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Preparation method of 13X molecular sieve and 13X molecular sieve

A technology of molecular sieve and mass percentage, applied in octahedral crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, etc., can solve the problems of limited popularization and application, large energy consumption, low mass transfer efficiency, etc.

Inactive Publication Date: 2020-10-30
CHINA UNIV OF MINING & TECH (BEIJING)
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  • Summary
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  • Description
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Problems solved by technology

Most of the fly ash pretreatment and molecular sieve synthesis process require a large amount of solution, which consumes water and produces difficult-to-degrade sewage, or requires alkali roasting activation during pretreatment, and consumes a lot of energy during the roasting activation process , and the currently synthesized 13X molecular sieve has a single channel, and the low mass transfer efficiency obviously limits its popularization and application

Method used

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  • Preparation method of 13X molecular sieve and 13X molecular sieve
  • Preparation method of 13X molecular sieve and 13X molecular sieve
  • Preparation method of 13X molecular sieve and 13X molecular sieve

Examples

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preparation example Construction

[0043] see figure 1 , The invention provides a preparation method of 13X molecular sieve. The preparation method comprises the following steps:

[0044] (1) Remove impurity iron, wash, filter and dry the fly ash of the circulating fluidized bed with a magnetic separator to obtain the fly ash raw material;

[0045] (2) this fly ash raw material is mixed with sodium hydroxide, silicon source, aluminum source, 13X molecular sieve crystal seed, hard formwork, obtain compound by grinding afterwards;

[0046] (3) crystallize the mixture in the range of 80-98° C. for 15-24 hours to obtain a crystallized product, and then cool the crystallized product to obtain the first product of 13X molecular sieve;

[0047] (4) Calcining the primary product at a temperature of 500-600°C for 4-8 hours to obtain a calcined product, after cooling the calcined product, washing and filtering, and then drying at a temperature of 50-70°C After 10-15 hours, 13X molecular sieves were obtained.

[0048]...

Embodiment 1

[0057] In this example, first, an appropriate amount of circulating fluidized bed fly ash containing a certain silicon-aluminum ratio is subjected to magnetic separation to remove iron, and then deionized water is added to wash and remove the floating matter in the fly ash, and the fly ash is filtered to remove soluble salt, and then dried in an oven at 110°C for 6 hours to obtain the raw material of fly ash. Then, mix and grind according to the ratio of 70% fly ash raw material, 10% sodium hydroxide, 7% sodium silicate, 2% aluminum hydroxide, 8% seed crystal and 3% hard template After uniformity, place it in a reaction kettle, crystallize in an oven at 95°C for 16 hours to obtain a crystallized product, and then cool the crystallized product to obtain a primary product. The primary product was calcined in a muffle furnace at 550°C for 6 hours. Finally, wash several times with deionized water, filter to remove the hard template, and dry in an oven at 60°C for 12 hours to obta...

Embodiment 2

[0060] In this example, firstly, an appropriate amount of circulating fluidized bed fly ash containing a certain silicon-aluminum ratio is subjected to magnetic separation to remove iron, then deionized water is added to wash to remove floating matter, and soluble salt is filtered to remove, and then heated in an oven at 110°C Dry for 6 hours to obtain the fly ash raw material. Then, mix and grind evenly according to the ratio of 78% of fly ash raw material, 10% of sodium hydroxide, 7% of sodium silicate, 2% of aluminum hydroxide and 3% of hard template, and then place it in the reactor , crystallized in an oven at 95°C for 16 hours, and cooled the crystallized product to obtain the primary product. The primary product was calcined in a muffle furnace at 550°C for 6 hours. Finally, wash with deionized water several times, filter, and dry in an oven at 60°C for 12 hours to obtain the final product microporous-mesoporous 13X molecular sieve.

[0061] Compared with Example 1, n...

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Abstract

The invention discloses a preparation method of a 13X molecular sieve and the 13X molecular sieve, and belongs to the technical field of solid waste treatment in the field of environmental protection.The preparation method comprises the following steps: providing a fly ash raw material, wherein the mass percentage of the fly ash is 66-85%, mixing the fly ash raw material with sodium hydroxide, asilicon source, an aluminum source, a 13X molecular sieve seed crystal and a hard template, grinding to obtain a mixture, wherein the range of the silica-alumina ratio in the mixture is 3-11, the masspercent of the 13X molecular sieve seed crystal is 8-15% and the mass percent of the hard template is 2-5%, crystallizing the mixture for 15-24 hours at the temperature of 80-98 DEG C to obtain a crystallized product, and cooling the crystallized product to obtain a primary product; and calcining the primary product for 4-8 hours at the temperature of 500-600 DEG C to obtain a calcined product, sequentially cooling, washing and filtering the calcined product, and drying for 10-15 hours at the temperature of 50-70 DEG C to obtain the 13X molecular sieve. According to the preparation method ofthe 13X molecular sieve and the 13X molecular sieve, a roasting activation link is not needed.

Description

technical field [0001] The invention relates to the technical field of solid waste treatment in the field of environmental protection, in particular to a preparation method of 13X molecular sieve and 13X molecular sieve. Background technique [0002] Fly ash is a kind of pozzolanic mixed material formed after coal powder is burned at high temperature. The main chemical composition of fly ash is SiO 2 and Al 2 o 3 aluminosilicate, and it also contains a small amount of Fe 2 o 3 , CaO, MgO, and unburned carbon. [0003] Fly ash belongs to bulk industrial solid waste, and its chemical composition is the basis of its resource utilization. Depending on the type of coal, how it is burned, and how it is collected, the composition of fly ash produced by burning coal varies from country to country, from type to type, and even from part of the same mine. [0004] Coal is the main energy source in my country. With the sharp increase in energy demand and the continuous growth of t...

Claims

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Application Information

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IPC IPC(8): C01B39/22
CPCC01B39/22C01P2006/16
Inventor 竹涛韩一伟张星边文璟王若男
Owner CHINA UNIV OF MINING & TECH (BEIJING)
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