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High-silicon MFI zeolite adsorbent without adhesive and preparation method thereof

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

Active Publication Date: 2014-11-19
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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  • High-silicon MFI zeolite adsorbent without adhesive and preparation method thereof
  • High-silicon MFI zeolite adsorbent without adhesive and preparation method thereof

Examples

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Effect test

Embodiment 1

[0031] Weigh silica sol (by weight percentage, containing 40%SiO 2 ) 9.0 kg, in a 30-liter reactor, add 9.0 kg of tetrapropylammonium hydroxide (TPAOH) solution (by weight percent, containing 20% ​​tetrapropylammonium hydroxide), stir for 30 minutes, then add MFI 360 grams of zeolite seed crystals (200 nanometers), continued to stir for 8 hours, then continued to stir, raised the temperature of the crystallization kettle to 160° C., and crystallized 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.

[0032] 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 by weight percentage, roll into a ball, and sieve the formed silicon ball , select 16-40 mesh silicon balls, that is, the adhesive-containing adsorbent; the...

Embodiment 2

[0039] Weigh ethyl silicate (by weight percent, containing 28.8%SiO 2 ) 12.5 kg, in a 30-liter reactor, add 9.0 kg of tetrapropylammonium bromide (TPABr) solid, add 19.5 kg of water, add 4.8 kg of sodium hydroxide (solid), stir for 30 minutes, and then add MFI zeolite seed ( 200 nanometers) 360 grams, continue 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, 0.02 kg of methyl cellulose, mix the above powder evenly, add 0.30 kg of water glass containing 10% sodium silicate in weight percentage, roll into a ball, and sieve the formed silicon ball. Select 20-40 mesh silicon balls, that is, the adhesive-containing adsorbent; the adhesive is transformed into a cr...

Embodiment 3

[0044] 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 g 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.

[0045] 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 adsorbent i...

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Abstract

The invention relates to a high-silicon MFI zeolite adsorbent without adhesive and a preparation method thereof, which mainly aim at solving the problems of small adsorption capacity of an adsorbent for PX in mixed xylene C8, as well as low adsorption rate and poor separation effect in the prior art. The high-silicon zeolite adsorbent without adhesive is prepared through the steps of adding high-silicon MFI powder in specific grain size distribution into a silicon adhesive for forming and performing crystal transformation, wherein the grain size of the adsorbent is 16-40 meshes; at room temperature, when a solid-liquid ratio is 3 to 5, the adsorption capacity of per gram of adsorbent for p-xylene in a 1,3,5-trimethylbenzene solution containing 10% of p-xylene based on weight percent is greater than 0.102g, the selectivity coefficient of p-xylene for ethylbenzene, o-xylene and m-xylene is higher than 9.0, and within initial three minutes, the adsorption rate of the per gram of adsorbent for p-xylene is greater than 22mg / minute. By virtue of the technical scheme, the technical problems are well solved and the high-silicon MFI zeolite adsorbent without adhesive can be used for separation of p-xylene in C8 arene.

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 Applications(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
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