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Dynamic hydrothermal synthesis method of exfoliated type MWW lamellar molecular sieve

A dynamic hydrothermal, exfoliating technology, applied in the direction of crystalline aluminosilicate zeolite, can solve the problems of complicated steps, high cost, difficult price, etc., and achieve the effect of low price and simple synthesis method

Active Publication Date: 2017-03-22
NORTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the cumbersome steps in the traditional synthesis method of ITQ-2 and the damage to the crystallinity and acidity of the MWW sheet by high temperature and high alkalinity, as well as the difficult and expensive synthesis of the structure directing agent in the one-step hydrothermal synthesis method. The problem is to provide a method for one-step synthesis of exfoliated MWW sheet molecular sieves using an industrialized and inexpensive cationic surfactant with a unique structure containing polyoxyethylene chains as a structure-directing agent

Method used

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  • Dynamic hydrothermal synthesis method of exfoliated type MWW lamellar molecular sieve
  • Dynamic hydrothermal synthesis method of exfoliated type MWW lamellar molecular sieve
  • Dynamic hydrothermal synthesis method of exfoliated type MWW lamellar molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0027] 1. According to the molar ratio of SiO 2 / Al 2 o 3 =50, OH / SiO 2 =0.14, Na / SiO 2 =0.14, HMI / SiO 2 =0.35,H 2 O / SiO 2 =45, CPAB / HMI=0.25, weigh 0.21g of sodium metaaluminate, 0.24g of sodium hydroxide, 6.22g of silica sol, 7g of CPAB, 1.45g of HMI, and 33.55mL of deionized water.

[0028] 2. Dissolve sodium hydroxide in 22.37mL deionized water to prepare sodium hydroxide aqueous solution, dissolve CPAB in 11.18mL deionized water to prepare CPAB aqueous solution; add HMI to the prepared CPAB aqueous solution, and stir for 5 hours at room temperature , to obtain a structure-directing agent mixture.

[0029] 3. Add sodium metaaluminate to the prepared sodium hydroxide aqueous solution under stirring. After the sodium metaaluminate is completely dissolved, add the silica sol and the structure-directing agent mixture in step 2 drop by drop, and then use Adjust the pH to 13.7-13.8 with 6 mol / L sodium hydroxide aqueous solution, and stir for 30 minutes at room temperatur...

Embodiment 2

[0034] 1. According to the molar ratio of SiO 2 / Al 2 o 3 =30, OH / SiO 2 =0.18, Na / SiO 2 =0.18, HMI / SiO 2 =0.5,H 2 O / SiO 2 =45, CPAB / HMI=0.25, weigh 0.28g of sodium metaaluminate, 0.42g of sodium hydroxide, 5.04g of silica sol, 5.25g of CPAB, 1.68g of HMI, and 24.19mL of deionized water.

[0035] 2. Dissolve sodium hydroxide in 16.13mL deionized water to prepare sodium hydroxide aqueous solution, and dissolve CPAB in 8.06mL deionized water to prepare CPAB aqueous solution; add HMI to the prepared CPAB aqueous solution, and stir for 5 hours at room temperature , to obtain a structure-directing agent mixture.

[0036] 3. Add sodium metaaluminate to the prepared sodium hydroxide aqueous solution under stirring. After the sodium metaaluminate is completely dissolved, add the silica sol and the structure-directing agent mixture in step 2 drop by drop, and finally Use 6 moles per liter of sodium hydroxide solution to adjust the pH of the mixture to 13.7-13.8, and stir for 30 ...

Embodiment 3

[0040] 1. According to the molar ratio of SiO 2 / Al 2 o 3 =100, OH / SiO 2 =0.2, Na / SiO 2 =0.2, HMI / SiO 2 =0.3,H 2 O / SiO 2 =50, CPAB / HMI=0.2, weigh 0.09g of sodium metaaluminate, 0.32g of sodium hydroxide, 5.72g of silica sol, 7.86g of CPAB, 1.14g of HMI, and 30.35mL of deionized water.

[0041] 2. Dissolve sodium hydroxide in 20.23mL deionized water to prepare sodium hydroxide aqueous solution, dissolve CPAB in 10.12mL deionized water to prepare CPAB aqueous solution; add HMI to the prepared CPAB aqueous solution, and stir for 8 hours at room temperature , to obtain a structure-directing agent mixture.

[0042] 3. Add sodium metaaluminate to the prepared sodium hydroxide aqueous solution under stirring. After the sodium metaaluminate is completely dissolved, add the silica sol and the structure-directing agent mixture in step 2 drop by drop, and finally Use 6 moles per liter of sodium hydroxide solution to adjust the pH of the mixture to 13.7-13.8, and stir for 30 minut...

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PUM

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Abstract

The invention discloses a dynamic hydrothermal synthesis method of an exfoliated type MWW lamellar molecular sieve. According to the method, silica sol is taken as a silicon source, sodium metaaluminate is taken as an aluminum source, HMI (hexamethyleneimine) and CPAB are taken as a structure-directing agent, and the exfoliated type MWW lamellar molecular sieve can be synthesized through dynamic hydrothermal synthesis with one step. The synthesis method is simple, and the structure-directing agent is industrialized, low in cost and suitable for industrial production of the exfoliated type MWW lamellar molecular sieve.

Description

technical field [0001] The invention belongs to the technical field of molecular sieves and porous materials, in particular to a method for dynamically hydrothermally synthesizing exfoliated MWW sheet molecular sieves. Background technique [0002] MCM-22 molecular sieve is a molecular sieve with MWW topology. The skeleton topology of MCM-22 has two different multi-dimensional channel systems, one is a two-dimensional sinusoidal network channel with an effective pore diameter of ten-membered rings (0.4nm×0.59nm); the other is composed of twelve-membered The supercage composition of the ring, the size of the cage is (0.71nm×0.71nm×1.82nm), and its opening is also a ten-membered ring. It is generally believed that the precursor of MCM-22 molecular sieve (MCM-22(P)) is a layered material formed by orderly arrangement of MWW nano-molecular sieve sheets (thickness is about 2.5nm, referred to as MWW sheet). It is a two-dimensional layered structure formed by orderly stacking of ...

Claims

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Application Information

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IPC IPC(8): C01B39/04
CPCC01B39/04C01P2002/20C01P2002/72C01P2004/03C01P2004/04
Inventor 郝青青赵东阳胡敏马晓迅陈汇勇徐龙孙鸣
Owner NORTHWEST UNIV
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