Process and equipment for synthesis of sub-micron 4A zeolite with continuous crystallization

A submicron, crystallization technology, applied in the direction of crystalline aluminosilicate zeolite, A-type crystalline aluminosilicate zeolite, etc., can solve the problems that large particles are easy to deposit into clothes or sewer pipes, and the application effect is poor, so as to achieve convenient Industrialized production, high crystallinity, repeatable effect

Inactive Publication Date: 2009-05-13
CHINA RES INST OF DAILY CHEM IND
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Problems solved by technology

The average particle size of 4A zeolite synthesized by these processes is usually 2-4 microns, and the distribution is wide, resulting in poor application effect in detergents (mainly because 4A zeolite is insoluble in water, and large particles are easy to deposit into clothes or sewer pipes)

Method used

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  • Process and equipment for synthesis of sub-micron 4A zeolite with continuous crystallization

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Experimental program
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Effect test

Embodiment 1

[0024] Dissolve sodium silicate with a modulus of 2.0 in water or alkaline water to form a sodium silicate solution (Na 2 O: 45g / L; SiO 2 : 120g / L), sodium aluminate is dissolved in NaOH solution to configure sodium aluminate solution (Na 2 O: 90g / L; AL 2 o 3 : 60g / L). The above two solutions are based on a silicon-aluminum molar ratio of 2:1, the flow rate of the sodium aluminate solution is 0.5L / h, and the flow rate of the sodium silicate solution is 0.28L / h, and they are respectively continuously fed into the online high-shear emulsifier through the pipeline Carry out mixed reaction gelation, after passing through the aging tank, enter the crystallization tube 3 from the feed port 7 of the temperature-controllable tubular flow crystallization reactor through a pump, and control the heating through the thermometer at the temperature measuring port 4 on the upper part of the constant temperature tank 2 The regulating valve of the steam port 1 reaches the temperature of th...

Embodiment 2

[0026] Dissolve sodium silicate with a modulus of 3.2 in water or alkaline water to form a sodium silicate solution (Na 2 O: 75g / L; SiO 2 : 180g / L), sodium aluminate is dissolved in NaOH solution to configure sodium aluminate solution (Na 2 O: 70g / L; AL 2 o 3 : 40g / L). The above-mentioned two kinds of solutions are carried out according to the silicon-aluminum molar ratio of 5:1, the flow rate of the sodium aluminate solution is 1L / h, and the flow rate of the sodium silicate solution is 0.65L / h. The mixed reaction is gelled, and after passing through the aging tank, it is pumped into a temperature-controllable tubular flow crystallization reactor for crystallization (heating to 65°C, flow rate 1m / min, residence time 30min). After crystallization, the mother liquor is removed by a continuous filter washing device and the pH value is washed with deionized water to 10 (the filtered mother liquor is reused in the preparation of sodium aluminate solution). Finally, it is dried...

Embodiment 3

[0028] Sodium silicate solution (Na 2 O: 90g / L; SiO 2 : 250g / L), sodium aluminate is dissolved in NaOH solution to configure sodium aluminate solution (Na 2 O: 120g / L; AL 2 o 3 : 40g / L). The above two solutions are prepared according to the silicon-aluminum molar ratio of 6:1, the flow rate of the sodium aluminate solution is 6L / h, and the flow rate of the sodium silicate solution is 3.39L / h. The mixed reaction is gelled, and after passing through the aging tank, it is pumped into a temperature-controllable tubular flow crystallization reactor for crystallization (heating to 95°C, flow rate 0.1m / min, residence time 15min). After crystallization, the mother liquor is removed by a continuous filter washing device and the pH value is washed with deionized water to 7 (the filtered mother liquor is reused in the preparation of sodium aluminate solution). Finally, it is dried into powder by drying equipment at 300°C to obtain a submicron 4A zeolite product. Others are with emb...

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Abstract

A process for synthesizing submicron 4A zeolite by a continuous crystallization method comprises steps as follows: a sodium silicate solution with a certain concentration and a sodium aluminate solution with a certain concentration rapidly react and gel in a linear high-shear emulsifying machine; the gelled product is heated for crystallization in a controllable temperature tubular flowing crystallization reactor; then the crystallized product is washed and filtrated by a continuous filtering apparatus; and finally submicron 4A zeolite is obtained after drying. The invention has the advantages of simple and easy process method for synthesizing zeolite, small device, high preparation efficiency, continuous operation, and average grain diameter of synthesized submicron 4A zeolite smaller than 1 micron.

Description

technical field [0001] The invention belongs to a synthesis process and equipment for submicron 4A zeolite, in particular to a method and equipment for synthesizing submicron 4A zeolite by continuous crystallization. Background technique [0002] The synthesis method of 4A zeolite is mainly completed under the agitation of the reactor, as reported in U.S. Patent 4469036, adopts two-step process to synthesize 4A zeolite; in Chinese Patent 1775675A (Notice No.), it is reported that 4A zeolite is synthesized by graded kettle type continuous crystallization process In addition, AkiraYoshida et al described the process of two-step synthesis of 4A zeolite in Zeolite Magazine, 1991, volume 11, page 94 "Preparation of 4A zeolite from water glass". The average particle size of 4A zeolite synthesized by these processes is usually 2-4 microns, and the distribution is wide, resulting in poor application effect in detergents (mainly because 4A zeolite is insoluble in water, and large par...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/14
Inventor 杨效益李小秋王万绪李萍胡青霞李永峰赵惠贤
Owner CHINA RES INST OF DAILY CHEM IND
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