Catalyst for hydrogenation reaction and preparation method for same

Patent metadata

Field	Value
Publication number	US-11878286-B2
Application number	US-201917299311-A
Country	US
Kind code	B2
Filing date	Oct 28, 2019
Priority date	Dec 31, 2018
Publication date	Jan 23, 2024
Grant date	Jan 23, 2024

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

The invention claimed is:

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 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.

9. 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.

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

11. A method for preparing the catalyst for the hydrogenation reaction according to claim 1 , 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.

12. The method of claim 11 , wherein a temperature of the hydrogen atmosphere is 200-500° C.

13. The method of claim 11 , further comprising, after the step (d), sintering the prepared dried product in an air atmosphere.

14. The method of claim 13 , wherein a temperature of the air atmosphere is 200-500° C.

15. The method of claim 11 , further comprising passivating the reduced product with a nitrogen mixed gas including 0.1-20% oxygen.

16. The method of claim 11 , further comprising passivating the reduced product by depositing the reduced product in an organic solvent.

17. The method of claim 11 , wherein a pH in the step (c) of preparing the precipitate is 7-9.

18. The method of claim 11 , wherein the drying in the step (d) is performed at 100-200° C. for 5-24 hours.

19. 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 .

20. The hydrogenation method of claim 19 , wherein the hydrocarbon resin comprises dicyclopentadiene (DCPD).

21. The hydrogenation method of claim 19 , 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