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5A molecular sieve absorbent for adsorptive separation of distillate containing n-alkane and preparation method of 5A molecular sieve adsorbent

A technology for adsorption and separation of normal alkanes, which is applied in the fields of refined hydrocarbon oil, chemical instruments and methods, and the petroleum industry, and can solve problems such as low active center utilization, long diffusion paths, and long adsorption/desorption cycles

Pending Publication Date: 2017-06-20
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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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] According to the following raw material molar ratio:

[0056] nNa 2 O: nSiO 2 : NAl 2 O 3 :NPQA:nH 2 O=3:2:1:0.010:150

[0057] Weigh polyquaternium, silicon source solution, NaOH, aluminum source solution and deionized water and mix them evenly. The specific synthesis steps are as follows:

[0058] 1) Weigh a certain amount of polyquaternary 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 molecular sieve crystals, which are washed 3 t...

Embodiment 2～18

[0062] The steps of the preparation method for the spherical adsorbent with multi-stage 5A molecular sieve are the same as in Example 1, except that the molar ratio of the components in the raw materials, the polyquaternary ammonium salt, the silicon source and the aluminum source, and the calcium salt for exchange are different. Shown in Tables 1 and 2.

[0063] Table 1

[0064]

[0065] Table 2

[0066] Example number Adsorbent name Silicon source type Type of aluminum source Types of polyquaternium Calcium ion solution Example 1A Water glass Sodium aluminate Polyquaternium-2 Calcium chloride Example 2B White carbon black Aluminum chloride Polyquaternium-6 Calcium chloride Example 3C Silica sol Sodium aluminate Polyquaternium-7 Calcium chloride Example 4D Methyl orthosilicate Aluminum Nitrate Polyquaternium-10 Calcium chloride Example 5E Water glass Aluminum sulfate Polyquaternium-22 Calcium chloride Example 6F Silica sol Aluminum isopropoxide Polyquaternium-32 Calcium c...

Embodiment 19

[0068] The 5A adsorbent samples prepared in Examples 1-18 were characterized and analyzed using a Micromeritics ASAP2020 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.

[0069] table 3

[0070]

[0071]

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Abstract

The invention discloses a 5A molecular sieve adsorbent for adsorptive separation of distillate containing n-alkane and a preparation method of the 5A molecular sieve adsorbent. The preparation method comprises the following steps: adding polyquaternary ammonium salt serving as a crystallization synthetic soft template agent into a sol system formed by mixing a silicon source with an aluminum source, and carrying out hydrothermal synthesis to obtain a hierarchically porous 4A molecular sieve with a microporous-mesoporous structure; after the 4A molecular sieve is subjected to soft template agent removal, carrying out roll forming on the treated 4A molecular sieve and a binder to obtain small balls with particle sizes of 0. 2 to 0.8mm; drying, roasting and then carrying out calcium ion exchange and activating to obtain the 5A molecular sieve adsorbent with the microporous-mesoporous structure, wherein the proportion of a 5A molecular sieve in the adsorbent is 90 to 97 weight percent, and the proportion of the binder is 3 to 10 percent. The preparation method of the adsorbent, provided by the invention, has the advantages that a diffusion coefficient of the n-alkane in the molecular sieve is remarkably improved while the synthesized hierarchically porous 5A molecular sieve maintains higher equilibrium adsorption capacity for the n-alkane, thereby increasing the rate of adsorptive separation.

Description

Technical field [0001] The invention relates to a 5A molecular sieve adsorbent for adsorption and separation containing n-alkane distillate oil and a preparation method thereof. Specifically, it is to synthesize a 4A molecular sieve with a microporous-mesoporous hierarchical pore structure and form it with a binder 5. The 5A molecular sieve adsorbent prepared by calcium ion exchange can be used to separate and purify n-alkanes from distillates containing n-alkanes. 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 significan...

Claims

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Application Information

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IPC IPC(8): B01J20/18B01J20/30C10G25/00
CPCB01J20/18C10G25/003
Inventor 王志光李小龙王涛李进王炳春刘国东王建青王庆吉
Owner CHINA CATALYST HLDG CO LTD
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