Method for preparing hierarchical pore Y zeolite through oxalic acid-ammonium hydroxide cotreatment

A molecular sieve and multi-stage pore technology, applied in the field of molecular sieves, can solve the problems of small external surface area and mesopore volume of multi-stage pore Y molecular sieves.

Inactive Publication Date: 2019-08-13
GUANGDONG UNIV OF PETROCHEMICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the external area and mesopore volume of the hierarchically porous Y molecular sieve prepared by the prior art are relatively small.

Method used

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  • Method for preparing hierarchical pore Y zeolite through oxalic acid-ammonium hydroxide cotreatment
  • Method for preparing hierarchical pore Y zeolite through oxalic acid-ammonium hydroxide cotreatment
  • Method for preparing hierarchical pore Y zeolite through oxalic acid-ammonium hydroxide cotreatment

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1: the method for preparing hierarchically porous Y molecular sieves by oxalic acid-ammonia co-treatment

[0022] Acid treatment of oxalic acid solution: Weigh 6g of NaY molecular sieve and prepare 100ml of H with a concentration of 0.12mol / L 2 C 2 o 4 The solution is ready for use. Add 15ml of H for every 1g of sample 2 C 2 o 4 The ratio of the solution, the above sample and the amount taken out of the H 2 C 2 o 4 The solution was mixed evenly in the flask, placed in an oil bath with a constant temperature of 363K, and stirred for 60 minutes. The mixed solution after the above oil bath treatment was filtered under reduced pressure until the filtrate was nearly neutral, and then put into a 337K oven to dry overnight. After H 2 C 2 o 4 Solution-treated samples were recorded as AT.

[0023] NH 3 ·H 2 Alkaline treatment of O solution: add 20ml of NH per 1g of sample 3 ·H 2 The ratio of O solution to the above sample and the amount of NH 3 ·H 2...

Embodiment 2

[0024] Embodiment 2: the method for preparing hierarchically porous Y molecular sieves by oxalic acid-ammonia co-treatment

[0025] Acid treatment of oxalic acid solution: Weigh 6g of NaY molecular sieve and prepare 100ml of H with a concentration of 0.12mol / L 2 C 2 o 4 The solution is ready for use. Add 15ml of H for every 1g of sample 2 C 2 o 4 The ratio of the solution, the above sample and the amount taken out of the H 2 C 2 o 4 The solution was mixed evenly in the flask, placed in an oil bath with a constant temperature of 363K, and stirred for 60 minutes. The mixed solution after the above oil bath treatment was filtered under reduced pressure until the filtrate was nearly neutral, and then put into a 337K oven to dry overnight. After H 2 C 2 o 4 Solution-treated samples were recorded as AT.

[0026] NH 3 ·H 2 Alkaline treatment of O solution: add 20ml of NH per 1g of sample 3 ·H 2 The ratio of O solution to the above sample and the amount of NH 3 ·H 2...

Embodiment 3

[0028] The method of oxalic acid-ammonia co-treatment was used to prepare hierarchically porous NaY molecular sieves. The concentration of oxalic acid was selected as 0.12mol / L and the treatment temperature was 90°C. The reaction time of ammonia water was adjusted to see the mesopore formation under different reaction times. The specific experimental conditions are shown in Table 1.

[0029] Table 1. Labeling and processing conditions of samples

[0030] Sample model Reagent pH T(K) t(h) AT h 2 C 2 o 4

1 363 1 E1 NH 3 ·H 2 o

11 328 4 E2 NH 3 ·H 2 o

11 328 8

[0031] (1) XRD of molecular sieve

[0032] figure 1 The XRD patterns of NaY and NaY-AT-E2 molecular sieves are given. By observing the crystal structure of Y molecular sieve before and after modification with oxalic acid-ammonia water, it can be seen that: NaY-AT-E2 molecular sieve is still the structure of Y-type molecular sieve, and no other miscel...

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Abstract

The invention discloses a method for preparing hierarchical pore Y zeolite through oxalic acid-ammonium hydroxide cotreatment. The method comprises the following steps of 1, acid treatment with an oxalic acid solution, wherein NaY zeolite is obtained to be evenly mixed with the H2C2O4 solution to obtain a mixture, and the mixture is put in an oil bath pan and stirred; the mixed liquid obtained after oil bath treatment is subjected to vacuum suction filtration until filter liquor is close to be neutral, a filter cake is put into a drying oven for overnight drying, and an oxalic acid treated sample is obtained; 2, alkaline treatment with a NH3 H2O solution, wherein the oxalic acid treated sample obtained in the step 1 is evenly mixed with the NH3 H2O solution to obtain a mixture, and the mixture is put into an oil bath pan and treated; the mixed liquid obtained after oil bath treatment is subjected to vacuum suction filtration until filter liquor is close to be neutral, a filter cake istaken out, put into a drying oven for drying and calcined by using a muffle furnace, and then the hierarchical pore Y zeolite is obtained. The hierarchical pore Y zeolite is prepared through the oxalic acid-ammonium hydroxide cotreatment, compared with NaY, the outer surface area of the hierarchical pore Y zeolite is increased by 3 times or above, and the mesoporous volume of the hierarchical poreY zeolite is increased by 4 times or above.

Description

technical field [0001] The invention relates to the technical field of molecular sieves, in particular to a preparation technology of multi-level porous Y molecular sieves. Background technique [0002] The pore size of microporous zeolite is small, the distribution is too wide, and the opening is not enough, which seriously affects the diffusion of larger heavy oil molecules and their intermediate products, resulting in the difficulty of mass transfer in catalytic reactions, which requires the development of new catalytic materials. Ordered mesoporous materials attracted people's attention in 1992. It has large pore size, pore volume, high specific surface area and highly ordered pore structure, which makes it prominent in catalytic reactions involving macromolecules. Excellent catalytic performance, but in practical applications, mesoporous materials have poor hydrothermal stability and lower catalytic activity than microporous zeolites, which seriously restricts their app...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/24C01B39/02
CPCC01B39/24C01B39/026C01P2002/72C01P2004/03C01P2006/12C01P2006/10C01P2006/14
Inventor 段林海孟秀红程丽华林存辉张尤华曹水秦慧博
Owner GUANGDONG UNIV OF PETROCHEMICAL TECH
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