Small moleoule rare-earth atom containing composite molecular sieve and preparing method thereof

A composite molecular sieve, molecular sieve technology, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolites, etc.

A composite molecular sieve, molecular sieve technology, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolites, etc.

CN1242917CInactive Publication Date: 2006-02-22CHINA PETROLEUM & CHEM CORP +1
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  • Small moleoule rare-earth atom containing composite molecular sieve and preparing method thereof
  • Small moleoule rare-earth atom containing composite molecular sieve and preparing method thereof
  • Small moleoule rare-earth atom containing composite molecular sieve and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0034] The preparation method of the gel mentioned in the step (a) is to fully mix the required substances in a certain order to obtain a homogeneous colloidal mixture. The mol ratio of each material in the gained gel is generally:

[0035] 0.8~2.0M 2 O / 1.0~5.0R / 0.01~1.0Al 2 o 3 / 10SiO 2 / 0.1~2.0NX / 50~600H 2 O / 0.01~2.0Re 2 o 3 , preferably:

[0036] 1.0~1.5M 2 O / 2.0~4.0R / 0.05~0.5Al 2 o 3 / 10SiO 2 / 0.2~1.0NX / 100~500H 2 O / 0.05~0.5Re 2 o 3 , more preferably:

[0037] 1.1~1.4M 2 O / 2.5~3.5R / 0.1~0.2Al 2 o 3 / 10SiO 2 / 0.2~0.5NX / 300~400H 2 O / 0.05~0.2Re 2 o 3 , where R is an organic template, M is a monovalent alkali metal ion, NX is a halide, and Re is a rare earth element.

[0038] The crystallization mentioned in the step (b) is carried out in a high-pressure reactor with autogenous pressure, and the crystallization temperature is 120 to 200°C, preferably 150 to 180°C, more preferably 160 to 170°C; the crystallization time is 10 ~240 hours, preferably 24~96 ho...

Embodiment 1

[0052] Using the gel with the same composition as that described in Comparative Example 2, under the condition of a stirring speed of 200 rpm, after the same crystallization and post-treatment process as in Comparative Example 2, the sample number E-1 was obtained.

[0053] Characterization: E-1 SiO 2 / Al 2 o 3 58, SiO 2 / La 2 o 3 for 92. The XRD result of sample E-1 has the characteristics of Table 1 and Table 2, see Figure 5 , see SEM Figure 6 . Depend on Figure 5 It can be seen that the product has two structural molecular sieve characteristics of MFI and TON, and the ratio of the content of molecular sieves with MFI structure and TON structure is 0.6; SEM results show that the product is needle-like crystals with an average length of about 0.4 microns.

Embodiment 2

[0058] The preparation steps of molecular sieve mainly include:

[0059] (a) The preparation process of the gel is: the same as in Example 1, except adding 20.50 grams of 82% KOH, 25.3 grams of 1,8-octanediamine, 10 grams of Al 2 (SO 4 ) 3 .18H 2 O replaces 4 g of AlCl 3 , 5.8 grams of KF, 17.4 grams of La (NO 3 ) 3 ·6H 2 O and 400 grams of water were mixed together and vigorously stirred for 20 minutes to obtain a homogeneous gel-like mixture. The molar composition of the obtained gel was:

[0060] 1.5K 2 O / 2.01R / 0.08Al 2 o 3 / 10SiO 2 / 1.0KF / 0.20La 2 o 3 / 300H 2 o

[0061] R = 1,8-octanediamine

[0062] (b) crystallization process: same as embodiment 1.

[0063] (c) Post-treatment process: Same as in Example 1, the obtained sample number is E-2.

[0064] (d) Characterization: SiO of E-2 2 / Al 2 o 3 104, SiO 2 / La 2 o3 for 44. The XRD result of sample has table 1 and table 2 characteristic, see Figure 9 , see SEM Figure 10 . Depend on Figure 9 It ...

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Abstract

A RE atoms contained composite molecular sieve in the form of small crystal grains has the characteristics of the crystalline molecular sieve with TON and MFI structures, acicular crystal grains and RE elements contained on its skeleton. It is prepared in dynamic hydrothermal condition. In the procedure of preparing gel, RE metal salt and halide are added.

Description

technical field [0001] The invention relates to a compound molecular sieve containing rare earth atoms in small grains and a preparation method thereof. More specifically, the molecular sieve provided by the present invention has the characteristics of TON and MFI structural molecular sieves, the molecular sieve framework contains rare earth elements, and the grains are needle-shaped, and the length of the grains is less than 0.8 microns. Background technique [0002] Molecular sieves are important members of crystalline materials and have regular pore structure crystal structures (which can be characterized by XRD). Channels and cavities of crystals can be characterized in different ways. Many kinds of molecular sieves have been found, such as zeolite A, ZSM series, β, X, Y, SAPO series and other microporous molecular sieves and MCM-41 and other medium pore molecular sieves. These natural or synthetic crystalline molecular sieves are widely used in the fields of catalysis...

Claims

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Application Information

Patent Timeline
22 Feb 2006
Publication
CN1242917C
IPC
C01B39/04; C01B39/48
Inventors
刘全杰; 徐会青