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Preparation method of catalyst containing small-grain Y-type molecular sieve

A molecular sieve, small-grain technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as poor thermal and hydrothermal stability, difficult elution of fluoride ions, and small batch size.

Active Publication Date: 2015-11-25
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN1382632A discloses a super-stabilizing method of small-grain Y-type zeolite, which is obtained by contacting the dry gas of silicon tetrachloride with small-grain NaY zeolite and washing it. Stability is just relatively poor, and this inventive method adopts the mode of vapor phase dealumination of silicon to process molecular sieve simultaneously, and this makes the thermal and hydrothermal stability of product worse, and activity is low; Small, high energy consumption and other disadvantages
Although the above two modification methods can increase the silicon-aluminum ratio of the molecular sieve skeleton, the fluoride ions introduced by the additives are difficult to elute from the slurry, and a large amount of fluoride ions remain in the liquid after the molecular sieve is washed, causing environmental problems in industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] This example illustrates the synthesis process of NaY molecular sieves.

[0038] 50.39g high alkali sodium metaaluminate solution (provided by Sinopec Catalyst Changling Branch, Al 2 o 3 The content is 40.2g / L, Na 2 O content is 255g / L, specific gravity is 1.324) joins 65.56g water glass (Sinopec Catalyst Changling Branch provides, SiO 2 The content is 260.6g / L, Na 2 The O content is 81.6g / L, the specific gravity is 1.2655, and the modulus is 3.3), aged with stirring at room temperature for 48 hours, then statically aged at 60°C for 5 hours, and finally added 15g of deionized water, the resulting directing agent has a final molar ratio of 15Na 2 O: A1 2 o 3 :15SiO2 2 :320H 2 O.

[0039] All the directing agents prepared were used in the preparation of the following reaction mixture, and the amount of the directing agent added was calculated according to the fact that the moles of aluminum in the directing agent accounted for 3% of the total moles of aluminum. ...

Embodiment 2

[0050] This example illustrates the synthesis process of NaY molecular sieves.

[0051] 50.39g high alkali sodium metaaluminate solution (provided by Sinopec Catalyst Changling Branch, Al 2 o 3 The content is 40.2g / L, Na 2 O content is 255g / L, specific gravity is 1.324) joins 65.56g water glass (Sinopec Catalyst Changling Branch provides, SiO 2 The content is 260.6g / L, Na 2 The O content is 81.6g / L, the specific gravity is 1.2655, and the modulus is 3.3), aged with stirring at 60°C for 5 hours, then statically aged at 60°C for 5 hours, and finally added 15g of Ionized water, the final molar ratio of the resulting directing agent is 15Na 2 O: A1 2 o 3 :15SiO2 2 :320H 2 O.

[0052] All the directing agents prepared were used in the preparation of the following reaction mixture, and the amount of the directing agent added was calculated according to the fact that the moles of aluminum in the directing agent accounted for 3% of the total moles of aluminum.

[0053] Under...

Embodiment 3

[0063] This example illustrates the synthesis process of NaY molecular sieves.

[0064] With 164.54g high alkali sodium metaaluminate solution (Sinopec Catalyst Changling Branch Company provides, Al 2 o 3 The content is 40.2g / L, Na 2 O content is 340g / L, specific gravity is 1.297) joins 291.37g water glass (Sinopec Catalyst Changling Branch provides, SiO 2 The content is 260.6g / L, Na 2 The O content is 81.6g / L, the specific gravity is 1.2655, and the modulus is 3.3), aged with stirring at 30°C for 20 hours, then statically aged at 40°C for 15 hours, and finally added 60g of ionized water. The resulting directing agent has a final molar ratio of 20Na 2 O: A1 2 o 3 :20SiO2 2 :380H 2 O.

[0065] All the directing agents prepared were used in the preparation of the following reaction mixture. The amount of the directing agent added was calculated according to the fact that the moles of aluminum in the directing agent accounted for 10% of the total moles of aluminum.

[...

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Abstract

The invention provides a preparation method of a catalyst containing a small-grain Y-type molecular sieve. The preparation method comprises steps of mixing raw materials including a small-grain Y-type molecular sieve, alumina sol, hydrated alumina, silica sol, clay, acid and water to obtain slurry and moulding to obtain the catalyst. The preparation method is characterized in that the small-grain Y-type molecular sieve is prepared from the following steps: successively adding a guiding agent, a silicon source, an aluminium source and water into a mixing tank under synthesis conditions of a NaY molecular sieve so as to obtain a mixture A, carrying out hydrothermal crystallization on the mixture A and recovering an obtained product, carrying out ammonium exchange for sodium reduction on the product, carrying out a hydro-thermal treatment, beating, adding silica sol with pH of 2-4 and C2-C4 organic alcohols, adjusting pH to 3-6 with citric acid, fully mixing at the temperature of 80-120 DEG C, washing and drying. The catalyst prepared by the above method has good mechanical strength and has better catalytic performance.

Description

technical field [0001] The present invention relates to a preparation method of a catalyst containing Y-type molecular sieves, more specifically to a preparation method of a catalyst containing small-grain Y-type molecular sieves. Background technique [0002] In the late 1950s, Milton and Breck successfully synthesized Y-type molecular sieves. Due to the SiO in the structure of the Y-type molecular sieve 2 with Al 2 o 3 The ratio is greater than that of X-type molecular sieve, so that the thermal stability and hydrothermal stability are improved. In the early 1970s, Grace Company developed the directing agent method to synthesize NaY molecular sieves. The raw material was water glass instead of expensive silica sol. The process was simplified and the growth cycle was shortened, so that NaY molecular sieves were rapidly and widely used in petrochemical industries Petroleum cracking catalysis field. So far, among the hundreds of molecular sieves that have been developed,...

Claims

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Application Information

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IPC IPC(8): B01J29/08C01B39/24C07C9/16C07C2/58
CPCY02P20/52
Inventor 鲁玉莹付强李永祥胡合新慕旭宏
Owner CHINA PETROLEUM & CHEM CORP
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