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Duplex metal phosphide catalyst for selective hydrogenation and olefin hydrocarbon removal as well as preparation method thereof

A catalyst and phosphide technology, applied in the field of solid catalyst and its preparation for selective hydrogenation of a small amount of olefins in aromatics, achieving good application prospects and high selective hydrogenation activity

Inactive Publication Date: 2009-07-08
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But so far there is no report on the application of phosphide catalysts in the selective hydrodeolefination

Method used

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  • Duplex metal phosphide catalyst for selective hydrogenation and olefin hydrocarbon removal as well as preparation method thereof
  • Duplex metal phosphide catalyst for selective hydrogenation and olefin hydrocarbon removal as well as preparation method thereof
  • Duplex metal phosphide catalyst for selective hydrogenation and olefin hydrocarbon removal as well as preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Preparation of TiO by coprecipitation method 2 -Ni 2 P catalyst precursor. 3.90 grams of nickel nitrate (Ni(NO 3 ) 2 ·6H 2 O) dissolved in 15 mL of deionized water, 2.70 g of titanium tetrachloride (TiCl 4 ) was dissolved in 100mL ethanol, and an appropriate amount of TiCl 4 Add the ethanol solution into the nickel nitrate solution and stir well. Added TiCl 4 The amount of ethanol solution is determined according to the total Ti / Ni molar ratio. Then 1.77 grams of diamine hydrogen phosphate ((NH 4 ) 2 HPO 4 ) was dissolved in 10mL deionized water and added dropwise to the above TiCl-containing 4 In the nickel nitrate solution in ethanol solution, a precipitate is formed. The resulting mixture was evaporated to dryness with stirring, the slurry was dried at 120° C. for 12 hours, and then calcined at 500° C. for 3 hours to obtain a catalyst precursor.

Embodiment 2

[0018] Preparation of CeO by impregnation method 2 -Ni 2 P catalyst precursor.

[0019] First, unsupported Ni was prepared by co-precipitation method 2 P catalyst precursor. Weigh 3.90 grams of nickel nitrate (Ni(NO 3 ) 2 ·6H 2 O) was dissolved in 15mL deionized water, 1.77 grams of diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) was dissolved in 10 mL of deionized water. Then the diammonium hydrogen phosphate solution was added dropwise to the nickel nitrate solution to form a precipitate. The water was evaporated to dryness, and the solid product was dried at 120°C for 12 hours, and then calcined at 500°C for 3 hours to obtain Ni 2 P precursor.

[0020] Ni will be produced 2 After the P precursor is finely ground, it is added to the metered Ce(NO 3 ) 3 ·6H 2 O aqueous solution (the concentration is determined by the catalyst Ce / Ni molar ratio), impregnated for 12 hours, then dried at 120°C for 12 hours, and calcined at 500°C for 3 hours to obtain CeO-containi...

Embodiment 3

[0022] Weigh 0.5 g of the catalyst precursor in Example 1 or 2, and put it into a fixed-bed reactor with an inner diameter of 8 mm. In a hydrogen atmosphere, raise the temperature from room temperature to 400°C at a rate of 2°C / min, then raise it to 500°C at a rate of 1°C / min, keep it for 2 hours, and then cool down to the reaction temperature naturally to prepare a bimetallic phosphide catalyst. The gas flow rate is 200mL / min, and the pressure is 1MPa. Table 1 lists the catalysts prepared by the method of the present invention.

[0023] Table 1 Catalyst prepared by the present invention

[0024]

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Abstract

The invention discloses a bi-metallic phosphide catalyst for selective hydrogenation for olefin removal and a preparation method thereof. The invention pertains to the hydrogenation refining technical field of the petroleum hydrocarbon products. The invention is characterized in that the cocatalyst of the catalyst is TiO2 or rare earth metal oxide and the main catalyst is the phosphide of one of the transition metal such as Mo, W, Fe, Co or Ni and the catalyst is prepared by conducting temperature programmed reduction on an oxidation state precursor thereof. When the molar ratio between the cocatalyst and the main catalyst is within 0.01-0.5, selective hydrogenation to the olefin of the aromatic hydrocarbon can be realized, with almost no loss of the aromatic hydrocarbon. The effect and benefit of the invention is to change the phosphide catalyst hydrogenation activity by simply changing the cocatalyst content, therefore, the bi-metallic phosphide catalyst is especially fit for the selective hydrogenation of olefin in reformate producing oil aiming at producing chemical grade BTX aromatic hydrocarbon in the refinery.

Description

technical field [0001] The invention belongs to the technical field of hydrofining of petroleum hydrocarbon products, more specifically, it relates to a solid catalyst mainly used for selective hydrogenation to remove a small amount of olefins in aromatics and a preparation method thereof. Background technique [0002] For the reforming unit in the refinery to produce chemical grade BTX (Benzene, Toluene and Xylene) aromatics, it is faced with the problem of how to remove a small amount of olefins in the condition that the aromatics are not saturated. Otherwise, the bromine value of the product and the color after pickling are unqualified, and the bromine index of the solvent oil and the copper sheet corrosion test are unqualified. At the same time, the presence of olefins in the oil will polymerize in the extraction solvent and contaminate the extraction solvent. In addition, the organic acids produced by the oxidation of olefins can cause corrosion of extraction system eq...

Claims

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Application Information

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IPC IPC(8): B01J27/185B01J21/06B01J23/10B01J37/18C10G49/04
Inventor 李翔张艳玲王安杰
Owner DALIAN UNIV OF TECH
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