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Preparation method for composite molecular sieves

A technology of composite molecular sieve and ion exchange, which is applied in the field of preparation of composite molecular sieves, can solve the problems of low shape selectivity, easy deactivation of naphthylation reaction catalysts, etc., and achieve the effect of long deactivation time

Inactive Publication Date: 2018-04-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem to be solved by the present invention is that there are problems in the prior art that the catalyst for naphthalene alkylation reaction is easily deactivated and the shape selectivity is not high.

Method used

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  • Preparation method for composite molecular sieves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Take 50g water glass (SiO 2 Content is 27.20wt%, modulus is 3.2), 0.67g aluminum sulfate, 96wt% sodium hydroxide 1.0g, deionized water 50g, 30wt% tetraethylammonium hydroxide aqueous solution 50g, mix into gel, use Adjust the pH to 13 with 10% aqueous sodium hydroxide solution and let stand for 6 hours. Then crystallization was carried out at 170° C. for 72 hours.

[0036] (2) Take the milky white slurry obtained in the previous step, wash it 5 times with deionized water, and then vacuum-dry it for 12 hours.

[0037] (3) Take the solid obtained in the previous step and bake it in a muffle furnace at 550° C. for 6 hours.

[0038] The mixed crystal raw powder obtained in the previous step is coded as A1, and it is detected by XRD powder diffraction as a mixture of ZSM-5 and ZSM-12. The ratio of ZSM-5 to ZSM-12 is 1:1.

[0039] (4) Take 10.3g of the powder obtained in the previous step, and use 1mol / L NH 4 NO 3 The 200ml solution was exchanged three times at room...

Embodiment 2

[0044] (1) 600 grams of 40% silica sol, 10.1 grams of sodium aluminate (alumina content 42%), 41.6 grams of 30wt% tetraethylammonium hydroxide (TEAOH), 168.0 grams of tetraethylammonium bromide (TEABr), 16.0 grams of sodium hydroxide and 925.1 grams of water were mixed, stirred evenly at room temperature, and left to stand for 6 hours. Then crystallization was carried out at 200° C. for 48 hours.

[0045] (2) Take the milky white slurry obtained in the previous step, wash it 5 times with deionized water, and then vacuum-dry it for 12 hours.

[0046] (3) Take the solid obtained in the previous step and bake it in a muffle furnace at 550° C. for 6 hours.

[0047] The mixed crystal raw powder obtained in the previous step is coded as A2, and it is detected by XRD powder diffraction as a mixture of ZSM-5 and ZSM-12. The ratio of ZSM-5 to ZSM-12 is 1:1.

[0048] (4) Take 200g of the powder obtained in the previous step, and use 1mol / L NH 4 NO 3 Solution 2000ml was exchanged th...

Embodiment 3

[0053] (1) Get 3.5g of aluminum tert-butoxide (wt97%), 160g of 30wt% tetraethylammonium hydroxide, 8g of sodium hydroxide mix, then add 160g TEOS (wt98%) and 140g deionized water therein, at room temperature Stir well and let stand for 4 hours. Then crystallization was carried out at 200° C. for 48 hours.

[0054] (2) Take the milky white slurry obtained in the previous step, wash it 5 times with deionized water, and then vacuum-dry it for 12 hours.

[0055] (3) Take the solid obtained in the previous step and bake it in a muffle furnace at 550° C. for 6 hours.

[0056] The mixed crystal raw powder obtained in the previous step is coded as A3, and it is detected by XRD powder diffraction as a mixture of ZSM-5 and ZSM-12. The ratio of ZSM-5 to ZSM-12 is 1:4.

[0057] (4) Take 35g of the powder obtained in the previous step, and use 2mol / L NH 4 500ml of Cl solution was exchanged three times at 80°C, each time for 8 hours.

[0058] (5) Take the solid obtained by the exchange...

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Abstract

The invention relates to a preparation method for composite molecular sieves. The method is mainly used for solving the problem in the prior art that a naphthalene alkylation catalyst is relatively poor in selectivity and meanwhile is prone to deactivation. The method comprises the following steps: mixing a silica source, an alumina source, alkali, water and a template agent so as to obtain initial gel, and then, carrying out hydrothermal crystallization, thereby preparing ZSM-5 / ZSM-12 composite molecular sieves, wherein the silica source comprises at least one of water glass, silica sol and white carbon black; the alumina source comprises at least one of aluminum alkoxide, sodium metaaluminate, aluminum sulfate and aluminum nitrate; the template agent comprises at least one of ammonium tetraethyl hydroxide, ammonium tetraethyl bromide and ammonium tetraethyl chloride; the hydrothermal crystallization is carried out for 36 to 144 hours at the temperature of 120 DEG C to 200 DEG C; thesilica-alumina ratio of the silica source SiO2 to the alumina source Al2O3 by mole is (62 to 150): 1; and the ratio of the template agent R to Si is (0.15 to 0.35): 1. Excellent catalysis performanceis displayed when the composite molecular sieves disclosed by the invention are applied to the naphthalene alkylation reaction.

Description

technical field [0001] The invention relates to the preparation of a compound molecular sieve. Background technique [0002] 2,6-dialkylnaphthalene can be oxidized to synthesize 2,6-naphthalene diacid (2,6-DNA), and 2,6-naphthalene diacid is a new type of high-performance polyester material-polyethylene naphthalate The raw material of glycol ester (PEN), compared with polybutylene terephthalate (PET), the performance of PEN is much better. PEN has superior heat resistance, mechanical properties, chemical stability, gas barrier and UV and radiation resistance; PEN has good transparency like PET, and the advantage of PEN over PET is that its use temperature is 35-55 °C higher , the tensile strength is 50% higher, and the barrier performance is 5 times higher; other markets of PEN are in the manufacture of laminates, copolymers and blends, and the application prospects are very broad. Since the 1990s, major foreign plastic manufacturers and application companies have invested...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02B01J29/80C07C2/66C07C15/24
CPCB01J29/80C01B39/023C01P2002/72C07C2/66C07C15/24
Inventor 刘远林高焕新季树芳姚晖王高伟
Owner CHINA PETROLEUM & CHEM CORP
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