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Method for synthesizing beta-ionone

A technology of ionone and synthesis method, applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problems of complex separation process, poor operating environment, and high equipment requirements

Inactive Publication Date: 2004-03-24
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to address the deficiencies in the prior art, break through the idea of ​​traditional concentrated sulfuric acid as a catalyst to synthesize β-ionone from pseudo-ionone, and propose a method using solid superacid as a catalyst, aiming at solving the problem of the original process equipment High requirements, harsh operating conditions, complicated subsequent separation process, poor operating environment and other shortcomings

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 10g of sodium ZSM-5 zeolite and add to 500ml of 10% NH 4 NO 3 The solution was exchanged 5 times. Calcined at 450°C for 2 hours to obtain HZSM-5 zeolite. The HZSM-5 zeolite was then added to 15 mL of 10% (wt%) ZrOCl 2 In the solution, stir vigorously to make it evenly mixed to obtain a suspension. In the above-mentioned suspension, gradually add dropwise the ammoniacal liquor of 28% by volume, make the zirconium hydroxide Zr(OH) of generation 4 Uniform deposition onto HZSM-5. After standing for 10 hours, the precipitate was filtered and washed to chloride ion Cl - Not detected; dry at 110°C for 12 hours, then use 500ml of 0.5mol L -1 impregnated with sulfuric acid for 12 hours; after filtering and drying, roasting at 550°C for 3 hours to obtain a solid superacid catalyst sample 10% (wt%) SO 4 2- / ZrO 2 / HZSM-5.

[0027] Wherein 1g10% (wt%) SO 4 2- / ZrO 2 / HZSM-5 catalyst was placed in a vacuum oven, dried at 80°C for 10 hours, and then added to a thre...

Embodiment 2

[0029] Weigh 10g of sodium ZSM-5 zeolite and add to 500ml of 10% NH 4 NO 3 The solution was exchanged 5 times. Calcined at 450°C for 2 hours to obtain HZSM-5. The HZSM-5 was then added to 60 mL of 10% (wt%) ZrOCl 2 solution, stir vigorously to mix well. Gradually add 28% ammoniacal liquor dropwise to above-mentioned suspension, make Zr(OH) 4 Uniform deposition onto HZSM-5. After standing for 11 hours, the precipitate was filtered and washed to Cl - Not detected; dry at 110°C for 12 hours, then use 500ml of 0.5mol L -1 impregnated with sulfuric acid for 12 hours; after filtering and drying, it was roasted at 550°C for 3 hours to obtain a catalyst sample of 40% (wt%) SO 4 2- / ZrO 2 / HZSM-5.

[0030] 2g of 40% SO 4 2- / ZrO 2 / HZSM-5 catalyst was placed in a vacuum oven, dried at 80°C for 10 hours, and then added to a three-necked flask. Then add 250 ml of dried acetone, and keep stirring at a temperature of 110-120°C. Under nitrogen protection, 10 g of pseudoionone ...

Embodiment 3

[0032] Weigh 10g of sodium ZSM-5 zeolite and add to 500ml of 10% NH 4 NO 3 The solution was exchanged 5 times. Calcined at 450°C for 2 hours to obtain HZSM-5. The HZSM-5 was then added to 120 mL of 10% (wt%) ZrOCl 2 solution, stir vigorously to mix well. Gradually add 28% ammoniacal liquor dropwise to above-mentioned suspension, make Zr(OH) 4 Uniform deposition onto HZSM-5. After standing for 12 hours, the precipitate was filtered and washed to Cl - Not detected; dry at 110°C for 12 hours, then use 500ml of 0.5mol L -1 impregnated with sulfuric acid for 12 hours; after filtering and drying, it was roasted at 550°C for 3 hours to obtain a catalyst sample with 80% (wt%) SO 4 2- / ZrO 2 / HZSM-5.

[0033] 0.7g 80% SO 4 2- / ZrO 2 / HZSM-5 catalyst was placed in a vacuum oven, dried at 80°C for 10 hours, and then added to a three-necked flask. Then add 100ml of dried acetone, and keep stirring at a temperature of 110-120°C. Under nitrogen protection, 10 g of pseudoionon...

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Abstract

Under the condition of constant temperature the prepared solid super acidic catalyst is added into the acetone solution, under the protection of nitrogen gas the pseudo ionone can be slowly added while stirring, after the reaction is completed, the solid super acidic catalyst is fertered and separated, then the acetone can be separated out in rotary evaporator, finally, the target product beta-ionone can be separated out by utilizing reduced pressure distillation process.

Description

Technical field: [0001] The invention relates to a method for synthesizing β-ionone, in particular to a method for synthesizing β-ionone from pseudoionone by utilizing a solid superacid catalyst, and belongs to the technical field of chemical engineering and catalysis. Background technique: [0002] In the industry, the synthesis of β-ionone is generally generated by ring closure of pseudo-ionone under strong acidic conditions. [0003] As early as the mid-19th century, the reaction was studied abroad, using 98% concentrated sulfuric acid as a catalyst. Alcohols are used as solvents and reacted at -20 to 0°C to obtain 95% β-ionones (OttoHertel, Hans Kiefer, Lothar Arnold. Preparation of ionones. US, 4565894.1986). In addition, esters are used as solvents to obtain β-ionone with a purity of 90%. The use of a single solvent, especially solvents with low density such as alcohols, is not conducive to the uniform mixing of the reaction solution with concentrated sulfuric acid w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/40C07C45/61C07C49/21
Inventor 蒋淇忠马紫峰李春波叶伟东沈旻
Owner SHANGHAI JIAO TONG UNIV
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