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Preparation method of citronellyl cyanide

A technology of citronellyl nitrile and citronellic acid, which is applied in the field of citronellyl nitrile preparation to achieve the effects of ensuring intrinsic safety, mild chemical properties and low risk

Active Publication Date: 2020-10-30
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The object of the present invention is to provide a kind of method for preparing citronellil, thereby solve many problems existing in the existing preparation citronellel technology, the present invention utilizes In-MOF catalyst to catalyze the high yield of citronellic acid under mild reaction conditions Efficient preparation of citronellonitrile, with a simpler reaction process, lower reaction cost, good environmental friendliness, and better industrialization prospects

Method used

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  • Preparation method of citronellyl cyanide
  • Preparation method of citronellyl cyanide
  • Preparation method of citronellyl cyanide

Examples

Experimental program
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Effect test

Embodiment 1

[0068] 1) Add 71.16ml polyvinyl alcohol aqueous solution (concentration 0.08g / ml, polyethylene 0.129mol) into 5ml indium trichloride aqueous solution (concentration 0.6g / ml, indium element 0.016mol) under vigorous stirring, Stir at -2 °C for 1 h; keep stirring, add 38.193 g of freshly prepared NaBH to the above solution 4 Aqueous solution (concentration 8wt%, wherein NaBH 4 0.08mol), forming a PVA-In nano-sol;

[0069] 2) Disperse 4.126g / 0.018mol 5-(1H-pyrazol-4-yl)isophthalic acid in 43.429ml water and vibrate ultrasonically (frequency 1500Hz) for 30h, then add to the PVA-In nano-sol prepared in step 1) , continue to stir at -2°C for 5h, then centrifuge, wash with deionized water three times, dry at 95°C for 3h, and then transfer to a roaster for 3.5h at 400°C to obtain the In-MOF catalyst. (The mass fraction of indium in the catalyst is about 18.2wt%)

Embodiment 2

[0071] 1) Add 64ml polyvinyl alcohol aqueous solution (concentration 0.1g / ml, polyethylene 0.145mol) into 3.75ml indium trichloride aqueous solution (concentration 0.8g / ml, indium element 0.016mol) under vigorous stirring, Stir at -1 °C for 1.5 h; keep stirring, add 37.344 g of freshly prepared NaBH to the above solution 4 Aqueous solution (concentration 9wt%, wherein NaBH 4 0.09mol), forming a PVA-In nano-sol;

[0072] 2) Disperse 3.952g / 0.021mol 3-(1H-pyrazol-4-yl)benzoic acid in 39.517ml of water and vibrate ultrasonically (frequency 1750Hz) for 33h, and then add it to the PVA-In nano-sol prepared in step 1), Continue to stir at -1°C for 5.5h, then centrifuge, wash with deionized water 4 times, dry at 100°C for 4h, and transfer to a roaster for 4h at 410°C to obtain the In-MOF catalyst. (The mass fraction of indium in the catalyst is about 17.985wt%)

Embodiment 3

[0074] 1) Add 33.55ml polyvinyl alcohol aqueous solution (concentration 0.1g / ml, polyethylene 0.076mol) to 3.75ml indium tribromide aqueous solution (concentration 0.8g / ml, indium element 0.008mol) under vigorous stirring , stirred at -1°C for 2 h; keeping stirring, added 19.56 g of freshly prepared NaBH to the above solution 4 Aqueous solution (concentration 9wt%, wherein NaBH 4 0.046mol), forming a PVA-In nano-sol;

[0075] 2) Disperse 2.554g / 0.014mol 5-(1H-pyrazol-4-yl)isophthalic acid in 25.54ml of water and vibrate ultrasonically (frequency 2000Hz) for 33h, then add to the PVA-In nano-sol prepared in step 1) , continue to stir at 0°C for 6h, then centrifuge, wash with deionized water five times, dry at 100°C for 4h, and then transfer to a roaster for 4h at 420°C to obtain In-MOF catalyst. (The mass fraction of indium in the catalyst is about 13.28wt%)

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Abstract

The invention discloses a preparation method of citronellyl cyanide, which comprises the following steps: under the action of an In-MOF catalyst, carrying out Mom rearrangement reaction on citronellylacid and aliphatic nitrile to obtain citronellyl cyanide. Under mild reaction conditions, the In-MOF catalyst is utilized to catalyze citronellyl acid to prepare citronellyl cyanide at high yield, and the method has the advantages of simpler reaction process, lower reaction cost, favorable environment friendliness and favorable industrial prospects.

Description

technical field [0001] The invention belongs to the field of citronellyl nitrile preparation, in particular to a method for preparing citronellel nitrile from citronellic acid through Mumm rearrangement reaction. Background technique [0002] Citronella nitrile has a unique aroma, not only has a strong flowery citrus aroma, but also has a lemon fruity aroma of fresh lemon fruit, and the aroma is strong and long-lasting. Citronellal nitrile is a colorless to pale yellow liquid, stable in weakly acidic and alkaline environments, safe and harmless to human skin, and has the functions of repelling mosquitoes and insects, especially suitable for soap flavors and synthetic detergent flavors In the formula, it is also suitable for flavoring and seasoning of other daily chemical products. It is an important nitrile fragrance with great development value. [0003] At present, the process for preparing citronellyl nitrile mainly adopts hydroxamin oximation method: citronellal is reac...

Claims

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Application Information

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IPC IPC(8): C07C255/07C07C253/00C07C253/20B01J31/22
CPCC07C253/00C07C253/20B01J31/1691B01J31/2239B01J2531/33C07C255/07Y02P20/584
Inventor 王亚新董菁张永振于磊李康王文李晶孙亚明程英
Owner WANHUA CHEM GRP CO LTD
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