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Molybdenum sulfide-zirconium phosphate catalyst for preparing allyl alcohol by hydrogenation of glycerin and its preparation method and application

A technology of zirconium phosphate and molybdenum sulfide, which is applied in the field of catalysis, can solve the problems of low yield of allyl alcohol, cumbersome separation process, and easy deactivation, and achieve the effects of high selectivity, simple and efficient synthesis, and high stability

Active Publication Date: 2020-05-19
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the process of directly synthesizing propylene alcohol from glycerin, the cost of formic acid and organic alcohol as hydrogen donors is high, the catalyst is expensive, toxic, and easily deactivated, and the products are complicated, the yield of propylene alcohol is low, and the separation process is cumbersome. The present invention provides A molybdenum sulfide-zirconium phosphate catalyst for the hydrogenation of glycerin to prepare allyl alcohol was prepared by mixing zirconium phosphate and molybdenum sulfide by a simple ball milling method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 10.3 grams of zirconium oxychloride octahydrate and dissolve it in 5 milliliters of deionized water, stir for 10 minutes to dissolve evenly, slowly add 11.1 grams of 85% phosphoric acid solution dropwise, the molar ratio of phosphorus to zirconium is 3:1, mix and stir After 1 hour, a gel-like precipitate was obtained; the gel-like precipitate was transferred to a stainless steel reactor with a polytetrafluoroethylene liner, and hydrothermally crystallized at 180°C for 48 hours, and the obtained product was cooled, washed and centrifuged until the pH was 7 or so, dry and grind to get white powder; transfer the above white powder to muffle furnace, calcinate at 450°C for 2 hours in a static air atmosphere, control the heating rate of 2°C / min, and get white zirconium phosphate solid. Then weigh 0.4 to 0.8 grams of zirconium phosphate and 0.4 to 0.8 grams of molybdenum sulfide, that is, control the mass ratio of molybdenum sulfide and zirconium phosphate to 1:2, 1:1 an...

Embodiment 2

[0033]The same catalyst preparation process in Example 1 was used to prepare a catalyst with a mass ratio of molybdenum sulfide to zirconium phosphate of 1:1, and the same method was used to load and activate the catalyst. The reaction temperature was 205°C, and the hydrogen pressure was 3MPa. The mass fraction of 40% glycerol solution was injected into the reaction tube at a flow rate of 0.01 ml / min, and the reaction started and stabilized for 1.5 hours; the reaction product was cooled by a cold trap at -5°C, and the resulting liquid product was measured by capillary gas chromatography, external standard Quantitative analysis. The conversion of glycerol and the selectivity of allyl alcohol in different solvents are shown in Table 2.

[0034] The conversion ratio of glycerol and the selectivity of propenyl alcohol in different solvents of table 2

[0035] solvent Isopropanol Methanol ethanol water Glycerin conversion rate (%) 64.4 57.6 81.9 63.7 ...

Embodiment 3

[0037] Adopt the same catalyzer among the embodiment 2 and the same method to load and activate the catalyzer, the reaction temperature is 185~225 ℃, and the hydrogen pressure is 3MPa, and the mass fraction is 40% glycerol isopropanol solution at 0.01 ml / min with a high pressure pump The flow rate is injected into the reaction tube, and the reaction starts and stabilizes for 1.5 hours; the reaction product is cooled by a -5°C cold trap, and the obtained liquid product is determined by capillary gas chromatography, and quantitatively analyzed by the external standard method. The conversion of glycerol and the selectivity of allyl alcohol at different temperatures are shown in Table 3.

[0038] Table 3 The conversion rate of glycerol and the selectivity of propenyl alcohol at different temperatures

[0039] temperature(℃) 185 205 225 Glycerin conversion rate (%) 49.5 64.4 82.8 Propyl Alcohol Selectivity (%) 33.4 40.5 30.5

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Abstract

The invention discloses a molybdenum sulfide-zirconium phosphate catalyst for preparing allyl alcohol through glycerin hydrogenation and a preparation method and application of the catalyst. The molybdenum sulfide-zirconium phosphate catalyst is prepared in the mode that zirconium phosphate and molybdenum sulfide are mixed through a ball milling method, and the mass ratio of the zirconium phosphate to the molybdenum sulfide is (0.5-2):1. The molybdenum sulfide-zirconium phosphate catalyst is applied to a gas-phase hydrogenation allyl alcohol preparation reaction for glycerinum, the reaction temperature is controlled within 185-225 DEG C, the hydrogen pressure is controlled within 1-3 MPa, the glycerinum conversion rate after the reaction can reach 49.5-82.8%, the selectivity of the allyl alcohol can reach 40.5%, and the highest time space yield of the allyl alcohol can reach 0.25 g-allyl alcohol / g-catalyst / h.

Description

technical field [0001] The invention relates to the technical field of catalysis, in particular to a molybdenum sulfide-zirconium phosphate catalyst for hydrogenating glycerin to prepare allyl alcohol, a preparation method and application thereof. Background technique [0002] At present, the industrial production routes of allyl alcohol mainly include four methods: hydrolysis of allyl chloride, isomerization of propylene oxide, reduction of acrolein and hydrolysis of propylene acetate. The hydrolysis of propylene chloride will produce a large amount of waste residue during the hydrolysis process; although the propylene oxide isomerization method has the characteristics of simple process, high yield, and no corrosion to equipment, due to the limitation of the source and price of propylene oxide, the output The advantage of the acrolein reduction method is that it does not need chlorine gas, but it is difficult to popularize due to the low yield, high toxicity of acrolein, an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/19C07C29/60C07C33/03
Inventor 姜媛媛赵怀远侯昭胤
Owner ZHEJIANG UNIV
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