Preparation method of copper-containing zeolite adsorbent used for separating olefin from alkane

An olefin alkane and adsorbent technology, applied in the field of chemical gas separation, can solve the problems of low copper reduction rate, high reduction temperature, difficult to control, etc., and achieve the effects of high monovalent copper content, improved olefin selectivity, and mild conditions

Inactive Publication Date: 2014-12-17
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the current prior art, the reduction of divalent copper on the zeolite adsorbent is obtained in two ways: (1) the divalent copper exchanged to the carrier zeolite is subjected to high temperature (>450°C) for a long time (>6h) in an inert atmosphere Heat treatment, this method has the disadvantages of high reduction temperature, long time, low reduction rate of copper, and extreme instability; (2) the divalent copper exchanged to the carrier zeolite under a reducing atmosphere (H 2 , CO or C 2 h 4 ) heat treatment, this method has the disadvantages of being difficult to control and easily excessively reduced to elemental copper

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Preparation of adsorbent: Weigh 10g of copper acetate and dissolve it in 500mL of deionized water, weigh 1g of zeolite ZSM-5 and dissolve it in the above 50mL of copper acetate solution, perform ion exchange at 30°C for 24 hours, filter, wash and dry to obtain Copper ion exchanged zeolite samples. Take 0.1g of copper ion-exchanged zeolite sample and put it in an open container and isolate it with 1mL of formaldehyde in a closed reaction kettle, put it in an oven at 180°C for 5h, and after cooling, the copper-containing zeolite adsorbent can be obtained.

[0017] Adsorption application experiment: the gas adsorption performance of the adsorbent was measured by the volumetric method (this method is used in the following examples). Take 500 mg of the above-mentioned adsorbent and place it in the ASAP2020 specific surface and pore analyzer of American Mike Company, and perform adsorption under a certain pressure and temperature, and finally measure the adsorption capacity o...

Embodiment 2

[0019] Preparation of adsorbent: Weigh 12.5g of copper sulfate and dissolve it in 500mL of deionized water, weigh 1g of zeolite ZSM-5 and dissolve it in the above 50mL of copper sulfate solution, perform ion exchange at 90°C for 12h, filter, wash and dry, A copper ion-exchanged zeolite sample was obtained. Take 0.8g copper ion-exchanged zeolite sample and put it in an open container and isolate it with 1mL methanol in a closed reaction kettle, put it in an oven at 210°C for 6h, and after cooling, the copper-containing zeolite adsorbent can be obtained.

[0020] Adsorption application experiment: The gas adsorption performance of the adsorbent was determined by the volumetric method. Take 500 mg of the above-mentioned adsorbent and place it in the ASAP2020 specific surface and pore analyzer of American Mike Company, and perform adsorption under a certain pressure and temperature. / ethane separation selectivity. Under normal temperature and pressure, the adsorption capacity of...

Embodiment 3

[0022] Preparation of adsorbent: Weigh 12.1g of copper nitrate and dissolve it in 500mL of deionized water, weigh 1g of zeolite ZSM-5 and dissolve it in the above 50mL of copper nitrate solution, perform ion exchange at 90°C for 24h, filter, wash and dry, A copper ion-exchanged zeolite sample was obtained. Take 0.8g copper ion-exchanged zeolite sample and put it in an open container and isolate it with 1mL hydrazine hydrate in a closed reaction kettle, put it in an oven at 200°C for 6h, and after cooling, the copper-containing zeolite adsorbent can be obtained.

[0023] Adsorption application experiment: The gas adsorption performance of the adsorbent was determined by the volumetric method. Take 500 mg of the above-mentioned adsorbent and place it in the ASAP2020 specific surface and pore analyzer of American Mike Company, and perform adsorption under a certain pressure and temperature, and finally measure the adsorption capacity of the adsorbent to butene and butane respecti...

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Abstract

The invention discloses a preparation method of a copper-containing zeolite adsorbent used for separating olefin from alkane. The preparation method of the copper-containing zeolite adsorbent used for separating olefin from alkane is capable of preparing relatively high content of cuprous active site with relatively low energy consumption in relatively short time, so that the separation performance of the copper-containing zeolite adsorbent during separation of olefin and alkane is improved. The preparation method of the copper-containing zeolite adsorbent used for separating olefin from alkane comprises the following steps: exchanging ions of a bivalent copper salt solution and a carrier zeolite, filtering reaction liquid to obtain solid, drying the solid to obtain bivalent cupric ion exchange zeolite, putting the obtained bivalent cupric ion exchange zeolite and a reducing agent in a sealed reaction kettle, separating the bivalent cupric ion exchange zeolite from the reducing agent by using an open container, enabling the zeolite to not be in direct contact with the reducing agent, introducing reducing agent steam and carrying out reduction reaction to obtain a zeolite adsorbent containing a cuprous active component.

Description

technical field [0001] The invention relates to a preparation method of an adsorbent, more specifically to a preparation method of a copper-containing zeolite adsorbent for the separation of alkenes and alkanes, and belongs to the technical field of chemical gas separation. Background technique [0002] Olefins and alkanes have relatively large output and demand in the chemical and petrochemical industry, and are the most important raw materials. Due to their similar physical properties, the separation of alkenes and alkanes is relatively difficult, and low-temperature distillation is mainly used in industry. This separation process requires a large investment in equipment and high energy consumption. Due to its advantages of high efficiency, energy saving and low cost, the adsorption separation method is considered to be a more suitable method among many separation methods at present. In particular, using some transition metals (Cu + 、Ag + etc.) and unsaturated hydrocarb...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/18B01J20/30
Inventor 刘晓勤孙林兵秦菊香刘定华
Owner NANJING TECH UNIV
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