of impregnating solution, and 1.0L of the catalyst carrier II was impregnated in the above impregnating solution, left to stand for 3h and dried at 100°C. 2 In the atmosphere,...

Embodiment 3

[0075] Preparation of hydroformylation catalyst carrier II: 0.80L of hydrofluoric acid aqueous solution containing 0.52gF and 1.0L of spherical SiO with a diameter of 5.6mm 2 Carriers were mixed and dried at 100° C. to obtain the catalyst carrier precursor I. Fully mix 0.16g of sodium oxide powder with 1.0g of silica sol with a concentration of 35wt% to obtain a coating solution, spray the coating solution evenly on 1.0L of catalyst carrier precursor I, dry at 100°C, and bake in a muffle furnace at 500°C Finally, the catalyst carrier II is obtained. The carrier was analyzed by IC and ICP, and the F content was 0.51g / L, and the Na content was 0.11g / L.

[0076] The preparation of hydroformylation main catalyst: the RhCl that will contain 6.50gRh 3 ·3H 2 O was dissolved in pure water to obtain 500ml of impregnating solution, and 1.0L of the catalyst carrier II was impregnated in the above impregnating solution, left to stand for 3h and dried at 100°C. 2 In the atmosphere, the...

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Abstract

The invention relates to a method used for synthesizing 1,3-propanediol. When 1,3-propanediol is prepared with vinyl acetate through the route of hydroformylation, hydrogenation and hydrolysis, 1,3-propanediol yield and selectivity are low. The invention mainly aims at solving the problems. According to the technical scheme of the invention, 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 subjected to alcoholysis, such that 1,3-propanediol is obtained. A hydroformylation catalyst comprises a main catalyst and an accelerant. The main catalyst comprises a carrier and an active component. The active component is a rhodium compound. The accelerant is at lease one selected from organic amine and organic phosphorus. The carrier is silicon dioxide with a coating on the surface, obtained after fluorine-containing compound modification. The coating is composed of a modification metal element and a silicon dioxide binding agent used for binding the modification metal element on the surface of the carrier. The modification metal element is at least one selected from alkali metal elements.

Description

technical field [0001] The present invention relates to a process for the synthesis 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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IPC IPC(8): C07C31/20C07C29/09C07C27/02B01J31/28B01J31/30C07C69/14C07C67/38
Inventor 查晓钟杨运信
Owner CHINA PETROLEUM & CHEM CORP