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Process for preparing NaY molecular sieve by using synthetic mother liquor

A technology for synthesizing mother liquor and molecular sieves, applied in the direction of crystalline aluminosilicate zeolite, octahedral crystalline aluminosilicate zeolite, etc., can solve the problems of slow filtration rate, reduce waste liquid discharge and improve production efficiency

Active Publication Date: 2006-11-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention overcomes the defects of the prior art, adds a pre-crystallization step before the conventional crystallization step in the molecular sieve synthesis process, and solves the problem of molecular sieve crystal grains being small , The problem of small particles and slow filtration rate during continuous exchange water washing not only improves industrial production efficiency, but also can prepare NaY molecular sieves with large grains and large particles

Method used

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  • Process for preparing NaY molecular sieve by using synthetic mother liquor
  • Process for preparing NaY molecular sieve by using synthetic mother liquor
  • Process for preparing NaY molecular sieve by using synthetic mother liquor

Examples

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Embodiment 1

[0040] This example is the preparation of the directing agent.

[0041] Get water glass 126ml (specific gravity 1.278kg / L, SiO 2 content 287 g / L, modulus 3.3) into a beaker, slowly add 105ml of sodium metaaluminate solution (Al 2 o 3 Content 38.7 g / L, Na 2 O content 291 g / L, specific gravity 1233 g / L), mix uniformly at room temperature, age at 35°C for 6 hours, and make a molar ratio of 16.85Na 2 O:Al 2 o 3 : 15.1SiO2 2 : 320.8H 2 O's directing agent.

Embodiment 2

[0043] This embodiment is the preparation of silica-alumina glue.

[0044] Get industrial NaY mother liquor 1500ml (Qilu Catalyst Factory, specific gravity 1.110, SiO 2 Content 53.3 g / L, Na 2 O content 26.6 grams / liter), while stirring mother liquor with the rotating speed of 700r / min, slowly add aluminum sulfate solution 154ml (Al 2 o 3 Content 98 g / L, specific gravity 1.291), forming silica-alumina glue slurry. After stirring evenly, put the silica-alumina glue slurry into a water bath at 95°C for heating and aging for 2 hours. Take out the aged silica-alumina glue slurry and filter it on a φ200 Buchner funnel with a vacuum of 0.05Mpa. Obtain silica-alumina gel filter cake.

Embodiment 3

[0046] This example is the preparation of NaY molecular sieves with large grains and large particles.

[0047] Pre-crystallization step: get water glass 210ml (specific gravity 1.278kg / L, SiO 2 Content 287 grams per liter, modulus 3.3) put into 2L enamel cup, add the silica-alumina gel filter cake 1087g in the embodiment 2 when stirring water glass, the directing agent 88ml in the embodiment 1, aluminum sulfate solution 33ml (Al 2 o 3 Content 98 g / L, specific gravity 1.291), sodium metaaluminate solution 77ml (Al 2 o 3 Content 102 g / L, Na 2 O content is 159 g / L, specific gravity is 1.240), mixed evenly, and pre-crystallized at 95° C. for 2 hours. Among them, the SiO provided by the silica-alumina gel filter cake 2 SiO in the precrystallization reaction mixture 2 The mass percentage is 55%, the Al in the directing agent 2 o 3 accounted for the total Al in the precrystallization reaction mixture 2 o 3 5% of the amount.

[0048] Crystallization step: take out 800g of p...

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Abstract

The invention relates to a method for preparing NaY molecular sieve by using the synthesis mother liquor, comprising the following steps: 1. adding the aluminium salt solution into the synthesis mother liquor to form a precipitating silicon-aluminium gel, then filtering it to obtain a silicon-aluminium gel filter cake; 2. mixing the silicon-aluminium gel filter cake with the soluble silica resource, aluminium resource and guiding agent evenly, after that, pre-crystallizing it under 30 to 100 degrees centigrade for 0.5 to 30 hours; 3. mixing the pre-crystallized product with the soluble silica resource, aluminium resource to form a crystallization mixture, after that, crystallizing it under 90 to 100 degrees centigrade for 8 to 65 hours, then filtering, washing and drying to obtain a NaY molecular sieve with large crystal grain and large granule. The invention overcomes the bias of the existed techniques by adding the pre-crystallizing step before the conventional crystallizing step to prepare NaY molecular sieve with large crystal grain and large granule, and solves slow filtering rate in post treatment.

Description

technical field [0001] The present invention relates to catalytic cracking catalyst, especially the preparation method of NaY molecular sieve. Background technique [0002] NaY molecular sieves are the main source of active components in catalytic cracking catalysts, and the composition of NaY molecular sieves is (0.9±0.2)Na 2 O:Al 2 o 3 :(3~6)SiO 2 :xH 2 O, where the value of x is generally 1-9. At present, the method for industrially producing Y-type molecular sieve basically adopts the directing agent method (US3639099, US3671191) proposed by Grace Company of the United States. That is to say, the soluble silicon source and aluminum source will be (15-17)Na according to a certain order of addition and composition. 2 O:Al 2 o 3 :(14~16)SiO 2 :(280~360)H 2 The directing agent with O grains smaller than 0.1μm is mixed to form a ratio of (1.8~4)Na 2 O:Al 2 o 3 :(7~12)SiO 2 :(120~350)H 2 The reaction mixture of O then crystallized at about 100 °C. The disadvant...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/24
Inventor 郭瑶庆马跃龙邓景辉
Owner CHINA PETROLEUM & CHEM CORP
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