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Adsorbent for olefin/alkane mixed gas separation and preparation method and application thereof

A technology of mixed gas and adsorbent, applied in adsorption purification/separation, chemical instruments and methods, other chemical processes, etc., can solve the problems of easily damaged material structure, complex operation process, collapse of pore structure, etc., to achieve good adsorption effect, The effect of high selectivity and easy regeneration

Active Publication Date: 2015-04-22
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Solution impregnation method (Bull Chem Soc Jpn, 1986,59:2217), because cuprous chloride has very low solubility in conventional solvents, only has larger solubility in high-concentration hydrochloric acid, and high-concentration acid solution is easy Destroy the material structure, even lead to the collapse of the pore structure
In addition, because cuprous chloride is quite unstable to light and air, the entire operation must be carried out under the protection of light and inert gas, so the operation process is quite complicated.

Method used

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  • Adsorbent for olefin/alkane mixed gas separation and preparation method and application thereof
  • Adsorbent for olefin/alkane mixed gas separation and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Preparation of metal-organic framework materials: add vanadium chloride, terephthalic acid, hydrofluoric acid and water into the reaction kettle according to a certain molar ratio (1:0.25:2:250), stir them evenly with ultrasonic waves, and then After 4 days of reaction at 200°C, MIL-47(V) containing impurities (mainly terephthalic acid in the channels) can be obtained, and the valence state of the initially synthesized metal vanadium is 3+;

[0045] (2) Activation of metal-organic frameworks: take 500 mg of initially synthesized MIL-47 (V 3+ ) into 100ml of DMF, ultrasonicated at 80°C for 2h, centrifuged and repeated ultrasonication twice, then exchanged with methanol for 3 times at 70°C, and finally dried in a vacuum oven at 80°C for 12h. Purified samples were stored in a desiccator. The following examples, unless otherwise specified, are samples purified by this activation method.

[0046] (3) Preparation of composite adsorbent material: get activated MIL-47 (V ...

Embodiment 2

[0051] Preparation of composite adsorbent material: get the activated MIL-47 (V 3+ ) into the container, add 2 mL of ethanol solution with a cupric chloride concentration of 200 mg / ml, stir for 6 h, filter, and dry in a vacuum oven at 80° C. for 1 h to obtain an adsorbent with a loading capacity of 38.5 wt%.

[0052] At 30°C and 1 bar, the adsorption capacity of the adsorbent to ethylene is 1.20 mmol / g, the adsorption capacity to ethane is 0.7 mmol / g, and the equilibrium separation selectivity is 1.71. At 8 bar, the adsorption capacity of the adsorbent to ethylene is 2.56 , the adsorption capacity of ethane is 1.45mmol / g, and the equilibrium separation selectivity is 1.76.

Embodiment 3

[0054] Preparation of composite adsorbent material: get the activated MIL-47 (V 3+ ) into the container, add 2 mL of ethanol solution with a cupric chloride concentration of 300 mg / ml, stir for 6 h, filter, and dry in a vacuum oven at 80° C. for 1 h to obtain an adsorbent with a loading capacity of 54.8 wt%.

[0055] At 30°C and 1 bar, the adsorption capacity of the adsorbent to ethylene is 1.01mmol / g, the adsorption capacity to ethane is 0.50mmol / g, the equilibrium separation selectivity is 1.95, and according to the ideal solution theory (IAST), the equimolar ratio The ideal selectivity of ethylene / ethane calculated under the following conditions is 5. The adsorption capacity of the adsorbent for ethylene at 8 bar is 2.35, the adsorption capacity for ethane is 1.2 mmol / g, and the equilibrium separation selectivity is 2.02. At 1 bar, the adsorption capacity of the adsorbent for The adsorption amount of propylene is 1.81mmol / g, the adsorption amount to propane is 0.91mmol / g, t...

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Abstract

The invention discloses a preparation method of an adsorbent for olefin / alkane mixed gas separation. the preparation method comprises the following steps: after vanadium chloride, terephthalic acid, hydrofluoric acid and water are mixed, a hydrothermal reaction is carried out to obtain MIL-47(V<3+>) containing impurities; under the assistance of ultrasonic wave, low temperature activation treatment is carried out to remove impurities so as to obtain MIL-47(V<3+>); and by a solution impregnation method, Cu<2+> is loaded on MIL-47(V<3+>), and autoxidation-reduction is carried out to reduce the loaded Cu<2+> to Cu<+> so as to obtain the adsorbent. By using MIL-47(V<3+>) obtained by low temperature activation treatment as a carrier, Cu<2+> is firstly loaded, and then the loaded Cu<2+> is reduced to Cu<+> by the process of autoxidation-reduction. The preparation process is simple, and conditions are mild. The prepared adsorbent can be used to realize high-selective separation of olefin / alkane mixed gases.

Description

technical field [0001] The invention relates to the technical field of adsorption materials, in particular to an adsorbent used for the separation of olefin / alkane mixed gas and its preparation method and application. Background technique [0002] The separation of olefins and alkanes is an important separation process in the petrochemical industry, among which the separation of ethylene-ethane and propylene-propane is the most representative. In olefins plants, cryogenic rectification has traditionally been used to separate olefins-alkanes. Although rectification is a very mature process, it consumes a lot of energy. Researchers have been working hard to find an efficient, energy-saving, and low-cost method to replace low-temperature distillation. The adsorption method is due to its high efficiency, energy saving, and low cost. Advantages, it is currently recognized as one of the methods most likely to replace cryogenic separation. [0003] The key to the adsorption separ...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30C07C7/12
CPCB01J20/22B01J20/3085B01J2220/4812C07C7/12C07C9/06C07C11/04C07C9/08C07C11/06
Inventor 鲍宗必任其龙常刚刚苏宝根邢华斌杨亦文张治国杨启炜
Owner ZHEJIANG UNIV
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