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Method for preparing C2 oxygen-containing compound through CO hydrogenation

A compound and catalyst technology, which is applied in the pretreatment field of Rh catalyst carrier silica gel, can solve problems such as the impact of treatment effects, achieve a simple and reliable method, and reduce the cost of catalysts

Active Publication Date: 2021-06-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these documents are basically soaked at room temperature, and most of the alcohols used are low-carbon normal monohydric alcohols, so the treatment effect is greatly affected.

Method used

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  • Method for preparing C2 oxygen-containing compound through CO hydrogenation
  • Method for preparing C2 oxygen-containing compound through CO hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh 10g of silica gel (product of Qingdao Haiyang Co., Ltd.) into a pressure vessel filled with 50ml of anhydrous ethanol, seal it and place it in a muffle furnace, raise it from room temperature to 150°C and keep it for 1h. After receiving, the liquid was poured out, and the obtained solid was dried at room temperature and then dried overnight at 110°C. Then bake at 350°C for 2h. Take by weighing gained sample 2.0g, join in containing certain amount RhCl3, MnCl 2 , LiCl ethanol solution, dried at 110°C for 4h, and calcined at 350°C for 4h, the obtained catalyst is marked as A. Catalyst composition Rh 1.5wt%; Mn0.5wt%; Li 0.05wt%.

[0018] The CO hydrogenation reaction was carried out in a fixed-bed stainless steel reactor (id=10mm), and the catalyst consumption was 1.0ml. Before the reaction, the catalyst was used at 350°C with 5NL / h of pure H 2 Restore 1h. The reactor was then lowered to 280 °C and switched to syngas (H 2 / CO=2), the flow rate is 12.5L / h, and ...

Embodiment 2

[0026] Weigh 10g of silica gel (product of Qingdao Haiyang Co., Ltd.) into a pressure vessel filled with 50ml of n-butanol, seal it, place it in a muffle furnace, raise it from room temperature to 80°C and keep it for 8h. After receiving, pour out the liquid, and dry the resulting solid at room temperature and then dry at 120°C for 12 hours. Then bake at 300°C for 4h. Take by weighing gained sample 2.0g, join in containing certain amount RhCl3, MnCl 2 , Methanol solution of LiCl, dried in the air, dried at 110°C for 16h, and calcined at 300°C for 8h, the obtained catalyst was designated as B. Catalyst composition Rh 1.0wt%; Mn 1.5wt%; Li 0.1wt%.

[0027] The evaluation of catalyst is the same as embodiment 1, reduction condition: 10%H 2 / N 2 , 300℃, 48h, 500h -1 ;Reaction conditions: 250℃, 5.0MPa, 8000h -1 , and the reaction results are shown in Table 1.

Embodiment 3

[0029]Weigh 10g of silica gel (product of Qingdao Haiyang Co., Ltd.) into an autoclave filled with 50ml of n-amyl alcohol, seal it and put it in a muffle furnace, and raise it from room temperature to 250°C and keep it for 4h. After receiving, the liquid was poured out, and the obtained solid was dried at room temperature and then dried overnight at 110°C. Then bake at 500°C for 4h. Weigh 2.0 g of the obtained sample, add it to an ethanol solution containing a certain amount of Rh, Mn, and Li nitrates, dry it in the air, dry it at 110°C for 4 hours, and calcinate it at 350°C for 4 hours. The obtained catalyst is designated as C. Catalyst composition Rh 1.5wt%; Mn 2.0wt%; Li 0.01wt%.

[0030] The evaluation of catalyst is the same as embodiment 1, reduction condition: 50%H 2 / N 2 , 500℃, 8h, 3000h -1 ;Reaction conditions: 300℃, 3.0MPa, 5000h -1 , and the reaction results are shown in Table 1.

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Abstract

The invention relates to a pretreatment method of a novel efficient catalyst carrier silica gel for preparing a C2 oxygen-containing compound through CO hydrogenation. Wherein the catalyst is composed of active components and a carrier silica gel, and the active components are Rh and additives such as Mn and Li. The preparation method comprises the following steps: carrying out alcohol heat treatment on silica gel for a period of time by using monohydric alcohols or dihydric alcohols with different carbon numbers (C1-C6) at different temperatures and under self-generated pressures, airing and roasting, then selecting a proper dipping solvent water or low-carbon alcohols with relatively low polarity, preparing a catalyst precursor by using a dipping method, and drying and roasting to obtain the final catalyst. And reduction activation is performed before use. In a fixed bed reactor, a reaction for preparing the C2 oxygen-containing compound through CO hydrogenation is carried out at a proper temperature and pressure under the action of the catalyst.

Description

technical field [0001] The present invention relates to a pretreatment method of Rh catalyst carrier silica gel for CO hydrogenation to produce C2 oxygen-containing compounds, in particular to commercial silica gel, which is subjected to alcohol heat treatment with monohydric or polyhydric alcohols with different carbon numbers at different temperatures and autogenous pressures Finally, choose a suitable solvent to prepare the catalyst by impregnation method. The catalyst is used in the reaction of CO hydrogenation to produce C2 oxygen compounds. [0002] technical background [0003] Ethanol, acetaldehyde, acetic acid or ethyl acetate, etc. C 2 Oxygenates are important chemical raw materials. With the increasing shortage of food supply and the depletion of oil resources, starting from coal, natural gas or biomass and producing C2 oxygenates through synthesis gas to replace food and oil routes, the strategy of replacing coal with oil or coal with grain has been realized, so...

Claims

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Application Information

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IPC IPC(8): B01J23/656B01J37/02C07C1/04C07C9/04C07C45/49C07C47/06C07C51/10C07C53/08C07C27/06
CPCB01J23/6562B01J37/0207B01J37/0213C07C1/043C07C1/0445C07C45/49C07C51/10C07C9/04C07C47/06C07C53/08
Inventor 陈维苗丁云杰宋宪根宁丽丽
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI