Production technique for preparing 2,3-butanedione from 2,3-butanediol by one-step oxidization and heterogeneous catalyst used by same

A heterogeneous catalyst and production process technology, applied in the direction of physical/chemical process catalysts, molecular sieve catalysts, carbon-based compound preparation, etc., can solve the problems of expensive selenium dioxide, low yield, and failure to achieve large-scale industrialization. Achieve the effect of high yield and liquid time, low reaction temperature, and green source

Inactive Publication Date: 2013-03-13
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The selenium dioxide ozonation method uses butanone as a raw material, and the yield can reach 40%, but the catalyst selenium dioxide is expensive and fails to realize large-scale industrialization; the air oxidation method is to use metals such as nickel or vanadium as a catalyst, and the Butanone is oxidized to butanedione, and because the yield is low, there is no production example report yet; the nitrosation method is to use butanone as a raw material, react with nitrous acid to generate butanone oxime, and then hydrolyze to obtain diacetyl
However, there are no patents and literature reports on the direct conversion of 2,3-butanediol to 2,3-butanedione by one-step oxidation at home and abroad

Method used

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  • Production technique for preparing 2,3-butanedione from 2,3-butanediol by one-step oxidization and heterogeneous catalyst used by same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: 0.5Mo / HZSM-5 (360) catalyst and reaction performance thereof

[0020] Mix HZSM-5 raw powder with a Si / Al ratio of 360, ammonium molybdate tetrahydrate and water in the following mass ratio: raw HZSM-5 powder: ammonium molybdate tetrahydrate: water=10:0.9:60. Immerse at room temperature for 24 hours under stirring conditions, dry at 110°C, and roast the solid material at 500°C to 550°C for 4 hours to obtain Mo 2 o 3 A 0.5Mo / HZSM-5(360) catalyst with a content (converted mass content) of 0.5wt%.

[0021] The catalyst prepared above is pressed into tablets, crushed and screened into 30-40 mesh particles, and used for one-step oxidation of 2,3-butanediol to prepare 2,3-butanedione. The reaction raw material is 60wt% 2,3-butanediol aqueous solution, and the liquid hourly space velocity is 2.4h -1 (calculated in butanediol), pure oxygen flow rate 8.3cm 3 / (g.min), the reaction temperature is 180°C, the conversion rate of 2,3-butanediol and the selectivity of...

Embodiment 2

[0022] Embodiment 2: 1.0Fe / HZSM-5 (120) and its reaction performance

[0023] Mix HZSM-5 raw powder with a Si / Al ratio of 120, ferric nitrate nonahydrate and water in the following mass ratio: HZSM-5 raw powder: ferric nitrate nonahydrate: water=10:0.5:40. Immerse at room temperature for 24 hours under stirring conditions, dry at 110°C, and roast the solid material at 500°C to 550°C for 4 hours to obtain Fe 2 o 3 A 1.0Fe / HZSM-5(120) catalyst with a content (converted mass) of 1.0wt%.

[0024] The catalyst prepared above is pressed into tablets, crushed and screened into 30-40 mesh particles, and used for one-step oxidation of 2,3-butanediol to prepare 2,3-butanedione. The reaction raw material is 60wt% 2,3-butanediol aqueous solution, and the liquid hourly space velocity is 2.4h -1 (calculated as butanediol), air velocity 12cm 3 / (g.min), the reaction temperature is 180°C, the conversion rate of 2,3-butanediol and the selectivity of main products are listed in Table 1.

Embodiment 3

[0025] Embodiment 3: 2.0Co / HZSM-5 (200) and its reaction performance

[0026] Mix HZSM-5 raw powder with a Si / Al ratio of 200, cobalt dichloride and water in the following mass ratio: HZSM-5 raw powder: cobalt dichloride: water=10:0.3:40. Immerse at room temperature for 24 hours under stirring conditions, dry at 110°C, and calcinate the obtained solid material at 500°C to 550°C for 4 hours to prepare a 2.0Co / HZSM-5(200) catalyst with a CoO content (converted mass) of 2.0wt%.

[0027] The catalyst prepared above is pressed into tablets, crushed and screened into 30-40 mesh particles, and used for one-step oxidation of 2,3-butanediol to prepare 2,3-butanedione. The reaction raw material is 60wt% 2,3-butanediol aqueous solution, and the liquid hourly space velocity is 2.4h -1 (calculated in butanediol), oxygen-argon gas mixture (oxygen content 50%) flow rate 12cm 3 / (g.min), the reaction temperature is 180°C, the conversion rate of 2,3-butanediol and the selectivity of main pro...

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PUM

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Abstract

The invention discloses a production technique for preparing 2,3-butanedione from 2,3-butanediol by one-step oxidization and a heterogeneous catalyst used by the same. The technique comprises the following steps: reacting 2,3-butanediol or water solution thereof in a fixed bed tubular reactor at 140-300 DEG C under atmospheric pressure at the liquid hourly space velocity of 0.6-6h<-1>, thereby converting the 2,3-butanediol into a liquid-phase product mainly composed of butanone and butanedione under the action of the heterogeneous catalyst. The heterogeneous catalyst is composed of 2-50 wt% of active metal constituent, 0-10 wt% of non-metal boron or phosphorus and HZSM-5 with the silica-alumina ratio of 100-500. By using the technique and catalyst disclosed by the invention, under optimized conditions, the conversion rate of the 2,3-butanediol is 100%, the yield of the 2,3-butanediol is greater than 57%, and the space-time yield is greater than 1.3g / (g.h).

Description

technical field [0001] The invention belongs to the field of catalysts, and relates to a production process for preparing 2,3-butanedione by one-step oxidation of 2,3-butanediol and a heterogeneous catalyst used therein. Background technique [0002] 2,3-Butanedione, also known as diacetyl, is a yellow to light green liquid with a sweet, creamy, buttery aroma. Naturally present in essential oils such as angelica, lavender, nutmeg, citronella, bay leaf, clove, magnolia, etc., and also detected in cream, milk, coffee, raspberry, strawberry, apple, tomato, wine, vinegar. Diacetyl is an important fragrance compound, which is widely used in various flavor formulations, such as daily flavors such as lavender, iris, sandalwood, and food flavors such as milk, cream, cheese, chocolate, coffee, cocoa, wine, etc. . In addition, diacetyl is an important intermediate in organic synthesis, which can be used to prepare spices such as 2,3,5-trimethylpyrazine and 2,3-dimethylpyrazine, and ...

Claims

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Application Information

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IPC IPC(8): B01J29/48B01J29/46C07C49/12C07C45/39
Inventor 余定华黄和章文贵李晓栓李正文张小伟
Owner NANJING UNIV OF TECH
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