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Method for preparing hydrogenated rosin through rosin hydrogenation and catalyst thereof

A technology for rosin hydrogenation and hydrogenation of rosin, which is applied in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of high catalyst cost, poor recycling effect, low catalytic activity, etc. The effect of improved efficiency, low cost and high catalytic activity

Active Publication Date: 2020-11-03
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the problems of high catalyst cost, low catalytic activity under mild conditions, and poor recycling effect in the prior art, the present invention provides a method for preparing hydrogenated rosin by hydrogenating rosin

Method used

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  • Method for preparing hydrogenated rosin through rosin hydrogenation and catalyst thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1 Catalyst Ni / CxNy@mSiO 2 preparation of

[0023] S 1 , Amphiphilic nano-mesoporous material CxNy@mSiO 2 The preparation of 0.16g CTAB (cetyltrimethylammonium bromide) and 5mLEDA (ethylenediamine) were weighed respectively and dispersed in the mixed solution of ethanol and water of 50mL (ethanol: water=3:7) , then add 0.12g resorcinol, ultrasonically disperse for 30min, add 0.24mL formaldehyde dropwise, stir for 2h, then add 50mg CTAB, add 0.8mLTEOS (tetraethyl orthosilicate) dropwise, continue stirring for 12h, and then stand for aging 48h, centrifugal separation, and finally high-temperature carbonization under argon atmosphere to obtain the amphiphilic nano-mesoporous material CxNy@mSiO 2 ;

[0024]S 2 , Amphiphilic nanocatalyst Ni / CxNy@mSiO 2 Preparation, weigh 200mg CxNy@mSiO 2 Add it into a three-necked flask, ultrasonically disperse in ethanol solution at room temperature, and then add 50mg NiCl 2 , continue to disperse for 10min, then weigh 30mgN...

Embodiment 2

[0025] Embodiment 2 rosin hydrogenation prepares hydrogenated rosin

[0026] Weigh 1g of rosin and add it to a stainless steel mechanically stirred tank, then add 4mL of water and 6mL of 200# solvent oil, and weigh 40mg of the amphiphilic catalyst Ni / CxNy@mSiO 2 Mix evenly, replace the gas in the kettle with 1MPa hydrogen for 4 times, then flush into 4MPa hydrogen, and react with mechanical stirring at 140°C for 4 hours. After the reaction, let stand for a period of time to separate the catalyst from the product, collect the upper product phase and use chromatography Quantitative analysis shows that the conversion rate of rosin reaches 94.78%, the selectivity of tetrahydroabietic acid in the product is 61.80%, and the selectivity of dihydroarginic acid is 35.12%, which meet the requirements of super-grade rosin.

Embodiment 3

[0027] Embodiment 3 rosin hydrogenation prepares hydrogenated rosin

[0028] Weigh 1g of rosin and add it to a stainless steel mechanically stirred tank, then add 4mL of water and 6mL of 200# solvent oil, and weigh 40mg of the amphiphilic catalyst Ni / CxNy@mSiO 2 Mix evenly, replace the gas in the kettle with 1MPa hydrogen for 4 times, then pour in 2MPa hydrogen, and react with mechanical stirring at 120°C for 2 hours. Quantitative analysis by chromatography shows that the conversion rate of rosin reaches 92.09%, the selectivity of tetrahydroabietic acid in the product is 61.17%, and the selectivity of dihydroarginic acid is 29.09%, which meets the requirements of super-grade rosin.

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Abstract

The invention belongs to the technical field of hydrogenated rosin preparation, and discloses a method for preparing hydrogenated rosin through rosin hydrogenation and a catalyst thereof. The method comprises the following steps: in a mixed solution of water and 200 # solvent oil, introducing H2 under the catalytic action of a Juans type hollow amphiphilic nano catalyst Ni / CxNy@mSiO2, and catalyzing rosin hydrogenation to prepare hydrogenated rosin. The Ni-based catalyst Ni / CxNy@mSiO2 provided by the invention shows good catalytic activity and product selectivity, so that the rosin hydrogenation reaction is mild in condition and is environment-friendly.

Description

technical field [0001] The invention relates to the technical field of hydrogenated rosin preparation, in particular to a method for preparing hydrogenated rosin by hydrogenating rosin and a catalyst thereof. Background technique [0002] Rosin is the solid left after distillation and cooling of pine oil exuded from pine plants. Its general color is yellow or brown. It is a renewable chemical raw material and is widely used in materials, medicine, rubber, graphite and other industries; my country is a major producer of rosin, with an output of 6.7987 million tons per year, but the utilization rate is low, and it is exported directly without further processing, causing a large amount of economic losses. Rosin is a kind of complex compound, its main component is abietic acid type resin acid, abietic acid type resin acid has a pair of conjugated double bonds and a three-membered phenanthrene ring skeleton structure, and has multiple isomers, Including pimaric acid, abietic acid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/08C09F1/04
CPCB01J27/24C09F1/04B01J35/396B01J35/51
Inventor 解从霞于凤丽吴方柱李雯袁冰于世涛
Owner QINGDAO UNIV OF SCI & TECH
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