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Hydrothermal synthesis method of 4A molecular sieve

A technology of hydrothermal synthesis and molecular sieve, which is applied in the direction of A-type crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, etc., can solve the problems of low crystallinity and purity of 4A molecular sieve, low solid phase yield, etc.

Active Publication Date: 2015-02-11
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] In the prior art, the 4A molecular sieve synthesized by the hydrothermal method has a low solid-phase yield, and the increase of the solid-phase yield by increasing the aluminum and silicon raw materials easily leads to the problem of low crystallinity and purity of the 4A molecular sieve, the purpose of the present invention To provide a method for hydrothermal synthesis of 4A molecular sieve with higher solid phase yield, the crystallinity and purity of the 4A molecular sieve prepared by the method are higher

Method used

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Embodiment 1

[0078] A kind of hydrothermal synthesis method of 4A molecular sieve, comprises the steps:

[0079] (1) Initial slurry preparation: crush natural kaolin with a kaolinite content of 93.5wt% through a 100-mesh sieve, and roast at 700°C for 3 hours to obtain roasted powder, which is silicon and aluminum raw materials; select roasted powder 20kg, add 50kg24wt % sodium hydroxide aqueous solution, stirring and mixing to obtain initial slurry;

[0080] (2) Aging treatment: aging the initial slurry prepared in step (1) at room temperature for 48 hours to obtain aged slurry;

[0081] (3) Initial crystallization: put the aged slurry obtained in step (2) in an insulated stirring mill for mechanochemical treatment by ball milling, the speed of the agitator is 150r / min, raise the temperature of the system and keep it at 90-100°C, Keep warm for 60 minutes;

[0082] (4) Late stage crystallization: Under the condition of 150r / min ball milling, make the temperature 80~100℃, reduce the ball m...

Embodiment 2

[0090] A kind of hydrothermal synthesis method of 4A molecular sieve, comprises the steps:

[0091] (1) Initial slurry preparation: crush natural kaolin with a kaolinite content of 93.5wt% through a 100-mesh sieve, and roast at 700°C for 3 hours to obtain roasted powder, which is silicon and aluminum raw materials; select roasted powder 20kg, add 40kg10wt % sodium hydroxide aqueous solution, stirring and mixing to obtain initial slurry;

[0092] (2) Aging treatment: aging the initial slurry prepared in step (1) at room temperature for 48 hours to obtain aged slurry;

[0093] (3) Initial crystallization: put the aged slurry obtained in step (2) in an insulated stirring mill for mechanochemical treatment by ball milling, the speed of the agitator is 150r / min, raise the temperature of the system and keep it at 90-100°C, Keep warm for 20 minutes;

[0094] (4) Later stage crystallization: Under the condition of 150r / min ball milling, slowly add 7kg of solid sodium hydroxide to th...

Embodiment 3

[0100] A kind of hydrothermal synthesis method of 4A molecular sieve, comprises the steps:

[0101] (1) Preparation of initial slurry: crush coal-series kaolin with a kaolinite content of 91.6wt% through a 100-mesh sieve, and roast at 850°C for 2 hours to obtain roasted powder, which is silicon and aluminum raw materials; select roasted powder 25kg, add Add 100 g of water reducer sodium hexametaphosphate to 40 kg of 15 wt % sodium hydroxide aqueous solution, stir and mix to obtain initial slurry;

[0102] (2) Aging treatment: aging the initial slurry prepared in step (1) at room temperature for 24 hours to obtain aged slurry;

[0103] (3) Initial crystallization: place the aged slurry obtained in step (2) in an insulated stirring mill, perform mechanochemical treatment, raise the temperature of the system and keep it at 80-95°C, keep it warm for 1 hour, and perform initial crystallization;

[0104] (4) Later stage crystallization: under the condition of 600r / min ball milling,...

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Abstract

The invention relates to a hydrothermal synthesis method of a 4A molecular sieve. The hydrothermal synthesis method is characterized in that a ratio of water to sodium is not more than 25, and mechanochemical treatment is carried out. The preparation method of the 4A molecular sieve improves the solid phase yield of the hydrothermal synthesized 4A molecular sieve, guarantees the phase purity of the 4A molecular sieve, reduces the amount of water and the emission of wastewater, and also reduces the device and personnel investment.

Description

technical field [0001] The invention relates to a hydrothermal synthesis method of 4A molecular sieve, in particular to a hydrothermal synthesis method capable of increasing the solid-phase yield of 4A molecular sieve. Background technique [0002] The chemical formula of 4A molecular sieve is Na 12 al 12 Si 12 o 48 27H 2 O is a three-dimensional framework compound composed of silicon-oxygen and aluminum-oxygen tetrahedra. It belongs to the cubic crystal system. It is composed of an 8-membered ring connected with 6 similar holes, and its channel size is about 0.4nm. Among them, the sodium ions of the 4A molecular sieve stable framework can interact with various ions (Ag + 、Ti 2+ 、K + , NH 4 + , Li + 、Cs + , Zn 2+ 、Ba 2+ , Ca 2+ 、Co 2+ 、Ni 2+ 、Cd 2+ , Hg 2+ , Mg 2+ and Cu 2+ etc.) for ion exchange, for example: 66.7% of sodium ions can be exchanged with potassium ions, and 75% of sodium ions can be exchanged with calcium ions to form 3A and 5A molecular si...

Claims

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Application Information

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IPC IPC(8): C01B39/14C01B39/18
CPCC01B39/14C01B39/18
Inventor 卢旭晨王体壮
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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