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KL molecular sieve and morphology regulation synthesis method thereof

A synthesis method and technology of molecular sieves, applied in the field of molecular sieves, can solve the problems of increased production costs of KL molecular sieves, and achieve the effects of synthesis and cost advantages, high yield and low synthesis cost

Active Publication Date: 2021-12-07
CHEM & CHEM ENG GUANGDONG LAB
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, if organic alcohols or amines are used as structure-directing agents, the production cost of KL molecular sieves will increase, and high-temperature roasting is required to remove the structure-directing agents.

Method used

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  • KL molecular sieve and morphology regulation synthesis method thereof
  • KL molecular sieve and morphology regulation synthesis method thereof
  • KL molecular sieve and morphology regulation synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Weigh 13.66g KOH and dissolve in appropriate amount of water, then weigh 4.50g Al(OH) 3 Add, stir and heat to reflux in a three-necked flask until Al(OH) 3 Dissolve completely to make the solution clear; after the solution is cooled, transfer it to a beaker, add 8.82g KCl and the remaining water and stir evenly, then weigh 68.11g of silica sol (SiO 2 content 30wt.%) was slowly added dropwise to the above solution, stirred and aged at room temperature for 20 hours to obtain a synthetic liquid of KL molecular sieve, and the molar ratio of each material in the synthetic liquid was 4.0KCl: 3.5K 2 O: 11.5SiO 2 : 1.0Al 2 o 3 : 292.65H 2 O. Transfer the above synthetic solution to a polytetrafluoroethylene-lined crystallization kettle, and conduct static hydrothermal crystallization at 175°C for 24 hours. The resulting product is filtered by suction, washed with deionized water until neutral, and then dried at 120°C for 24 hours to obtain KL molecular sieve. Raw powder, ...

Embodiment 2

[0039] Weigh 13.66g KOH and dissolve in appropriate amount of water, then weigh 4.50g Al(OH) 3 Add, stir and heat to reflux in a three-necked flask until Al(OH) 3 Dissolve completely to make the solution clear; after the solution is cooled, transfer it to a beaker, add 17.64g KCl and the remaining water and stir evenly, then weigh 68.11g of silica sol (SiO2 content 30wt.%) was slowly added dropwise to the above solution, stirred and aged at room temperature for 20h to obtain a KL molecular sieve synthetic liquid, and the molar ratio of each material in the synthetic liquid was 8.0KCl: 3.5K 2 O: 11.5SiO 2 : 1.0Al 2 o 3 : 292.65H 2 O. Transfer the above synthetic solution to a polytetrafluoroethylene-lined crystallization kettle, and conduct static hydrothermal crystallization at 175°C for 24 hours. The resulting product is filtered by suction, washed with deionized water until neutral, and then dried at 120°C for 24 hours to obtain KL molecular sieve. Raw powder, the yield...

Embodiment 3

[0042] Weigh 13.66g KOH and dissolve in appropriate amount of water, then weigh 4.50g Al(OH) 3 Add, stir and heat to reflux in a three-necked flask until Al(OH) 3 Dissolve completely to make the solution clear; after the solution is cooled, transfer it to a beaker, add 26.46g KCl and the remaining water and stir evenly, then weigh 68.11g of silica sol (SiO 2 content 30wt.%) was slowly added dropwise to the above solution, stirred and aged at room temperature for 20h to obtain a KL molecular sieve synthetic liquid, and the molar ratio of each material in the synthetic liquid was 12.0KCl: 3.5K 2 O: 11.5SiO 2 : 1.0Al 2 o 3 : 292.65H 2 O. Transfer the above synthetic solution to a polytetrafluoroethylene-lined crystallization kettle, and conduct static hydrothermal crystallization at 175°C for 24 hours. The resulting product is filtered by suction, washed with deionized water until neutral, and then dried at 120°C for 24 hours to obtain KL molecular sieve. Raw powder, the yi...

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Abstract

The invention discloses a KL molecular sieve and a morphology control synthesis method thereof. The method comprises the following steps: mixing potassium salt, potassium hydroxide, an aluminum source, a silicon source and water according to a molar ratio of (1-15):(2-4):1:(6-15):(150-350), sequentially conducting stirring, aging and hydrothermal crystallization, and conducting separating, washing and drying to obtain the KL molecular sieve. Compared with other KL molecular sieve morphology regulation and control methods, the technical scheme provided by the invention does not need to add an organic alcohol or amine structure-directing agent, does not need to change the silica-alumina ratio and alkalinity of a synthesis system to a great extent, is simple in method, wide in raw material source and low in cost, and has remarkable synthesis and cost advantages, and the maximum yield of a single synthesis kettle can reach 80% or above.

Description

technical field [0001] The invention relates to the technical field of molecular sieves, in particular to a KL molecular sieve and a synthesis method for controlling its morphology. Background technique [0002] KL molecular sieve (skeleton structure code is LTL) was developed and synthesized by Union Carbide Company in 1965, and its typical chemical composition is K 9 [Al 9 Si 27 o 72 ]·nH 2 O (n = 0 ~ 36), the silicon aluminum ratio (atomic ratio) is generally 2.6 ~ 3.5. Its crystals are composed of hexagonal column cages (D6R) and cancia stone cages (CAN cages) stacked alternately in the direction of the C-axis. Six sets of centrally symmetrical cage columns are connected to form a ring, forming a wavy profile around the direction of the C-axis. The one-dimensional twelve-membered ring channel structure, the diameter of the channel is (macroporous molecular sieve), belonging to the hexagonal system (P6 / mmm, ). KL molecular sieve with alkali metal ion K + It is ...

Claims

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Application Information

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IPC IPC(8): C01B39/32
CPCC01B39/32C01P2004/30C01P2004/54C01P2004/61C01P2004/62Y02P20/52
Inventor 王熙陈会民李珂王苹王海丽丁湘浓
Owner CHEM & CHEM ENG GUANGDONG LAB
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