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A kind of separation method of ethylene ethane

A separation method, ethylene technology, applied in the purification/separation of hydrocarbons, chemical instruments and methods, adsorption purification/separation, etc., can solve the problems of unfavorable industrial applications, easy deactivation of materials, low adsorption capacity, etc., and achieve precise pore size The effects of regulation, easy availability of raw materials, and high adsorption capacity

Active Publication Date: 2020-06-05
ZHEJIANG UNIV
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The core is to choose a good adsorbent. The ideal adsorbent should have the characteristics of large adsorption capacity, large separation factor and long service life. However, the currently used molecular sieve or porous material adsorbents have low adsorption capacity or low selectivity. Disadvantages, such as the capacity of NaY molecular sieve to ethylene at normal temperature and pressure is 2.1mmol / g, but the separation selectivity of ethylene / ethane is only 1.4 (AICHE Journal,1995,41(3):509-517); metal organic framework MaterialCu(BTC) 2 Although the adsorption capacity to ethylene is 6mmol / g at normal temperature and pressure, the ethylene / ethane separation selectivity is only 1.2 (Micropor.Mesopor.Mater., 2002,55(2):217-230); all-silicon molecular sieve ITQ-55 achieves ethylene / ethane separation through the kinetic difference of ethylene and ethane diffusion, but the adsorption capacity for ethylene is only 1.3mmol / g at normal temperature and pressure; patent CN 105251442A reports a loaded CuCl adsorbent, ethylene ethane The separation ratio can reach 8.25, but the adsorption capacity for ethylene is only 1.25mmol / g, and this kind of material is easy to deactivate, which is not conducive to industrial application

Method used

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  • A kind of separation method of ethylene ethane
  • A kind of separation method of ethylene ethane
  • A kind of separation method of ethylene ethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1mmol Ni(BF 4 ) 2 , 1mmol (NH 4 ) 2 GeF 6 and 10mmol of pyrazine were placed in a strain bottle, 3ml of water and 1ml of methanol were added, and stirred at room temperature for 48h. After suction filtration, the obtained slurry was activated for 12h under vacuum at 140°C to obtain GeFSIX-3-Ni material.

[0045] Fill the obtained GeFSIX-3-Ni material into a 5cm adsorption column, and pass 0.2Mpa ethylene: ethane (93.7:6.3) mixed gas into the adsorption column at 25°C at 1mL / min, and high purity can be obtained in the outflow gas Ethane (greater than 99.99%) gas, when ethylene breaks through, stops adsorption. The adsorption column adopts vacuum desorption at 100°C to obtain ethylene (purity greater than 98%), and the adsorption column can be recycled.

[0046] figure 1 CO for GeFSIX-3-Ni material at 298K and 1atm 2 The adsorption isotherm;

[0047] figure 2 is the crystal unit structure diagram of GeFSIX-3-Ni material, where Inorganic anion GeF 6 2- , i...

Embodiment 2

[0054] 1mmol Ni(NO 3 ) 2 , 1mmol (NH 4 ) 2 GeF 6 and 3 mmol of pyrazine were placed in a ball mill jar, and after ball milling at 800 r / min for 15 min, the resulting material was washed with 10 ml of methanol, then suction-filtered, and vacuum activated at 100°C for 12 hours to obtain GeFSIX-3-Ni material.

[0055] The obtained GeFSIX-3-Ni material was packed into a 10cm adsorption column, and 0.5Mpa ethylene: ethane (50:50) mixed gas was passed into the adsorption column at 0.5mL / min at 25°C, and high Purity ethane (greater than 99.99%) gas, when ethylene breaks through, the adsorption stops. The adsorption column adopts vacuum desorption at 100°C to obtain ethylene (purity greater than 95%), and the adsorption column can be recycled.

[0056] The breakthrough curve of GeFSIX-3-Ni material for ethylene / ethane (50 / 50) gas mixture at 298K and 1atm is as follows Figure 4 shown.

Embodiment 3

[0058] 1mmol Co(NO 3 ) 2 , 1mmol (NH 4 ) 2 TiF 6 and 12.5 mmol of pyrazine were placed in a strain bottle, 2 ml of methanol and 1 ml of water were added, and stirred at room temperature for 48 h. After suction filtration, the obtained slurry was vacuum activated at 140°C for 24 h to obtain TIFSIX-3-Co material.

[0059] The obtained TIFSIX-3-Co material was filled into a 15cm adsorption column, and a 0.2Mpa ethylene: ethane: methane (49:49:2) gas mixture was passed into the adsorption column at 30°C at 2mL / min. When transparent, stop adsorption. The adsorption column adopts vacuum desorption at 130°C to obtain ethylene (purity greater than 90%), and the adsorption column can be recycled.

[0060] The adsorption isotherms of TIFSIX-3-Co material for ethylene and ethane at 298K are as follows: Figure 5 shown;

[0061] The thermogravimetric curve of TIFSIX-3-Co material is as follows Figure 6 shown.

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Abstract

Disclosed is a method for separating ethylene from ethane, comprising the following steps: bring a mixture of ethylene and ethane into contact with an ultramicroporous anion-pillared hybrid material, and selectively adsorbing ethylene molecules so as to separate ethylene from ethane, wherein the ultramicroporous anion-pillared hybrid material is expressed by the general formula of [L2-M-A]n, where same is constructed by an organic ligand L, an inorganic fluorine-containing anion A and a metal ion M through coordination bonds, in which n is a positive integer, representing the fact that the ultramicroporous anion-pillared hybrid material is formed by regularly arranging several structural units composed of L2-M-A; the organic ligand L is pyrazine; the inorganic fluorine-containing anion A is any one of SiF6 2-, GeF6 2-, TiF6 2-, SnF6 2-, and NbF6 -; and the metal ion M is any one of Fe2+, Co2+, and Ni2+. The invention realizes the selective identification of ethylene, and at the same time, the selective separation of ethylene and ethane can also be realized by means of a kinetic diffusion rate, and as such, a high-purity (99.99%) of ethylene and ethane can be obtained.

Description

technical field [0001] The invention belongs to the technical field of chemical separation, and in particular relates to an anion hybrid ultramicroporous material used for the separation of ethylene and ethane. Background technique [0002] As an important basic chemical raw material, ethylene mainly comes from the cracking of natural gas and petroleum hydrocarbons. It is one of the chemical products with the largest output in the world. The ethylene industry is the core of the petrochemical industry. Ethylene products account for more than 75% of petrochemical products. As one of the important symbols to measure the development level of a country's petrochemical industry, it has a pivotal position. Ethylene is mainly used to produce polymers such as polyethylene and ethylene-propylene rubber, and high purity is required in the utilization process. In addition, ethane can be used as the main raw material for steam cracking to produce ethylene, which has a high demand. [0...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C7/12C07C7/00C07C9/06C07C11/04
CPCC07C7/00C07C7/12C07C9/06C07C11/04
Inventor 邢华斌张照强崔希利
Owner ZHEJIANG UNIV
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