Preparation method of ITQ-13 molecular sieve in non-concentrated-gel system

A molecular sieve and non-condensing technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of increased synthesis cost, poor repeatability, high cost, etc., and achieve the effects of reduced loss, good crystallinity and purity, and low price

Inactive Publication Date: 2012-06-20
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The resulting gel is very viscous and difficult to handle, which also results in poor reproducibility of thi

Method used

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  • Preparation method of ITQ-13 molecular sieve in non-concentrated-gel system
  • Preparation method of ITQ-13 molecular sieve in non-concentrated-gel system
  • Preparation method of ITQ-13 molecular sieve in non-concentrated-gel system

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0033] Example 1:

[0034] First, pipette 1.5mL deionized water and 3.0mL TMHDA, mix them evenly, add 0.104g GeO to them 2 , 0.20mL ethyl orthosilicate (TEOS), add 0.12mL hydrofluoric acid (40wt%) under stirring, continue stirring until a uniform silicon germanium gel is formed, and then transfer to a polytetrafluoroethylene reactor at 180°C Under the conditions of static crystallization for 7 days. The ratio of reaction raw materials is 0.5SiO 2 :0.5GeO 2 :7TMHDA: 42H 2 O: 1.4HF. After the reaction kettle is cooled to room temperature, the product is suction filtered, washed with water 4 times, and dried at 85° C., product 1 can be obtained. The BET specific surface area of ​​product 1 measured by nitrogen adsorption is 296.87m 2 / g, the pore volume of the micropore is 0.126mL / g, and the pore diameter is

[0035] The XRD spectrum of product 1 is as follows figure 1 . It can be seen that product 1 has a typical ITH molecular sieve structure and has a high degree of crystallinit...

Example Embodiment

[0037] Example 2:

[0038] Mix 1.5mL deionized water and 3.0mL TMHDA evenly, add 0.104g GeO to it 2 , 0.22mL silica sol, add 0.12mL hydrofluoric acid (40wt%) under stirring, continue stirring until a uniform silicon-germanium gel is formed, then transfer it to a polytetrafluoroethylene reactor, and statically crystallize at 180℃. day. The ratio of reaction raw materials is 0.5SiO 2 :0.5GeO 2 :7TMHDA: 42H 2 O: 1.4HF. After the reaction kettle is cooled to room temperature, the product is suction filtered, washed with water 4 times, and dried at 85° C., product 2 can be obtained.

[0039] The XRD spectrum of product 2 is as follows image 3 . The baseline of product 2 is relatively flat, indicating that product 2 has high crystallinity.

[0040] SEM of product 2 such as Figure 4 . Product 2 has a typical bar-shaped crystal morphology, with a size of about 20-30 μm.

Example Embodiment

[0041] Example 3:

[0042] Measure 1.5mL deionized water and 3.0mL TMHDA, mix well and add 0.104g GeO 2 , 0.20mL TEOS, add 0.15g ammonium fluoride under stirring, continue stirring until a uniform silicon-germanium gel is formed, then transfer to a polytetrafluoroethylene reactor, and statically crystallize at 180°C for 7 days. The ratio of reaction raw materials is 0.5SiO 2 :0.5GeO 2 :7TMHDA:42H 2 O: 1.4NH 4 F. After the reaction kettle is cooled to room temperature, the product is filtered off with suction, washed with water 4 times, and dried at 85°C to obtain product 3.

[0043] The XRD spectrum of product 3 is as follows Figure 5 . The baseline of product 3 is relatively flat, indicating that product 3 has high crystallinity.

[0044] SEM of product 3 such as Image 6 . Product 3 has a bar-shaped crystal morphology with a size of about 20-30 μm.

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Abstract

The invention belongs to the technical field of inorganic chemistry, and relates to a method for preparing an ITQ-13 molecular sieve in a non-concentrated-gel system by taking TMHDA (Tetramethylethylenediamine) as a template agent. The method comprises the following steps of: uniformly mixing deionized water with TMHDA, adding a germanium source and a silicon source to obtain a uniform solution, adding a fluorine source, continually stirring at the room temperature to form uniform silicon-germanium sol, transferring into a reaction kettle, and standing and crystallizing at the temperature of 160-230 DEG C for 1-14 days; and cooling the reaction kettle to the room temperature, performing suction filtration on a product, washing with water, and drying to obtain the ITQ-13 molecular sieve. The method is simple and practicable, and has low price; an entire process is performed under a hydrothermal condition; and compared with the conventional process, the preparation method has the advantages that: the preparation time and crystallization time of gel are shortened, so that unnecessary loss in a production process is reduced. The obtained ITQ-13 molecular sieve keeps a high crystallinity degree and high purity, and has high thermal stability and a large specific surface area.

Description

technical field [0001] The invention belongs to the technical field of inorganic chemistry, and in particular relates to a method for preparing ITQ-13 molecular sieve in a non-concentrated gel system by using N,N,N',N'-tetramethyl-1,6-hexamethylenediamine as a template Methods. Background technique [0002] Microporous molecular sieves are widely used in adsorption, separation, ion exchange, catalysis and other fields due to their regular pore structure and nanoscale pore size. ITQ-13 molecular sieve is a zeolite with a medium pore size and an ITH-type framework structure. It has a three-dimensional intersecting channel system, in which the size of the nine-membered ring channel parallel to the [100] plane is The channel size of the ten-membered ring parallel to the [001] plane is The channel size of the ten-membered ring parallel to the [010] plane is ITQ-13 molecular sieve can be applied to the selective conversion process of hydrocarbons, such as the catalytic crac...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 徐如人于吉红任晓燕
Owner JILIN UNIV
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