Synthesis method of nano fibrous mordenite

A technology of mordenite and nanofiber, which is applied in the field of catalytic chemistry, can solve the problems of complex preparation process of nano-mordenite, environmental pollution, high synthesis cost, etc., and achieve the effect of improving mass transfer and diffusion, simple synthesis process and good application potential

Inactive Publication Date: 2012-08-22
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Moreover, the synthesis system and preparation process of nano-mordenite are usually relatively complicated, and the organic templates and organic solvents added in some synthesis processes will also cause relatively high synthesis costs and serious environmental pollution, which limits its large-scale production to a certain extent. industrial production

Method used

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  • Synthesis method of nano fibrous mordenite
  • Synthesis method of nano fibrous mordenite
  • Synthesis method of nano fibrous mordenite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 18.2g sodium aluminate solution (NaOH 31.2wt.%, Al 2 o 3 16.8wt.%, H 2 O 52.0wt.%, the same below), 14.5g dilute sulfuric acid solution (0.3g H 2 SO 4 / ml, the same below) and 99.7g of deionized water were added to the reaction kettle and mixed evenly, then 19.6g of solid silica gel (SiO 2 92.0wt.%, H 2 O 8.0wt.%, hereinafter the same), and finally add 0.2g of mordenite as a seed crystal. The molar ratio of the reaction mixture is SiO 2 / Al 2 o 3 =10, Na 2 O / Al 2 o 3 = 1.0, H 2 O / Al 2 o 3 =225, the seed crystal addition amount is 1.0% of the total mass of the raw material silicon aluminum oxide. The reaction vessel was sealed and placed in a synthesis oven for dynamic crystallization at 164°C for 60 hours. After the reaction, the reactor was cooled, the solid and the mother liquor were centrifuged, the solid was washed with deionized water to pH 8-9, and dried in air at 100° C. for 8 hours to obtain a molecular sieve powder. The final product is pure mo...

Embodiment 2

[0022] The water content in embodiment 1 is increased by 50%, that is, the molar ratio of the reaction mixture is SiO 2 / Al 2 o 3 =10, Na 2 O / Al 2 o 3 = 1.0, H 2 O / Al 2 o 3 =337.5, the crystallization time was extended to 96 hours, and other conditions remained unchanged. The final product is pure mordenite as tested by XRD, and the XRD spectrum is shown in figure 1 C; see its SEM photo Figure 4 , TEM photo see Figure 5 , the product is in the form of nanofibers with a grain length of 3-7 microns and a width of about 40 nanometers.

[0023] Compared figure 1 A, B, and C can be seen (wherein A is the XRD spectrum of the industrially produced mordenite sample provided by Fushun Petrochemical Company): although the XRD peak positions of the three samples are the same, and they are all pure mordenite, there are obvious differences in the peak intensity and width of the three samples. difference, the peak intensity order corresponding to the crystal planes [020], [200...

Embodiment 3

[0025]Keep the raw material ratio of Example 1, change sulfuric acid into hydrochloric acid (0.2g HCl / ml), the amount of seed crystals is changed into 2.1g (add-on is 10% of the raw material silicon-aluminum oxide gross mass), and crystallization temperature is changed into At 180°C, the crystallization time was shortened to 30 hours, and other conditions remained unchanged. The final product was tested as pure mordenite by XRD, and its SEM photo is shown in Image 6 , the product is a divergent nanofiber with a grain length of 1-2 microns and a width of about 30 nanometers.

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Abstract

The invention discloses a synthesis method of nano fibrous mordenite. In the method, a silicon source, an aluminium source, inorganic acid and deionized water are utilized as reaction raw materials. The method comprises: adding a proper amount of molecular sieve seed crystal into the reaction raw materials; crystallizing for 30-160 hours at generated pressure under the hydrothermal condition of crystallization temperature of 130-200 DEG C; and synthetizing mordenite with high crystallinity. The synthetized mordenite has a regular c-axis lengthening fibrous feature, the width of the synthetized mordenite is 20-100 nanometers, and the length of the synthetized mordenite is 1-8 micronmeters. The synthesis method has the characteristics of environmental friendliness, simple process, pure crystal phase, high crystallinity, good repeatability and the like and is suitable for mass production.

Description

technical field [0001] The invention belongs to the technical field of catalytic chemistry, and in particular relates to a synthesis method of nanofibrous mordenite with elongated c-axis. Background technique [0002] Mordenite was first synthesized by Barrer et al. in 1948. It is one of the few molecular sieves that have been industrialized and has been widely used because of its good adsorption, separation and catalytic properties. The pore system of mordenite consists of 12-membered rings along the c-axis and 8-membered ring The channel, and the 8-membered ring connected to it along the b-axis direction Pore ​​composition. Mordenite is often considered to be a 12-membered ring with one-dimensional straight channel structure along the c-axis direction due to its relatively small orifice in the direction perpendicular to the c-axis and relatively tortuous channels. [0003] As an emerging material, nanomaterials can effectively accelerate reaction mass transfer, he...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/26B01J29/18B01J35/06
Inventor 徐龙伢张玲谢素娟刘盛林王清遐
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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