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Method for preparing methyl-ethyl ketone

A technology of methyl ethyl ketone and molecular sieve, which is applied in the field of preparation of methyl ethyl ketone, can solve problems such as lack of industrial production prospects, difficult separation of products, unfavorable continuous production, etc., achieve high substrate conversion rate and target product yield, not easy to deactivate, and produce low cost effect

Inactive Publication Date: 2008-10-29
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As early as 1982, Emerson et al. used 2.5-10% (v / v) sulfuric acid to homogeneously catalyze the dehydration of various concentrations of 2,3-butanediol (prepared from pure 2,3-butanediol) to prepare Methyl ethyl ketone (Emerson R R, Flicklnger M C, Tsao G T.Industrial & Engineering Chemistry Product Research and Development, 1982, 21 (3): 473-477); Preparation of methyl ethyl ketone from 2,3-butanediol fermentation broth obtained by Klebsiella oxytoca fermentation of glucose (Wang Di, Wang Fanqiang, Wang Jianhua. Fine and Specialty Chemicals, 2000, 8(9): 19-20), However, these two methods do not have the prospect of industrialized production due to the use of sulfuric acid as a catalyst, which severely corrodes the equipment, and the acid waste liquid is more polluting to the environment, and the products are difficult to separate.
In order to overcome the above-mentioned shortcoming, Tran etc. use the solid acid (aluminum oxide) that is made up of sulfonic acid covalent group and inorganic support as catalyst instead, and catalyzes and obtains 2,3-butanediol fermented liquid by Klebsiella pneumoniae fermentation Dehydration produces methyl ethyl ketone (Tran A V, Chambers R P. Biotechnology and Bioengineering, 1987, 29 (3): 343-351), but the catalyst (alumina) used in the reaction process is obviously affected by impurities in the fermentation broth, Easier to inactivate, not conducive to large-scale continuous production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] step 1:

[0025] Preparation of reaction solution: 200 mL of 200 g / L aqueous solution was prepared with 40 g of 2,3-butanediol (chemically pure) for later use.

[0026] Step 2:

[0027] Put 1.2g of 30-50 mesh ZSM-5 (Si / Al=25) molecular sieve catalyst into the constant temperature section of the tubular fixed-bed reactor, and fill the rest with quartz sand. After the system checks the seal, when the volumetric space velocity is 3h -1 N 2 Under the gas flow rate, the temperature of the catalytic bed layer is programmed to 300 ° C, and then the reaction solution obtained in step 1 is 2 h according to the mass space velocity -1 Inject into the gasification system, and react through the catalytic bed layer after gasification. After the product is cooled in an ice-water bath and separated from gas and liquid, the gas is evacuated, and the liquid collected after 1.5 hours of reaction is sampled for analysis. According to the content of the reaction product components, The ...

Embodiment 2

[0029] step 1:

[0030]Preparation of reaction solution: collect 200mL of Klebsiella oxytoca (Klebsiella oxytoca) CCTCC M 207023 (from application number 200710021641.5, publication number CN101063095A, titled "A Klebsiella oxytoca and its application" 2,3-butanediol fermented liquid (wherein the concentration of 2,3-butanediol is 125g / L) that fermented the 2,3-butanediol fermented liquid (the bacterial strain preserved in the patent application document of ) , the fermented liquid is removed bacteria through chitosan flocculation The clear liquid was obtained after the body, and the pH was adjusted with NaOH to make the pH 7.0.

[0031] Step 2:

[0032] Put 1.2g of 30-50 mesh ZSM-5 (Si / Al=30) molecular sieve catalyst into the constant temperature section of the tubular fixed-bed reactor, and fill the rest with quartz sand. After the system checks the seal, when the volumetric space velocity is 3h -1 N 2 Under the gas flow rate, the temperature of the catalytic bed layer i...

Embodiment 3

[0034] step 1:

[0035] Collect 200mL of 2,3-butanediol fermented liquid produced by Klebsiella pneumoniae (Klebsiellapneumoniae) CICC 10011 (provided by China Industrial Microorganism Culture Collection Management Center) (wherein the concentration of 2,3-butanediol 92.4g / L), the fermented liquid was centrifuged to remove the thallus to obtain a clear liquid, and the pH was adjusted to 7.0 with NaOH.

[0036] Step 2:

[0037] Put 1.2g of 30-50 mesh ZSM-5 (Si / Al=38) molecular sieve catalyst into the constant temperature section of the tubular fixed-bed reactor, and fill the rest with quartz sand. After the system checks the seal, when the volumetric space velocity is 3h -1 N 2 Under the gas flow rate, the temperature of the catalytic bed layer is programmed to 250 ° C, and then the reaction solution obtained in step 1 is 2 h according to the mass space velocity. -1 Inject into the gasification system, and react through the catalytic bed layer after gasification. After the ...

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Abstract

The invention belongs to the chemical technology field, and discloses a method for preparing methyl ethyl ketone. The methyl ethyl ketone is prepared from 2,3-butanediol by dehydrating in the presence of ZSM-5 or NaY molecular sieve catalyst. Under process conditions, the catalyst is not easily deactivated and has good stability. The method has the advantages of high substrate conversion and product yield, simple process, low production cost and less environmental pollution, and can satisfy industrial requirement. With the method, the conversion rate of 2,3-butanediol is 90.5%-100%, and the selectivity of methyl ethyl ketone is 83.7%-91.3%.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of methyl ethyl ketone. Background technique [0002] Methyl ethyl ketone is an excellent solvent for polymer compounds such as nitrocellulose, polyurethane, vinyl resin, acrylic resin, alkyd resin, phenolic resin, pharmaceutical production and lubricating oil dewaxing, and is the best substitute for "triphenyl" solvent. In addition, methyl ethyl ketone is also an important fine chemical raw material, which is widely used in industrial fields such as oil refining, coatings, adhesives, inks, magnetic tapes, medicine and electronic components. At present, the main industrialization routes of methyl ethyl ketone are: n-butene method, n-butane liquid phase oxidation method and isobutylbenzene method, etc. (Cui Xiaoming. Fine Chemical Raw Materials and Intermediates, 2006, 4(4): 20-26). However, these methods have a large amount of three was...

Claims

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Application Information

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IPC IPC(8): C07C45/66C07C45/67C07C49/10C12P7/18
Inventor 黄和闫婕纪晓俊李霜胡耀池
Owner NANJING UNIV OF TECH
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