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Supported heteropolyacid catalyst, preparation method and application of supported heteropolyacid catalyst in preparation of convallaria majalis pyrane

A technology of heteropolyacids and catalysts, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve problems such as destruction, reduced selectivity, and unfavorable product quality.

Pending Publication Date: 2022-03-22
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the disclosed method of patent CN105175372A, solid superacid is used as a catalyst. Although solid superacid can achieve a faster conversion rate, because the acidity is too strong, the newly generated lily of the valley pyran product will also be destroyed by superacid, resulting in selection Sexuality is reduced, and more by-products will be generated, which is not conducive to the improvement of product quality
[0007] In the method disclosed in the patent CN104529969A, a strongly acidic cation exchange resin is used as a catalyst, and the acidity is too strong, and the newly generated lily of the valley pyran product will also be destroyed by the super acid, resulting in a decrease in selectivity and more by-products. Problems that are not conducive to the improvement of product quality

Method used

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  • Supported heteropolyacid catalyst, preparation method and application of supported heteropolyacid catalyst in preparation of convallaria majalis pyrane
  • Supported heteropolyacid catalyst, preparation method and application of supported heteropolyacid catalyst in preparation of convallaria majalis pyrane
  • Supported heteropolyacid catalyst, preparation method and application of supported heteropolyacid catalyst in preparation of convallaria majalis pyrane

Examples

Experimental program
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Effect test

Embodiment 1

[0073] Preparation of supported heteropolyacid catalyst 1:

[0074] 1) Weigh 150g of KH-560 (γ-glycidyl etheroxypropyltrimethoxysilane) to prepare a 15wt% aqueous solution, add 112.5g of aluminum hydroxide powder (10-50nm) to the solution, and rotate at room temperature at 1100rpm / min fully stirred for 15 minutes, then transferred to the evaporator for evaporative dehydration, after removing 55wt% of the total water, added 9g of polyvinyl alcohol and methyl cellulose, raised the temperature to 75°C, stirred at 1100rpm / min for 15min, and stirred evenly. Shaped into a spherical shape, dried at 120°C to constant weight, transferred to a muffle furnace, and roasted at 750°C for 5 hours in a nitrogen atmosphere to obtain SiO 2 -Al 2 O 3 Composite carrier, the particle size is 4mm.

[0075] 2) Weigh 30g of phthalimide derivative 2 with an acidic group, dissolve it in 180g of ethyl acetate, and then add SiO 2 -Al 2 O 3 Composite carrier 105g, fully stirred, refluxed and dehydr...

Embodiment 2

[0078] Preparation of supported heteropolyacid catalyst 2:

[0079] 1) Weigh 150g of tetraethoxysilane to prepare a 10wt% aqueous solution, add 90g of aluminum hydroxide powder (10-50nm) to the solution, stir at room temperature at 500rpm / min for 5min, then transfer to an evaporator for evaporation and dehydration After removing 40wt% of the total water, add 7.5g of methyl cellulose, heat up to 60°C, stir at 500rpm / min for 25min, after stirring evenly, shape and granulate into a spherical shape, dry at 100°C to constant weight, and transfer to In a muffle furnace, calcined at 600°C for 3 hours under a nitrogen atmosphere to obtain SiO 2 -Al 2 O 3 Composite carrier, the particle size is 2mm.

[0080] 2) Weigh 30g of phthalimide derivative 2 with an acidic group, dissolve it in 570g of ethyl acetate, and then add SiO 2 -Al 2 O 3 Composite carrier 150g, fully stirred, refluxed and dehydrated at 70°C for 5h, then transferred the solution after the reflux reaction to an evapo...

Embodiment 3

[0083] Preparation of supported heteropolyacid catalyst 3:

[0084] 1) Weigh 200g of KH-560 (γ-glycidyl etheroxypropyltrimethoxysilane) to prepare a 20wt% aqueous solution, add 180g of aluminum hydroxide powder (10-50nm) to the solution, and rotate at room temperature at 1500rpm / min Fully stir for 20 minutes, then transfer to the evaporator for evaporative dehydration, remove 70wt% of the total water, add 40g of polyvinyl alcohol, heat up to 90°C, stir at 1500rpm / min for 20min, after stirring evenly, shape and granulate into a spherical shape , dried at 150°C to constant weight, transferred to a muffle furnace, and calcined at 900°C for 12h under a nitrogen atmosphere to obtain SiO 2 -Al 2 O 3 Composite carrier, the particle size is 6mm.

[0085] 2) Weigh 30g of phthalimide derivative 3 with an acidic group, dissolve it in 120g of ethyl acetate, and then add SiO 2 -Al 2 O 3 Composite carrier 60g, fully stirred, refluxed and dehydrated at 140°C for 10h, then transferred t...

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Abstract

The invention provides a supported heteropolyacid catalyst, a preparation method and application of the supported heteropolyacid catalyst in preparation of convallaria majalis pyrane. The supported heteropolyacid catalyst comprises a SiO2-Al2O3 composite carrier and a supported phthalimide derivative active component with an acidic group, and has the advantages of simplicity in synthesis, low cost, high strength, good stability, long service life and the like. The supported heteropolyacid catalyst is used for catalytic synthesis of lily pyran, and has the characteristics of high raw material conversion rate, good selectivity, high catalyst strength, long service life, simple process, obvious application value and the like.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a supported heteropolyacid catalyst, a preparation method and its application in a method for synthesizing lily of the valley pyran. Background technique [0002] Lily-of-the-valley type spices are synthetic spices with lily scent, which are currently used in food, perfume, cosmetics, cleaning agents and other fields. Lilial is the most widely used lily-type spice, followed by neolilial, hydroxycitronellal and lilipyran. The first three lily-of-the-valley-type spices have been included in the list of banned or restricted use by many countries and organizations due to their allergenicity, and lily-of-the-valley-type spices are considered to be the best choice for other lily-of-the-valley spices in the future because they have no allergenicity. most powerful substitute. [0003] Lily of the valley pyran (structure as follows), alias lily of the valley ether, wh...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J31/04C07D309/10
CPCB01J31/0269B01J31/0271B01J31/0247B01J31/0254B01J31/04C07D309/10Y02P20/584
Inventor 蔺海政赵振华张德旸姜鹏刘连才
Owner WANHUA CHEM GRP CO LTD
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