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Method of quickly synthesizing super fine 4A zeolite

A zeolite, rapid technology, applied in the direction of A-type crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, etc., can solve the problems of A-type zeolite grain size increase, reaction speed acceleration, reaction rate slowing down, etc., to achieve Narrow particle size distribution, short crystallization time, and the effect of reducing the amount of waste liquid

Inactive Publication Date: 2005-03-23
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CharnellJF. et al reported the method of changing the crystallization size of A-type zeolite in "Journal of Crystal Growth" magazine 1971, page 291, volume 8 (called the Charnell method, that is, adding triethanolamine in the gel, which can make A-type zeolite crystallization Particle size increases, and the reaction rate slows down); Schoeman BJ. etc. reported adding tetramethylammonium hydroxide to the reaction system to accelerate the reaction rate in the 1994 volume 110 page of "Zeolites" magazine, and the 4A type zeolite particle size decreased Small method; Werner Stober et al reported the method of adding ethanol in the gel to reduce the particle size of zeolite in Colloid and Interfacial Chemistry Journal, 26th page 62 in 1968; Prabir K.Dutta et al. Volume 507 page "Solvent influences on synthetic A-type and X-type zeolite" article reports the method that adds hexamethylphosphoric acid amide and dimethyl sulfoxide to make synthetic A-type and X-type zeolite particle size reduction; Chinese patent CN1453212A (publication number ) reported that adding surfactants can speed up the reaction and reduce the particle size of 4A zeolite; while adding inorganic salts to speed up the reaction of 4A zeolite and reduce the particle size has not been reported yet

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Water glass is dissolved in NaOH solution to prepare sodium silicate solution (Na 2 O: 117g / L, SiO 2 : 366g / L), aluminum hydroxide was dissolved in NaOH solution to prepare sodium aluminate solution (Na 2 O: 75g / L, Al 2 o 3 : 74g / L). Put 400mL of the above sodium aluminate solution into the crystallizer, then add 30g of sodium chloride, stir well, and then press SiO 2 / Al 2 o 3 =2 After adding the above sodium silicate solution, stir for 8 minutes, raise the temperature to 90°C, carry out crystallization under static or stirring, and the residence time is 120 minutes. After crystallization, the mother liquor is removed by a filter washing device and the pH value is washed with deionized water to 9, and the filtered mother liquor can be reused in the preparation of sodium aluminate solution. Finally, it is dried into powder by drying equipment at 120°C to obtain ultrafine 4A zeolite products.

Embodiment 2

[0024] Sodium silicate is dissolved in NaOH solution to prepare sodium silicate solution (Na 2 O: 100g / L, SiO 2 : 300g / L), sodium metaaluminate solution was dissolved in NaOH solution to prepare sodium aluminate solution (Na 2 O: 110g / L, Al 2 o 3 : 100g / L). Put 400mL of the above sodium aluminate solution into the crystallizer, then add 30g of sodium chloride, stir well, and then press SiO 2 / Al 2 o 3 =2 After adding the above sodium silicate solution, stir for 8 minutes, heat up to 82°C, carry out crystallization statically or under stirring, and the residence time is 100 minutes. After crystallization, the mother liquor is removed by a filter washing device and the pH value is washed with deionized water to 10, and the filtered mother liquor can be reused in the preparation of sodium aluminate solution. Finally, it is dried into powder by drying equipment at 180°C to obtain ultrafine 4A zeolite products.

Embodiment 3

[0026] Silica particles were dissolved in NaOH solution to prepare sodium silicate solution (Na 2 O: 130g / L, SiO 2 : 400g / L), aluminum hydroxide was dissolved in NaOH solution to prepare sodium aluminate solution (Na 2 O: 150g / L, Al2O3: 150g / L). Put 400mL of the above-mentioned sodium aluminate solution into the crystallizer, then add 7.6g of sodium chloride, stir well, and press SiO 2 / Al 2 o 3 =3 After adding the above-mentioned sodium silicate solution, stir for 8 minutes, raise the temperature to 90°C, carry out crystallization under static or stirring, and the residence time is 50 minutes. After crystallization, the mother liquor is removed by a filter washing device and the pH value is washed with deionized water to 8, and the filtered mother liquor can be reused in the preparation of sodium aluminate solution. Finally, it is dried into powder by drying equipment at 200°C to obtain ultrafine 4A zeolite products.

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Abstract

A process for quickly synthesizing superfine 4A zeolite includes such steps as dissolving Si source in the solution of sodium hydroxide to obtain solution of sodium silicate, dissolving Al source in the solution of sodium hydroxide to obtain solution of sodium aluminate, adding inorganic sodium salt to said solution of sodium aluminate, stirring, adding the solution of sodium silicate, regulating pH greater than II, stirring to become colloid, heating, crystallizing, filtering water washing and drying at 100-300 deg.C.

Description

technical field [0001] The invention belongs to a synthesis method of 4A zeolite, in particular to a rapid synthesis method of ultrafine 4A zeolite. Background technique [0002] There are few studies on the effects of additives on the crystallization rate and physicochemical properties of zeolites. CharnellJF. et al reported the method of changing the crystallization size of A-type zeolite in "Journal of Crystal Growth" magazine 1971, page 291, volume 8 (called the Charnell method, that is, adding triethanolamine in the gel, which can make A-type zeolite crystallization Particle size increases, and the reaction rate slows down); Schoeman BJ. etc. reported adding tetramethylammonium hydroxide to the reaction system to accelerate the reaction rate in the 1994 volume 110 page of "Zeolites" magazine, and the 4A type zeolite particle size decreased Small method; Werner Stober et al reported the method of adding ethanol in the gel to reduce the particle size of zeolite in Colloi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/14C01B39/16
Inventor 吴刚张高勇杨效益张威王万绪杨秀全赵郁梅谷浩
Owner CHINA RES INST OF DAILY CHEM IND
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