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Solid phosphoric acid catalyst, preparation method and recovery method of Saucy-Marbet reaction light component

A technology of phosphoric acid catalyst and recovery method, which is applied in the fields of fine chemicals and flavors and fragrances. It can solve the problems of large consumption and complex components of light components, and achieve the effects of simple operation, simplified separation and purification, and convenient operation.

Active Publication Date: 2021-03-16
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to reduce costs, it is necessary to recover the light components of the Saucy-Marbet reaction, but the components of the light components are complex, and a large amount of steam needs to be consumed for rectification in order to recover relatively pure 2-alkoxypropene and 2,2- Dialkoxypropane

Method used

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  • Solid phosphoric acid catalyst, preparation method and recovery method of Saucy-Marbet reaction light component
  • Solid phosphoric acid catalyst, preparation method and recovery method of Saucy-Marbet reaction light component
  • Solid phosphoric acid catalyst, preparation method and recovery method of Saucy-Marbet reaction light component

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Preparation of Solid Phosphoric Acid Catalyst by Blending Method

[0041]Preparation of diatomite-supported phosphoric acid catalyst by blending method: Weigh zinc oxide (0.41g), ammonium oxalate (0.62g), diatomite (230.58g) and deionized water (243.13g), and mix them uniformly to obtain a suspension Turbid liquid, finally add phosphoric acid (85wt%, 11.53g), under slow stirring (200 rpm) oil bath evaporates most of the water in the suspension to dryness, obtain the semi-dry solid catalyst precursor, the gained solid extrudes Shaped and then calcined at 300°C to obtain catalyst samples. Based on the mass of the carrier diatomite, the mass fraction of phosphoric acid supported in the catalyst is about 5%, and the catalyst is named as 5% phosphoric acid-0.2% zinc-0.3% ammonium oxalate-diatomite catalyst.

Embodiment 2

[0043] Preparation of Solid Phosphoric Acid Catalyst by Blending Method

[0044] Prepare diatomite-supported phosphoric acid catalyst by blending method: Weigh zinc oxide (0.41g), sodium silicate (0.61g), diatomite (230.6g) and deionized water (243.12g), and mix them uniformly to obtain Suspension liquid, add phosphoric acid (85wt%, 11.53g) at last, under slow stirring (200 rpm) oil bath evaporates most of water in the suspension liquid, obtain the semi-dry solid catalyst precursor, squeeze the gained solid Compression molding, and then roasting at 300 ° C to obtain catalyst samples. Based on the mass of carrier diatomite, the mass fraction of phosphoric acid supported in the catalyst is about 5%, and the catalyst is named as 5% phosphoric acid-0.2% zinc-0.3% sodium silicate-diatomite catalyst.

Embodiment 3

[0046] Preparation of Solid Phosphoric Acid Catalyst by Blending Method

[0047] Prepare diatomite-supported phosphoric acid catalyst by blending method: Weigh magnesium oxide (0.2g), sodium silicate (0.61g), diatomite (230.6g) and deionized water (242.92g), and mix them uniformly to obtain Suspension liquid, add phosphoric acid (85wt%, 11.53g) at last, under slow stirring (200 rpm) oil bath evaporates most of water in the suspension liquid, obtain the semi-dry solid catalyst precursor, squeeze the gained solid Compression molding, and then roasting at 300 ° C to obtain catalyst samples. Based on the mass of carrier diatomite, the mass fraction of phosphoric acid supported in the catalyst is about 5%, and the catalyst is named as 5% phosphoric acid-0.1% magnesium-0.3% sodium silicate-diatomite catalyst.

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Abstract

The invention discloses a solid phosphoric acid catalyst, a preparation method and a recovery method of a Saucy-Marbet reaction light component. The catalyst provided by the invention comprises a carrier, and phosphoric acid, a metal oxide and an auxiliary agent which are loaded on the carrier. By utilizing the solid phosphoric acid catalyst disclosed by the invention, the 2-alkoxy propylene in the light components of the Saucy-Marbet reaction can be efficiently converted into the 2, 2-dialkoxy propane, and the converted light components are subjected to rectification separation, so that high-yield and high-purity recovery of high-added-value components in the light components is realized. The method adopts a tubular reactor, is carried out in a continuous manner, and has the advantages ofsimple process, convenience in operation, easiness in large-scale production and the like.

Description

technical field [0001] The invention belongs to the fields of fine chemicals and flavors and fragrances, and in particular relates to a solid phosphoric acid catalyst, a preparation method and its application in the recovery of light components of Saucy-Marbet reaction. Background technique [0002] The Saucy-Marbet reaction is the rearrangement reaction of propargyl alcohol and 2-alkoxypropylene under the action of an acid catalyst to obtain a ketene product, which was first reported by chemists Saucy and Marbet et al. (R.Marbet, G.Saucy , Helv. Chim. Acta. 1967, 50, 1158-1167; US3029287, US6184420). In the earliest reports, strong acids such as p-toluenesulfonic acid, methanesulfonic acid, and sulfuric acid were used to catalyze the reaction, and allenone products could be obtained in high yields. Because the starting material 2-alkoxypropene of this reaction is simple and easy to obtain, the price is low, the rearrangement reaction speed is fast, and the selectivity is h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/16B01J37/00B01J37/08C07C41/54C07C43/303
CPCB01J27/16B01J37/0018C07C41/54C07C43/303Y02P20/584
Inventor 谢硕王永军马文成孙媛媛陈江黄文学
Owner WANHUA CHEM GRP CO LTD
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