Method for preparing pyruvic aldehyde

A technology of glyoxal and titanium-silicon molecular sieve is applied in the preparation of heterocyclic compounds, the preparation of carbon-based compounds, chemical instruments and methods, etc. It can solve the problems of difficulty in obtaining hydroxyacetone and high cost, and achieve high sugar conversion rate and separation energy consumption. Low, process safe and efficient effect

Active Publication Date: 2020-06-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Catalytic dehydrogenation of glycerol also requires the use of expensive noble metal catalysts
The product yield and reactant conversion rate of hydroxyacetone gas-phase catalytic oxidation are high, but the reactant hydroxyacetone is not easy to obtain

Method used

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  • Method for preparing pyruvic aldehyde

Examples

Experimental program
Comparison scheme
Effect test

preparation Embodiment 1

[0043] This preparation example prepares Sn-MFI molecular sieve, and specific preparation method is:

[0044] tin tetrachloride pentahydrate (SnCl 4 .5H 2 O) Dissolve in water, add this aqueous solution to tetraethyl orthosilicate (TEOS) and stir, add tetrapropylammonium hydroxide (TPAOH, 20% aqueous solution) and water under stirring, and continue stirring for 30 minutes to obtain a chemical composition of 0.03SnO 2 : SiO 2 :0.45TPA: 35H 2 The clear liquid of O was then crystallized at 433K for 2 days, and then the obtained solid was filtered, washed with distilled water, dried at 393K for 5 hours, and then calcined at 823K for 10 hours to obtain a molecular sieve sample. Among them, the amount of TEOS is 15.31g, the amount of TPAOH is 33.67g, SnCl 4 .5H 2 The amount of O used is 0.38g, and the amount of water used is 39.64g.

preparation Embodiment 2

[0046] This preparation example references "Nemeth L, Moscoso J, Erdman N, et al.Synthesis and characterization of Sn-Beta as a selective oxidation catalyst [J]. Studies in Surface Science & Catalysis, 2004, 154 (04): 2626-2631" Method prepares Sn-Beta molecular sieve, the preparation method of the adopted Sn-Beta molecular sieve is:

[0047] tin tetrachloride pentahydrate (SnCl 4 .5H 2 O) Dissolve in water, add tetraethyl ammonium hydroxide (TEAOH) to this aqueous solution and stir with tetraethyl ammonium hydroxide (TEAOH), stir until TEOS evaporates to obtain alcohol, add hydrogen fluoride (HF) to the clarified liquid , forming a paste-like thin layer. Finally, a suspension of dealuminated nano Beta seeds (20nm) and water is added to obtain a chemical composition of 0.03SnO 2 : SiO 2 :6TEA:15H 2 O: 10HF clear liquid, then crystallized at 413K for 10 days, then filtered the obtained solid, washed with distilled water, dried at 393K for 5 hours, and then roasted at 823K ...

preparation Embodiment 3

[0049] References for this preparation example "Yang X, Wu L, Wang Z, et al. Conversion of dihydroxyacetone to methyl lactate catalyzed by highly active hierarchical Sn-USY at room temperature [J]. Catalysis Science & Technology, 2016, 6 (6): 1757- 1763" method to prepare Sn-USY molecular sieve, the preparation method of the Sn-USY molecular sieve adopted is:

[0050] H-USY molecular sieve was mixed with nitric acid, treated at 85°C for 8h, the sample was filtered and washed with deionized water, and dried at 120°C for 12h to obtain a solid sample. This solid sample was mixed with tin tetrachloride pentahydrate (SnCl 4 .5H 2 O) mixed for 1h to obtain a chemical composition of 0.03SnO 2 : 100SiO2 2The mixed liquid was dried at 100°C for 12 hours, and finally calcined at 550°C for 3 hours to obtain a molecular sieve sample. Among them, the amount of H-USY is 2.0g, the amount of nitric acid is 50mL, the amount of SnCl 4 .5H 2 The amount of O used is 0.6 g.

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Abstract

The invention relates to a method for preparing pyruvic aldehyde. The method comprises the following steps of: contacting sugar with a catalyst in a reactor in the presence of alcohol, and reacting toobtain a pyruvic aldehyde-containing product, wherein the molar ratio of the sugar to the alcohol is 1:1, the reaction temperature is 100 DEG C or above and lower than 150 DEG C, the reaction time is10-50 h, the catalyst contains a mixture of a titanium-silicon molecular sieve and a tin-silicon molecular sieve, and the weight ratio of the sugar to the mixture of the titanium-silicon molecular sieve and the tin-silicon molecular sieve based on the dry basis weight is 1:(0.1-6). The method provided by the invention has high sugar conversion rate and high pyruvic aldehyde yield.

Description

technical field [0001] The invention relates to a method for preparing methylglyoxal. Background technique [0002] Methylglyoxal is an aldehyde compound, also known as methylglyoxal, 2-oxopropanal. The form is yellow or yellow-brown transparent liquid with pungent smell and hygroscopicity. Density 1.200g / cm 3 , a melting point of 25°C, a boiling point of 72°C, and a refractive index of 1.4209. This substance is easily polymerized into viscous semi-solid, dissolves in water, releases heat, and returns to monomer solution. Heating at 72°C forms a yellow-green gas, which can last for several days in a closed tube. The commercial product is generally 20%-40% aqueous solution. It is used as medicine, pesticide intermediate and biochemical reagent, and can also be used as raw material of cimetidine, lactic acid, pyruvic acid, analgesic, anticancer, antihypertensive drug, desensitizer and cosmetics. [0003] Traditional production methods of methylglyoxal include acetone meth...

Claims

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Application Information

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IPC IPC(8): C07C45/61C07C49/185B01J29/80
CPCC07C45/61C07C45/60C07C45/673B01J29/80B01J35/19C07C49/185C07C49/17
Inventor 刘聿嘉赵毅夏长久林民朱斌罗一斌舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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