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Activated carbon-loaded type ruthenium catalyst and preparation and application thereof

A ruthenium catalyst and activated carbon technology, applied in the field of activated carbon supported ruthenium catalysts, can solve the problems of poor catalyst selectivity and versatility, low yield of catalytic series of sugar alcohols, unsatisfactory catalyst selectivity, etc. Conversion and product selectivity, low cost effect

Inactive Publication Date: 2019-03-12
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN105859522A discloses a general-purpose precious metal catalyst to catalyze the reduction of glucose, fructose, galactose, xylose, and arabinose to prepare a series of sugar alcohols. The reaction uses formate as the hydrogen donor and is environmentally friendly, but the catalyst selectivity is not ideal. Low sugar alcohol yield between 44-83%
In summary, the current sugar alcohol preparation process has the problems of poor catalyst selectivity and versatility, and low yields for the preparation of catalytic series of sugar alcohols.

Method used

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  • Activated carbon-loaded type ruthenium catalyst and preparation and application thereof
  • Activated carbon-loaded type ruthenium catalyst and preparation and application thereof
  • Activated carbon-loaded type ruthenium catalyst and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Preparation of Ru / C catalyst

[0025] (1) Pretreatment of activated carbon: Add 20 g of activated carbon to a round bottom ground flask, and then add 300 mL of 10% nitric acid solution. Place the flask in a water bath thermostat, install a reflux condenser on it, turn on the power, set the water bath thermostat to 90°C, and reflux at constant temperature for 3 hours. After the constant temperature is over, it is naturally cooled to room temperature and then filtered, then washed with distilled water until the filtrate is neutral, and dried under vacuum at 60°C.

[0026] (2) Load: add 1.0g of activated carbon treated with nitric acid to 100mL of ultrapure water, add 0.14g of ruthenium trichloride, add 20mL of ethylene glycol, heat up to 80°C, stir and reflux for 12h. After the precipitation is complete, the solution is filtered hot, and the catalyst is washed with distilled water to neutrality. Dry under vacuum at 60°C to prepare a catalytically active Ru / C catal...

Embodiment 2

[0027] Example 2: Sugar conversion rate and selective detection method of sugar alcohol

[0028] Take 20μL of the reactant before sealing the reactor and the product after hydrogenation, and dilute it to 1mL with ultrapure water. Detect the concentration of sugar in the reactant, the residual sugar concentration and sugar alcohol concentration in the product by high performance liquid chromatography .

[0029] The high performance liquid chromatographic instrument used for detection is the 2414 differential detector of waters system, the chromatographic column is AminexHPX-87H column (300×7.8mm), the mobile phase is 5mM H 2 SO 4 , The flow rate is 0.6mL / min, the column temperature is 60.0℃, and the injection volume is 20μL.

[0030] The formula for calculating sugar conversion rate and sugar alcohol selectivity is as follows:

[0031]

[0032]

Embodiment 3

[0033] Example 3: Hydrogenation of xylose to produce xylitol

[0034]

[0035] Weigh 5.0 g of anhydrous xylose, add it to 45 mL of ultrapure water, prepare a 10% xylose solution, transfer the xylose solution to a 100 mL reactor, add 0.5 g of Ru / C catalyst, and seal the reactor. Replace the reactor with nitrogen three times to remove the air in the reactor. Adjust the temperature of the reaction kettle to 120°C and the stirring speed to 500 rpm. After the temperature stabilizes, hydrogen is charged to 4.0 MPa to start the reaction. After 120 minutes of reaction, the reactor was rapidly cooled, and when the temperature dropped to room temperature, hydrogen was vented to end the hydrogenation reaction.

[0036] Using the method of Example 2 for detection, the conversion rate of xylose was 99.2%, and the selectivity of xylitol was 99.1%.

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Abstract

The invention relates to an activated carbon-loaded type ruthenium catalyst and a preparation method and application thereof in preparation of sugar alcohols by catalytic hydrogenation of saccharides.The preparation method comprises the following steps of loading metal ruthenium onto the activated carbon by a simple impregnating reduction method, so as to prepare the loaded type Ru / C (ruthenium / carbon) catalyst with high dispersion degree; further applying the Ru / C catalyst into the hydrogenation process of a series of saccharides, such as xylose, arabinose, glucose, mannose and maltose, so as to prepare xylitol, arabitol, sorbitol, mannitol and maltitol at high efficiency. The activated carbon-loaded type ruthenium catalyst has the advantages that under certain reaction conditions, the high conversion rate of series saccharides and the high selectivity of sugar alcohols can be realized, the stability of the catalyst is good, the recycling is convenient, and the frequency of cyclic use is high; the preparation technology is simple, the production cost is low, the catalytic activity is high, and the preparation technology is suitable for preparing multiple types of sugar alcohols,has good universality and is suitable for being popularized.

Description

(1) Technical field [0001] The invention relates to an activated carbon supported ruthenium catalyst, a preparation method thereof and its application in sugar alcohol preparation by catalytic hydrogenation of sugar. (2) Background technology [0002] Sugar alcohol refers to a polyhydric alcohol produced by reducing the aldehyde and ketone carbonyl groups of sugars to hydroxyl groups. Sugar alcohol has moderate sweetness and low calorific value. It is a green and healthy new sweetener; generally does not affect insulin secretion, does not cause blood sugar fluctuations, and has the effect of protecting the liver and lowering lipids. It can be used as an auxiliary treatment for diabetes, etc. In addition, sugar alcohol has good hygroscopicity and no irritation to the skin. It can be used as a moisture regulator and is widely used in cosmetics. [0003] Except for erythritol, the main sugar alcohols are all prepared by hydrogenating corresponding sugars under high temperature and hi...

Claims

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Application Information

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IPC IPC(8): B01J23/46B01J37/02B01J37/16C07C31/18C07C31/26C07C29/132C07H15/04C07H1/00
CPCB01J23/462B01J37/0207B01J37/16C07C29/132C07H1/00C07H15/04C07C31/18C07C31/26Y02P20/584
Inventor 柳志强张晓健郑裕国李海伟汤晓玲
Owner ZHEJIANG UNIV OF TECH
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