Secondary growth preparation method of X type molecular sieve film on stainless steel metal net

A secondary growth, molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, membrane technology, etc., can solve problems such as blocked pores, low molecular sieve membrane permeability, and molecular sieve membrane permeability decline.

Inactive Publication Date: 2008-12-10
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

While in the porous α-Al 2 o 3 Molecular sieve membranes synthesized on ceramic sheets or tubes have only very low permeability, because during the synthesis process, α-Al 2 o 3 The aluminum and silicon on the ceramics are easy to dissolve into the reaction solution, and the molecular sieve crystals are also easy to nucleate and crystallize in the pores of the sheet and tube to block the pores. These factors all lead to a decrease in the permeability of the molecular sieve membrane.

Method used

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  • Secondary growth preparation method of X type molecular sieve film on stainless steel metal net
  • Secondary growth preparation method of X type molecular sieve film on stainless steel metal net
  • Secondary growth preparation method of X type molecular sieve film on stainless steel metal net

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Processing of metal mesh carrier:

[0048] Select 300-mesh stainless steel metal mesh (No. 540 Factory, Xinxiang, China) as the carrier, soak it in tap water, sonicate for 10 minutes under the condition of ultrasonic (ultrasonic power 100 watts, temperature 20 ℃), and finally rinse it with deionized water 3 times.

[0049] attached figure 1 It is an optical microscope photo of a 300-mesh stainless steel wire mesh.

[0050] Synthesis of seed crystals:

[0051] First, add 2.49 grams of sodium metaaluminate to 33.16 grams of water, add 2.99 grams of sodium hydroxide after dissolving, add 2.4 grams of white carbon black after dissolving, stir well and put it into a stainless steel reaction kettle lined with polytetrafluoroethylene , 2.5 days at 85°C. The product was suction-filtered and dried to obtain a seed crystal powder of X, the size of which was about 1 micron.

[0052] Preparation of the seed film:

[0053] Add 5 grams of X-type molecular sieve seed crystal powd...

Embodiment 2

[0061] The effects of different reaction times on the synthesis of X-type molecular sieve membranes were investigated.

[0062] The preparation of the seed crystal film was the same as in Example 1.

[0063] Membrane Synthesis:

[0064] Different from Example 1, the reaction time was changed into 1, 2, 3, 4, 5, 6, 7 days, with Figure 6 SEM photographs of X-type zeolite membranes obtained for different reaction times. 1 to 7 are SEM photos of X-type molecular sieve membranes reacted for 1 to 7 days, respectively.

[0065] It can be seen from the figure that after 1 day of reaction, no obvious growth of the seed layer can be seen, but the molecular sieve membrane can be washed with deionized water without separation of the seed layer on the metal mesh from the metal mesh. On the second day of reaction, the growth of the seed layer was clearly seen, but the molecular sieve membrane was still discontinuous, with many voids and defects. On the third day of the reaction, the mo...

Embodiment 3

[0067] The effects of different solution concentrations on the synthesis of X-type molecular sieve membranes were investigated.

[0068] The preparation of the seed crystal film was the same as in Example 1.

[0069] Membrane Synthesis:

[0070] Different from Example 1, in the solution ratio (molar ratio) 6.4mol NaOH: 4mol SiO 2 : 2mol NaAlO 2 : x mol H 2 In O, the values ​​of x are 190, 356, 600, 1187, 1662 and 2375 respectively. attached Figure 7SEM photographs of X-type molecular sieve membranes obtained for different solution concentrations. Among them, 1 to 6 are the SEM photos corresponding to the values ​​of x of 190, 356, 600, 1187, 1662 and 2375, respectively.

[0071] It can be seen from the figure that too high or too low solution concentration is not conducive to the growth of X-type zeolite molecular sieve membrane. When the concentration is too high, the solution is prone to homogeneous nucleation, and it is easy to crystallize and grow X-type zeolite mo...

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Abstract

The invention pertains to the preparation field of an X-type molecule sieve membrane, which in particular relates to a secondary growth method for preparing the X-type molecule sieve on a stainless steel metal mesh using pre-coated seeds. The method comprises the steps of preparing a seed suspension liquid for X-type molecule sieve, dripping the suspension liquid on the pre-treated stainless steel metal mesh, baking the mesh on a resistance wire furnace for drying with forming a seed layer covering the stainless steel metal mesh so as to obtain the seed membrane and then placing the seed membrane in a secondary reaction solution synthesized by a molecule sieve membrane to carry out a reaction for 1 to 20 days at the temperature ranging from 70 to 85 DEG C so as to obtain the X-type molecule sieve membrane. In the method, the adoption of baking for pre-coating the seeds perfectly addresses the difficult issue of coating the seeds coating on metal carriers. The X-type molecule sieve membrane prepared in the method is thin and has good continuity and few defects. The X-type molecule sieve membrane with the stainless metal mesh as carrier is much thinner than those synthesized by using other carriers. Furthermore, the molecule sieve crystal membrane has a greater permeability due to a large effective area.

Description

technical field [0001] The invention belongs to the field of preparation of X-type molecular sieve membranes, and in particular relates to a secondary growth method for preparing X-type molecular sieve membranes on stainless steel metal nets by using precoated crystal seeds. technical background [0002] X-type molecular sieve belongs to FAU-type molecular sieve, and the other type of FAU-type molecular sieve is Y-type, and the silicon-aluminum ratio (Si / Al) of the two is different. Si / Al greater than 3.0 is Y type, and less than 3.0 is X type. FAU type molecular sieve has regular microporous channels with a size of 7.4 angstroms, which is larger than that of general molecular sieves such as LTA type and MFI type molecular sieves. Therefore, the preparation and research of FAU-type molecular sieve membranes have also aroused widespread interest. There are many literatures reporting the synthesis of FAU-type molecular sieve membranes, mainly studying the separation of hydro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02B01D67/00C01B39/22B01J29/08
Inventor 朱广山裘式纶王正阳
Owner JILIN UNIV
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