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Vanadium-titanium-based catalyst for synthesizing n,n-dimethylformamide from methanol, oxygen and dimethylamine and preparation method thereof

A technology of dimethylformamide and catalyst, which is applied in the field of vanadium-titanium-based catalyst and its preparation, which can solve the problems of catalyst instability, high reaction temperature, and short life, and achieve good dispersion, high porosity, and good sintering resistance performance effect

Active Publication Date: 2021-01-26
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above two methods require high reaction temperature and high energy consumption, and there are dangerous gases such as carbon monoxide and hydrogen in the reaction process, and the catalyst is unstable and has a short life.
Chinese patent CN104447381A adopts copper-based composite catalyst to synthesize N,N-dimethylformamide, and its optimal reaction temperature is as high as 250°C. At the same time, the reaction will generate a large amount of hydrogen, which has high energy consumption and great danger.

Method used

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  • Vanadium-titanium-based catalyst for synthesizing n,n-dimethylformamide from methanol, oxygen and dimethylamine and preparation method thereof
  • Vanadium-titanium-based catalyst for synthesizing n,n-dimethylformamide from methanol, oxygen and dimethylamine and preparation method thereof
  • Vanadium-titanium-based catalyst for synthesizing n,n-dimethylformamide from methanol, oxygen and dimethylamine and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Dissolve 5.0 g of vanadyl sulfate and 20.0 g of titanium sulfate in 500 ml of deionized water, stir fully in a three-necked flask to mix the solution evenly, place the above solution in an ice-water bath, and use ammonia (25%) solution at 40 r / min Velocity titration to pH = 8 gave a slurry containing a tan precipitate. Continue to stir for 0.5h to allow it to fully react, then leave it to age for 2h. The aged slurry was separated by filtration and washed with 100 mL of deionized water to obtain a tan solid; the obtained solid was dried at 100°C for 2 hours, and calcined at 400°C for 5 hours to obtain a vanadium-titanium-based catalyst.

[0037] figure 1 Shown as the XRD spectrum of the catalyst, it can be seen that the catalyst support titanium is anatase TiO 2 form, vanadium is highly dispersed on the surface of the carrier.

[0038] figure 2 It is a transmission electron microscope photograph of the catalyst, and it can be seen that the particle size of the catal...

Embodiment 2

[0043] Dissolve 0.895g of vanadyl sulfate and 28.5g of titanium sulfate in 500ml of deionized water, fully stir in a three-necked flask to mix the solution evenly, place the above solution in an ice-water bath, and use ammonia (5%) solution at 40r / min Velocity titration to pH = 7 gave a slurry containing a tan precipitate. Continue to stir for 0.5h to make it fully react, then let it stand for aging for 1h. The aged slurry was separated by filtration and washed with 100 mL of deionized water to obtain a yellow-brown solid; the obtained solid was dried at 60°C for 10 hours and calcined at 300°C for 8 hours to obtain a vanadium-titanium-based catalyst.

[0044] The prepared catalyst is pressed into tablets, crushed and sieved to get 20-40 mesh particles, the prepared catalyst 0.1g is filled into the reactor, and the oxygen content is 10% ( vol.) inert gas, activated at 500°C for 1h. The catalytic reaction temperature was controlled at 120°C, methanol was passed in at a flow ra...

Embodiment 3

[0046] Dissolve 7.16g of vanadyl sulfate and 18.0g of titanium sulfate in 500ml of deionized water, stir fully in a three-necked flask to mix the solution evenly, place the above solution in an ice-water bath, and use ammonia (28%) solution at 40r / min Velocity titration to pH = 10 yielded a slurry containing a tan precipitate. Continue to stir for 0.5h to allow it to fully react, then leave it to age for 12h. The aged slurry was separated by filtration and washed with 100 mL of deionized water to obtain a tan solid; the obtained solid was dried at 120°C for 2 hours and calcined at 600°C for 4 hours to obtain a vanadium-titanium-based catalyst.

[0047] The prepared catalyst is pressed into tablets, crushed and sieved to get 20-40 mesh particles, the prepared catalyst 1.0g is filled into the reactor, and the oxygen content is 30% ( vol.) inert gas, activated at 300°C for 5h. The catalytic reaction temperature was controlled at 150°C, methanol was passed in at a flow rate of 0...

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Abstract

The invention provides a vanadium-titanium based catalyst for synthesizing N, N-dimethyl formamide from methanol, oxygen and dimethylamine and a preparation method thereof. The vanadium-titanium basedcatalyst comprises, by mass, 5-40% of vanadium oxide and 60-95% of titanium oxide. When the vanadium-titanium based catalyst is applied in reaction for synthesizing N, N-dimethyl formamide from methanol, oxygen and dimethylamine, conversion rate of methanol reaches 32-50%, conversion rate of dimethylamine can reach 80-99%, selectivity of N, N-dimethyl formamide reaches 82.5-99.5%, one-way servicelife of the vanadium-titanium based catalyst is longer than 1000h, and the vanadium-titanium based catalyst is long in service time.

Description

technical field [0001] The invention relates to the field of catalyst preparation methods, in particular to a vanadium-titanium-based catalyst used for synthesizing N,N-dimethylformamide from methanol, oxygen and dimethylamine and a preparation method thereof. Background technique [0002] DMF is N,N-dimethylformamide. It is a colorless, high boiling point, hygroscopic and fishy liquid at room temperature. It is a polar aprotic and high dielectric organic solvent. It is widely used In the field of chemical industry, it can be used not only as a chemical raw material, but also as an excellent reaction solvent. Dimethylformamide is a good solvent for various high polymers such as polyethylene, polyvinyl chloride, polyacrylonitrile, polyamide, etc., and can be used for wet spinning of synthetic fibers such as polyacrylonitrile fibers and synthesis of polyurethane; It is used for making plastic films; it can also be used as a paint remover for removing paint; it can also dissol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/22C07C233/03C07C231/10
CPCB01J23/22C07C231/10C07C233/03
Inventor 曾高峰吴平刘国娟孙予罕刘子玉陈新庆
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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