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Mordenite preparation method

A technology of mordenite and pseudo-boehmite, which is applied in the direction of crystalline aluminosilicate zeolite, can solve the problems of unreported mordenite, high yield of unreported mordenite, specific surface area, acid density and catalytic activity reduction, etc. To achieve the effect of enriching acid center density, increasing crystallinity and improving activity

Active Publication Date: 2012-06-20
山东荣创催化新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although it has been reported that gelatinized starch has been used as the template to make the resulting mordenite than the crystallinity of the TEA template product can be increased by 10% to 30%, as described in CN100364889C, but due to the relatively high silicon-aluminum ratio of its product, and further During the process of roasting to remove the starch in the pores, it will further dealuminate and lose part of the skeleton structure, resulting in a decrease in its specific surface area, acid density and catalytic activity.
How to obtain high crystallinity and acid density, the preparation of large surface area mordenite has not been reported in the prior art, and green zeolite that does not use organic additives, high yield and mother liquor circulation to reduce emissions in the prior art has not been reported , efficient preparation method

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0033] This example is to illustrate the preparation process of mordenite provided by the present invention without mother liquor circulation.

[0034] Add 3.5 grams of 37 weight percent concentrated hydrochloric acid (chemically pure, Beijing Reagent Company) in 1 liter of chemical water and stir evenly, add pseudo-boehmite powder (industrial product, produced by China Aluminum Corporation Shandong Aluminum Factory, solid content 66.1 weight percent) ) 121 grams and stirred for 30 minutes, added silica gel (industrial products, produced by Qingdao Ocean Chemical Co., Ltd., 99.7 weight percent of silicon dioxide, 0.18 weight percent of sodium oxide, 0.085 weight percent of calcium oxide, 92.7 weight percent of solid content) 600 grams, and then Rinse with about 220ml of water, stir well and dry at 120°C / 2 hours. The chemical composition is: 13.2% by weight of aluminum oxide, 0.16% by weight of sodium oxide, 0.40% by weight of chlorine, and 87.6% by weight of solid content.

...

Embodiment 2

[0038] This example is to illustrate the preparation process of mordenite provided by the present invention under the mode of mother liquor circulation.

[0039] Get 650 milliliters of crystallization mother liquors obtained in Example 1, add 131 grams of sodium hydroxide (chemically pure reagent, Beijing Reagent Company, 95% by weight) and 11 grams of sodium chloride (same as above) and stir to make it dissolve, then add according to implementation 650 g of the silicon-aluminum mixture prepared in the manner of Example 1 was stirred at room temperature for 4 hours, crystallized at 120° C. for about 10 hours, and then crystallized at 200° C. for 65 hours.

[0040] The X-ray diffraction pattern of embodiment 2 sample sees specification sheet appendix figure 2 , sodium oxide 7.9% by weight, silicon-aluminum molar ratio 10.9, grain size distribution range of 10-20 microns.

Embodiment 3

[0042] This example provides the process of preparing mordenite by using the mother liquor after multiple cycles in the present invention.

[0043] Get 650 milliliters of crystallization mother liquors obtained after 10 synthetic crystallization cycles, add 130 grams of sodium hydroxide (same as above) and 10 grams of sodium chloride (same as above) and stir to make it dissolve, then add the prepared by the method of embodiment 1 650 g of the silicon-aluminum mixture was stirred at room temperature for 6 hours, crystallized at 120°C for about 12 hours, and then crystallized at 200°C for 49 hours.

[0044] The X-ray diffraction pattern of embodiment 3 samples and description attached figure 2 Similarly, the sodium oxide is 7.9% by weight, the molar ratio of silicon to aluminum is 10.9, and the grain size distribution range is 10-20 microns.

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Abstract

A mordenite preparation method is characterized in that after being reacted with diluted hydrochloric acid according to molar ratio of HCl / Al203 ranging from 0.04 to0.05 and molar ratio of H2O / Al203 ranging from 70-75, pseudo-boehmite is added into silica gel powder according to silicon to aluminum molar ratio ranging from 11.0 to 12.5 to realize pulping, uniform mixing and drying, then mixture is added into liquor mixture added with crystallized mother liquor, sodium chloride and sodium hydroxide according to molar ratio of Na2O / SiO2 ranging from 0.25 to 0.30, molar ratio of H2O / Na2O rangingfrom 25.0 to 30.0 and molar ratio of Cl / Al203 ranging from 0.4 to 0.5 and is stirred for 1 hour to 8 hours, and then two sections of thermal crystallization are realized at the temperature of 120 DEGC for 8 hours to 14 hours and at the temperature of 200 DEG C for 36 hours to 72 hours; and mordenite with the grain size ranging from 10 micrometers to 20 micrometers, silicon to aluminum molar ratio ranging from 11.0 to12.0 and a pure MOR (mordenite) structure is prepared. Compared with a conventional product, the mordenite prepared by the method has the advantages that crystallinity is improved by 30%, Langmuir specific surface area is larger than or equal to 400 square meters per gram, the mordenite is extremely rich in acid site density, and activity is improved when the mordenite is used in catalyst. In addition, any organic additives are not added in a preparation process, yield of a single kettle is high, the mother liquor can be recycled, emission is reduced, and the mordenite preparation method belongs to clean, high-efficiency, safe and green preparation technology.

Description

technical field [0001] The invention relates to a preparation method of mordenite, more precisely, relates to a high-efficiency and green preparation method of mordenite with high crystallinity, acid density and large specific surface area. Background technique [0002] Mordenite is a molecular sieve with MOR structure (zeolite molecular sieve structure symbol recommended by International Union for Pure and Applied Chemistry), which contains eight-membered ring and twelve-membered ring channels, and has good heat resistance, acid resistance and water vapor resistance. It has been widely used as an adsorbent for separating gases and liquids, as well as in catalytic cracking, hydrocarbon isomerization, alkylation, aromatics disproportionation, transalkylation, lipidation and etherification of alcohols, dewaxing and pour point reduction, and olefin selection Hydrogenation, reforming and other petrochemical processes, especially in the industrial catalysts of toluene disproporti...

Claims

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Application Information

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IPC IPC(8): C01B39/02
Inventor 王淑瑜陈谱忠曲令多
Owner 山东荣创催化新材料有限公司
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