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A method for removing organic amine templates in borosilicate β molecular sieves

A technology of beta molecular sieve and template agent, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of large loss of crystallinity, poor structural stability of borosilicate beta molecular sieve, ineffective removal, etc. The effect of surface area

Active Publication Date: 2018-04-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, compared with silica-alumina β-molecular sieve, borosilicate β-molecular sieve raw powder contains more templates, and the structural stability of borosilicate β-molecular sieve is worse
Either the above method cannot effectively remove the template agent in the borosilicate β molecular sieve, or the loss of crystallinity is large

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0024] Preparation of borosilicate β molecular sieves.

[0025] 1.0g of borax, 1.1g of sodium hydroxide and 104.7g of tetraethylammonium hydroxide solution with a concentration of 25% by mass were mixed evenly, and then 20g of ultrafine silicon dioxide (produced by Cabot Company, brand name CAB-O-SILM-5) was added. ), stirred evenly, moved into the reaction kettle, crystallized at 140°C for 15 days, cooled rapidly to 40°C after the crystallization was completed, and after the product was centrifuged and washed, the obtained solid was dried at 90°C for 10 hours to obtain borosilicate β molecular sieve powder S 0 , its anhydrous chemical composition (based on oxide molar ratio) is: 0.5Na 2 O·B 2 o 3 22SiO2 2 . The original powder was used as the standard sample, and its relative crystallinity was set as 100%. The characterization data are shown in Table 1.

example 2

[0027] (1) Three-stage roasting

[0028] The S prepared by 10g example 1 0 Molecular sieves were dried at 120°C for 12 hours. In an air atmosphere, the temperature was raised to 180°C at a rate of 5°C / min, calcined for 2 hours, and then heated to 260°C at a rate of 5°C / min for 2 hours, and then heated at a rate of 10°C / min. The heating rate was raised to 420°C for 4 hours.

[0029] (2) Oxidation treatment

[0030] Take 5g (1) step roasted powder, 5g perchloric acid, and 20ml deionized water into the hydrothermal reaction kettle, let it stand at 140°C for 12h, cool to 25°C, the product is separated by centrifugation, and the obtained solid is deionized Wash with water for 3 to 5 times, dry at 120°C for 12 hours, and obtain borosilicate molecular sieve S with organic amine template removed 1 , and its characterization data are shown in Table 1.

example 3

[0032] Remove borosilicate β molecular sieve S by the method for example 2 0 The organic amine template in (1) is different from the molecular sieve S 0 After drying at 120°C for 12 hours, three-stage calcination in a nitrogen atmosphere, and then oxidation treatment according to step (2), the obtained borosilicate molecular sieve S with organic amine template removed 2 The characterization data are shown in Table 1.

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PUM

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Abstract

A method for removing an organic amine template in a borosilicate β molecular sieve, comprising drying the borosilicate β molecular sieve, roasting in air or nitrogen at 150 to 420°C in sections, and then reacting in an aqueous solution of an oxidizing agent. After the reaction, The obtained solid is washed and dried, and the oxidizing agent is selected from one or more of perchloric acid, hypochlorous acid, perchlorate and hypochlorite, and the mass ratio of the oxidizing agent to borosilicate β molecular sieve is 0.5~ 2.0. The method is simple to operate and can effectively remove the template agent in the borosilicate β molecular sieve.

Description

technical field [0001] The invention relates to a method for removing an organic amine template in a molecular sieve, in particular to a method for removing an organic amine template in a β molecular sieve. Background technique [0002] Borosilicate molecular sieve is a kind of silicon-aluminum heteroatom molecular sieve, that is, a molecular sieve in which the aluminum on the framework of the silicon-alumina molecular sieve is completely replaced by boron atoms. Borosilicate β molecular sieves are usually hydrothermally synthesized in a system containing organic templates. Commonly used templates include tetraethylammonium hydroxide, tetraethylammonium bromide or their mixtures, and other organic amine compounds. Separating the organic template from the inorganic framework of the molecular sieve is an essential step to obtain unobstructed pores and increase the specific surface area before the molecular sieve is used as an adsorbent or catalyst. The commonly used method fo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 王嘉欣马爱增张大庆臧高山张玉红王涛
Owner CHINA PETROLEUM & CHEM CORP
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