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Exchange modification method for reducing content of sodium oxide in beta-type molecular sieve

A molecular sieve, sodium oxide technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of difficult implementation, ammonia nitrogen pollution, difficulty and so on

Active Publication Date: 2012-11-28
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Visible, K + The exchange capacity is strong, and the Na in the zeolite can be easily exchanged + , but since K + The exchange capacity of NH is stronger than that of NH 4 + , use the ammonium salt to further exchange the K that has been exchanged to the zeolite + Obviously it is more difficult, and the exchanged K + It needs to be further exchanged by subsequent ammonium salts before zeolite can be used for catalytic cracking
This method is difficult to implement in industry, and needs to be exchanged with ammonium salt, and there is still the problem of ammonia nitrogen pollution

Method used

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  • Exchange modification method for reducing content of sodium oxide in beta-type molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 12.8 grams of citric acid, add an appropriate amount of cold water and stir to dissolve it, then add 5.07 grams of 36% by weight hydrochloric acid, then continue to add cold water to dilute the solution to 1000ml to form a low-concentration mixed acid, control the solution temperature: 2 ± 0.5 ° C, at During stirring, add 143 grams of Naβ molecular sieve former powder dry basis (in the molecular sieve exchange liquid, H 2 O: the weight ratio of molecular sieve raw powder dry basis=7:1), then stirred and reacted at 2±0.5°C for 1.5 hours, then filtered the slurry, and the filter cake was drenched with deionized water 5 times the dry basis weight of Naβ molecular sieve raw powder Wash and dry to obtain a β-molecular sieve sample exchanged once with a low-temperature acidic solution, which is denoted as S1. Its properties and exchange water consumption are shown in Table 1.

Embodiment 2

[0021] Weigh 10.1 grams of oxalic acid, add an appropriate amount of cold water and stir to dissolve it, then add 15.75 grams of nitric acid with a concentration of 20% by weight, then continue to add cold water to dilute the solution to 1000 ml to form a low-concentration mixed acid, control the solution temperature: 1 ± 0.5 ° C, Add 133 grams of Naβ molecular sieve former powder dry base (in the molecular sieve exchange liquid, H 2O: the weight ratio of molecular sieve raw powder dry basis=7.5:1), then stirred and reacted at 1±0.5°C for 2 hours, then filtered the slurry, and the filter cake was drenched with deionized water 5 times the dry basis weight of Naβ molecular sieve raw powder Wash and dry to obtain a β-molecular sieve sample exchanged once with a low-temperature acidic solution, which is denoted as S2. Its properties and exchange water consumption are shown in Table 1.

Embodiment 3

[0023] Weigh 6.9 grams of acetic acid, add an appropriate amount of cold water and stir to dissolve it, then add 3.92 grams of phosphoric acid with a concentration of 50% by weight, then continue to add cold water to dilute the solution to 1000 ml to form a low-concentration mixed acid, control the solution temperature: 3 ± 0.5 ° C, Add Naβ molecular sieve former powder dry base 167 grams (in the molecular sieve exchange liquid, H 2 O: the weight ratio of molecular sieve raw powder dry basis=6:1), then stirred and reacted at 3±0.5°C for 2 hours, then filtered the slurry, and the filter cake was drenched with deionized water 5 times the dry basis weight of Naβ molecular sieve raw powder Wash and dry to obtain a β molecular sieve sample exchanged once with a low-temperature acidic solution, which is denoted as S3. Its properties and exchange water consumption are shown in Table 1.

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Abstract

The invention discloses an exchange modification method for reducing the content of sodium oxide in a beta-type molecular sieve. The exchange modification method is characterized by comprising the following steps of contacting the molecular sieve of which the content of Na is relatively high and an aqueous solution containing inorganic acid and organic acid at the temperature of 0 to 5 DEG C for 0.5 to 2 hours; and separating, washing and drying to obtain the exchanged molecular sieve, wherein the weight ratio of H2O to the molecular sieve is (2.5-7.5):1. By the exchange modification method, the content of Na2O in the beta-type molecular sieve of which the content of the Na is relatively high can be reduced from 2.6 weight percent to less than 0.4 weight percent at one time, so that the actual requirement of industrial production is met; the relative crystallinity of the molecular sieve is not increased; the nitrogen-ammonia pollution is eliminated at the source; and water consumption in the molecular sieve exchange process is obviously reduced.

Description

technical field [0001] The invention relates to a method for reducing the content of sodium oxide in β-type molecular sieves. More precisely, it is a molecular sieve exchange modification method involving the use of low-temperature mixed acid to exchange molecular sieves to eliminate ammonia nitrogen pollution and reduce the content of sodium oxide in β-type molecular sieves. Background technique [0002] β molecular sieve was synthesized by the classic hydrothermal crystallization method for the first time in 1967 (Wadlinger R.L, Kerr G.T, Rosinski E.J.US 3308069). The zeolite has a unique three-dimensional pore structure and high catalytic activity for hydrocracking and hydroisomerization. After modification or loading of certain metal components, it can be used for catalytic cracking, hydrocracking, hydroisomerization, and In petroleum refining and petrochemical processes such as hydrogen refining, hydrodewaxing, diesel oil decondensation, etc. [0003] However, in the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02
Inventor 周灵萍张蔚琳李峥许明德朱玉霞田辉平
Owner CHINA PETROLEUM & CHEM CORP
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