Separation of nitrogen from hydrocarbon gas using pyrolyzed sulfonated macroporous ion exchange resin

Patent metadata

Field	Value
Publication number	US-2017368493-A1
Application number	US-201615535434-A
Country	US
Kind code	A1
Filing date	Jan 6, 2016
Priority date	Jan 27, 2015
Publication date	Dec 28, 2017
Grant date	—

Abstract

A method for separating N 2 from a hydrocarbon gas mixture containing N 2 comprising the steps of: i) providing a bed of adsorbent selective for N 2 ; (ii) passing the hydrocarbon gas mixture through the bed of adsorbent to at least partially remove N 2 from the gas mixture to produce: (a) N 2 -loaded adsorbent and (b) N 2 -depleted hydrocarbon gas mixture; iii) recovering the N 2 -depleted hydrocarbon gas mixture; iv) regenerating the N 2 -loaded adsorbent by at least partially removing N 2 from the adsorbent; and v) sequentially repeating steps (ii) and (iii) using regenerated adsorbent from step (iv); wherein the adsorbent comprises a pyrolized sulfonated macroporous ion exchange resin.

First claim

1 . A method for separating N 2 from a hydrocarbon gas mixture containing N 2 comprising the steps of:
i) providing a bed of adsorbent selective for N 2 ; ii) passing the hydrocarbon gas mixture through the bed of adsorbent to at least partially remove N 2 from the gas mixture to produce: (a) N 2 -loaded adsorbent and (b) N 2 -depleted hydrocarbon gas mixture; iii) recovering the N 2 -depleted hydrocarbon gas mixture; iv) regenerating the N 2 -loaded adsorbent by at least partially removing N 2 from the adsorbent; and v) sequentially repeating steps (ii) and (iii) using regenerated adsorbent from step (iv); wherein the adsorbent comprises a pyrolized macroporous sulfonated ion exchange resin having an average micropore diameter of from 3.64 Å to 3.80 Å.

2 . The method of claim 1 wherein step (i) occurs in an adsorption chamber, and step (iv) occurs in a desorption chamber, and wherein N 2 -loaded adsorbent is continuously transferred from the adsorption chamber to the desorption chamber, and regenerated adsorbent is continuously transferred from the desorption chamber to the adsorption chamber.

3 . The method of claim 2 wherein the adsorbent located in the adsorption chamber forms a packed moving bed.

4 . The method of claim 1 wherein the step of regenerating the N 2 -loaded adsorbent comprises irradiating the adsorbent with microwaves.

5 . The method of claim 1 wherein the sulfonated macroporous ion exchange resin comprises a crosslinked macroporous copolymer matrix formed from polymerizing a reaction mixture of styrene and divinylbenzene, and wherein the resin is pyrolized at a temperature from 1225° C. to 1300° C.

6 . The method of claim 1 wherein the adsorbent has a N 2 /CH 4 selectivity of greater than 5.

7 . The method of claim 1 wherein the adsorbent as a N 2 capacity of greater than 0.5 wt %.

8 . The method of claim 1 wherein the adsorbent has a t 0.5N2 of less than 5 minutes.

9 . The method of claim 1 wherein the sulfonated macroporous ion exchange resin has a dry weight capacity of from 4.0 to 5.0 millequivalents per gram.

10 . A method for making an adsorbent having an average micropore diameter of from 3.64 Å to 3.80 Å comprising the step of pyrolizing a sulfonated macroporous ion exchange resin having a dry weight capacity of from 4.0 to 5.0 millequivalents per gram under an inert atmosphere at a temperature of from 1225° C. to 1300° C.

Assignees

• Dow Global Technologies Llc

Inventors

• Liu Junqiang
• Han Chan
• Goltz H Robert
• Rodgers Matthew L
• Matteucci Scott T
• Kem Brandon J

Classifications

• B01D2253/308

  Pore size · CPC title

• B01J20/28092

  Bimodal, polymodal, different types of pores or different pore size distributions in different parts of the sorbent · CPC title

• B01J2220/4812

  the starting material being of organic character · CPC title

• B01D2256/24

  Hydrocarbons · CPC title

• B01D2257/102

  Nitrogen · CPC title