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Binder-free high-silica MFI zeolite adsorbent and preparation method thereof

A binder-free and adsorbent-free technology, applied in chemical instruments and methods, and other chemical processes, can solve the problems of small adsorption capacity, poor separation effect, and low adsorption rate, achieve high para-selectivity, reduce bed The number of layers and the effect of simplifying the process flow

Active Publication Date: 2016-06-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] One of the technical problems to be solved by the present invention is that existing high-silicon MFI zeolite adsorbents have the problems of small adsorption capacity, low adsorption rate and poor separation effect due to the use of binders. High-silica MFI zeolite adsorbent, which has the advantages of large adsorption capacity, high adsorption rate and good separation effect

Method used

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  • Binder-free high-silica MFI zeolite adsorbent and preparation method thereof
  • Binder-free high-silica MFI zeolite adsorbent and preparation method thereof
  • Binder-free high-silica MFI zeolite adsorbent and preparation method thereof

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Embodiment 1

[0032] Take by weighing silica sol (by weight percent, containing 40% SiO 2 ) 9.0 kilograms, in 30 liters of reactors, add 9.0 kilograms of tetrapropyl ammonium hydroxide (TPAOH) solution (by weight percent, containing tetrapropyl ammonium hydroxide 20%), stir 30 minutes, add MFI 360 grams of zeolite seed crystals (200 nanometers) were stirred for 8 hours, then the stirring was continued, the temperature of the crystallization kettle was raised to 160° C., and the crystallization was carried out for 28 hours. The product was taken out, filtered, washed with deionized water until neutral, and dried at 120°C for 6 hours to obtain high-silicon MFI zeolite powder 1. The properties of the powder are shown in Table 1.

[0033] Weigh 1.0 kg of powder 1, 0.030 kg of carboxymethyl cellulose, mix the above powder evenly, add 0.15 kg of water glass containing 10% sodium silicate in weight percentage, roll into a ball, and sieve the formed silicon ball , select 16-40 mesh silicon balls, ...

Embodiment 2

[0039] Take ethyl silicate (by weight percent, containing 28.8% SiO 2 ) 12.5 kilograms, in 30 liters of reactors, add 9.0 kilograms of tetrapropylammonium bromide (TPABr) solids, add 19.5 kilograms of water, add 4.8 kilograms of sodium hydroxide (solids), stir 30 minutes, add MFI zeolite crystal seed ( 200 nanometers) 360 grams, after continuing to stir for 8 hours, continue to stir, raise the temperature of the crystallization kettle to 140°C, and crystallize for 48 hours. The product was taken out, filtered, washed with deionized water until neutral, and dried at 120°C for 6 hours to obtain high-silicon MFI zeolite powder 2. The properties of the powder are shown in Table 1.

[0040] Weigh 1.0 kg of powder 2 and 0.02 kg of methyl cellulose, mix the above powder evenly, add 0.30 kg of water glass containing 10% sodium silicate in percentage by weight, roll into a ball, and sieve the formed silicon ball. Select 20-40 mesh silicon balls, that is, the adhesive-containing adsorb...

Embodiment 3

[0043] Weigh silica gel (SiO 2 ) 3.6 kg, in a 160-liter reactor, add 1.62 kg of ethylenediamine, add 108 kg of water, add 4.8 kg of sodium hydroxide (solid), stir for 30 minutes, then add 360 grams of MFI zeolite seed crystals (200 nanometers), continue After stirring for 8 hours, continue stirring, raise the temperature of the crystallization tank to 170° C., and crystallize for 28 hours. The product was taken out, filtered, washed with deionized water until neutral, and dried at 120°C for 6 hours to obtain high-silicon MFI zeolite powder 3. The properties of the powder are shown in Table 1.

[0044] Weigh 1.0 kg of powder 3, 0.10 kg of hydroxymethyl cellulose, mix the above powder evenly, add 0.03 kg of water glass containing 10% sodium silicate by weight percentage, roll into a ball, and sieve the formed silicon ball , select 16-30 mesh silicon balls, that is, the adhesive-containing adsorbent; the adhesive is transformed into a crystal, and the adhesive-containing adsorbe...

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Abstract

The invention relates to a binder-free high-silicon MFI zeolite adsorbent and a preparation method thereof, which mainly solves the problems in the prior art that the adsorbent has small adsorption capacity for PX in mixed xylene C8, low adsorption rate and poor separation effect . The present invention uses silicon adhesive to add high-silicon MFI powder with specific particle size distribution to form and transform crystals to prepare a binder-free high-silica zeolite adsorbent. The particle size of the adsorbent is 16-40 mesh, and at room temperature, the solid-to-liquid ratio is 3: At 5 o'clock, the adsorption capacity of p-xylene in 1,3,5-trimethylbenzene solution containing 10% p-xylene in weight percentage is greater than 0.102 g / g adsorbent, p-xylene, p-ethylbenzene, and o- and m-xylene The technical scheme that the selectivity coefficient of xylene is greater than 9.0, and the initial 3-minute adsorption rate is greater than 22 mg / g adsorbent / min solves the above technical problems well, and can be used for the separation of p-xylene in C8 aromatics.

Description

technical field [0001] The invention relates to a binder-free high-silicon MFI zeolite adsorbent and a preparation method thereof. Background technique [0002] Mixed xylene (C8) is mainly composed of p-xylene, o-xylene, m-xylene and ethylbenzene. Mixed C8 aromatics mainly come from catalytic reforming, gasoline cracking and other production processes. It is o-xylene (OX), m-xylene A mixture of xylene (MX), para-xylene (PX) and ethylbenzene (EB). In the past two decades, with the rapid development of the polyester industry, the market demand for p-xylene at home and abroad has increased rapidly. Since the boiling points of the four main components in C8 aromatics are very close, especially the difference between the boiling points of m-xylene and p-xylene is only 0.75°C, high-purity p-xylene cannot be obtained by traditional distillation methods. [0003] The industrial methods for separating high-purity PX mainly include adsorption separation and freeze crystallization. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/18B01J20/30
Inventor 钱斌孔德金刘仲能姜向东王德举余强王辉黄琴琴
Owner CHINA PETROLEUM & CHEM CORP