Preparation method for naphthalene alkylation catalyst

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

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Problems solved by technology

[0010] The technical problem to be solved by the present invention is that the catalyst is easily dea

Method used

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  • Preparation method for naphthalene alkylation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Take 50g of water glass (SiO 2 The content is 27.20wt%, the modulus is 3.2), 0.67g aluminum sulfate, 96wt% sodium hydroxide 1.0g, deionized water 50g, 30wt% tetraethylammonium hydroxide aqueous solution 50g, mixed into a gel, with Adjust the pH to 13 with 10% sodium hydroxide aqueous solution and let it stand for 6 hours. Then it was crystallized at 170°C for 72 hours.

[0032] (2) Take the milky white slurry obtained in the previous step and wash it with deionized water 5 times, and then vacuum dry for 12 hours.

[0033] (3) Take the solid obtained in the previous step and calcinate in a muffle furnace at 550°C for 6 hours.

[0034] The original mixed crystal powder obtained in the previous step is numbered as A1, and it is detected as a mixture of ZSM-5 and ZSM-12 by XRD powder diffraction. The ratio of ZSM-5 to ZSM-12 is 1:1.

[0035] (4) Take 10.3g of the powder obtained in the previous step and use 1mol / L of NH 4 NO 3 Exchange the 200ml solution three times at room t...

Embodiment 2

[0041] (1) 600 grams of 40% silica sol, 10.1 grams of sodium aluminate (42% alumina content), 41.6 grams of 30% by weight tetraethylammonium hydroxide (TEAOH), 168.0 grams of tetraethylammonium bromide (TEABr), Mix 16.0 grams of sodium hydroxide with 925.1 grams of water, stir evenly at room temperature, and let stand for 6 hours. Then it was crystallized at 200°C for 48 hours.

[0042] (2) Take the milky white slurry obtained in the previous step and wash it with deionized water 5 times, and then vacuum dry for 12 hours.

[0043] (3) Take the solid obtained in the previous step and calcinate in a muffle furnace at 550°C for 6 hours.

[0044] The mixed crystal powder obtained in the previous step is numbered as A2, and it is detected as a mixture of ZSM-5 and ZSM-12 by XRD powder diffraction. The ratio of ZSM-5 to ZSM-12 is 1:1.

[0045] (4) Take 200g of the powder obtained in the previous step and use 1mol / L of NH 4 NO 3 The 2000ml solution was exchanged three times at 80°C for 8 h...

Embodiment 3

[0051] (1) Take 3.5g of aluminum tert-butoxide (wt97%), 160g of 30wt% tetraethylammonium hydroxide, 8g of sodium hydroxide and mix, then add 160g of TEOS (wt98%) and 140g of deionized water, at room temperature Stir well and let stand for 4 hours. Then it was crystallized at 200°C for 48 hours.

[0052] (2) Take the milky white slurry obtained in the previous step and wash it with deionized water 5 times, and then vacuum dry for 12 hours.

[0053] (3) Take the solid obtained in the previous step and calcinate in a muffle furnace at 550°C for 6 hours.

[0054] The original mixed crystal powder obtained in the previous step was numbered as A3, and it was detected as a mixture of ZSM-5 and ZSM-12 by XRD powder diffraction. The ratio of ZSM-5 to ZSM-12 is 1:4.

[0055] (4) Take 35g of the powder obtained in the previous step and use 2mol / L of NH 4 Exchange 500 ml of Cl solution three times at 80°C for 8 hours each time.

[0056] (5) Take the solid obtained in the previous step, dry, and ...

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Abstract

The invention relates to a preparation method and an application for a naphthalene alkylation catalyst. The invention is mainly to solve the problems of poor selectivity and easy deactivation of a naphthalene alkylation catalyst in the prior art. The preparation method comprises the following steps: mixing a silicon source, an aluminum source, alkali, water and a template agent so as to obtain aninitial colloid, and carrying out hydrothermal crystallization so as to prepare a ZSM-5/ZSM-12 composite molecular sieve; and modifying the prepared composite molecular sieve through ion exchange, andcarrying out calcination and silylation modification so as to obtain the naphthalene alkylation catalyst, wherein the silicon source is an alkaline ammonia stable silicon sol; the aluminum source issodium metaaluminate; the inorganic alkali is sodium hydroxide or potassium hydroxide; the template is one or more selected from the group consisting of tetraethylammonium hydroxide or tetraethylammonium bromide and tetraethylammonium chloride; and in the colloid, the mol ratio of SiO2 to Al2O3 is 62 to 150, the mol ratio of R to SiO2 is 0.15 to 0.35 and the mol ratio of H2O to SiO2 is 13 to 30,wherein R represents the template agent. The modified composite molecular sieve provided by the invention shows excellent catalytic performance when used in a naphthalene alkylation reaction.

Description

Technical field [0001] The invention relates to a preparation method and application of a naphthalene alkylation catalyst. 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 excellent heat resistance, mechanical properties, chemical stability, gas barrier properties and resistance to ultraviolet and radiation; PEN has good transparency like PET. The advantage of PEN to PET is that its use temperature is 35~55℃ higher. , The tensile strength is 50% higher, and the barrier performance is 5 times higher; PEN's other markets are in the manufacture of laminates, copolymers and blends, and its application prospects are very broad. Since the 1990s, major foreign plastic manufacturers ...

Claims

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Application Information

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IPC IPC(8): B01J29/80C01B39/04C07C2/66C07C15/24
CPCB01J29/40B01J29/7034B01J29/80B01J2229/40C01B39/023C01B39/04C07C2/66C07C15/24
Inventor 刘远林高焕新季树芳姚晖王高伟胥明方华顾瑞芳魏一伦
Owner CHINA PETROLEUM & CHEM CORP
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