A preparation method of organic-inorganic hybrid porous material for separating propylene propane

A porous material, propylene propane technology, applied in organic chemistry, chemical instruments and methods, adsorption purification/separation, etc., can solve the problems of difficult separation, low relative volatility, etc., achieve simple preparation process, low equipment requirements, high The effect of adsorption capacity

Active Publication Date: 2022-06-24
杭州市富阳区浙工大银湖创新创业研究院 +2
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  • Description
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Problems solved by technology

The difference between the boiling points of propylene and propane is only 5.3 K, so the relative volatility is low (1.14), and the separation is difficult

Method used

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  • A preparation method of organic-inorganic hybrid porous material for separating propylene propane
  • A preparation method of organic-inorganic hybrid porous material for separating propylene propane
  • A preparation method of organic-inorganic hybrid porous material for separating propylene propane

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preparation example Construction

[0033] A preparation method of an organic-inorganic hybrid porous material for separating propylene propane, comprising the following steps:

[0034] 1) Put nickel hydroxide in a container, and then dropwise add an aqueous solution of hexafluorosilicic acid with a concentration of 20-30 wt%, the molar ratio of nickel hydroxide and hexafluorosilicic acid is 1.1-1.3:1; stirring reaction at room temperature 3 -5h, the obtained reaction product was suction filtered to obtain a green solution and dried at 40-60°C to obtain green nickel salt crystals.

[0035]2) Add 2-mercaptopyrazine into methanol according to the solid-liquid ratio of 0.1-0.15g / 10-30mL, and ultrasonicate for 20-40min to completely dissolve 2-mercaptopyrazine to obtain solution A; Liquid ratio 0.14-0.16g / 6-10mL is dissolved in methanol solution to obtain solution B; after solution A and solution B are mixed, add in the reactor, the mol ratio of described 2-mercaptopyrazine and green nickel salt crystal is ( 1-2): ...

Embodiment 1

[0038] Preparation of Nickel Hexafluorosilicate:

[0039] Weigh 4.2 g of nickel hydroxide into a 100 mL round-bottomed flask, then add 20 mL of a 25wt% hexafluorosilicic acid aqueous solution, wherein the molar ratio of hexafluorosilicic acid and nickel hydroxide is 1:1.1, and the reaction is stirred at room temperature for 4 h. The green solution was obtained by suction filtration with a Buchner funnel, and dried at 50° C. to remove water to obtain green hexafluorosilicate crystals, which were used for later use.

[0040] Embodiment 1 prepares the above-mentioned method of nickel hexafluorosilicate is optimal condition, as figure 1 As shown, it has high phase purity, and the nickel hexafluorosilicate in the subsequent examples is prepared by the above method.

[0041] Organic-inorganic hybrid porous materials [Ni(pyz-SH) 2 (SiF 6 )] n Preparation and activation of:

[0042] Dissolve 0.154g of nickel hexafluorosilicate in 6mL of methanol solution and 0.112g of organic lig...

Embodiment 2

[0046] Dissolve 0.154g nickel hexafluorosilicate in 6mL methanol solution and dissolve 0.056g organic ligand 2-mercaptopyrazine in 12mL methanol solution (with ultrasound for 30min), wherein nickel hexafluorosilicate and 2-mercaptopyrazine The molar ratio of pyrazine is 1:1. After mixing the two solutions, add them into 25mL polytetrafluoroethylene liner, put them into the reaction kettle, heat up 75°C at 10°C / min, react at 75°C for 72h, and finish After cooling down to room temperature, turn off the instrument and take out the sample. The solid yellow powder was obtained by suction filtration through a Buchner funnel, which was a microporous organic-inorganic hybrid porous material. Gas adsorption isotherms were measured by a Micromeritics ASAP 2020 Surface Area Analyzer. To remove all guest solvent from the backbone, fresh powder samples were first solvent-exchanged with anhydrous methanol multiple times over two days. The solvent-exchanged samples were evacuated at room t...

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Abstract

The invention relates to the technical field of chemical separation, and discloses a method for preparing an organic-inorganic hybrid porous material for separating propylene propane. The organic-inorganic hybrid porous material of the present invention is based on the inorganic metal ion Ni 2+ , Inorganic anion SiF 6 2‑ The microporous metal-organic framework material obtained under solvothermal conditions with the organic ligand 2-mercaptopyrazine has a relatively large specific surface area, and exhibits more suitable channels with shrinking pore sizes, which is more conducive to the capture of C 3 h 6 molecule, while restricting C to some extent 3 h 8 The capture in the channel has the characteristics of fast and efficient, high adsorption capacity, high selectivity and reuse after desorption. In addition, the present invention combines bifunctional groups ("-SH and SiF 6 2‑ ”) into the framework structure of hybrid porous materials, which can generate multiple binding environments to improve C 3 h 6 specific identification.

Description

technical field [0001] The invention relates to the technical field of chemical separation, in particular to a preparation method of an organic-inorganic hybrid porous material for separating propylene propane. Background technique [0002] Today, the efficient separation and purification of gases such as olefins, alkanes and alkynes is one of the key processes for sustainable development in the petrochemical industry. Light hydrocarbon compounds have similar structures and physicochemical properties, with only slight differences in carbon number and degree of unsaturation. The separation process of traditional cryogenic rectification has low selectivity and high energy consumption. Propylene is mainly used in the production of polypropylene, which is the basic raw material for the three major synthetic materials. Removal of propane from propylene is a key step to obtain high-purity propylene. The boiling point difference between propylene and propane is only 5.3 K, so the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/30C07C7/12C07C9/08C07C11/06
CPCB01J20/226C07C7/12C07C9/08C07C11/06
Inventor 胡军温慧敏廖才俊
Owner 杭州市富阳区浙工大银湖创新创业研究院
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