Method for hydrogenation utilization of linalool rectification kettle residual liquid

A linalool and rectifying kettle technology, which is applied in the field of hydrogenation and utilization of linalool rectifying kettle residue liquid, can solve the problems affecting product yield and purity, more stringent control of product purity and content of harmful substances, complex components, etc. The problem is to achieve the effect of improving the selectivity of raw materials and product yield, wide production and application value, and high product purity and yield.

Active Publication Date: 2020-05-29
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Due to the complex components of the linalool vacuum distillation raffinate, impurities and heavy components will affect the life of the catalyst and the catalytic selectivity, the prior art still has no information on the hydrogenation and utilization selectivity of the linalool vacuum distillation raffinate Reports of generating dihydrolinalool or tetrahydrolinalool, and there is a large amount of dehydrolinalool containing carbon-carbon triple bonds in the vacuum distillation raffinate of linalool, which will produce heavy components in the process of hydrogenation utilization By-products affect the yield and purity of the product, especially if the product is a precious spice, the control of product purity and harmful substance content is more stringent

Method used

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  • Method for hydrogenation utilization of linalool rectification kettle residual liquid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 100 g of n-hexane, 100 g of linalool rectification raffinate, 2 g of 1,2-propylenediamine, 1.0 g of w(Ru)=5% ruthenium carbon catalyst to the autoclave, seal the autoclave, and replace with 4.0 MPa nitrogen 6 times . Use hydrogen pressure (gauge pressure) 4.0MPa to replace 6 times, turn on the stirring paddle, keep hydrogen pressure (gauge pressure) 4.0MPa, and keep the inner temperature of the reactor at 120°C for 6h. After cooling down, stop stirring and release the pressure. Filtration separation reclaims catalyst, and gas chromatographic analysis product is composed of: tetrahydrolinalool 96.5%, linalool 0.1%, dihydrolinalool 0.1%, other 3.3% (wherein the component content of molecular weight greater than 200 accounts for 0.08%). Raw material conversion rate: 99.79%, tetrahydrolinalool selectivity: 99.69%.

Embodiment 2

[0036] Add 100 g of ethanol, 100 g of linalool rectification raffinate, 2 g of ethylenediamine, and 1.0 g of w(Ru)=5% ruthenium carbon catalyst to the autoclave, seal the autoclave, and replace with 6.0 MPa nitrogen 6 times. Use hydrogen pressure (gauge pressure) 6.0MPa to replace 6 times, turn on the stirring paddle, keep the hydrogen pressure (gauge pressure) 6.0MPa, and keep the inner temperature of the reactor at 80°C for 12h. After cooling down, stop stirring and release the pressure. The catalyst was separated and recovered by filtration, and the gas chromatographic analysis product consisted of: tetrahydrolinalool 96.8%, dihydrolinalool 0.1%, and others 3.1% (the content of components with a molecular weight greater than 200 accounted for 0.12% in liquid phase detection). Conversion rate: 99.90%, tetrahydrolinalool selectivity: 99.90%.

Embodiment 3

[0038] Add toluene 150g, linalool rectification raffinate 100g, ethylenediamine 0.2g, w(Ru)=1% ruthenium carbon catalyst 0.5g to autoclave, autoclave is sealed, 0.5MPa nitrogen replacement 6 times. Use a pressure (gauge pressure) of 0.5 MPa hydrogen to replace 6 times, turn on the stirring paddle, keep the hydrogen pressure (gauge pressure) 0.5 MPa, and keep the inner temperature of the reactor at 180°C for 24 hours. After cooling down, stop stirring and release the pressure. Filtration separation reclaims catalyst, and gas chromatographic analysis product is composed of: tetrahydrolinalool 95.8%, dihydrolinalool 0.2%, linalool 0.5%, other 3.5% (wherein the component content of molecular weight greater than 200 accounts for 0.19%). Conversion rate: 99.28%, tetrahydrolinalool selectivity: 99.48%.

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Abstract

The invention provides a method for hydrogenation utilization of linalool rectification kettle residual liquid. According to the method, the linalool rectification kettle residual liquid with heavy components removed is taken as a raw material and is subjected to a hydrogenation reaction to synthesize dihydrolinalool or tetrahydrolinalool. According to the method, a ruthenium-carbon catalyst is used for carrying out hydrogenation reaction on the linalool rectification kettle residual liquid, and when no metal salt is added for modifying the catalyst, tetrahydrolinalool can be prepared with high selectivity; when a metal salt is added to modify the catalyst, dihydrolinalool can be prepared with high selectivity, so that productivity regulation and control of different hydrogenation productsare realized according to market demand conditions, and the method has wide actual production and application values. Besides, diamine substance can stabilize hydrogen ions at the carbon-carbon triple bond end position in the dehydrolinalool and inhibit the polymerization reaction, thereby inhibiting the generation of heavy component byproducts and being beneficial to enhancing the selectivity ofthe raw material and the yield of the product.

Description

technical field [0001] The invention relates to a method, in particular to a method for hydrogenation and utilization of linalool rectification still residual liquid, and belongs to the technical field of waste liquid recovery and utilization. Background technique [0002] Linalool is an important fragrance product and can synthesize vitamin E and dozens of fragrances, such as linalyl acetate, linalyl propionate, Erinthal, dihydrolinalool and its esters, tetrahydrolinalyl Alcohols and their esters, etc. The synthetic method of linalool is shown in the following formula, is to take dehydrolinalool as raw material through selective hydrogenation to synthesize linalool, unavoidably have excessive hydrogenation product to generate (dihydrolinalool and tetrahydrolinalool) in the reaction process Hydrolinalool). Dehydrolinalool has a higher boiling point than linalool, so the linalool rectification still raffinate mainly contains components such as dehydrolinalool, linalool, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/17C07C31/125C07C33/025B01J23/652B01J23/656
CPCC07C29/172C07C29/17B01J23/6562B01J23/6522C07C31/125C07C33/025
Inventor 鲍元野张永振黎源
Owner WANHUA CHEM GRP CO LTD
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