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Nano compound oxide preparation method

A composite oxide and nano-composite technology, which is applied in the field of preparation of nano-composite oxides, can solve problems such as difficult separation, high price, and large amount of surfactant

Active Publication Date: 2006-11-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN1316486A discloses a method for preparing a hydrogenated nano-titanium-silicon composite oxide carrier. The method uses techniques such as sol-gel method and supercritical drying to prepare a titanium-silicon composite body with a high specific surface and 2-40nm. The disadvantage is that more expensive alkoxides are used as raw materials
CN 1334243A discloses a method for preparing nano-zirconia by reverse-phase microemulsion. The amount of surfactants, hydrocarbons and water required in this method is large, the yield is extremely low, and the shortcomings of difficult separation

Method used

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  • Nano compound oxide preparation method

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Experimental program
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Effect test

Embodiment 1

[0076] Mix 50g of second-line oil and 8g of SP-80, heat to dissolve at 80°C, and mix well; heat 249g of ferric nitrate hexahydrate to 80°C to melt, slowly add to the above mixture, and mix for 15 minutes to form a uniform supersolubilized colloid. Add 300g of anhydrous aluminum chloride to 90g of ethanol to dissolve, add to the above colloid and mix evenly. 303 g of saturated ammonia water at 20° C. was added dropwise and aged for 10 hours to obtain a nano-iron-aluminum oxide gel. The composite oxide gel was calcined at 300° C. for 2 hours by flowing nitrogen gas, and then calcined at 550° C. for 8 hours by flowing nitrogen gas, that is, the nano-iron-aluminum composite oxide of this embodiment. BET specific surface: 320m 2 / g, pore volume: 0.52ml / g, average pore diameter: 5nm, average particle diameter: 32nm.

Embodiment 2

[0078] Heat and dissolve 56g of four-line oil, 4g of light deasphalted oil and 2g of SP-60 at 100°C, and mix well; heat 650g of aluminum nitrate nonahydrate to 100°C to melt, slowly add to the above mixture, and mix for 30 minutes to form a uniform super To solubilize the colloid, add 143 g of titanium tetrachloride at room temperature to the above-mentioned super solubilized colloid and mix for 18 minutes. The reactor was closed, and 145 g of ammonia gas was added at a temperature of 120° C. to obtain a nano-titanium-aluminum gel. The titanium-aluminum gel is calcined at 280° C. for 2.5 hours and 580° C. for 10 hours by blowing air into it, which is the nano-titanium-aluminum composite oxide of this embodiment. BET specific surface: 260m 2 / g, pore volume: 0.44ml / g, average pore diameter: 4.2nm, average particle diameter: 45nm.

Embodiment 3

[0080] Heat 35g of common three-line oil, 5g of minus three-line wax paste, and 15g of polyisobutenyl diethylene glycol maleate at 120°C to dissolve and mix evenly; mix 248g of aluminum chloride, 225g of zirconium oxychloride octahydrate, 260g of urea and 212g of water Mix and heat to 120°C to melt, slowly add to the above mixture, and mix for 20 minutes to form a uniform supersolubilized colloid. Seal the reactor, react at 80° C. for 4 hours, and age for 5 hours to obtain nano zirconium aluminum hydroxide gel. The zirconium-aluminum hydroxide gel is baked in air at 250°C for 2 hours, and at 600°C for 5 hours, which is the nano-zirconium-aluminum composite oxide of this embodiment. BET specific surface: 300m 2 / g, pore volume: 0.58ml / g, average pore diameter: 5nm, average particle diameter: 30nm.

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Abstract

This invention discloses a method for producing nanometer composite oxides. The procedures comprise: solubilise the molten substance in the mixture of hydrocarbon component and surfactantto form the molten salt-in-oil super solubilising colloidal group, which limits the hydroxide generated by the reaction of molten substance and precipitant in the colloidal group, so as to avoid the increase of particle size, and then obtain the nanometer composite oxides by burning.This invention is characterized of low cost of surfactant and hydrocarbon component, single distributed colloidal groups, narrow particle size distribution range and high yield. Besides, the process is simple and is adapted for industrial mass production. The nanometer composite oxide produced by this invention has large specific surface area and pore size, which makes it suitable for being used as catalyst carrier.

Description

technical field [0001] The invention relates to a preparation method of a nanocomposite oxide, in particular to a preparation method of a nanocomposite oxide used as a catalyst carrier. Background technique [0002] As an important process in petroleum refining and synthetic ammonia production using petroleum as raw material, hydrodesulfurization has always been valued by people. However, in recent years, the quality of petroleum has become heavier and worse, while the quality of products has become more stringent, and the requirements for feed materials in subsequent processes have become more and more stringent. In addition, since mankind entered the 21st century, people's awareness of environmental protection has been continuously enhanced, and environmental protection legislation has become more and more stringent. x , SO x And the restrictions on aromatics content are more stringent. In the early 1990s, the sulfur content of the European diesel standard was 2000ppm, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G1/02B01J32/00B01J37/03C04B35/622
Inventor 王鼎聪
Owner CHINA PETROLEUM & CHEM CORP
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