Preparation method of metal-organic framework porous adsorption material for normal paraffin and isoparaffin adsorption separation

A metal-organic framework and porous adsorption material technology, applied in the direction of adsorption purification/separation, organic chemistry, alkali metal compounds, etc., can solve the problems of low yield per unit adsorbent, low adsorption capacity, etc., and achieve controllable surface potential energy, adsorption The effect of large capacity and excellent selectivity

Inactive Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to prepare a new metal-organic framework porous material for the disadvantages of low adsorption capacity of existing adsorbents and low yield per unit adsorbent, and use it for pressure swing adsorption to separate C4-C8 normal alkanes and isoparaffins. Mixture of paraffins

Method used

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  • Preparation method of metal-organic framework porous adsorption material for normal paraffin and isoparaffin adsorption separation
  • Preparation method of metal-organic framework porous adsorption material for normal paraffin and isoparaffin adsorption separation
  • Preparation method of metal-organic framework porous adsorption material for normal paraffin and isoparaffin adsorption separation

Examples

Experimental program
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Effect test

Embodiment 1

[0030] 1.0g of 2-methylimidazole and 1.0g of zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O) Dissolve in a mixed solvent prepared by 50ml N,N-dimethylformamide and 50ml N,N-diethylformamide, mix evenly and pour into a polytetrafluoroethylene reactor, the reaction temperature is 150°C, and the reaction time is 12h , to synthesize three-dimensional cage-like metal-organic frameworks by hydrothermal synthesis. Its three-dimensional structure is as figure 1 As shown, the framework structure consists of dodecahedral Zn(ClbIm) 2 and polycyclic rings. At a temperature of 180°C and a pressure of 0.5Mpa, the binary mixture components n-hexane and 2,2-dimethylbutane are completely separated, 2,2-dimethylbutane is hardly adsorbed, and the adsorption capacity of n-hexane reaches 15.6g / 100g ads , showing excellent selectivity and high adsorption capacity of the adsorbent.

Embodiment 2

[0032]2.0g nickel nitrate (Ni(NO 3 ) 2 6H2O), 4.0g 1,3,5-triethyl benzenetricarboxylate (C 15 h 18 o 6 ) and 8.0g imidazole mixed components were dissolved in 200ml N,N-dimethylformamide and 250ml N,N-diethylformamide solvent, stirred at 30°C for 30min, kept the reaction temperature at 80°C for 24h, passed Synthesis of three-dimensional metal-organic frameworks by hydrothermal synthesis. The three-dimensional structure of the adsorbent described in Example 2 is composed of 1,3,5-triethyl benzenetricarboxylate, imidazole, nickel atoms and oxygen atoms, such as figure 2 shown. At a temperature of 110°C and a pressure of 0.15Mpa, the ternary mixed components of n-pentane, 2-methylbutane and methylcyclopentane were successfully separated, and the adsorbent in Example 2 hardly adsorbed isoparaffins , The adsorption capacity for n-pentane reaches 18.5g / 100gads.

Embodiment 3

[0034] 2.0g aluminum nitrate (Al(NO 3 ) 3 ) and 30g of 1,4-benzenedicarboxylate, add solvent 40mllN,N-dimethylformamide and 200mlN,N-diethylformamide mixed solution, stir for 12h, mix well and pour into polytetrafluoroethylene to react In the kettle, keep the reaction temperature at 215°C, and react for 120h. Through the hydrothermal synthesis method, the three-dimensional network topology structure is obtained, and the adsorption isotherms of the three-dimensional organic framework material to n-pentane and n-hexane in Example 3 are as follows image 3 shown. The synthesized MOFs have an adsorption capacity of 20.0g / 100gads for the mixed component of n-pentane and n-hexane at a certain temperature and pressure, and have almost no adsorption capacity for multi-branched isoparaffins.

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Abstract

The invention relates to a preparation process of a metal-organic framework porous adsorption material for C4-C8 normal paraffin and isoparaffin adsorption separation. According to the preparation method of the synthesized metal-organic framework porous adsorption material, metal ion nitrate and an organic ligand are dissolved according to the mass ratio of 1:1-15 in a mixed solution of N,N-dimethylformamide and N,N-diethyl formamide; stirring is carried out for 0.5-12 h; reaction temperature is controlled to 80-250 DEG C, and reaction time is 12-120 h; and by a hydrothermal synthesis method, the metal-organic framework porous adsorption material is prepared. The material has characteristics as follows: specific surface area is large; pore structure height is ordered; pore size is controllable; surface potential energy is controllable; and adsorption capacity of normal paraffin is large. The material can selectively adsorb normal paraffin from mixed materials of normal paraffin and isoparaffin, has high selectivity and has a wide practical application prospect in normal paraffin and isoparaffin separation.

Description

technical field [0001] The invention relates to a preparation method of a metal-organic framework porous adsorption material, which is used for the adsorption and separation of C4-C8 normal paraffins and isoparaffins in light naphtha. Background technique [0002] Pressure swing adsorption is based on the principle of shape-selective adsorption of adsorbents to separate normal alkanes and isoparaffins. Adsorbents generally have regular and uniform micropore distribution, and the mixed components can be separated according to the relationship between their pore size and molecular size. The effective kinetic diameter of n-paraffin molecules is about 0.49nm, and the effective diameter of isoparaffin molecules is above 0.52nm. At present, the adsorbents usually used for pressure swing adsorption to separate alkanes and n-isomeric hydrocarbons are mainly type A molecular sieves and β molecular sieves. A-type molecular sieves generally use 5A molecular sieves. 5A molecular sieve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30B01J20/28C07C9/00C07C7/12
CPCB01J20/226B01J20/28002B01J20/3085B01J2220/44C07C7/12C07C9/12C07C9/14
Inventor 王海燕陈韶辉崔群刘宗健贺春尧汪洋殷飞李晓强戚龙浩王亚
Owner CHINA PETROLEUM & CHEM CORP
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