Method of preparing catalyst for oxidative dehydrogenation and method of performing oxidative dehydrogenation using catalyst

Patent metadata

Field	Value
Publication number	US-11247195-B2
Application number	US-201816307676-A
Country	US
Kind code	B2
Filing date	Apr 26, 2018
Priority date	May 4, 2017
Publication date	Feb 15, 2022
Grant date	Feb 15, 2022

Abstract

A method of preparing a catalyst for oxidative dehydrogenation that includes coprecipitation and injecting inert gas or air at a specific time point to reduce the ratio of an inactive α-Fe2O3 crystal structure, thereby improving the activity of the catalyst. Also provided is a method of performing oxidative dehydrogenation using the catalyst. When oxidative dehydrogenation of butene is performed using the catalyst, side reaction may be reduced, and selectivity for butadiene may be improved, providing butadiene with high productivity.

First claim

The invention claimed is:

1. A method of preparing a catalyst for oxidative dehydrogenation, comprising:
preparing an aqueous metal precursor solution by adding a trivalent cationic iron (Fe) precursor and a divalent cationic metal (A) precursor to water;
coprecipitating iron and the metal (A) by adding the aqueous metal precursor solution and a basic aqueous solution to a coprecipitation bath containing an aqueous solution having a pH of 6 or more or water while agitating the aqueous solution or water in the coprecipitation bath and injecting nitrogen as an inert gas through a tube or pipe located below the surface of the aqueous solution or water in the coprecipitation bath to form a coprecipitate and a coprecipitation solution; and
burning the coprecipitate to yield the catalyst, wherein during coprecipitating, the aqueous metal precursor solution is supplied beneath the surface of the aqueous solution or water in the coprecipitation bath, and wherein the injecting nitrogen to the coprecipitation bath is performed at a speed of 0.1 to 2 L/min.

2. The method according to claim 1 , wherein the method further comprises aging the coprecipitation solution formed during coprecipitating.

3. The method according to claim 1 , wherein the trivalent cationic iron (Fe) precursor and the divalent cationic metal (A) precursor are independently one or more selected from the group consisting of a nitrate, an ammonium salt, a sulfate, and a chloride.

4. The method according to claim 1 , wherein the divalent cationic metal (A) is one or more metals selected from the group consisting of copper (Cu), radium (Ra), barium (Ba), strontium (Sr), calcium (Ca), beryllium (Be), zinc (Zn), magnesium (Mg), manganese (Mn), and cobalt (Co).

5. The method according to claim 1 , wherein a pH of the coprecipitation solution is maintained at 7 to 10 during coprecipitating.

6. The method according to claim 1 , wherein the catalyst comprises an AFe 2 O 4 crystal structure.

7. The method according to claim 1 , wherein the catalyst exhibits mixed phases comprising an AFe 2 O 4 crystal structure and an α-Fe 2 O 3 crystal structure.

8. The method according to claim 1 , wherein the coprecipitate is obtained by drying, filtering, or drying and filtering the coprecipitation solution.

9. The method according to claim 7 , wherein the catalyst satisfies Equation 1:
0≤ T 2/ T 1≤0.80,  Equation 1

wherein:
T2 is an amount of an α-Fe 2 O 3 crystal structure contained in the catalyst based on 100% by weight of a total amount of the catalyst;
T1 is an amount of an α-Fe 2 O 3 crystal structure contained in a catalyst prepared in an identical manner to that in the method of claim 7 , except that the process of supplying nitrogen as an inert gas or air is omitted, based on 100% by weight of a total content of the catalyst; and
the amount of the α-Fe 2 O 3 crystal structure is determined by measuring an intensity of a peak (2theta: 33 to 34°) corresponding to the α-Fe 2 O 3 crystal structure in an XRD diffraction analysis of the catalyst.

10. The method according to claim 1 , further comprising injecting nitrogen to the coprecipitation bath after completion of coprecipitating.

Assignees

• Lg Chemical Ltd

Inventors

• Han Sang Jin
• Ko Dong Hyun
• Cha Kyong Yong
• Han Jun Kyu
• Hwang Sun Hwan

Classifications

• B01J35/70

  characterised by their crystalline properties, e.g. semi-crystalline (catalysts comprising carbon B01J21/18; molecular sieves B01J29/00) · CPC title

• B01J2235/15

  X-ray diffraction · CPC title

• C01G49/0063

  containing zinc · CPC title

• C07C11/167

  1, 3-Butadiene · CPC title

• B01J37/03 Primary

  Precipitation; Co-precipitation · CPC title