Method for rapidly preparing h0h oriented MFI molecular sieve membrane by microwave heating method

A technology of microwave heating and molecular sieves, which is applied in separation methods, molecular sieves and alkali exchange compounds, chemical instruments and methods, etc., can solve the problems of complex seed crystal coating methods, expensive and other problems, and achieve shortened synthesis time, cost savings, and good repeatability sexual effect

Active Publication Date: 2018-10-12
NANJING UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the disadvantages of using expensive structure-directing agent tetrapropylammonium hydroxide, relatively complicated seed crystal coating method and long synthesis time required by ordinary heating.

Method used

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  • Method for rapidly preparing h0h oriented MFI molecular sieve membrane by microwave heating method
  • Method for rapidly preparing h0h oriented MFI molecular sieve membrane by microwave heating method
  • Method for rapidly preparing h0h oriented MFI molecular sieve membrane by microwave heating method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A kind of microwave heating method preparation hoh The method for orientation MFI type molecular sieve film, comprises the steps:

[0030] (1) Preparation of seed crystals: Mix silicon powder, sodium hydroxide, structure-directing agent tetrapropylammonium bromide and water to form a sol with a molar ratio of: H 2 O / SiO 2 =20, SDA / SiO 2 =0.05, NaOH / SiO 2 = 5, after the sol was aged, it was synthesized under microwave heating at a controlled reaction temperature of 110°C for 0.5 h, and the prepared crystals were washed with deionized water and centrifuged to obtain molecular sieve crystal seeds;

[0031](2) Support coating seed crystals: Weigh 1.0 g ellipsoidal MFI molecular sieve crystals and add them to 1000 g ethanol solution (99.9 wt%). After ultrasonic and vibration treatment, the crystals are evenly dispersed in ethanol solution to form a uniform The molecular sieve suspension, the suspension mass fraction is 0.25%. Put the porous carrier vertically into the m...

Embodiment 2

[0043] (1) Preparation of seed crystals: Mix sodium silicate, sodium hydroxide, structure directing agent tetrapropylammonium hydroxide and water to form a molar ratio of sol: H 2 O / SiO 2 =100, SDA / SiO 2 =0.5, NaOH / SiO 2 = 20, after the sol was aged, it was synthesized under microwave heating at a controlled reaction temperature of 200°C for 5 h, and the prepared crystals were washed with deionized water and centrifuged to obtain molecular sieve crystal seeds;

[0044] (2) Support coated with seed crystals: the preparation process is the same as step 2 of Example 1, except that the suction pressure is 0.08 MPa and the time is 20 seconds.

[0045] (3) hoh Synthesis of oriented MFI molecular sieve membrane: the preparation process is the same as Step 3 of Example 1, except that the structure directing agent in the synthesis sol is tetrapropylammonium iodide, and the aging time of the sol is 12 h. The synthetic sol in the reactor submerged the support body by 3 cm, the microw...

Embodiment 3

[0048] (1) Preparation of seed crystals: the preparation process is the same as Step 1 of Example 1.

[0049] (2) Support coated with seed crystals: the preparation process was the same as step 2 of Example 1, except that the suction pressure was 0.08 MPa, the time was 5 seconds, and the concentration of the seed crystal suspension was 4%.

[0050] (3) hoh Oriented MFI type molecular sieve membrane synthesis: the preparation process is the same as in Example 1 step (3), except that the molar ratio of each component of the synthetic sol is: H 2 O / SiO 2 =600, TPABr / SiO 2 =0.1, NaOH / SiO 2 = 0.5. The silicon source used was tetramethyl orthosilicate.

[0051] The prepared membrane M3 was used for n- / i-C 4 h 10 The gas separation performance was characterized in the (50 / 50) system, and the test results are shown in Table 1.

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Abstract

The invention relates to a method for rapidly preparing an h0h oriented MFI molecular sieve membrane by a microwave heating method, and is characterized in that a continuous dense crystal seed layer is formed on the surface of a porous ceramic support body pre-coated with a MFI molecular sieve. Crystal seeds are attached to the support body by a way of vacuum suction coating, and then the h0h oriented MFI molecular sieve membrane is prepared rapidly by a way of microwave heating in dilute synthetic sol. The synthetic time of the method is greatly shortened, and the cost of synthesis is greatlyreduced. The prepared h0h oriented molecular sieve membrane is applied to separation of n-butane/isobutane and n-pentane/isopentane mixed components, and has high separation performance.

Description

technical field [0001] The invention relates to the synthesis of MFI molecular sieve membranes, in particular to a kind of low-cost raw material, simple synthesis method and rapid synthesis of high performance by microwave heating. hoh Method for Orienting MFI Type Molecular Sieve Membranes. Background technique [0002] As a new type of separation membrane material, zeolite molecular sieve membrane has a regular pore structure, fine and controllable pore size distribution, good thermal and chemical stability and excellent catalytic performance, making molecular sieve membranes widely used in membrane separation, membrane reactors and other fields. It has very important application value. At present, the molecular sieve membranes reported in the literature mainly include MFI type, T type, CHA type, LTA type, MOR type and FAU type, among which the research on MFI type molecular sieve membrane is the most extensive. The main reasons are as follows: First, the pore size of th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D67/00B01D69/10B01D71/02B01D53/22C01B39/00
CPCB01D53/228B01D67/0041B01D67/0044B01D67/0048B01D69/105B01D71/028C01B39/00C01P2002/72C01P2004/03
Inventor 周荣飞马韵升宋世超崔丽云梅伟亮张骞吴阿妹吴天雷杜洋
Owner NANJING UNIV OF TECH
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