A kind of method for preparing aluminide silicon borate molecular sieve in situ

A technology for preparing silicon aluminide and molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, etc., which can solve the problems of crystal structure damage, loss of active sites, and increased cost, etc., to achieve a large range of silicon-aluminum ratio, improve efficiency, and save time Effect

Inactive Publication Date: 2014-10-22
TAIYUAN UNIVERSITY OF SCIENCE AND TECHNOLOGY +2
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Problems solved by technology

Not only does this extra step add more cost in terms of time, reagents, and waste disposal, but post-processing results in partial disruption of the crystal structure and partial loss of linked active sites
Therefore, if the aluminum source is directly added to the raw material of SSZ-33 molecular sieve, it will be a low-cost and high-efficiency method to prepare aluminum-containing SSZ-33 molecular sieve in situ (no need for post-treatment borosilicate SSZ-33). Synthetic method, this scheme was not found after searching

Method used

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  • A kind of method for preparing aluminide silicon borate molecular sieve in situ
  • A kind of method for preparing aluminide silicon borate molecular sieve in situ
  • A kind of method for preparing aluminide silicon borate molecular sieve in situ

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Effect test

Embodiment 1

[0033] 1. Prepare Al-SSZ-33 molecular sieve seed crystals according to the traditional method (refer to US 5120425)

[0034] 0.14 g sodium tetraborate, 34.80 g hydroxide N,N,N-trimethyl-8-ammonium-tricyclo[5.2.1.0 2.6 ] Decane (concentration 5.69wt%) and 3.75 g sodium hydroxide solution (concentration 9.61wt%) were added to 9.20 g water and stirred evenly to obtain reaction mixture I; 3.60 g white carbon black was added to reaction mixture I and stirred evenly to obtain Reaction mixture II; the reaction mixture II was placed in a closed reactor, and crystallized in a homogeneous reactor with a rotational speed of 30 rpm. Crystallized at 160°C for 6 days to obtain B-SSZ-33 molecular sieve. B-SSZ-33 molecular sieves were calcined at 600 °C for 4 h to remove the template, and 1 mol L -1 In the aluminum nitrate solution (solid: liquid = 1:50), react at 90 °C for 3 days to obtain the Al-SSZ-33 molecular sieve sample, which is recorded as A (as the seed crystal required later).

[...

Embodiment 2

[0038] 0.22 g aluminum hydroxide, 2.00 g iodide N,N,N-trimethyl-8-ammonium-tricyclo[5.2.1.0 2.6 ] Decane, 3.20 g of sodium hydroxide solution (concentration 9.61wt%) were added to 45.00 g of water, and stirred evenly to obtain reaction mixture I; 33 molecular sieve sample A) and 1.50 g tetraethylammonium hydroxide solution (concentration 27.43wt%) were added to the reaction mixture I, stirred evenly to obtain the reaction mixture II; The crystallization was carried out in a homogeneous reactor at rpm. The crystallization is divided into two stages, the heating rate is raised to 150 °C at a rate of 1.5 °C / min, and the crystallization is carried out at 150 °C for 60 hours, and then the temperature is increased to 190 °C at a rate of 4.0 °C / min, and continued at 190 °C After crystallization for 48 hours, Al-SSZ-33 was obtained.

Embodiment 3

[0040] 0.22 g aluminum hydroxide, 1.80 g iodide N,N,N-trimethyl-8-ammonium-tricyclo[5.2.1.0 2.6 ] decane, 8.50 g N,N,N-trimethyl-8-ammonio-tricyclohydroxide [5.2.1.0 2.6 ] Decane (concentration 5.69wt%), 3.20 g sodium hydroxide solution (concentration 9.61wt%) were added in 37.00g water, stirred evenly to obtain reaction mixture I; 3.72 g white carbon black, 0.50 g seed crystal (using example 1 Self-made Al-SSZ-33 molecular sieve sample A) and 0.40 g concentrated ammonia water (concentration 28wt%) were added to the reaction mixture I, and stirred evenly to obtain the reaction mixture II; The crystallization was carried out in a homogeneous reactor at rpm. The crystallization is divided into two stages, the heating rate is raised to 160 °C at a rate of 2.0 °C / min, and the crystallization is carried out at 160 °C for 40 hours, and then the temperature is rapidly raised from 160 °C to 190 °C at 4.5 °C / min, and at 190 °C The crystallization was continued for 48 hours to obtain ...

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Abstract

The invention provides a method for preparing aluminized silicon boric acid molecular sieves in situ. The method comprises the following steps of: adding aluminum source, boron source, template and sodium hydroxide into water, uniformly stirring to obtain a reaction mixture I; adding silicon source, seed crystal and accelerator into the reaction mixture I, and uniformly stirring to obtain a reaction mixture II; and putting the reaction mixture II into a closed reaction kettle to react for 16-144 hours through process control to obtain the aluminized silicon boric acid molecular sieves. The method has the advantages of simple process, low cost, high efficiency, and in-situ synthesizing of aluminum-containing SSZ-33.

Description

technical field [0001] The invention belongs to a method for preparing molecular sieves, in particular to a method for directly preparing aluminide silicon borate molecular sieves in one step. Background technique [0002] With the increase of car ownership, the problem of air pollution caused by cars has become increasingly serious. According to the US Federal Test Cycle (FTP) test, 80% of the hydrocarbons emitted by gasoline engines come from the first 200 seconds after a cold start. This is because the exhaust temperature of the engine is low during the cold start stage, and the three-way catalyst responsible for treating exhaust gas has not yet reached its light-off temperature, so it cannot effectively catalyze the conversion of hydrocarbons and directly discharge them into the atmosphere, causing serious air pollution. Therefore, the control of cold-start hydrocarbon emissions has received increasing attention. Installing a hydrocarbon capture catalyst in the automob...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 潘瑞丽李晓峰贾妙娟晋春樊卫斌窦涛
Owner TAIYUAN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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