High-efficiency catalyst for preparing 1,3-butadiene by using carbon dioxide to oxidize 1-butene to dehydrogenate and preparation method thereof

A carbon dioxide and catalyst technology, applied in the field of high-efficiency loaded iron-based composite oxide catalyst and its preparation, can solve the problems of poor stability and low catalyst activity

Active Publication Date: 2019-04-19
TIANJIN UNIV OF SCI & TECH
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Problems solved by technology

However, these catalysts have low activity and poor stability.

Method used

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  • High-efficiency catalyst for preparing 1,3-butadiene by using carbon dioxide to oxidize 1-butene to dehydrogenate and preparation method thereof
  • High-efficiency catalyst for preparing 1,3-butadiene by using carbon dioxide to oxidize 1-butene to dehydrogenate and preparation method thereof
  • High-efficiency catalyst for preparing 1,3-butadiene by using carbon dioxide to oxidize 1-butene to dehydrogenate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～7

[0032] In traditional Fe 2 o 3 / Al 2 o 3 On the basis of the catalyst, a single element doping modification is carried out, wherein the doping element is selected from one of Co, Cr, Cu, Mn, Ni, V or Zn. The specific preparation method is as follows:

[0033] Weigh γ-Al 2 o 3 3g, Fe(NO 3 ) 3 9H 2 O 3.2464g (0.0080mol), nitrates of doping elements (wherein V is NH 4 VO 3 ) 0.00089mol, that is, the molar ratio of Fe to doping elements is 9:1, measure 100mL of distilled water, put it in an eggplant-shaped bottle at 60°C and continuously stir for 4h. After the water solvent was removed by rotary evaporation, it was dried in an oven at 120°C for 4 hours. Then put the above samples in a muffle furnace and bake them at 600°C for 4h (heating rate 5°C / min) to obtain the samples, respectively denoted as FeCoO x / Al 2 o 3 , FeCrO x / Al 2 o 3 , FeCuO x / Al 2 o 3 , FeMnO x / Al 2 o 3 , FeNiO x / Al 2 o 3 、FeVO x / Al 2 o 3 , FeZnO x / Al 2 o 3 .

Embodiment 8

[0035] Catalyst activity evaluation was carried out in the atmospheric pressure micro-reaction system, and the reactants were fed 6mL / min 1-butene and 54mL / min CO 2 , that is, the ratio of intake air to CO 2 / C 4 h 8 =9:1, using 0.2g of the catalysts of Examples 1 to 7 respectively, that is, the space velocity is 4.5h -1 , the reaction was carried out at 600°C under normal pressure, and the product was analyzed by gas chromatography. Carry out 1-butene conversion rate when carrying out 10min with reaction, the selectivity of 1-butene to 1,3-butadiene and the space-time yield of 1,3-butadiene are index, and gained reaction performance is as shown in table 1 . It can be clearly seen from the results that the selectivity of 1,3-butadiene can be effectively improved by doping V elements, thereby increasing the space-time yield of 1,3-butadiene, and the highest space-time yield of 1,3-butadiene 1054.3 mg / g / h. Therefore, V element is selected as the first element to be doped. ...

Embodiment 9～10

[0039] Under the reaction condition of embodiment 8, adopt the catalyzer among the embodiment 6 (FeVO x / Al 2 o 3 ) to investigate the reaction temperature in the reaction conditions of synthesizing 1,3-butadiene, to explore the optimum reaction temperature. Set the reaction temperature as 500°C and 550°C respectively. Carry out 1-butene conversion ratio when carrying out 10min with reaction, 1-butene is to 1, the selectivity of 3-butadiene and the space-time yield of 1,3-butadiene as index, and gained reaction performance is as shown in table 2 . It can be seen from Table 2 that the activity of the catalyst is not as high as that at 600° C. (the reaction conditions of Example 8) when the reaction temperature is 500° C. or 550° C. Therefore, 600°C is the optimal temperature for the reaction.

[0040] Table 2 FeVO at different reaction temperatures x / Al 2 o 3 Catalytic performance of the catalyst

[0041]

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Abstract

The invention discloses a high-efficiency catalyst for preparing 1,3-butadiene by using carbon dioxide to oxidize 1-butene to dehydrogenate and a preparation method thereof, wherein the catalyst consists of a carrier and an active component, a compound oxide of metal iron and a doping element is taken as the active component, and a precipitation roasting mode is adopted for preparation. The catalyst disclosed by the invention can be used for preparing for preparing 1,3-butadiene by using carbon dioxide to oxidize 1-butene to dehydrogenate, and is high in activity, good in selectivity, good instability and low in preparation cost, and the preparation method is simple in process. Compared with a traditional aluminum oxide loaded iron oxide catalyst, the crystal lattice oxygen fluidity and the crystal lattice oxygen content of the catalyst can be effectively improved, so that the activity and the stability of the catalyst are improved.

Description

technical field [0001] The invention belongs to the catalytic technology for synthesizing 1,3-butadiene gas phase synthesis, more specifically, relates to a method for CO 2 A high-efficiency loaded iron-based composite oxide catalyst for oxidizing 1-butene to dehydrogenate 1,3-butadiene and a preparation method thereof. Background technique [0002] 1,3-Butadiene is an important organic chemical raw material, which is widely used in the petrochemical industry to produce rubber, resin, and plastics. It is also an intermediate for the preparation of adiponitrile, sulfolane, and cyclooctadiene. With the development of the global economy, the market demand for 1,3-butadiene is increasing. According to the previous technology, the production of 1,3-butadiene is mainly extracted from naphtha steam cracking C4. However, the development of more and more light hydrocarbons from natural gas and refinery gas to ethylene, propylene, and coal to olefins will not be conducive to the dev...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/75B01J23/755B01J23/80B01J23/847B01J23/86B01J23/887B01J23/889C07C5/42C07C11/167
CPCB01J23/002B01J23/75B01J23/755B01J23/80B01J23/8472B01J23/862B01J23/8878B01J23/8892B01J2523/00C07C5/42C07C2523/75C07C2523/755C07C2523/80C07C2523/847C07C2523/86C07C2523/887C07C2523/889B01J2523/31B01J2523/55B01J2523/67B01J2523/68B01J2523/842B01J2523/845B01J2523/17B01J2523/72B01J2523/847B01J2523/27C07C11/167
Inventor 闫冰高越王博龙姜涛
Owner TIANJIN UNIV OF SCI & TECH
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