Fast synthesis process of high-crystallinity zeolite molecular sieve

A zeolite molecular sieve, high crystallinity technology, applied in the directions of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc. short cycle effect

Inactive Publication Date: 2003-05-14
SYNFUELS CHINA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is a pity that the author did not give the crystal morphology
In the actual research work, we found that using alcohols as templates to synthesize zeolite molecular sieves, in order to obtain high-purity and high-crystallinity zeolite molecular sieves, it must be possible within a narrow range of silicon-aluminum ratio, and α- SiO 2 and heterocrystalline phases such as mordenite

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 240g water glass (SiO 2 : 30.56wt%, Na 2 (2:10.4wt%) joins 407g deionized water, mixes and is solution A; 11.7g Al 2 (SO 4 ) 3 18H 2 O, 462g water and 31.5g concentrated sulfuric acid (98wt%) are mixed uniformly to be solution B.

[0025] The ingredients are operated in the following order: under vigorous stirring, add solution B to solution A dropwise, and stir evenly. Then add 7 g of n-butylamine and 18.3 ml of ammonia water with a concentration of 7 mol / L, adjust the pH to 10.5, and stir evenly. Finally, transfer the prepared gel mixture into a synthesis kettle and seal it. The molar ratio of each component consists of:

[0026] 14.6NH 3 : 7.9Na 2 O:Al 2 o 3 : 69SiO 2 : 5.45n-C 4 h 9 NH 2

[0027] First heat up to 100°C and age for 20 hours. Continue to raise the temperature to 185°C, and crystallize for 28 hours. Cool rapidly with ice water to stop the crystallization, and remove the mixture in the synthesis kettle.

[0028] The above mixtu...

Embodiment 2

[0031] 165g of water glass (SiO 2 : 30.56wt%, Na 2 (2:10.4wt%) joins 380g deionized water, mixes and is solution A; 9.3g Al 2 (SO 4 ) 3 18H 2 O, 219g of water and 21.7g of concentrated sulfuric acid (98wt%) were mixed uniformly to form solution B.

[0032] The ingredients are operated in the following order: under vigorous stirring, add solution B to solution A dropwise, and stir evenly. Then add 3.4 g of n-butylamine and 14.2 ml of aqueous ammonia with a concentration of 7 mol / L, adjust the pH to 10.5, and stir evenly. Finally, transfer the prepared gel mixture into a synthesis kettle and seal it. The molar ratio of each component consists of:

[0033] 14.2NH 3 : 6.6Na 2 O:Al 2 o 3 : 60SiO 2 : 3.34 n-C 4 h 9 NH 2

[0034] First raise the temperature to 90°C and age for 22 hours. Continue to raise the temperature to 170°C for 36 hours of crystallization. Cool rapidly with ice water to stop the crystallization, and remove the mixture in the synthesis ke...

Embodiment 3

[0038] l25g water glass (SiO 2 : 30.56wt%, Na 2 (2:10.4wt%) joins 104g deionized water, mixes and is solution A; 10.5g Al 2 (SO 4 ) 3 18H 2 O, 362g water and 15.8g concentrated sulfuric acid (98wt%) are mixed uniformly to be solution B.

[0039] The batching sequence is the same as Example 1, and the add-on of n-butylamine and ammoniacal liquor is respectively 2.7g and 13.4ml (7mol / L). The molar ratio of each component consists of:

[0040] 11.9NH 3 : 4.34Na 2 O:Al 2 o 3 : 40SiO 2 : 2.7n-C 4 h 9 NH 2

[0041] First raise the temperature to 90°C and keep it at a constant temperature for 24 hours. Then continue to heat up to 185 ° C, and keep the temperature for 28 hours to complete. Rapidly cool down to stop the crystallization, and remove the mixture in the synthesis kettle.

[0042] The above mixture is separated, washed and dried according to Example 1 to obtain a zeolite molecular sieve. The crystal phase was analyzed by X powder ray diffractometer and...

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PUM

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Abstract

High-crystallinity H-type zeolite molecular sieve is synthesized through the fast process including: adding dropwise mixed solution B comprising Al2(SO4)3.18H2O, water and concentrated sulfuric acid to mixed solution A comprising water glass and deionized water while stirring drastically; adding fatty amine and inorganic ammonia solution to form gel mixture; sealing, ageing, crystallizing, cooling, solid-liquid separation, washing to filter cake pH value of 8-9, drying, calcining and HCl exchange. The process has the advantages of short synthesis period, high crystallinity, low organic template agent content in crystallized zeolite and low sodium ion content.

Description

[0001] Field: [0002] The invention belongs to a method for synthesizing zeolite molecular sieves, in particular to a method for quickly synthesizing ZSM-5 zeolite molecular sieves with a small amount of organic template and inorganic ammonia. Background technique: [0003] The main feature of zeolite molecular sieve is that it is a solid material with regular pore structure. Its uniqueness determines that zeolite molecular sieve has a wide range of uses. Such as: (1) catalyst, (2) detergent, (3) adsorbent and desiccant, (4) others (including sewage treatment, etc.). The economic and social benefits of zeolite catalysts are the most significant. It can not only improve the yield and quality of products in petrochemical processes, but also significantly shorten the process flow and reduce process costs. [0004] In 1972, U.S. Patent 3,702,866 first introduced the preparation method of ZSM-5 zeolite molecular sieve, and the molar ratio of its oxides was: 0.9±0.2M 2 / n O:Al 2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04C01B39/38
Inventor 孙予罕任杰王锋胡津仙房克功
Owner SYNFUELS CHINA TECH CO LTD
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