New method for preparing molybdenum phosphide by reducing molybdenum trioxide precursor

A technology of molybdenum trioxide and molybdenum phosphide, which is applied in the fields of chemical instruments and methods, catalyst activation/preparation, phosphide, etc., can solve the problems of high preparation temperature and difficult realization of programmed temperature reduction, and achieve low preparation temperature and equipment Effect of low cost, good HDS and HDN activity

Inactive Publication Date: 2010-03-03
NANKAI UNIV
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  • Claims
  • Application Information

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Problems solved by technology

Although this method is a traditional method for preparing phosphide catalysts, this method needs to break the P-O bond in the phosphate during the preparation, thus

Method used

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  • New method for preparing molybdenum phosphide by reducing molybdenum trioxide precursor
  • New method for preparing molybdenum phosphide by reducing molybdenum trioxide precursor
  • New method for preparing molybdenum phosphide by reducing molybdenum trioxide precursor

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Experimental program
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Effect test

Embodiment 1

[0015] First, 16.06 g of sodium hypophosphite (NaH 2 PO 2 .H 2 O) was added to 50mL deionized water, and after dissolving for 10min, 4.34g of MoO was added 3 . After continuing to stir for 2 hours, the resulting solution was put into a petri dish and dried at 100°C. Then put the dried precursor powder into the reactor, heat treatment at 300°C for 10 minutes under the protection of static nitrogen, and then wash the product with water and then dry it. The obtained sample is named A, and A has attached figure 1 Characteristics.

Embodiment 2

[0017] First, 2.50 g of ammonium molybdate ((NH 4 ) 6 Mo 7 o 24 .4H 2 O) was added to 27mL deionized water, and after dissolving for 10min, 4.48g of MCM-41 molecular sieves were added. After continuing to stir for 2 hours, the resulting solution was put into a petri dish and dried at 100°C. Then put the dried precursor powder into a muffle furnace, and bake it in an air atmosphere at 550°C for 2 hours to obtain a supported molybdenum trioxide (MoO 3 / MCM-41). With stirring at room temperature, 7.50 g of NaH 2 PO 2 .H 2 O was added to 27mL deionized water, and after dissolving for 10min, the supported molybdenum trioxide (MoO 3 / MCM-41). After continuing to stir for 2 hours, the resulting solution was put into a petri dish and dried at 100°C. Then put the dried precursor powder into the reactor, heat treatment at 300°C for 10min under the protection of static nitrogen, and then wash the product with water and then dry it. The obtained sample is named B, and B has att...

Embodiment 3

[0019] The preparation process is the same as that of sample B, only changing the NaH 2 PO 2 .H 2 The amount of O is 9.00 g, and other conditions remain unchanged. The obtained sample was named C, and C has attached image 3 Characteristics.

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Abstract

The invention provides a new method for preparing molybdenum phosphide by reducing the precursor of molybdenum trioxide by utilizing the phosphine generated by hypophosphite in thermal decomposition.The method comprises the steps of: adopting ammonium molybdate as a, roasting the Mo source to obtain molybdenum trioxide, and then by dipping the molybdenum trioxide in solution, and obtaining the precursor; and synthesizing loaded and unloaded molybdenum phosphide by simple thermal decomposition of the precursor at low temperature. The method is characterized in that the adopted process is simple, the preparation temperature of the molybdenum phosphide is low, the production period is short, and the preparing process needs no flowing protective gas and complex steps such as temperature raising of program and the like except simple thermal treatment at constant pressure; the used raw materials are safe and low in cost, and equipment has low cost; and due to the better HDS and HDN activity, the catalyst can be widely used in the hydrotreating of oils.

Description

technical field [0001] The invention proposes a new method for preparing molybdenum phosphide (MoP) by using phosphine produced by thermal decomposition of hypophosphite to reduce molybdenum trioxide precursor. In this method, ammonium molybdate is used as the molybdenum source to obtain molybdenum trioxide after roasting, and the obtained molybdenum trioxide is impregnated with hypophosphite solution to obtain a precursor, and the precursor is subjected to simple low-temperature heat treatment to synthesize supported and non-supported phosphating molybdenum. The present invention is characterized by simple process, low molybdenum phosphide preparation temperature, short production cycle, no need to use flowing protective gas in the preparation process, no complicated steps such as temperature program, and only simple heat treatment under normal pressure . The raw materials used are cheap and safe, and the cost of required equipment is low. This type of catalyst can be wide...

Claims

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Application Information

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IPC IPC(8): B01J27/19B01J29/78B01J37/02B01J37/08B01J37/16C01B25/08
Inventor 李伟关庆鑫张明慧
Owner NANKAI UNIV
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