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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

A carbon dioxide and catalyst technology, applied in the field of high-efficiency catalysts and their preparation, can solve the problems of catalyst activity, low selectivity, poor stability, etc., and achieve the effects of abundant pores, good electrical conductivity, and avoiding agglomeration and sintering

Active Publication Date: 2019-04-19
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, such catalysts have low activity, low selectivity, and relatively 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 1～5

[0033] A single iron element is loaded on the activated carbon carrier. The specific preparation method is as follows:

[0034] Weigh 3g of activated carbon, Fe(NO 3 ) 3 ·9H 2 O 1.0821g, that is, the loading amount of Fe (mass of iron element / mass of carrier activated carbon) is 5wt%, measure 100 mL of distilled water, and place it in an eggplant-shaped flask at 60° C. for continuous stirring for 4 hours. After the water solvent was removed by rotary evaporation, it was dried in an oven at 120°C for 4 hours. Put the above sample in the tube furnace N 2 The samples are calcined at 600℃ for 4h (heating rate 3℃ / min), which are marked as FeO X / AC.

Embodiment 2～5

[0036] Under the condition that the other experimental conditions are exactly the same as in Example 1, the Fe(NO 3 ) 3 ·9H 2 The O mass is changed to 2.1643g, 3.2464g, 4.3286g, 5.4105g. That is, the loading amount of the modulating catalyst is 10wt%, 15wt%, 20wt%, and 25wt% respectively. The optimal catalyst loading can be obtained by comparing the activity test.

Embodiment 6～10

[0038] The catalyst activity is evaluated in an atmospheric micro-reaction system, with 6mL / min 1-butene and 54mL / min CO as reactants 2 , The intake air ratio CO 2 / C 4 H 8 =9:1, respectively use 0.2g of the catalyst of Examples 1-5, that is, the space velocity is 4.5h -1 , The reaction was carried out at 600°C and atmospheric pressure, and the product was analyzed by gas chromatography. Taking the conversion rate of 1-butene when the reaction is carried out for 10 minutes, the selectivity of 1-butene to 1,3-butadiene and the space-time yield of 1,3-butadiene are indicators. The obtained reaction performance is shown in Table 1. . From the results, it can be concluded that the 1,3-butadiene space-time yield of the catalyst is the highest when the iron loading is 15wt%, which is 849.1mg / g / h. Therefore, 15wt% is preferably the optimal loading of iron.

[0039] Table 1 Catalysts catalyze CO 2 The result of the dehydrogenation of 1-butene oxide to 1,3-butadiene

[0040]

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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, a carrier and an oxidizingacid are mixed for heating and stirring to obtain a mixture, the mixture is washed with deionized water to be neutral, and dried to obtain a granular sample, the granular sample is mixed with a soluble ferric salt, one or two same-period metal soluble salt and an alkali metal salt, deionized water is added to uniformly disperse, heating is performed to remove water to obtain a granular sample, heat preservation roasting is performed on the granular sample at 500-600 DEG c, and the granular sample is naturally cooled to room temperature. Compared with the prior art, activated carbon is adoptedas a catalyst carrier to prepare an iron-based catalyst, due to the fact that the activated carbon is large in specific surface area, rich in pore channels, and good in conductivity, and has rich andadjustable oxygen-containing groups on the surface, compared with a traditional aluminum oxide supported iron-based catalyst, active component iron oxide can be effectively dispersed, agglomeration and sintering of the active component can be avoided, the transmission capacity of electrons in the catalyst can be improved, so that the activity, the selectivity and the stability of the catalyst areimproved.

Description

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

Claims

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Application Information

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IPC IPC(8): B01J23/745B01J23/86B01J37/02C07C5/42C07C11/167
CPCB01J23/745B01J23/862B01J37/0207C07C5/42C07C2523/745C07C2523/86C07C11/167
Inventor 闫冰王博龙王璐怡姜涛
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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