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Method for performing ion exchange on molecular sieve containing exchangeable ions

A technology of ion exchange and ion exchange, applied in chemical instruments and methods, semi-permeable membrane separation, membrane technology, etc., can solve problems such as high cost, complicated operation, and high energy consumption of the process, so as to reduce usage and improve economic benefits , the effect of reducing pollution

Active Publication Date: 2013-06-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The main problem of the ammonium exchange method is: in the molecular sieve production process, the molecular sieve raw powder needs to be exchanged with ammonium to make NH 4 Type molecular sieves, which can be converted into hydrogen type molecular sieves by high-temperature roasting
During the ammonium exchange process, due to the NH 4 + There is a concentration gradient and Na in the molecular sieve + Position Limits, NH 4 + Cannot completely replace Na at one time + , so in order to get low Na 2 For molecular sieves with O content, the ammonium exchange process needs to be repeated many times, making this process produce a large amount of ammonium nitrogen wastewater exceeding the standard
In order to meet the national sewage discharge standard GB 8978-1996, which stipulates that the ammonium nitrogen discharge is less than 15mg / L, catalyst plants generally use alkali in wastewater, and then strip NH 3 process to treat the wastewater, but the process consumes a lot of energy, is complicated to operate and has high costs

Method used

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  • Method for performing ion exchange on molecular sieve containing exchangeable ions
  • Method for performing ion exchange on molecular sieve containing exchangeable ions
  • Method for performing ion exchange on molecular sieve containing exchangeable ions

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] 100g of NH 4 NaY molecular sieve (Na 2 The O content is 4.3% by weight, the silicon-alumina ratio is 5, and the relative crystallinity is 90.3%) and 1000 g of water are stirred evenly, and the temperature is raised to 95°C. 20 g of an aqueous solution of 90% by weight of ammonium hexafluorosilicate was added, and the mixture was treated at 95° C. for 2 hours to obtain a molecular sieve slurry with a high silicon-to-aluminum ratio. The SiO of the molecular sieve with high silicon-aluminum ratio 2 and Al 2 O 3 The molar ratio was 12, and the relative crystallinity was 95%.

[0065] The above-mentioned high silicon-aluminum ratio molecular sieve slurry was filtered to obtain 300 g of solid phase (the weight ratio of molecular sieve to water was 1:2) and 800 g of liquid phase containing high silicon-aluminum ratio molecular sieve. Add 4 g of Na to the liquid phase 2 SO 4 , and fill the liquid phase into the acid chamber storage tank of the bipolar membrane electrodia...

Embodiment 2

[0067] Put 200g of NH 4 NaY molecular sieve (Na 2 O content is 3.5 wt%, silicon-aluminum ratio is 5, relative crystallinity is 90%) and 15 g of rare earth chloride, treated at 90 °C for 1 hour, and calcined at 550 °C for 2 hours to obtain a high silicon-aluminum ratio. Molecular Sieve. The SiO of the molecular sieve with high silicon-aluminum ratio 2 and Al 2 O 3 The molar ratio was 11, and the relative crystallinity was 56.0%.

[0068] Weigh 100g of the molecular sieve with the above-mentioned high silicon-aluminum ratio and stir well with 1000g of deionized water to obtain the slurry of the molecular sieve, filter, and obtain 400g of the solid phase containing the high-silicon-aluminum ratio molecular sieve (the weight ratio of molecular sieve and water is 1:3) and 700g of liquid phase. 3.8 g of Na were added to the liquid phase 2 SO 4 , and fill the liquid phase into the acid chamber storage tank of the bipolar membrane electrodialyzer, and at the same time add 1000...

Embodiment 3

[0070] 200g of NaX (Na 2 The O content is 11.6 wt%, the silicon-aluminum ratio is 1.26, and the relative crystallinity is 81.3%) and 15 g of rare earth chloride were treated at 90 °C for 1 hour, and calcined at 550 °C for 2 hours to obtain a high silicon-aluminum ratio molecular sieve . The Si / Al ratio of the high silicon-aluminum ratio molecular sieve is 10, and the relative crystallinity is 76.2%.

[0071] Weigh 100g of the molecular sieve with the high silicon-aluminum ratio and 1000g of deionized water and stir to obtain the slurry of the molecular sieve, filter, and obtain 300g of the solid phase of the molecular sieve containing the high silicon-to-aluminum ratio (the weight ratio of molecular sieve and water is 1:2) and 800g of liquid phase. Add 5 g of Na to the liquid phase 2 SO 4 , and fill the liquid phase into the acid chamber storage tank of the bipolar membrane electrodialyzer, and at the same time add 1000 g of deionized water to the alkali chamber storage ta...

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Abstract

The invention provides a method for performing ion exchange on a molecular sieve containing exchangeable ions. The method comprises the following steps of: performing dealumnization and / or silicon reinsertion on the molecular sieve containing the exchangeable ions to obtain a molecular sieve with high ratio of silicate to aluminum; performing bipolar membrane electrodialysis on ion-containing solution to obtain acid liquor; contacting the molecular sieve with high ratio of silicate to aluminum and the acid liquor and performing ion exchange to obtain slurry of the molecular sieve which is subjected to ion exchange; performing solid-liquid separation on the slurry of the molecular sieve which is subjected to ion exchange to obtain a solid phase and a liquid phase; and circulating the liquid phase obtained through solid-liquid separation to serve as ion-containing solution in the step of bipolar membrane electrodialysis, wherein the content of negative ions in the ion-containing solution in the step of bipolar membrane electrodialysis is 0.01 to 10 mol / L. Zero emission of waste liquid is realized by the method, ions for ion exchange are not needed to be added and the molecular sievewith high crystallinity can be obtained.

Description

technical field [0001] The invention relates to a method for performing ion exchange on a molecular sieve containing exchangeable ions, in particular to a method for performing ion exchange on a molecular sieve containing exchangeable ions in a clean and low-cost manner. Background technique [0002] Molecular sieves are widely used in catalytic cracking, hydrocracking, isomerization and other oil refining processes as catalyst active components or catalyst supports. Synthetic molecular sieves are usually Na-type molecular sieves, while Na + The presence of has a great influence on the activity of the molecular sieve, the Na in the MgHY molecular sieve + When the content is reduced from 1.1% by weight to 0.1% by weight, the activity of the MgHY molecular sieve can be increased by about 100 times. For general industrial catalysts, Na in molecular sieves + The content is required to be below 0.25% by weight. Therefore, the molecular sieve synthesized at one time needs to b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D61/44
Inventor 周丽娜罗一斌刘中清舒兴田
Owner CHINA PETROLEUM & CHEM CORP