Ruthenium-based adsorbent for deeply removing thiophene of benzene as well as preparation method and application of ruthenium-based adsorbent

A deep adsorption, adsorbent technology, applied in adsorption purification/separation, chemical instruments and methods, other chemical processes, etc., can solve the problem that the adsorption sulfur capacity cannot be further improved, and achieve good application prospects, easy industrialization, and simple preparation process. Effect

Active Publication Date: 2015-01-28
SHANGHAI XUNKAI NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Considering the economy in industrial applications, the load of metal palladium is generally controlled within 1wt%, which determines that its adsorption sulfur capacity cannot be further improved. The loss of heteroelements in the medium will affect the activity, selectivity and lifespan of the ruthenium catalyst in the subsequent partial hydrogenation of benzene. Therefore, it is very important and necessary to find a new and efficient benzene deep desulfurization adsorbent with a relatively cheap price.

Method used

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  • Ruthenium-based adsorbent for deeply removing thiophene of benzene as well as preparation method and application of ruthenium-based adsorbent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0100] (1) Carrier pretreatment

[0101] Accurately weigh the bulk density to 0.60g / ml and the specific surface area to 110m 2 / g, the pore volume is 0.6ml / g, the diameter is 500g of the spherical alumina carrier of 2.0mm, is placed in the 5000mL beaker, adds 3wt% boric acid-methanol aqueous solution 1500mL, the volume ratio of methanol and water is 1:5. Immerse at a temperature of 50°C for 4 hours, take it out and dry it at 80°C for 8 hours, bake it in an air atmosphere at 350°C for 4 hours, and cool to obtain a treated carrier.

[0102] (2) Adsorbent preparation

[0103] Accurately weigh RuCl with a Ru content of 37.0wt% 3 .nH 2 O 5.41g, put in 1000mL beaker, add 20mL deionized water to dissolve, dilute to 120ml with 1.0wt% PVP-K30 aqueous solution, adjust solution pH value to 2.0 with 5wt% sodium hydroxide aqueous solution, add 100g processed carrier , soaked at a temperature of 30°C for 18 hours. Add 500mL of 10wt% sodium hydroxide aqueous solution, and invert and pre...

Embodiment 2

[0105] (1) Carrier pretreatment

[0106] Prepared supports were prepared as described in Example 1.

[0107] (2) Adsorbent preparation

[0108] Accurately weigh RuCl with a Ru content of 37.0wt% 3 .nH 2 O 5.41g, be placed in the 1000mL beaker, add 20mL deionized water and dissolve, adjust solution pH value to 2.0 with 2wt% sodium hydroxide aqueous solution, be diluted to 120 milliliters with 0.5wt% PVP-K30 aqueous solution, add 100g as embodiment 1 The treated carrier was soaked at a temperature of 60° C. for 6 hours. Add 500mL of 6wt% sodium hydroxide aqueous solution, and invert and precipitate at 50°C for 4 hours. At a temperature of 80°C, slowly add 200mL of 6wt% sodium borohydride aqueous solution (containing 0.1wt% sodium hydroxide), and reduce for 1 hour. After the reduction, rinse with 40°C deionized water until the washing liquid does not contain chloride ions (Aqueous solution of silver nitrate is detected), placed in a vacuum oven for 8 hours at 110°C and dried...

Embodiment 3

[0110] (1) Carrier pretreatment

[0111] Accurately weigh the bulk density to 0.70g / ml and the specific surface area to 180m 2 / g, the pore volume is 0.75ml / g, the spherical alumina support 500g that diameter is 1.3mm is placed in the 5000mL beaker, adds 5wt% boric acid-ethanol aqueous solution 2000mL, the volume ratio of ethanol and water is 1:4, in Immerse at a temperature of 70°C for 4 hours, take it out and dry it at 100°C for 8 hours, bake it in an air atmosphere at 400°C for 6 hours, and cool to obtain a treated carrier.

[0112] (2) Adsorbent preparation

[0113] Accurately weigh RuCl with a Ru content of 37.0wt% 3 .nH 2 O 5.41g, put in 1000mL beaker, add 20mL deionized water to dissolve, add 2ml 1:1 hydrochloric acid to dissolve Pd content 59.0wt%PdCl 2 0.169g, adjust the pH value of the solution to 1.5 with 5wt% sodium bicarbonate aqueous solution, dilute to 150 milliliters with 1.0wt% PEG-600 aqueous solution, add 100g processed carrier, and soak for 12 hours at ...

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Abstract

The invention provides a ruthenium-based adsorbent for deeply removing thiophene of benzene as well as a preparation method and application of the ruthenium-based adsorbent. The ruthenium-based adsorbent comprises metal ruthenium loaded on a carrier, wherein the carrier is selected from aluminum oxide, silicon oxide, titanium oxide and a molecular sieve, and a mixture of any two or more thereof. The preparation method comprises the following steps: adopting a molded porous grain-shaped carrier; carrying out modification treatment on the carrier in advance and loading pre-blended ruthenium-containing compound slurry by an immersion or spraying method; adding an inorganic alkali solution to carry out sedimentation and transformation; and carrying out liquid-phase reduction and/or gas-phase reduction to obtain the ruthenium-based adsorbent. The benzene, which is treated by the novel ruthenium-based adsorbent, can meet the requirements on content and quality of thiophene in the raw material benzene in a process of preparing cyclohexene through hydrogenating the benzene. Compared with the prior art, the ruthenium-based adsorbent has high thiophene removal precision, high sulfur capacity, low price and simple production process and equipment; and industrialized production is easy to realize and the ruthenium-based adsorbent has good application prospect and great economic benefits.

Description

technical field [0001] The invention relates to a novel high-efficiency ruthenium-based adsorbent for deep dethiophene removal of benzene, in particular to a ruthenium-based adsorbent for deep dethiophene removal of raw material benzene in the production process of benzene hydrogenation to cyclohexene, and a preparation method and application thereof. technical background [0002] Benzene is partially hydrogenated under the action of ruthenium-zinc catalyst to produce cyclohexene. The only by-product is cyclohexane, which is a reaction with a utilization rate close to 100%. Cyclohexene is further hydrated to produce cyclohexanol, cyclohexene, cyclohexane and Cyclohexanol is an important chemical raw material, mainly used in the production of caprolactam, adipic acid, hexamethylenediamine, cyclohexanone, etc. [0003] At present, the raw material benzene is mainly coking benzene, and the content of thiophene in benzene is relatively high. However, the ruthenium catalyst in th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/06B01J20/28B01J20/08B01J20/18C07C15/04C07C7/12
CPCB01J20/0211B01J20/0229B01J20/08B01J20/103B01J20/165B01J20/28016B01J20/28019C07C7/12C07C15/04
Inventor 国海光戴连欣孙兵
Owner SHANGHAI XUNKAI NEW MATERIAL TECH
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