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Method for preparing ethyl methyl ketone by dehydrating 2,3-butanediol efficiently

A technology of butanediol and methyl ethyl ketone, which is applied in 2 fields, can solve the problems of high energy consumption and low concentration of raw materials, and achieve the effects of low reaction temperature, high catalyst activity and no corrosion of equipment

Inactive Publication Date: 2009-11-18
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Huang He et al. (patent CN101293817A) adopt ZSM-5 or NaY molecular sieve catalyst to catalyze the dehydration of 2,3-butanediol to methyl ethyl ketone, which can realize higher conversion rate and selectivity, but its raw material concentration is low, and in the reaction process , a large amount of water that does not participate in the reaction must be heated to 200-300 ° C, and the energy consumption is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 10g of ZSM-5 molecular sieve with a silicon-aluminum ratio of 25 is impregnated in an equal volume of ferric sulfate solution (wherein, according to Fe 2 o 3 The mass ratio to ZSM-5 is 10%), impregnated at room temperature for 1 h, and then dried at 110 ° C; the dried catalyst was placed in a muffle furnace and roasted for 3 h at a temperature of 350 ° C; Fe / ZSM-5 improved property catalyst; Fe / ZSM-5 modified molecular sieve is 1mol / L H with 20ml concentration 2 SO 4 The solution was impregnated, treated at room temperature for 30min, and then dried at 110°C; the dried catalyst was calcined in a muffle furnace at 600°C for 3h; ZSM-5 supported SO 4 2- / Fe 2 o 3 superacid catalyst.

[0016] Get 2g of the catalyst prepared above and put it into a stainless steel fixed-bed tubular reactor (φ10mm×2mm×300mm). The catalyst is filled with inert small ceramic balls or quartz sand up and down. Under the protection of flow rate 0.08L / min nitrogen, in After activation at 400...

Embodiment 2

[0019] Get 2g of the catalyst prepared in Example 1 and pack it into a stainless steel fixed-bed tubular reactor (φ10mm × 2mm × 300mm). The upper and lower parts of the catalyst are filled with inert small ceramic balls or quartz sand. After activation at 400°C for 2 hours, the temperature was lowered to 250°C. The 2,3-butanediol solution with a concentration of 10wt% is injected into the gasification section of the reactor by a peristaltic pump, and the mass space velocity of 2,3-butanediol is 2.3h -1 . The gasified raw material gas is reacted through the catalyst layer, and the liquid phase product is collected for analysis after the gas-liquid separation of the material at the outlet of the reactor. According to analysis and calculation, the molecular sieve type solid superacid catalyst catalyzes the dehydration of 2,3-butanediol to produce methyl ethyl ketone with a conversion rate of 100% and a selectivity of methyl ethyl ketone of 91.73%.

Embodiment 3

[0021] Get 2g of the catalyst prepared in Example 1 and pack it into a stainless steel fixed-bed tubular reactor (φ10mm × 2mm × 300mm). The catalyst is filled with inert small ceramic balls or quartz sand up and down. After activation at 400°C for 2 hours, the temperature was lowered to 200°C. The 2,3-butanediol solution with a concentration of 90wt% is injected into the gasification section of the reactor by a peristaltic pump, and the mass space velocity of 2,3-butanediol is 2.3h -1 . The gasified raw material gas is reacted through the catalyst layer, and the liquid phase product is collected for analysis after the gas-liquid separation of the material at the outlet of the reactor. According to analysis and calculation, the molecular sieve type solid superacid catalyst catalyzes the dehydration of 2,3-butanediol to produce methyl ethyl ketone with a conversion rate of 94.7% and a selectivity of methyl ethyl ketone of 70.1%.

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Abstract

The invention discloses a method for preparing an ethyl methyl ketone by dehydrating a 2,3-butanediol, belonging to the technical field of chemical product preparation. The method is to prepare the ethyl methyl ketone by dehydrating the 2,3-butanediol under the action of molecular sieve solid acid catalyst. The method comprises the following steps: taking the 2,3-butanediol of 10-90 wt% as a raw material, pre-heating and vaporizing the raw material at a reaction temperature of 200-300 DEG C, the raw material gas after being aerified reacting through a catalyst layer with the 2,3-butanediol mass airspeed of 1.5-3.4h, and separating reactor outlet materiels by liquid-vapor separation to obtain the ethyl methyl ketone. The conversion rate of the 2,3-butanediol is 94.2-100%, and the selectivity of the ethyl methyl ketone can reach 70.1-94.2%. The catalyst adopted in the invention has high activity and high airspeed, thereby having high conversion rate of 2,3-butanediol with different concentration; the ethyl methyl ketone has high selectivity and productivity and is environmentally friendly, the process is simple and the catalyst has good stability.

Description

technical field [0001] The invention belongs to the technical field of chemical product preparation, and in particular relates to a method for preparing methyl ethyl ketone by dehydrating 2,3-butanediol. Background technique [0002] Methyl ethyl ketone (MEK for short) is an important low-boiling point solvent, which is miscible with most hydrocarbon solvents, has no adverse effect on high solid content and viscosity, has excellent solubility and drying characteristics, and can form azeotropes with many solvents. Various cellulose derivatives, synthetic rubber, oils, and higher fatty acids have strong solubility, and are widely used in industrial sectors such as coatings, tapes, adhesives, synthetic leather, inks, and magnetic tapes. In addition, methyl ethyl ketone itself contains a carbonyl group and active oxygen adjacent to the carbonyl group, and is prone to various chemical reactions. It is an important fine chemical raw material and intermediate, which can produce hig...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/10C07C45/52B01J29/46B01J29/76B01J27/02B01J37/02B01J37/08
Inventor 张建安谢杨程可可周玉杰刘宏娟刘德华
Owner TSINGHUA UNIV
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