Solid acid catalyst for synthesizing 2-propyl-1,3-dioxocyclo-5-pentene and preparation method thereof and method for using solid acid catalyst to synthesize 2-propyl-1,3-dioxocyclo-5-pentene

A technology of solid acid catalyst and dioxane, applied in the direction of catalyst activation/preparation, organic compound/hydride/coordination complex catalyst, chemical instrument and method, etc., which can solve the inconvenience of post-processing and corrosion of reaction equipment in production , Large waste water discharge and other problems, to achieve the effect of low cost and no waste water discharge

Inactive Publication Date: 2018-05-18
ZHEJIANG OCEAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the important intermediate as a dienophile is 2-alkyl-4,7-dihydro-1,3-diheptin (dioxane for short), which is composed of n-butyraldehyde or isobutyraldehyde and butyraldehyde The acetal compounds obtained by the condensation reaction of enediols, the acid catalysts currently used are liquid acids that are easily soluble in organic solvents such as hydrochloric acid, sulfuric acid, p-toluenesulfonic acid, sulfamic acid, and citric acid. Too strong acidity will seriously corrode the reaction equipment, discharge a large amount of waste water, and produce sticky residues, which will bring inconvenience to the post-processing during production and seriously affect the yield and quality of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] This implementation case shows the solid acid catalyst to make dioxane according to the following steps:

[0048] Will 10 grams than surface 350m 2 The silicon dioxide powder carrier of / g is placed in the oven of 150 ℃ and dries for 12 hours; Later, it is added in 50 milliliters of anhydrous toluene solution containing 1 gram of (3-mercaptopropyl) trimethoxysilane, heated and refluxed for 4 hours, Cool, filter, wash with toluene more than 3 times, and dry the obtained solid at 120°C for 6 hours; 2 o 250 ml of aqueous solution, heated to reflux for 4 hours, filtered, washed with deionized water for more than 3 times, dried at 120 degrees for 6 hours, then placed in 50 ml of 1wt% sulfuric acid solution, stirred and acidified at 90 ° C for 4 hours, filtered , washed with deionized water until the filtrate was neutral, dried at 150°C for more than 6 hours, and the obtained solid catalyst was sealed and stored for future use.

[0049] The solid acid catalyst prepared abo...

Embodiment 2

[0051] This implementation case shows the solid acid catalyst to make dioxane according to the following steps:

[0052] In addition to using (3-mercaptopropyl) triethoxysilane instead of (3-mercaptopropyl) trimethoxysilane in Example 1, the catalyst preparation conditions and reaction conditions are the same as those in Example 1 to obtain the product dioxane ring, the yield reached 92.5%. After the catalyst was reused 8 times, the yield of dioxane was 90.7%.

Embodiment 3

[0054] This implementation case shows the solid acid catalyst to make dioxane according to the following steps:

[0055] In addition to using 10 grams of specific surface area of ​​721m 2 The mesoporous SBA-15 silica material of / g replaces specific surface 350m in embodiment 1 2 / g of silica powder carrier, catalyst preparation conditions and reaction conditions were the same as those in Example 1 to obtain the product dioxane with a yield of 96.5%. After the catalyst was reused 8 times, the yield of dioxane was 92.6%.

[0056] Compared with the prior art, the beneficial effect of the present invention is that the solid acid catalyst of the present invention has the characteristics of environmental friendliness, low cost, high yield, simple operation, easy recovery and reusability.

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PUM

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Abstract

The invention discloses a solid acid catalyst for synthesizing 2-propyl-1,3-dioxocyclo-5-pentene. A sulfonic acid group is grafted on the surface of a carrier silicon dioxide, and the preparation method of the solid acid catalyst comprises the steps that an organosilicone coupling agent containing a mercapto group is grafted to a carrier material loading silicon dioxide by adopting a post graftingmethod, and then the solid acid catalyst is prepared through the processes of oxidation, acidification and the like. The method for using the solid acid catalyst to synthesize the 2-propyl-1,3-dioxocyclo-5-pentene comprises the steps that the solid acid catalyst reacts with 1, 4-butylene glycol, n-butanal and a water-carrying agent, heating is conducted till no water is generated in the water diversion backflowing process, filtering and reduced pressure distillation are conducted, cut fraction under the vacuum degree of -0.098MPa and at the boiling point of 100-120 DEG C is collected, and theproduct 2-propyl-1,3-dioxocyclo-5-pentene is obtained. The provided solid acid catalyst has the advantage that equipment is not corroded, no waste water is drained out, the cost is low, the yield ishigh, and the catalyst is liable to being recycled and used repeatedly.

Description

technical field [0001] The invention relates to the technical field of vitamin production, in particular to a solid acid catalyst for synthesizing vitamin B6 intermediate dioxane, a preparation method thereof, and a method for synthesizing dioxane using the solid acid catalyst. Background technique [0002] Domestic production of vitamins is mainly based on the Diels-Alder reaction between the aza-conjugated diene structure of the azole ring and the dienophile, that is, the oxazole synthesis. Among them, the important intermediate as a dienophile is 2-alkyl-4,7-dihydro-1,3-diheptine (referred to as dioxane), which is composed of n-butyraldehyde or isobutyraldehyde and butyraldehyde The acetal compounds obtained by the condensation reaction of enediols, the acid catalysts currently used are liquid acids that are easily soluble in organic solvents such as hydrochloric acid, sulfuric acid, p-toluenesulfonic acid, sulfamic acid, and citric acid. If the acidity is too strong, th...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J37/12C07D321/06
CPCB01J31/0275B01J37/12C07D321/06
Inventor 莫流业
Owner ZHEJIANG OCEAN UNIV
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