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Method for utilizing molecular sieve systhesis mother liquor

A technology for synthesizing mother liquor and molecular sieve, which is applied in the field of utilization of molecular sieve synthesis mother liquor, which can solve problems such as difficulty in accurate measurement and difficult control of formula stability, and achieve the effects of saving production time, overcoming temperature drop, and stable quality

Inactive Publication Date: 2011-10-26
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0038] However, there are still many difficulties in using the mother liquor directly for molecular sieve synthesis
On the one hand, it is difficult to accurately measure the main components in the mother liquor, which makes it difficult to control the stability of the formula after the mother liquor is circulated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Repeat Comparative Example 1, but filter the slurry after peeling treatment while hot at 80°C to obtain solid product A1 and filtrate B1, because the feed liquid temperature is high during the suction filtration process, there is no surfactant precipitation, and the suction filtration speed is fast. It takes less time. The solid product C1 and the filtrate D1 were isolated after the filter B1 was cooled at 10° C. for 4 h. The solid product A1 was dried and calcined to be a molecular sieve product with a product yield of 77%. X-ray diffraction analysis proved that the molecular sieve was ITQ-2 with a relative crystallinity of 96%. Analyze the content of CTAB and TPAOH in the solid product C1 and filtrate D1 according to the surfactant determination method and acid-base titration method in GB / T 5174-2004, and then use it as a circulating raw material, by supplementing CTAB, TPAOH, H 2 O and MCM-22 (P), make the reaction mixture according to the initial formula, prepare t...

Embodiment 2

[0063] Repeat Example 1, but change the hot filtration temperature to 90°C, 80°C, 60°C and 50°C, then the obtained product is proved to be pure ITQ-2 molecular sieve through X-ray diffraction analysis, and its relative crystallinity is 100%, respectively. 99%, 94% and 91%, and the product yields are 84%, 83%, 78% and 75% respectively.

Embodiment 3

[0065] Repeat Example 1, but change the cooling temperature to 15°C, 8°C and 0°C, then the obtained product is proved to be pure ITQ-2 molecular sieve through X-ray diffraction analysis, and its relative crystallinity is 97%, 98%, 99% respectively. %, the product yields were 79%, 80% and 82% respectively.

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Abstract

The invention provides a method for complete cyclic utilization of ITQ-2 molecular sieve mother liquor with zero discharge. The key points of the invention are as follows: ITQ-2 molecular sieve mother liquor undergoes separation at first, then a cetyl trimethyl ammonium bromide surfactant and alkali lye obtained from the separation are analyzed and determined, and finally the surfactant and alkali lye are reused as raw materials to reprepare ITQ-2 molecular sieves with a high degree of crystallization. According to the invention, a method of recycling mother liquor is formulated by ingeniously utilizing the rule of temperatures for a cetyl trimethyl ammonium bromide surfactant to crystallize and precipitate in the mother liquor. In the invention, ITQ-2 molecular sieve mother liquor is recycled, thereby reducing cost, protecting environment and enabling mother liquor recycle formula and the quality of the obtained products to be stabilized.

Description

technical field [0001] The invention belongs to the field of zeolite molecular sieve catalysts, and relates to a method for utilizing molecular sieve synthesis mother liquor. Background technique [0002] ITQ-2 molecular sieve is prepared by expansion and exfoliation of MCM-22 molecular sieve. It has a single-layer structure of MCM-22 molecular sieve and belongs to the MWW topology. MCM-22 molecular sieve has three independent pore systems: a pore system connected by a supercage (0.71×0.71×1.82nm) and an interlayer 10-membered ring (0.4×0.59nm), and a two-dimensional sinusoidal pore system with an intralayer 10-membered ring. And the 12-membered ring hole (0.71×0.71×0.71nm) on the outer surface of the crystal. In contrast, ITQ-2 molecular sieve has two independent pore systems: a 10-membered ring two-dimensional sinusoidal channel system in the layer and a 12-membered ring hole (0.71×0.71×0.71nm) on the outer surface of the crystal. Disorder and short-range order. At the ...

Claims

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Application Information

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IPC IPC(8): C01B39/02B01J29/06B01J37/00B01D9/02
Inventor 郭洪臣聂彬剑钱吉
Owner DALIAN UNIV OF TECH
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