Method of using modified alumina catalyst to continuously prepare methyl vinyl ketone

A kind of alumina and catalyst technology, applied in the direction of physical/chemical process catalysts, carbon-based compound preparation, chemical instruments and methods, etc., can solve the problems of high pressure resistance and leakage prevention requirements of production equipment, large safety hazards in the production process, and corrosion resistance Higher requirements and other issues, to achieve the effect of safe and reliable production, improved conversion rate and selectivity, and stable production process

Inactive Publication Date: 2014-04-16
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production capacity of the equipment is low and the volume of the equipment is large
The one-step synthesis of butenone is carried out at relatively high temperature and pressure, so the requirements for the pressure resistance and leakage prevention of the production equipment are high, the equipment investment is large, and the production process has great potential safety hazards
[0005] In the two-step method, oxalic acid or calcium chloride is used as a catalyst for the dehydration of butanone alcohol. Before dehydration, the butanone alcohol must be dried and distilled, and the requirements for the corrosion resistance of the equipment are relatively high. Reaction, equipment volume is large, production capacity is poor, and there is a large amount of waste water or waste residue generated

Method used

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  • Method of using modified alumina catalyst to continuously prepare methyl vinyl ketone
  • Method of using modified alumina catalyst to continuously prepare methyl vinyl ketone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Weigh Ti(SO 4 ) 2 50.0g, add 3000ml distilled water, stir to dissolve, and weigh another commercially available powdered γ-Al 2 o 3 (A: specific surface area 2900m 2 / g) 950.0g, pour the above Ti(SO 4 ) 2 solution, stir to form a paste. Put it at room temperature for 5 hours, then rotary evaporate under vacuum to obtain a solid, extrude it into a clover shape, then dry it at 110°C for 2 hours, and finally bake it at 450°C for 1.5 hours to make Ti(SO 4 ) 2 Modified γ-Al 2 o 3 , to obtain catalyst B, the resulting modified γ-Al 2 o 3 Contains SO 4 2- 4wt%.

Embodiment 2

[0024] Weigh (NH 4 ) 2 SO 4 27.1g, add 2000ml distilled water, stir to dissolve, and weigh another commercially available powdered γ-Al 2 o 3 (A: specific surface area 2900m 2 / g) 490.0g, pour the above (NH 4 ) 2 SO 4 solution, stir to form a paste. Place it at room temperature for 5 hours, and rotate it under vacuum to obtain a solid, extrude it into a clover shape, then dry it at 110°C for 2 hours, and finally bake it at 450°C for 1.5 hours to make (NH 4 ) 2 SO 4 Modified γ-Al 2 o 3 , to obtain catalyst C, the resulting modified γ-Al 2 o 3 Contains SO 4 2- 4wt%.

Embodiment 3

[0026] Add 20g of Catalyst B into a shell and tube reactor with a diameter of 8mm and a length of 400mm, start to use a metering pump to input the crude butanone alcohol into the reactor at a speed of 5ml / min, and keep the outlet temperature of the preheater at 95--100°C. The temperature of the reactor is maintained at 100--105°C, and the reaction is continued for 100 hours. The product is collected and dried. The product has a purity of 99.5% (GC), moisture: 0.16% (KF), and a yield of 90%.

[0027] The composition of the product was detected by gas chromatography (GC): DB~5MS capillary column (30m*0.25mm*0.25um) was selected and analyzed on an Agilent6890 gas chromatograph with a hydrogen flame ion detector. Detection conditions: initial temperature of 40°C, maintained for 5 minutes, programmed temperature increase at 10°C / min, final temperature of 120°C, maintained for 5 minutes. Injection port temperature: 220°C, detector temperature: 260°C.

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Abstract

The invention relates to a method of using a modified alumina catalyst to continuously prepare methyl vinyl ketone, which includes the steps: reacting crude methylolacetone in the existence of the modified alumina catalyst at the temperature of 80-150 DEG C, and condensing and drying effluence to obtain the methyl vinyl ketone. Crude methyl vinyl ketone high in water content can be treated by the method, selectivity of the methyl vinyl ketone can be higher than 95%, and conversion rate of the methyl vinyl ketone is effectively increased while selectivity of the methyl vinyl ketone is effectively improved. Further, the method using the continuous production process is simple in procedure, stable in production process, easy to control, safe and reliable in production, low in energy consumption and less in waste water.

Description

technical field [0001] The invention relates to a method for continuously preparing butenone with a modified alumina catalyst. The crude butanone alcohol is reacted at 80--150°C in the presence of a modified alumina catalyst, and the effluent is condensed. Dry to give butenone. Background technique [0002] Methyl Vinyl Ketone (MVK for short), also known as butenone, is a typical α, β unsaturated ketone, which has a strong reaction ability and is used as an alkylating agent and a polymerization monomer. It is used as an intermediate in the synthesis of steroids and vitamin A, and can also be used to prepare anionic resins, film emulsifiers, alkylating agents, poisonous gases, etc. It is considered to be an important raw material for the plastics industry, pharmaceutical industry and fine organic synthesis industry. [0003] Butenone has a variety of synthetic methods. Since the raw materials of acetone and formaldehyde are easy to obtain and the cost of synthesizing buteno...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/205C07C45/66B01J21/04
Inventor 刘桂龙郑占英张树军许寒李华斌
Owner NANKAI UNIV
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