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Method for preparing nerol and geraniol from citral

A technology of nerol and citral, which is applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of unenvironmental protection and large waste water in the production process, and achieve good industrial application value, high quality, The effect of eliminating bitterness

Active Publication Date: 2020-04-07
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method produces a large amount of waste water, and the production process is not environmentally friendly. In addition, the patent does not involve the impact of impurities in the product on the smell

Method used

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  • Method for preparing nerol and geraniol from citral
  • Method for preparing nerol and geraniol from citral

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] According to the metal element: organic ligand: solvent molar ratio 3:1:20, weigh 2.07g ruthenium trichloride, 0.55g terephthalic acid and 4.87g N,N-dimethylformamide in tetrafluoroethylene In the lined autoclave, stir evenly, tighten and seal the autoclave, heat to 160 °C, keep the temperature for 72 hours, then cool down to 30 °C at a rate of 4 °C / min, open the autoclave and take a sample, which is recorded as MOFs-1.

[0059] The MOFs-1 were immersed in a petroleum ether solution with a silicon content of 5 wt%. The silicon source was tetraethyl orthosilicate. After vacuum impregnation for 15 hours, it was dried at 30°C for 15 hours, and then placed in a muffle furnace at a temperature of 3°C / Slowly raise the temperature to 500°C at a heating rate of min, and then calcine for 2 hours. At this point, a silicon deposition operation is completed. After the deposition is repeated 2 times, the finished catalyst 1# is obtained.

[0060] The molar ratio of ruthenium, terep...

Embodiment 2

[0063] According to the metal element: organic ligand: solvent molar ratio 2:1:30, weigh 6.22g ruthenium trichloride, 2.49g terephthalic acid and 32.89g N,N-dimethylformamide in a PTFE liner In a pressure-resistant environment, stir evenly, tighten and seal the autoclave, heat it to 180°C, keep it warm for 12 hours, then cool it down to 30°C at a rate of 6°C / min, open the autoclave to take a sample, and record it as MOFs-2.

[0064] The MOFs-2 were immersed in a petroleum ether solution with a silicon content of 2wt%. The silicon source was tetraethyl orthosilicate. After vacuum impregnation for 20 hours, it was dried at 30°C for 20 hours, and then placed in a muffle furnace at 2°C / Slowly raise the temperature to 550°C at a heating rate of min, and then calcine for 1 hour. At this point, a silicon deposition operation is completed. After the deposition is repeated 3 times, the finished catalyst 2# is obtained.

[0065] The molar ratio of ruthenium, terephthalic acid and Si in...

Embodiment 3

[0068] According to the metal element: organic ligand: solvent molar ratio 4:1:25, weigh 10.37g ruthenium trichloride, 2.08g terephthalic acid and 22.84g N,N-dimethylformamide in a PTFE liner In a pressure-resistant environment, stir evenly, tightly seal the autoclave, heat it to 150°C, keep it warm for 50 hours, then cool it down to 30°C at a rate of 10°C / min, open the autoclave to take a sample, and record it as MOFs-3.

[0069] According to the method of equal volume impregnation, MOFs-3 was impregnated in petroleum ether solution with a silicon content of 8wt%. The silicon source was tetraethyl orthosilicate. After vacuum impregnation for 10 hours, it was dried at 30°C for 10 hours, and then placed in a muffle furnace. In the process, the temperature was slowly raised to 520°C at a heating rate of 4°C / min, and then calcined for 1.5 hours. At this point, a silicon deposition operation was completed, and the finished catalyst 3# was obtained after repeating the deposition 4 t...

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Abstract

The invention relates to a method for preparing nerol and geraniol from citral. The citral serving as a raw material undergoes a hydrogenation reaction under the action of a catalyst to generate neroland geraniol; and the catalyst comprises an MOFs material (metal-organic framework compound) and a passivation component Si element, and the Si element exists in the form of an oxide. The bitter taste is eliminated by controlling the generation amounts (the total amount is lower than 0.5 wt%) of citronellol and dihydrocitronellol in impurities. The method has the advantages of simplicity in operation, low device requirement, high selectivity, realization of pure aroma temperature and high quality of the prepared product, and excellent industrial application value.

Description

technical field [0001] The invention relates to the field of hydrogenated citral, in particular to a method for preparing nerol and geraniol from citral. Background technique [0002] Citral is a typical α, β-unsaturated aldehyde, which is a mixture of neral and geranial (the structural formula is shown below), and its selective hydrogenation product is a mixture of nerol and geraniol . Nerol and geraniol (structural formula shown below) have a mild sweet smell and a rose fragrance, and are widely used in the deployment of various floral flavors. The raw material of vitamin A is widely used in flavor, medicine and other industries. [0003] [0004] The difficulty of preparing nerol and geraniol by hydrogenation of citral is that the reaction of hydrogenation citral is difficult to achieve very high requirements for product selectivity, the impurities produced are difficult to separate, and there will still be an unpleasant smell in the product after separation ( Such ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/149C07C33/02B01J31/22C11B9/00
CPCC07C29/149B01J31/1691B01J31/2239C11B9/0015B01J2531/822B01J2531/821B01J2231/643C07C33/02
Inventor 方文娟于磊董菁王联防张永振王文丰茂英
Owner WANHUA CHEM GRP CO LTD
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