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Ammonia modification method of calcium squarate and application thereof in efficient separation of ethylene and ethane

A technology of ethylene ethane and calcium squaraine, which is applied in ethylene production, adsorption purification/separation, chemical instruments and methods, etc. The effect of increasing retention time and increasing adsorption capacity

Active Publication Date: 2020-08-07
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, comparing the research of Professor Chen Banglin's research group (Nat.Mater.2018, 18, 1128.) and Professor Bao Zongbi of Zhejiang University (Chem.Eng.J.2019, 358, 446.) found that in the process of using calcium squarylate, accurate Only by adjusting the activation conditions can good separation performance be achieved. Once the pore structure is not properly controlled during the activation process, the separation effect will be significantly reduced.
Therefore, the two for the C of calcium squarylate 2 h 4 / C 2 h 6 Separation jobs have large performance differences

Method used

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  • Ammonia modification method of calcium squarate and application thereof in efficient separation of ethylene and ethane
  • Ammonia modification method of calcium squarate and application thereof in efficient separation of ethylene and ethane
  • Ammonia modification method of calcium squarate and application thereof in efficient separation of ethylene and ethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The ammonia modification method of calcium squarylate comprises the following steps:

[0027] ① Place the prepared calcium squarylate material in a high vacuum environment (1×10 -5 bar) heated at 160°C and kept for more than 3 hours. The preparation method of calcium squarylate material is well known in the art, and will not be repeated here.

[0028] ② After the activation is completed, cool the material to room temperature naturally, and then pass ammonia gas (purity above 99.99%) to 1 bar at a rate of 200 mbar / min.

[0029] ③The modification of the above steps is more critical. The material modification temperature should be between 20-30°C, and the retention time during the ammonia modification process should be more than 1 hour. The above process ensures that the ammonia adsorption of the material is saturated. In this embodiment, the mass of the calcium squarylate material remains constant when the ammonia adsorption is saturated.

[0030] ④ After the ammonia a...

Embodiment 2

[0033] The ethylene adsorption properties of calcium squarylate materials with different ammonia modification amounts were tested.

[0034] Get ten calcium squarylate materials that the amount of ammonia modification in Example 1 is 0.05%, 0.5%, 1%, 1.6%, 3.2%, 3.7%, 4.8%, 6.6%, 8.2% and 10% at room temperature The ethylene adsorption test was carried out under the following conditions, and the final adsorption capacity was compared with that of the calcium squarylate material without ammonia modification. The results are shown in Table 1. In this example, the calcium squarylate material that has not been modified by ammonia has only completed the high-vacuum and high-temperature activation in step ① in Example 1.

[0035] Table 1 Effect of different amounts of ammonia modification on ethylene adsorption of calcium squarate materials

[0036]

[0037] Due to the dual effects of pore volume and ammonia modification position, too large ammonia modification amount or too low ...

Embodiment 3

[0039] Application testing of ethylene ethane separation using ammonia-modified calcium squarylate material.

[0040] ① Take 0.9 g of the calcium squarylate material in Example 1 with an ammonia modification amount of 1% and fill it into a separation column of Φ4×120 mm, and take 0.9 g of the calcium squarylate material without ammonia modification and fill it into a separation column of Φ4×120 mm The separation column was used as a control.

[0041] ②Purge the separation column with helium gas for 30 minutes at the set temperature of 80°C, and the flow rate of the purge is 100ml / min.

[0042] ③After purging, cool down to room temperature naturally, and use ethaneethylene (1:1 volume ratio) feed gas to penetrate the adsorption column at room temperature (25°C), and set the flow rate to 1.5mL / min.

[0043] ④ Take samples from the gas outlet every 2-3 minutes and inject them into the chromatographic analyzer to analyze the effluent components.

[0044] ⑤ Carry out content anal...

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Abstract

The invention relates to an ammonia modification method of calcium squarate and application thereof in efficient separation of ethylene and ethane. The calcium squarate material is activated for morethan 3 hours under the high vacuum condition of 160 DEG C or above, so that the water molecules in the structure of the calcium squarate material are removed, calcium metal vacancies are exposed, andammonia modification of the calcium squarate material is achieved through modification of ammonia gas. After the calcium squarate material is activated and dehydrated, ammonia gas is used for modifying the structure of the material, so that a saturated adsorption effect is achieved. After a proper amount of ammonia molecules are removed subsequently, 1% of ammonia modification amount is reserved as an optimal modification condition, more adsorption space and sites can be provided for ethylene, and 33% of adsorption amount is increased. When the modified calcium squarate material is used for separating ethane and ethylene, more retention time is achieved, so that the separation performance can be improved by nearly one time.

Description

technical field [0001] The invention relates to the field of modification of calcium squarylate adsorbent materials and the separation of low-carbon hydrocarbons, in particular to a method of modifying the structure of calcium squarylate materials by using ammonia gas, and selectively increasing the adsorption capacity of ethylene, through ammonia to the structure Controlled, and finally realize the high-efficiency separation of ethylene and ethane. Background technique [0002] Ethylene (C 2 h 4 ) is one of the chemical products with the largest output and consumption in the world, and is known as the "mother of the petrochemical industry". Ethylene production capacity is one of the important indicators to measure the development level of a country's petrochemical industry. my country's ethylene production capacity has long been ranked second in the world, second only to the United States. In 2018, my country's total ethylene production capacity reached ~25 million tons...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30C07C7/12C07C11/04C07C11/06
CPCB01J20/226B01J20/28054C07C7/12C07C11/04C07C11/06Y02P30/40
Inventor 陈杨李立博贺朝辉刘普旭李晋平
Owner TAIYUAN UNIV OF TECH
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