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High-selectivity amino acid decarboxylation catalyst and preparation method thereof

A high-selectivity, amino acid technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, preparation of amino compounds from amines, etc., can solve the problem of low selectivity of 2-methylbutylamine, to improve decarboxylation selectivity, High conversion rate, easy to realize the effect of industrialization

Active Publication Date: 2020-04-28
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved in the present invention is aimed at the prior art, the problem that isoleucine decarboxylation prepares 2-methylbutylamine selectivity is lower, provides A highly selective amino acid decarboxylation catalyst and preparation method thereof

Method used

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  • High-selectivity amino acid decarboxylation catalyst and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0028] Place 100 mL of 2% dilute nitric acid solution in a 50°C water bath. Add 8g TiOSO while stirring 4 , where TiOSO 4 The volume ratio with the nitric acid aqueous solution is 1:20. While maintaining stirring, 6 mL of polyethylene glycol-2000 was added dropwise. The resulting mixture was stirred at 50° C. for 6 h, and the suspension was centrifuged and filtered. Then wash with water and wash with alcohol three times each, dry at 50°C for 12h, and then roast at 450°C in air atmosphere for 4h to obtain 3.52g of prepared TiO 2 , the target amount is obtained after repeated accumulation.

[0029] 1.3g RuCl 3 ·3H 2 O was dissolved in 80ml of absolute ethanol, ultrasonically dissolved, and then 20g of TiO was added 2 -1, strongly stirred and impregnated for 16 hours; the obtained material was desolventized, dried, fully washed with deionized water, dried at 100°C, calcined at 350°C for 4 hours in an air atmosphere, and cooled in a dry environment to room temperature. Af...

Embodiment 2

[0031] TiO 2 -1 is prepared with embodiment 1. 3.6g RuCl 3 ·3H 2 O was dissolved in deionized water, ultrasonically dissolved, and then 20 g TiO 2 -1, strongly stirred and impregnated for 24 hours; the obtained material was desolventized, dried, fully washed with deionized water, dried at 100°C, granulated, shaped and dried again, then placed in air at 450°C Under roasting for 8h, cooled to room temperature in a dry environment. The sample was then placed in a hydrogen atmosphere and reduced at 500° C. for 3 hours to obtain catalyst B for amino acid decarboxylation.

Embodiment 3

[0033] TiO 2 -1 is prepared with embodiment 1. 3.9g RuCl 3 ·3H 2 O was dissolved in deionized water, ultrasonically dissolved, and then 20 g of commercially available anatase TiO 2 , vigorously stirred and impregnated for 24 hours; the obtained material was desolventized, dried, fully washed with deionized water, dried at 100°C, granulated, shaped and dried again, then roasted at 350°C in air atmosphere 8h, cooled to room temperature in a dry environment. The sample was then placed under a hydrogen atmosphere and reduced at 500° C. for 3 hours to obtain Catalyst C for decarboxylation of amino acid.

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Abstract

The invention discloses an isoleucine decarboxylation catalyst and a preparation method thereof. A catalyst precursor comprises the following components in percentage by mass: 0.1-10% of Ru and the balance of TiO2, wherein TiO2 is a self-made anatase phase carrier and has a Ti < 3 + > structure. The anatase phase carrier is adopted, the dispersity of loaded Ru is improved, and the electronic states of Ru and Ti are fixed in a state which is most beneficial to decarboxylation of amino acid through a specific reduction step so that the highest selectivity of preparing amine through direct decarboxylation is achieved. The catalyst is high in conversion rate, and the conversion rate of the isoleucine decarboxylation reaction can be stably kept at 97.0% or above. The catalyst is applied to a reaction for preparing 2-methylbutylamine through catalytic decarboxylation of isoleucine, and the selectivity of generated amine can be stably kept at 90.0% or above under the reaction conditions thatthe initial pressure is 2 Mpa, the reaction temperature is 150-180 DEG C and the reaction time is 4-8 h.

Description

technical field [0001] The invention belongs to the field of catalysts, and in particular relates to a highly selective amino acid decarboxylation catalyst and a preparation method thereof. Background technique [0002] Amino acids are attractive bio-based materials for the synthesis of complex organisms, but the preparation of chemicals from amino acids through catalytic conversion pathways still faces many challenges. Since amino acids have multiple functional groups, that is, the special structure of an amino group and a carboxyl group, amino acids produce different products under different reaction conditions. The decarboxylation of amino acids to synthesize amines is a hot topic in the research of catalytic conversion of amino acids (Chemical Communications, 2017, 53(42): 5682-5693.), because the main by-product is carbon dioxide, and the generated products are easy to separate and the process is simple to operate. [0003] However, there are few reports on catalysts f...

Claims

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Application Information

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IPC IPC(8): B01J23/46B01J37/02B01J35/10B01J21/06C07C209/68C07C211/07
CPCB01J23/462B01J37/0201B01J21/063C07C209/68B01J35/695C07C211/07
Inventor 杨建明吕剑李佳霖张前石坚余秦伟王为强梅苏宁赵锋伟袁俊惠丰寇联岗
Owner XIAN MODERN CHEM RES INST