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Preparation method of tin based catalyst, tin based catalyst and application of tin based catalyst

A catalyst, tin-based technology, applied in the field of catalysis in biomass conversion, can solve the problems of complex catalyst preparation process, difficult molecular sieve preparation, low selectivity, etc., achieve good industrial application prospects, single active site of catalyst, and space-time conversion rate high effect

Active Publication Date: 2017-06-20
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the main isomerization method is alkaline isomerization, but under alkaline conditions, fructose is unstable, easy to decompose, rearrange, and generate a large number of by-products, and the yield of fructose is low.
Another isomerization method is acidic isomerization, which mainly utilizes the acidic effect of molecular sieve skeleton tin, but there are disadvantages such as difficult preparation of molecular sieves, long cycle time, and low selectivity (Green Chem., 2013, 15, 2777-2785 )
[0004] Esben Taarning and others used Sn-Beta molecular sieves to realize the direct conversion of glucose and fructose to prepare lactate (Science, 2010, 602-605), but the preparation process of this catalyst is complicated and difficult to realize the application
In the later research, Bert F. Sels et al. used Beta molecular sieve dealumination and tinning method to introduce tin into the molecular sieve framework (ACS Catal., 2015, 5, 928-940). However, the dealumination process of this method is uncontrollable. There are disadvantages of incomplete dealumination and a certain amount of B acid, so a certain amount of by-products will be generated in the conversion of carbohydrates

Method used

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  • Preparation method of tin based catalyst, tin based catalyst and application of tin based catalyst
  • Preparation method of tin based catalyst, tin based catalyst and application of tin based catalyst
  • Preparation method of tin based catalyst, tin based catalyst and application of tin based catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Preparation of SBA-15: Dissolve 16g of P123 in 120g of water and 472mL of hydrochloric acid (2M) aqueous solution at 40℃. Crystallize in a hydrothermal kettle at 100°C for 24h, filter and wash with water, dry at 100°C, and roast at 550°C to obtain white powder SBA-15.

[0027] Preparation of MCM-41: Dissolve 25g of sodium silicate in a beaker with 30ml of distilled water, heat and dissolve 6.4g of cetyltrimethyl bromide surfactant (CTAB) in 20ml of distilled water, and cool to room temperature , after mixing, stir for 10 min, adjust the pH value of the mixture to 10 with sulfuric acid solution (5 mol / L), and continue stirring for 80 min, so that the solution becomes a viscous transparent gel. Then put it into a 100ml stainless steel hydrothermal kettle with a polytetrafluoroethylene liner, place it in an oven, crystallize at 130°C for 72 hours, take it out, cool it and filter it, wash until neutral, and then dry it at 90°C Overnight, the resulting semi-finished product...

Embodiment 2

[0030] Preparation of tin-based molecular sieve catalyst:

[0031] The precursor of tin: one or more of tin tetrachloride, tin dichloride, dimethyl tin, dioctyl tin, tetraphenyl tin, tributyl tin acetate, triphenyl tin, dissolved in ethanol in solution. At a certain temperature, pure silicon molecular sieves were added, stirred for 5 hours, filtered, dried and calcined at 600°C to obtain a Sn-molecular sieve catalyst.

[0032] The precursor of tin: one or more of tin tetrachloride, tin dichloride, dimethyl tin, dioctyl tin, tetraphenyl tin, tributyl tin acetate, triphenyl tin, dissolved in ethanol in solution. At a certain temperature, pure silicon molecular sieves were added, stirred for 12 hours, filtered, dried and calcined at 600° C. to obtain a Sn-molecular sieve catalyst.

[0033] The precursor of tin: one or more of tin tetrachloride, tin dichloride, dimethyl tin, dioctyl tin, tetraphenyl tin, tributyl tin acetate, triphenyl tin, dissolved in iso in propanol solutio...

Embodiment 3

[0037] Isomerization experiment: Add 0.5g of carbohydrates, 0.15g of catalyst and 5ml of water or alcohol solution into a 20ml reaction kettle, pass through nitrogen to replace the gas three times, program the temperature to 100-120°C, and react for 5-200min. After the reaction, cool down to room temperature, take the centrifuged supernatant, separate it on a high-performance liquid chromatography calcium-type ion-exchange column and detect it with a differential refraction detector. Products such as fructose and HMF are calculated in the product yield.

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Abstract

The invention provides preparation of a tin based catalyst and an application of the tin based catalyst in catalytic conversion of carbohydrates. According to the method, the tin based catalyst is prepared by an ion exchange method and is applied in a reaction for preparation of lactic acid ester through isomerization and catalytic conversion of the carbohydrates, and at the temperature of 80-210 DEG C and through a one-step catalytic conversion process, fructose or lactic acid ester is prepared from the carbohydrates with high efficiency, high selectivity and high yield. The reaction provided by the invention has the remarkable advantages of raw materials as renewable resources and high atom economy. At the same time, the catalyst preparation process has the advantages of being simple and feasible to implement and low in cost. In addition, compared with other technologies for preparing fructose or lactic acid ester by using biomass as raw material, the process has the advantages of simple reaction process, high space-time yield and convenience in industrialized production.

Description

technical field [0001] The invention belongs to the field of catalysis in biomass conversion, in particular to the preparation of a tin-based catalyst and its application in the catalytic conversion of carbohydrates, specifically the isomerization of carbohydrates under the tin-based catalyst and the catalytic conversion of carbohydrates Prepared as lactate reaction. Background technique [0002] Immobilized tin-based catalysts have unique Lewis acidity and exhibit unique reactivity in many catalytic reactions, thus attracting widespread attention from researchers. At present, the preparation of tin-based molecular sieve catalysts still has the characteristic of long preparation time. Avelino Corma et al. (Nature, 2001,412:424-425) utilize tetraethyl orthosilicate, SnCl 4 ·H 2 O is used as a raw material to obtain a tin-containing Sn-Beta molecular sieve after hydrolysis and crystallization, which has good Lewis acidity, but this method requires a long preparation period,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/035B01J23/14C07C67/39C07C69/68
CPCB01J21/06B01J23/14B01J29/0308B01J29/035B01J2229/18C07C67/39C07C69/68
Inventor 庞纪峰郑明远张涛姜宇孙睿岩王爱琴王晓东
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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