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Method for synthesizing and forming UTSA-280 adsorbent materials on large scale

A technology of UTSA-280 and synthesis method, which is applied in the field of preparation of UTSA-280 adsorbent material, can solve the problems of affecting the economic benefit of enterprises, large process energy consumption, etc., and achieve the effect of convenient and accurate addition amount control and fast speed.

Active Publication Date: 2020-01-03
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Cryogenic distillation is usually used in conventional 2 h 4 / C 2 h 6 Separation, but the energy consumption of the process is large, accounting for more than 75% of the production cost of ethylene, and the high separation cost significantly affects the economic benefits of the enterprise

Method used

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  • Method for synthesizing and forming UTSA-280 adsorbent materials on large scale
  • Method for synthesizing and forming UTSA-280 adsorbent materials on large scale
  • Method for synthesizing and forming UTSA-280 adsorbent materials on large scale

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Through the improvement of the prior art method, switch to NH 3 ·H 2 O promotes the dissolution of squaraine in the early stage, helps to form a high-concentration and uniform squaraine solution, and forms UTSA-280 with high crystallinity (improved synthesis 1):

[0032] ①Add 10.944g squaraine to 200mL distilled water and stir well to form a supersaturated squaraine solution.

[0033] ②Add 12mL NH 3 ·H 2 O (25%), add while stirring. Now, 95% of squaraine can be dissolved to form a high-concentration squaraine solution of 48g / L.

[0034] ③Add 200mL of 22.656g calcium nitrate tetrahydrate solution to the high-concentration squaraine solution in ②, and mix thoroughly.

[0035] ④React at room temperature for a few minutes, and you can see the process of the mixed solution becoming clear and then crystals precipitate out immediately. The reaction can be completed in 5 minutes to obtain strip-shaped high-crystallinity UTSA-280.

[0036] ⑤ Filtrate the product and wash ...

Embodiment 2

[0038] Through the improvement of Example 2, the yield is increased by increasing the reactant concentration. Conditioning solvent and NH 3 ·H 2 O addition amount to synthesize UTSA-280 (improved synthesis 2):

[0039] ①Add 10.944g squarylium into 100mL distilled water, stir well to form a supersaturated squarylium solution.

[0040] ②Add 16mL NH 3 ·H 2 O (25%), add while stirring. At this point, most of the squaraine is soluble, forming a high-concentration squaraine solution.

[0041] ③Add 100mL of 22.656g calcium nitrate tetrahydrate solution to the high-concentration squaraine solution in ②, and mix thoroughly.

[0042] ④React at room temperature for a few minutes, and you can see the process of the mixed solution becoming clear and then crystals precipitate out immediately. The reaction can be completed in 5 minutes to obtain strip-shaped high-crystallinity UTSA-280.

[0043] ⑤ Filtrate the product and wash it three times with distilled water, and obtain the corre...

Embodiment 3

[0045] After the UTSA-280 with high crystallinity is obtained through a large-scale synthesis method, the molding technology of PMMA binder is used to form UTSA-280:

[0046] ① Put 1 g of the UTSA-280 crystal obtained in Example 2 into a small beaker.

[0047] ②Add 5%, 10% or 15% PMMA to 5mL of ethyl acetate solution, stir well to form PMMA ethyl acetate solution.

[0048] ③ Add the ethyl acetate solution of PMMA to the UTSA-280 crystal in ①, and mix thoroughly for half an hour.

[0049] ④ Draw up the mixture in ③ with a syringe, and then inject the mixture slowly.

[0050] ⑤ Wait for the injection to dry naturally, dissolve and remove to get the nearly spherical shaped UTSA-280. The thermal stability and water stability of the formed product are guaranteed, which is enough to meet the requirements of general adsorption environment.

[0051] Table 1 Molding process of UTSA-280 with different amounts of binder added

[0052]

[0053] Table 2 The stability of molding UTSA...

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Abstract

The invention relates to the field of preparation of a UTSA-280 adsorbent material, particularly relates a method for synthesizing and forming UTSA-280 adsorbent materials on a large scale, and particularly relates to a method for preparing UTSA-280 MOFs materials in batches by regulating reaction raw materials and regulators. The materials are subjected to molding granulation by additives. The method comprises the following steps: adding NH3*H2O into a squaric acid supersaturated aqueous solution to promote dissolution of squaric acid, adding a calcium nitrate aqueous solution into the formedsquaric acid aqueous solution, maintaining stirring in the process of adding the calcium nitrate aqueous solution, and obtaining a strip-shaped UTSA-280 crystal with high crystallization degree at room temperature. Compared with addition of the original NaOH, the rate of promoting dissolution of the squaric acid by the NH3*H2O is higher, the adding amount is convenient and accurate to control, and the method is a method capable of synthesizing the UTSA-280 with high crystallization degree efficiently and rapidly.

Description

technical field [0001] The present invention relates to the field of preparation of UTSA-280 adsorbent materials, in particular to a large-scale synthesis and molding method of UTSA-280 adsorbent materials, in particular to a method for preparing UTSA-280MOFs materials in batches by adjusting reaction raw materials and regulators , and use additives to shape and granulate the material. Background technique [0002] Ethylene (C 2 h 4 ) is an important petrochemical basic raw material. The capacity and production technology level of ethylene is an important symbol of a country's petrochemical development level. C that is widespread in the petrochemical industry 2 h 6 and C 2 h 4 The physical properties and molecular size are very close, and the conventional separation process consumes a lot of energy, resulting in C in the dry gas 2 h 4 difficult to recycle. In the practical application of ethylene, in order to obtain a polymer grade ethylene product with a purity hig...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30
CPCB01J20/226B01J20/3028
Inventor 陈杨李立博刘普旭杜亚丹李晋平
Owner TAIYUAN UNIV OF TECH
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