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A kind of preparation method of citronellonitrile

A technology of citronellyl nitrile and fatty nitrile, which is applied in the field of citronellyl nitrile preparation, and achieves the effects of reducing equipment investment cost, low risk, and mild chemical properties

Active Publication Date: 2022-07-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A kind of preparation method of citronellonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0069] 2) Disperse 4.126g / 0.018mol 5-(1H-pyrazol-4-yl)isophthalic acid in 43.429ml water with ultrasonic (frequency 1500Hz) vibration for 30h, then add to the PVA-In nanosol prepared in step 1) , continue stirring at -2 °C for 5 h, then centrifuged, washed with deionized water for 3 times, dried at 95 °C for 3 h, and then transferred to a calciner and calcined at 400 °C for 3.5 h to obtain In-MOF catalyst. (The mass fraction of indium in the catalyst is about 18.2wt%)

Embodiment 2

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

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

Embodiment 3

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

[0075] 2) Disperse 2.554g / 0.014mol 5-(1H-pyrazol-4-yl)isophthalic acid in 25.54ml water with ultrasonic (frequency 2000Hz) vibration for 33h, then add to the PVA-In nanosol prepared in step 1) , continue to stir at 0 °C for 6 h, centrifuge, wash with deionized water for 5 times, dry at 100 °C for 4 h, and then transfer to a calciner for 420 °C for 4 h 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 citronellonitrile. The method is to prepare citronellonitrile by carrying out a Moum rearrangement reaction between citronellic acid and aliphatic nitrile under the action of an In-MOF catalyst. The present invention utilizes In-MOF catalyst to catalyze citronellic acid to prepare citronellonitrile with high yield under mild reaction conditions, has simpler reaction process, lower reaction cost, good environmental friendliness, and has better industrialization prospect.

Description

technical field [0001] The invention belongs to the field of preparation of citronellonitrile, in particular to a method for preparing citronellonitrile from citronellic acid through Mummy rearrangement reaction. Background technique [0002] The citronella nitrile aroma is specific, not only has the citrus aroma of strong flowery notes, but also the lemon fruit aroma of fresh lemon fruit, and the aroma is strong and lasting. Citronellonitrile is a colorless to pale yellow liquid, stable in weak acid and alkaline environments, safe and harmless to human skin, and has the functions of repelling mosquitoes and insects, especially suitable for soap essence and synthetic detergent essence In the formula, it is also suitable for flavoring of other daily chemical products. It is an important nitrile flavor with great development value. [0003] At present, the process for preparing citronellonitrile mainly adopts hydroxylamine oximation method: citronellal is reacted with hydroxy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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