Catalyst for hydrogenation reaction and preparation method for same

Patent metadata

Field	Value
Publication number	US-2022023842-A1
Application number	US-201917299311-A
Country	US
Kind code	A1
Filing date	Oct 28, 2019
Priority date	Dec 31, 2018
Publication date	Jan 27, 2022
Grant date	—

Abstract

The present invention relates to a catalyst for a hydrocarbon resin hydrogenation reaction and a preparation method for the same, wherein the catalyst is a nickel powder catalyst including nickel (Ni), copper (Cu), and sulfur (S), and more particularly, a nickel-based catalyst for a hydrogenation reaction, which is added to a hydrogenation reaction in order to improve the color of the hydrocarbon resin. According to an embodiment of the present invention, provided is a catalyst for a hydrogenation reaction, includes 40-80 parts by weight of nickel, 0.01-5 parts by weight of copper, 1-10 parts by weight of sulfur, and 10-60 parts by weight of a silica support based on 100 parts by weight of the entire dried catalyst including a support. Therefore, the catalyst can improve the quality of hydrocarbon resin. Furthermore, the catalyst can provide colorless, odorless, and transparent water-white hydrocarbon resin with improved thermal stability by removing unsaturated bonds in the hydrocarbon resin.

First claim

1 . A catalyst for a hydrogenation reaction, comprising 40-80 parts by weight of nickel, 0.01-5 parts by weight of copper, 1-10 parts by weight of sulfur, and 10-60 parts by weight of a silica support based on 100 parts by weight of the entire dried catalyst including a support.

2 . The catalyst of claim 1 , wherein the catalyst for the hydrogenation reaction has a degree of nickel reduction of 90% or more.

3 . The catalyst of claim 1 , wherein an average size of crystals of the nickel is 3-10 nm.

4 . The catalyst of claim 1 , wherein, in the catalyst particle size distribution, an average particle size is 3-10 μm, and a proportion of particles having a size of 1 μm or less is 0-10 vol %.

5 . The catalyst of claim 1 , wherein the catalyst has a specific surface area of 150-300 m 2 /g.

6 . The catalyst of claim 1 , wherein the silica support is a porous support having a specific surface area of 200-400 m 2 /g and a pore size of 10-30 nm.

7 . The catalyst of claim 1 , wherein the nickel forms a precipitate with the copper and the sulfur, is supported on the silica support, and is deposited and precipitated.

8 . The catalyst of claim 2 , wherein the degree of nickel reduction is measured by hydrogen-temperature program reduction (H 2 -TPR).

9 . The catalyst of claim 1 , wherein the catalyst has a hydrogen adsorption amount per sample weight in a range of 0.01-0.3 (mmol-H 2 /g-catalyst) through an H 2 -chemisorption measurement.

10 . The catalyst of claim 1 , wherein the catalyst has an electron absorption peak by Ni—S bond in a range of 159-166 eV (binding energy or bonding energy) through an X-ray photoelectron spectroscopy (XPS) analysis.

11 . The catalyst of claim 1 , wherein the hydrogenation reaction has a higher selectivity to olefin relative to aromatic.

12 . The catalyst of claim 1 , wherein a reactant of the hydrogenation reaction is a hydrocarbon resin.

13 . The catalyst of claim 12 , wherein, when the hydrogenation reaction is completed, the hydrocarbon resin has an APHA value of 30 or less.

14 . The catalyst of claim 1 , wherein a reactant of the hydrogenation reaction is a hydrocarbon resin including dicyclopentadiene (DCPD).

15 . The catalyst of claim 1 , wherein a reactant of the hydrogenation reaction is a hydrocarbon resin including C5 fraction.

16 . The catalyst of claim 1 , wherein a reactant of the hydrogenation reaction is a hydrocarbon resin including C9 fraction.

17 . The catalyst of claim 1 , wherein the catalyst is at least one selected from a powder form, a particle form, and a granular form.

18 . A method for preparing a catalyst for a hydrogenation reaction, the method comprising the steps of:
(a) preparing a first solution by dissolving, in a solvent, 40-80 parts by weight of nickel, 0.01-5 parts by weight of copper, and 10-60 parts by weight of a silica support based on 100 parts by weight of the entire dried catalyst including a support; (b) adding the first solution to a precipitation container, stirring the first solution, and heating the first solution to a temperature of 60-100° C.; (c) after the heating, preparing a second solution by adding a pH control agent and a sulfur precursor in a precipitation container, and preparing a precipitate by adding the second solution dropwise to the first solution; (d) washing and filtering the precipitate and drying the precipitate to prepare a dried product; and (e) reducing the dried product in a hydrogen atmosphere to prepare a reduced product.

19 . The method of claim 18 , wherein a temperature of the hydrogen atmosphere is 200-500° C.

20 . The method of claim 18 , further comprising, after the step (d), sintering the prepared dried product in an air atmosphere.

21 . The method of claim 20 , wherein a temperature of the air atmosphere is 200-500° C.

22 . The method of claim 18 , further comprising passivating the reduced product with a nitrogen mixed gas including 0.1-20% oxygen.

23 . The method of claim 18 , further comprising passivating the reduced product by depositing the reduced product in an organic solvent.

24 . The method of claim 18 , wherein a pH in the step (c) of preparing the precipitate is 7-9.

25 . The method of claim 18 , wherein the drying in the step (d) is performed at 100-200° C. for 5-24 hours.

26 . A hydrogenation method for contacting a hydrocarbon resin with hydrogen in the presence of the catalyst for the hydrogenation reaction prepared by the method of claim 18 .

27 . The hydrogenation method of claim 26 , wherein the hydrocarbon resin comprises dicyclopentadiene (DCPD).

28 . The hydrogenation method of claim 26 , wherein, when the hydrocarbon resin contacts the hydrogen and the hydrogenation reaction is completed, the hydrocarbon resin has an APHA value of 30 or less.

Assignees

• Hanwha Solutions Corp

Inventors

• Park Woo Jin
• Lee Yong Hee
• Jeon Bong Sik
• Jung Eui Geun
• Myeong Wan Jae

Classifications

• C10G45/06

  containing nickel or cobalt metal, or compounds thereof · CPC title

• B01J37/20

  Sulfiding · CPC title

• B01J37/18

  with gases containing free hydrogen · CPC title

• B01J37/08

  Heat treatment {(B01J37/0009, B01J37/0018 take precedence)} · CPC title

• B01J35/77

  Compounds characterised by their crystallite size · CPC title