Ultra-stable Y-type molecular sieve as well as preparation method and application thereof

A technology of molecular sieve and B acid, applied in the direction of molecular sieve catalysts, including molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of poor activity and selectivity of low-temperature liquid-phase transalkylation catalysts, improve the diffusion of reactants, and reduce side reactions , The effect of high proportion of B acid

Pending Publication Date: 2022-05-13

CHINA PETROLEUM & CHEM CORP +1

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AI-Extracted Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is the problem of poor activity ...

Method used

[0094] Wherein, it can be seen from the XRD spectrum that the faujasite characteristic peak intensity USY-A and USY-B molecular sieve of...

Abstract

The invention discloses an ultra-stable Y-type molecular sieve as well as a preparation method and application thereof. According to the ultra-stable Y-type molecular sieve provided by the invention, the pore volume of mesopores accounts for more than 50% of the total pore volume; and the amount of the strong B acid accounts for 40-70% of the total amount of the B acid. The ultra-stable Y-type molecular sieve has the characteristics of high proportion of strong B acid and abundant mesopores, can complete the reaction at a lower reaction temperature when being used for the transalkylation reaction of benzene and polyalkylbenzene, not only can improve reactant diffusion and enhance the accessibility of activity, but also can reduce the occurrence of side reactions, and has good activity and selectivity.

Application Domain

Molecular sieve catalystsMolecular sieve catalyst +5

Technology Topic

Molecular sieveTransalkylation +6

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Examples

Experimental program(5)
Comparison scheme(5)
Effect test(1)

Example Embodiment

[0071] [Example 1]

[0072] Take 1.2g of HF and add it to 150g of 0.2mol/L ammonium fluorosilicate solution. After stirring evenly, add 30g of SiO 2 /Al 2 O 3 The Y-type molecular sieve of 5.8 was heated to 60° C. and stirred for 30 minutes, and then filtered, washed and dried to obtain pretreated Y-type molecular sieve.

[0073] Get 20g of pretreated molecular sieves and be dispersed in 200g of ammonium chloride aqueous solution with a concentration of 9% by weight (in terms of ammonium chloride), beating and stirring, adding 1mol/L oxalic acid solution after 20min for acid treatment, the acid treatment temperature is 90 ° C, pickling The time is 1h; finally wash with 20 times deionized water and dry at 120℃ for 12h;

[0074] Then put it into a hydrothermal furnace, heat up to 650°C, the constant heating rate is 8°C/min during the hydrothermal ultra-stabilization treatment, calcinate with 100% steam by volume for 2h, and dry at 120°C for 12h to prepare the USY type molecular sieve. , labeled as sample USY-A.

[0075] NH on USY-A 3 - Characterization of TPD, Py-IR and XRD, the results of which can be found in Figure 1-4.

[0076]The physical parameters that characterize USY-A: the relative crystallinity is 94%; the skeleton silicon-aluminum molar ratio is 16:1; the acid content of strong B acid is 460 μmol/g; the total acid content of B acid is 735 μmol/g; the total acid content of B acid The ratio to the total acid content of L acid is 1.5, and the characterization of acid content is shown in Table 1; the specific surface area is 664m 2 /g; pore volume is 0.53cm 3 /g; the mesoporous pore volume is 0.29ml/g, and the mesoporous pore volume accounts for 55% of the total pore volume.

Example Embodiment

[0077] [Example 2]

[0078] Take 0.7g NH 4 F was added to 190g of 0.2mol/L ammonium fluorosilicate solution, after stirring evenly, 36g of SiO was added 2 /Al 2 O 3 The Y-type molecular sieve of 5.4 was heated to 80° C. and stirred for 15 minutes, and then filtered, washed and dried to obtain the pretreated Y-type molecular sieve.

[0079] Get 25g of pretreated molecular sieves and be dispersed in 220g of ammonium sulfate aqueous solution with a concentration of 9% by weight (in terms of ammonium chloride), beating and stirring, adding 0.6mol/L acetic acid solution after 20min for acid treatment, the acid treatment temperature is 75 ° C, pickling The time was 1.5h; finally washed with 20 times deionized water and dried at 120°C for 12h; then placed in a hydrothermal furnace, heated to 670°C, and the uniform heating rate during the hydrothermal ultra-stabilization treatment was 5°C/min , calcined in 80 vol% water vapor for 2h, and dried at 120°C for 12h to prepare USY type molecular sieve, which is marked as sample USY-B.

[0080] NH for USY-B 3 - Characterization of TPD, Py-IR and XRD, the results of which can be found in Figure 1-4.

[0081] The physical parameters that characterize USY-B: the relative crystallinity is 92%; the skeleton silicon-aluminum molar ratio is 13:1; the acid content of strong B acid is 425 μmol/g; the total acid content of B acid is 749 μmol/g; the total acid content of B acid The ratio to the total acid content of L acid is 1.4, and the characterization of acid content is shown in Table 1; the specific surface area is 652m 2 /g; pore volume is 0.51cm 3 /g; the mesoporous pore volume is 0.27ml/g, and the mesoporous pore volume accounts for 53% of the total pore volume.

Example Embodiment

[0082] [Example 3]

[0083] Take 1.0g of HF and add it to 165g of 0.2mol/L ammonium fluorosilicate solution. After stirring evenly, add 40g of SiO 2 /Al 2 O 3 Y-type molecular sieve of 6.5, heated to 50 °C and stirred for 1 h, then suction filtered, washed and dried to obtain pretreated Y molecular sieve.

[0084] Get 30g of pretreated molecular sieves and be dispersed in 280g of ammonium nitrate aqueous solution with a concentration of 10% by weight (in terms of ammonium chloride), beating and stirring, adding 1.4mol/L oxalic acid solution after 20min for acid treatment, the acid treatment temperature is 90 ℃, pickling The time was 2h; finally washed with 20 times deionized water and dried at 120°C for 12h; then placed in a hydrothermal furnace, heated to 630°C, and the uniform heating rate during the hydrothermal ultra-stabilization treatment was 10°C/min, Passing 100% by volume of steam to calcinate for 2 hours, and drying at 120° C. for 12 hours to prepare USY type molecular sieves, which are marked as sample USY-C.

[0085] USY-C for NH 3 - Characterization by TPD, Py-IR and XRD with results similar to Figure 1-4. The physical parameters characterizing USY-C: the relative crystallinity is 95%; the skeleton silicon-aluminum molar ratio is 23:1; the acid content of strong B acid is 546 μmol/g; the total acid content of B acid is 782 μmol/g; the total acid content of B acid The ratio to the total acid content of L acid is 1.3; the specific surface area is 683m 2 /g; pore volume is 0.54cm 3 /g; the mesoporous pore volume is 0.31ml/g, and the mesoporous pore volume accounts for 57% of the total pore volume.

PUM

Property	Measurement	Unit
Acidity	460.0	µmol/g
Specific surface area	664.0	m²/g
Pore volume	0.53	cm³/g

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Owner:ANHUI UNIVERSITY OF TECHNOLOGY

Ultra-stable Y-type molecular sieve as well as preparation method and application thereof

AI-Extracted Technical Summary

Problems solved by technology

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Example Embodiment

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Example Embodiment

PUM

Description & Claims & Application Information

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