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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

AI Technical Summary

Problems solved by technology

The resulting gel is very viscous and difficult to handle, which also results in poor reproducibility of this method
In addition, the organic template R(OH) 2 The cost is expensive, which increases the synthesis cost

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
Effect test

Embodiment 1

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

[0036] SEM of produ...

Embodiment 2

[0038] Mix 1.5mL deionized water and 3.0mL TMHDA well, add 0.104g GeO 2 , 0.22mL of silica sol, add 0.12mL of hydrofluoric acid (40wt%) under stirring, continue to stir until a uniform silicon germanium gel is formed, then transfer it to a polytetrafluoroethylene reactor, and statically crystallize at 180°C for 7 sky. The proportion of reaction raw materials is 0.5SiO 2 : 0.5GeO2 :7TMHDA:42H 2 O: 1.4HF. After the reactor was cooled to room temperature, the product was suction filtered, washed with water for 4 times, and dried at 85°C to obtain product 2.

[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 a high degree of crystallinity.

[0040] The SEM of Product 2 as Figure 4 . Product 2 has a typical strip crystal morphology with a size of about 20-30 μm.

Embodiment 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 to stir until a uniform silicon germanium gel is formed, then transfer to a polytetrafluoroethylene reactor, and statically crystallize at 180°C for 7 days. The proportion of reaction raw materials is 0.5SiO 2 : 0.5GeO 2 :7TMHDA:42H 2 O: 1.4NH 4 F. After the reaction kettle was cooled to room temperature, the product was filtered with suction, washed with water for 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 a high degree of crystallinity.

[0044] The SEM of product 3 as Image 6 . Product 3 has a bar-shaped crystal morphology, and the size is 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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