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Preparation method of 3A molecular sieve

A molecular sieve, secondary exchange technology, applied in chemical instruments and methods, A-type crystalline aluminosilicate zeolite, other chemical processes, etc. question

Inactive Publication Date: 2017-02-01
汇盈化学品实业(泉州)有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Chinese patent document CN102351213A discloses a method for preparing 3A-type zeolite molecular sieves, which includes the following steps: 1) Calcination of kaolin: Calcining soft kaolin in Lincang, Yunnan Province at 550-700° C. for 3-5 hours to obtain metakaolin; 2. ), the preparation of 4A molecular sieve: according to the proportioning of metakaolin and NaOH aqueous solution: 1530g: 100mL, select metakaolin and NaOH aqueous solution, wherein, the concentration of NaOH aqueous solution is 2-5mol / L; Metakaolin and NaOH aqueous solution are mixed uniformly , raise the temperature to 60-80°C, age under strong stirring for 3-5 hours, then raise the temperature to 90-100°C, and stir at a medium speed for 4-6 hours to obtain the mixture; filter the mixture, wash the filter cake with distilled water and filter again , filter the obtained filter cake again and dry at 90-100°C for 2-4 hours to obtain 4A molecular sieve; 3), the preparation of 3A type zeolite molecular sieve: according to the ratio of 4A molecular sieve and KCl solution: 5-10g: 100mL, select 4A Molecular sieve and KCl solution, wherein the concentration of KCl solution is 2-5mol / L; 4A molecular sieve and KCl solution are reacted in a reactor at 70-90°C for 3-5 hours, and then cooled, washed and filtered. The filtered cake was dried at 90-100°C for 2-4 hours to obtain 3A zeolite molecular sieves; in the preparation process of the above-mentioned 3A molecular sieves, K ions could not be completely exchanged with Na ions in 4A molecular sieves, and the utilization rate of K ions was low. The exchange rate of ions and Na ions is low, and after filtering and washing, the washing water containing K ions will be drained, polluting the environment
[0003] In addition, the exchange rate of existing 3A molecular sieves is generally between 38-55%, and the relative water adsorption value is between 25-23.5%, and the higher the exchange rate, the lower the water adsorption value, which is a big defect. The technical problem is that it is impossible to increase K ions to replace more Na ions. When more K ions replace Na ions, more adsorption pores will be blocked, resulting in low water adsorption value.

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  • Preparation method of 3A molecular sieve

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Embodiment 1

[0018] Embodiment one, with reference to figure 1 Shown, a preparation method of 3A molecular sieves, including one-time exchange and two-time exchange.

[0019] An exchange includes the following steps: 4A molecular sieve (Na 2 O·Al 2 o 3 2SiO2 2 9 / 2H2O) and the potassium-containing washing water recovered by the secondary exchange are mixed and stirred evenly in the primary exchange tank according to the solid-to-liquid mass ratio of 1:4, then the temperature is raised to 80°C, and the exchange is performed under dynamic stirring for 30 minutes. After the exchange is completed, press filter and wash Obtain the primary filter material and washing water containing sodium ions, chloride ions and a small amount of potassium ions, discharge the washing water, and send the primary filter material into the secondary exchange;

[0020] The secondary exchange includes the following steps: first put water into the secondary exchange tank, and then put in potassium chloride, put in...

Embodiment 2

[0021] Embodiment two, refer to figure 1 Shown, a preparation method of 3A molecular sieves, including one-time exchange and two-time exchange.

[0022] An exchange includes the following steps: 4A molecular sieve (Na 2 O·Al 2 o 3 2SiO2 2 9 / 2H2O) and the potassium-containing washing water recovered by the secondary exchange are mixed and stirred evenly in the primary exchange tank according to the solid-to-liquid mass ratio of 1:4, then the temperature is raised to 75°C, and the exchange is performed under dynamic stirring for 30 minutes. After the exchange is completed, press filter and wash Obtain the primary filter material and washing water containing sodium ions, chloride ions and a small amount of potassium ions, discharge the washing water, and send the primary filter material into the secondary exchange;

[0023] The secondary exchange includes the following steps: first put water into the secondary exchange tank, and then put in potassium chloride, put in a press ...

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Abstract

The invention provides a preparation method of a 3A molecular sieve. The preparation method includes the steps of primary exchange and secondary exchange. Primary exchange includes the following steps that a 4A molecular sieve and potassium-containing washing water recycled through secondary exchange are mixed and stirred in a primary exchange tank for exchange, filter-press washing is carried out after exchange is completed, and a primary filter-press material is obtained. Secondary exchange includes the following steps that the primary filter-press material, water and potassium chloride are mixed and stirred in a secondary exchange tank for exchange, press-filter washing is carried out after exchange is completed, and a secondary press-filter material and potassium-containing washing water are obtained, the potassium-containing washing water is recycled into primary exchange to participate in exchange, and after the secondary press-filter material is subjected to press-filter washing with water, the 3A molecular sieve is prepared through drying.

Description

technical field [0001] The invention relates to a preparation method of 3A molecular sieve. Background technique [0002] Chinese patent document CN102351213A discloses a method for preparing 3A-type zeolite molecular sieves, which includes the following steps: 1) Calcination of kaolin: Calcining soft kaolin in Lincang, Yunnan Province at 550-700° C. for 3-5 hours to obtain metakaolin; 2. ), the preparation of 4A molecular sieve: according to the proportioning of metakaolin and NaOH aqueous solution: 1530g: 100mL, select metakaolin and NaOH aqueous solution, wherein, the concentration of NaOH aqueous solution is 2-5mol / L; Metakaolin and NaOH aqueous solution are mixed uniformly , raise the temperature to 60-80°C, age under strong stirring for 3-5 hours, then raise the temperature to 90-100°C, and stir at a medium speed for 4-6 hours to obtain the mixture; filter the mixture, wash the filter cake with distilled water and filter again , filter the obtained filter cake again a...

Claims

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Application Information

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IPC IPC(8): C01B39/14B01J20/18
CPCC01B39/14B01J20/186
Inventor 林成基
Owner 汇盈化学品实业(泉州)有限公司
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