Porous material and its synthesis method

Abstract

A process material with compound artery is prepared from the Si source chosen from amorphous SiO2, si sol, silicon oxide solid, silicon gel, diatomite and water glass, the Al source chosen from sodium aluminate, sodium metaaluminate, aluminium sulfate, aluminium nitrate, etc, at least one of lithium hydroxide, sodium hydroxide, potassium hydroxide, rubidium hydroxide and cesium hydroxide, and template agent through proportional mixing, reaction, ageing and crystallizing.

Description

technical field

[0001] The invention relates to a porous material and a synthesis method thereof. Background technique

[0002] In industry, porous materials are widely used as catalysts and catalyst supports. Porous materials can be divided into three categories: Microporous (<2nm), Mesoporous (2-50nm) and Macroporous (>50nm). Porous materials have relatively high specific surface area and smooth pore structure, so they are good catalytic materials or catalyst supports.

[0003] Microporous materials such as zeolites can only be used as small molecule adsorbents or catalysts due to their small pore size. The basic framework structure of crystalline microporous zeolites is based on the rigid three-dimensional TO 4 (SiO 4 , AlO 4 etc.) unit structure; in this structure TO 4 Oxygen atoms are shared in a tetrahedral manner, and the skeleton tetrahedron such as AlO 4 The charge balance of is through surface cations such as Na + , H + ...

Examples

Embodiment 1

[0019] Sodium aluminate (Al 2 o 3 42.0% by weight) 16.0 grams are dissolved in 180 grams of water, add 8.0 grams of sodium hydroxide and make it dissolve, then add n-hexadecylamine R under the condition of stirring 1 120.5 g, tetrapropylammonium hydroxide R 2 40 g and cetyltrimethylammonium bromide R 3 7.3 grams, then add silica sol (SiO 2 40% by weight) 300 grams, after stirring evenly, aging at 40°C for 72 hours. The reactant mixture is in molar ratio: SiO 2 / Al 2 o 3 =30,OH - / SiO 2 = 0.1, R 1 / SiO 2 =0.25,R 2 / SiO 2 =0.10,R 3 / SiO 2 =0.01,H 2 O / SiO 2 =10. Then put it into a stainless steel reaction kettle, and crystallize at 175°C for 5 hours under agitation. After taking out, it is filtered, washed and dried. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 28.6. The specific surface area is 550 meters 2 / gram. In terms of volume percentage, the macropores of 0.1 to 10 microns account for 57.4%, the micropores of 0.4 to 2...

Embodiment 2

[0021] Sodium metaaluminate (Al 2 o 3 40% by weight) 6.07 grams are dissolved in 468 grams of water, add 48 grams of sodium hydroxide and make it dissolve, then add hexamethyleneimine R under stirring condition 4 79.2 g and cetyltrimethylammonium bromide R 3 7.3 grams, then add silica sol (SiO 2 40% by weight) of 300 grams, after stirring evenly, aged at 80° C. for 120 hours. The reactant mixture is in molar ratio: SiO 2 / Al 2 o 3 =80,OH - / SiO 2 =0.6,R 4 / SiO 2 = 0.4, R 3 / SiO 2 =0.01,H 2 O / SiO 2 =18. Then put it into a stainless steel reaction kettle, and crystallize at 150° C. for 50 hours under agitation. After taking out, it is filtered, washed and dried. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 76.6. The specific surface area is 420 meters 2 / gram. In terms of volume percentage, the macropores of 0.1 to 10 microns account for 84.4%, the micropores of 0.4 to 2 nanometers account for 15.6%, and the total pore volume is...

Embodiment 3

[0023] Dissolve 21.3 grams of aluminum nitrate in 612 grams of water, add 48 grams of sodium hydroxide to dissolve it, and then add hexamethyleneimine R under stirring 4 79.2 g and cetyltrimethylammonium bromide R3 14.6 grams, then add silica sol (SiO 2 40% by weight) 300 grams, 30 grams of seed crystals, after stirring evenly, age at 50° C. for 2 hours. The reactant mixture is in molar ratio: SiO 2 / Al 2 o 3 =40,OH - / SiO 2 =0.6,R 4 / SiO 2 = 0.4, R 3 / SiO 2 =0.02,H 2 O / SiO 2 =22. Then put it into a stainless steel reaction kettle, and crystallize at 160°C for 15 hours under agitation. After taking out, it is filtered, washed and dried. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 42.5. The specific surface area is 435 meters 2 / gram. In terms of volume percentage, the macropores of 0.1-10 micrometers account for 76.0%, and the micropores of 0.4-2 nanometers account for 29.0%. XRD analysis presents a specific zeolite structure. ...

technical field

[0001] The invention relates to a porous material and a synthesis method thereof. Background technique

[0002] In industry, porous materials are widely used as catalysts and catalyst supports. Porous materials can be divided into three categories: Microporous (<2nm), Mesoporous (2-50nm) and Macroporous (>50nm). Porous materials have relatively high specific surface area and smooth pore structure, so they are good catalytic materials or catalyst supports.

[0003] Microporous materials such as zeolites can only be used as small molecule adsorbents or catalysts due to their small pore size. The basic framework structure of crystalline microporous zeolites is based on the rigid three-dimensional TO 4 (SiO 4 , AlO 4 etc.) unit structure; in this structure TO 4 Oxygen atoms are shared in a tetrahedral manner, and the skeleton tetrahedron such as AlO 4 The charge balance of is through surface cations such as Na + , H + ...

Examples

Embodiment 1

[0019] Sodium aluminate (Al 2 o 3 42.0% by weight) 16.0 grams are dissolved in 180 grams of water, add 8.0 grams of sodium hydroxide and make it dissolve, then add n-hexadecylamine R under the condition of stirring 1 120.5 g, tetrapropylammonium hydroxide R 2 40 g and cetyltrimethylammonium bromide R 3 7.3 grams, then add silica sol (SiO 2 40% by weight) 300 grams, after stirring evenly, aging at 40°C for 72 hours. The reactant mixture is in molar ratio: SiO 2 / Al 2 o 3 =30,OH - / SiO 2 = 0.1, R 1 / SiO 2 =0.25,R 2 / SiO 2 =0.10,R 3 / SiO 2 =0.01,H 2 O / SiO 2 =10. Then put it into a stainless steel reaction kettle, and crystallize at 175°C for 5 hours under agitation. After taking out, it is filtered, washed and dried. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 28.6. The specific surface area is 550 meters 2 / gram. In terms of volume percentage, the macropores of 0.1 to 10 microns account for 57.4%, the micropores of 0.4 to 2...

Embodiment 2

[0021] Sodium metaaluminate (Al 2 o 3 40% by weight) 6.07 grams are dissolved in 468 grams of water, add 48 grams of sodium hydroxide and make it dissolve, then add hexamethyleneimine R under stirring condition 4 79.2 g and cetyltrimethylammonium bromide R 3 7.3 grams, then add silica sol (SiO 2 40% by weight) of 300 grams, after stirring evenly, aged at 80° C. for 120 hours. The reactant mixture is in molar ratio: SiO 2 / Al 2 o 3 =80,OH - / SiO 2 =0.6,R 4 / SiO 2 = 0.4, R 3 / SiO 2 =0.01,H 2 O / SiO 2 =18. Then put it into a stainless steel reaction kettle, and crystallize at 150° C. for 50 hours under agitation. After taking out, it is filtered, washed and dried. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 76.6. The specific surface area is 420 meters 2 / gram. In terms of volume percentage, the macropores of 0.1 to 10 microns account for 84.4%, the micropores of 0.4 to 2 nanometers account for 15.6%, and the total pore volume is...

Embodiment 3

[0023] Dissolve 21.3 grams of aluminum nitrate in 612 grams of water, add 48 grams of sodium hydroxide to dissolve it, and then add hexamethyleneimine R under stirring 4 79.2 g and cetyltrimethylammonium bromide R3 14.6 grams, then add silica sol (SiO 2 40% by weight) 300 grams, 30 grams of seed crystals, after stirring evenly, age at 50° C. for 2 hours. The reactant mixture is in molar ratio: SiO 2 / Al 2 o 3 =40,OH - / SiO 2 =0.6,R 4 / SiO 2 = 0.4, R 3 / SiO 2 =0.02,H 2 O / SiO 2 =22. Then put it into a stainless steel reaction kettle, and crystallize at 160°C for 15 hours under agitation. After taking out, it is filtered, washed and dried. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 42.5. The specific surface area is 435 meters 2 / gram. In terms of volume percentage, the macropores of 0.1-10 micrometers account for 76.0%, and the micropores of 0.4-2 nanometers account for 29.0%. XRD analysis presents a specific zeolite structure. ...

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