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ZSM-5 molecular sieve loaded Ru (ruthenium) catalyst as well as preparation and application thereof

A technology of ZSM-5 and ruthenium catalyst, which is applied in the direction of molecular sieve catalyst, catalyst activation/preparation, hydroxyl compound preparation, etc., can solve the problems of increasing production cost of sugar alcohol, poor catalyst stability, complicated preparation method, etc., to improve utilization rate, Good stability and simple preparation process

Inactive Publication Date: 2019-02-22
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the nickel-based catalyst selected by this method has the disadvantages of being sensitive to the pH of the solution and being easily deactivated; the activated carbon and oxide carrier used to load the active metal have problems such as uneven pore size distribution and poor mechanical properties, resulting in poor stability of the catalyst. The amount of catalyst used in the hydrogenation process is relatively large, which increases the production cost of sugar alcohols
[0006] To sum up, the current catalysts used in the sugar alcohol production process have problems such as complex preparation methods, high preparation costs, poor stability, and poor versatility.

Method used

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  • ZSM-5 molecular sieve loaded Ru (ruthenium) catalyst as well as preparation and application thereof
  • ZSM-5 molecular sieve loaded Ru (ruthenium) catalyst as well as preparation and application thereof
  • ZSM-5 molecular sieve loaded Ru (ruthenium) catalyst as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1: the preparation of Ru / ZSM-5 catalyst

[0022] Add 10mL of ethanol, 1.0g of ZSM-5 molecular sieve (pore size range of 0.5-5.0nm, Si / Al of 40), 0.18g of ruthenium trichloride into a 100mL three-necked flask, and ultrasonically disperse the resulting mixture at 45°C for 15min. in N 2 Stir at 60°C for 4 h under atmosphere, add 3 mL of 1 mol / L sodium borohydride solution, and continue stirring for 10 h. After the reaction was completed, it was centrifuged at 8000rpm for 3min, washed three times with ultrapure water, and then dried in a vacuum oven at 60°C for 12h to obtain the Ru / ZSM-5 catalyst, wherein the average particle size of ruthenium was 2.0nm, and the ruthenium The loading was 4.0 wt%.

Embodiment 2

[0023] Embodiment 2: the conversion rate of sugar and the selective detection method of sugar alcohol

[0024] Take 20 μL of the reactant before the sealed reactor and the product after the hydrogenation reaction, dilute to 1 mL with ultrapure water, and detect the sugar concentration in the reactant, the residual sugar concentration and the sugar alcohol concentration in the product by high performance liquid chromatography .

[0025] The high-performance liquid chromatographic instrument used for detection is a waters system 2414 differential detector, and the chromatographic column is an AminexHPX-87H column (300 × 7.8mm), and the mobile phase is 5mM H 2 SO 4 , flow rate 0.6 mL / min, column temperature: 60.0°C, injection volume: 20 μL.

[0026] The conversion rate of sugar and the selectivity calculation formula of sugar alcohol are as follows:

[0027]

[0028]

Embodiment 3

[0029] Embodiment 3: Preparation of xylitol by hydrogenation of xylose

[0030]

[0031] Weigh 10.0g of anhydrous xylose, add it to 40mL ultrapure water, prepare a xylose solution with a mass fraction of 20%, transfer the xylose solution to a 100mL reactor, add 1.0g of Ru / ZSM-5 catalyst, and seal the reaction kettle. The reactor was replaced three times with nitrogen, and the air in the reactor was removed. Adjust the temperature of the reactor to 110° C., and the stirring speed to 500 rpm. After the temperature is stabilized, hydrogen gas is charged to 4.0 MPa to start the reaction. After reacting for 100 minutes, the reactor was rapidly cooled, and when the temperature dropped to room temperature, the hydrogen gas was vented to end the hydrogenation reaction.

[0032] Using the method of Example 2 to detect, the conversion rate of xylose is 100%, and the selectivity of xylitol is 99.2%.

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Abstract

The invention relates to a ZSM-5 molecular sieve loaded Ru (ruthenium) catalyst, a preparation method of the ZSM-5 molecular sieve loaded Ru catalyst and application of the ZSM-5 molecular sieve loaded Ru catalyst to sugar alcohol preparation through sugar catalytic hydrogenation. Metal Ru is loaded on a ZSM-5 molecular sieve with high specific surface area by a simple impregnation reduction method; a Ru / ZSM-5 catalyst with high dispersity and high activity is prepared. The catalyst is applied to preparation of series sugar alcohol such as xylitol, arbaitol, sorbitol, mannose and maltol; the product selectivity is high; the yield is high; the catalyst has high activity and good stability; the multiple-batch repeated utilization can be realized; the comprehensive cost is low. In a word, thepreparation process of the catalyst is simple; the catalytic efficiency is high; the stability is high; the catalyst is applicable to the preparation process of various kinds of sugar alcohol; the universality is high; the popularization is facilitated.

Description

(1) Technical field [0001] The invention relates to a ZSM-5 molecular sieve-supported ruthenium catalyst, a preparation method thereof and an application thereof in sugar alcohol catalytic hydrogenation preparation. (2) Background technology [0002] Sugar alcohols refer to a class of polyols formed after the aldehyde and ketone carbonyl groups of sugars are reduced to hydroxyl groups. Sugar alcohol has moderate sweetness and low calorific value. It is a green and healthy new sweetener; it has high heat resistance and does not produce Maillard reaction at high temperature, so it can be used as an additive for baked food. The metabolism of sugar alcohols in the body does not affect insulin secretion, does not cause fluctuations in blood sugar, and has the effect of protecting the liver and reducing fat. It can be used as an auxiliary therapeutic agent and special nutritional agent for patients with diabetes; it is not suitable as a nutrition for oral microorganisms Source, c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/44B01J37/34B01J37/02B01J37/16C07C29/141C07C31/26C07H1/00C07H15/04
CPCB01J29/44B01J37/0201B01J37/16B01J37/343B01J2229/18C07C29/141C07H1/00C07H15/04C07C31/26Y02P20/584
Inventor 柳志强张晓健郑裕国李海伟王友亮金利群
Owner ZHEJIANG UNIV OF TECH