Multi-stage pore 5A molecular sieve adsorbent for n-alkane adsorption separation and preparation method thereof

A technology for adsorption and separation of normal alkanes, applied in chemical instruments and methods, refined hydrocarbon oil, and other chemical processes, can solve problems such as long diffusion paths, low active center utilization, and long adsorption/desorption cycles. To achieve the effect of improving the adsorption separation efficiency and the adsorption rate

Pending Publication Date: 2017-07-04
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The 5A molecular sieve synthesized by the traditional method only has a micropore channel structure, and the limited molecular diffusion rate, long diffusion path and low active center utilization in the micropore greatly limit the adsorption / desorption rate, making the adsorption / desorption long cycle time

Method used

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  • Multi-stage pore 5A molecular sieve adsorbent for n-alkane adsorption separation and preparation method thereof
  • Multi-stage pore 5A molecular sieve adsorbent for n-alkane adsorption separation and preparation method thereof
  • Multi-stage pore 5A molecular sieve adsorbent for n-alkane adsorption separation and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] According to the following raw material molar ratio:

[0036] nNa 2 O: nSiO 2 : NAl 2 O 3 :NDQA:nH 2 O=3:2:1:0.015:150

[0037] Weigh the long-chain double quaternary ammonium salt, silicon source solution, NaOH, aluminum source solution and deionized water and mix uniformly. The specific synthesis steps are as follows:

[0038] 1) Weigh a certain amount of long-chain diquaternary ammonium salt solution according to the ratio, dissolve it in 100ml of water, add sodium silicate solution and NaOH and stir to dissolve as a silicon source. Sodium metaaluminate was dissolved in 50 ml of water as an aluminum source. The aluminum source solution was added dropwise to the silicon source solution at 40° C., stirred vigorously for 10 minutes, and then allowed to stand and age for 2 hours. Move the silicon-aluminum mixture into a crystallization kettle for crystallization at 99±1°C for 4 hours, and cool naturally. The product after crystallization is suction filtered to obtain molecul...

Embodiment 2～18

[0042] The preparation method of the spherical adsorbent with multi-stage 5A molecular sieve is the same as in Example 1, except that the molar ratio of the components in the raw materials, the long-chain double quaternary ammonium salt, the silicon source and the aluminum source, and the types of calcium salts for exchange are different. Details are shown in Tables 1 and 2.

[0043] Table 1

[0044]

[0045] Table 2

[0046]

[0047]

Embodiment 19

[0049] The 5A adsorbent samples prepared in Examples 1-18 were characterized and analyzed using a Micromeritics ASAP 2020 nitrogen physical adsorption instrument. The pretreatment method of the sample before analysis is as follows: vacuumize the molecular sieve sample at room temperature. When the vacuum condition is reached, treat it at 130°C for 2h; then treat it at 350°C for 2h. Nitrogen physical adsorption results show that the pore diameters of samples 1-20 are 0.3-0.5nm, all of which contain mesopore pore diameter distribution, mesopore average pore diameter, mesopore volume and specific surface area as shown in Table 3.

[0050] table 3

[0051]

[0052]

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Abstract

The invention discloses a multi-stage pore 5A molecular sieve adsorbent for n-alkane adsorption separation and a preparation method thereof. The preparation method comprises adding a long-chain double biquaternary ammonium salt as a soft template agent into a silicon source-aluminum source mixed sol system, carrying out hydrothermal synthesis to obtain a microporous-mesoporous structure multi-stage pore 4A molecular sieve, removing the soft template agent in the 4A molecular sieve, rolling to mold the 4A molecular sieve and a binder so that small particles having diameters of 0.2-0.8mm are obtained, carrying out drying and calcination, and carrying out calcium ion exchange and activation to obtain a microporous-mesoporous structure multi-stage pore 5A molecular sieve, wherein a ratio of the 5A molecular sieve in the adsorbent is 90-97wt% and a ratio of the binder is 3-10%. In the preparation method of the adsorbent, the multi-stage pore 5A molecular sieve has a high equilibrium adsorption capacity of n-alkane, improves a diffusion coefficient of the n-alkane in the molecular sieve and improves an adsorption separation rate.

Description

Technical field [0001] The invention relates to a n-alkane adsorption and separation adsorbent and a preparation method thereof. Specifically, it synthesizes a 4A molecular sieve with a microporous-mesoporous hierarchical pore structure, which is formed by rolling with a binder and exchanged with calcium ions. The prepared 5A molecular sieve adsorbent can be used to separate and purify normal paraffins from distillate oil containing normal paraffins. Background technique [0002] It is of great significance to separate and purify n-paraffins from petroleum refining product fractions. For example, the separation of normal paraffins and other hydrocarbons (isoparaffins, naphthenes, and aromatics) in naphtha can optimize feedstocks and improve the efficiency of downstream ethylene and reformers. NC separated from kerosene fraction 10 ~nC 14 Normal alkanes are raw materials for the preparation of detergents. Separating n-alkanes from gasoline fractions can significantly increase th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30C10G25/08
CPCB01J20/0248B01J20/041B01J20/103B01J20/22C10G25/08
Inventor 王志光王涛李小龙李进王炳春王建青王庆吉刘国东
Owner CHINA CATALYST HLDG CO LTD
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