Monolithic column

• US 7,473,367 B2
• Filed: 08/10/2005
• Issued: 01/06/2009
• Est. Priority Date: 06/26/2002
• Status: Active Grant

• Current Assignee: Dionex Corporation (Thermo Fisher Scientific Incorporated)
• Original Assignee: Dionex Corporation (Thermo Fisher Scientific Incorporated)
• Inventors: Xie, Shaofeng
• Primary Examiner(s): Therkorn; Ernest G
• Application Number:
  US11/200,773
• Publication Number:
  US 20050274662A1
• Time in Patent Office: 1,245 Days
• Field of Search: 210/635, 210/656, 210/659, 210/198.2, 210/502.1, 95/88, 961/01
• US Class Current: 210/635
• CPC Class Codes: B01D 15/20 relating to the conditioning of the sorbent material
• CPC Class Codes: B01D 15/206 Packing or coating
• CPC Class Codes: B01J 19/0013 Controlling the temperature of the process
• CPC Class Codes: B01J 19/18 Stationary reactors having moving elements inside B01J19/08, B01J19/26 take precedence
• CPC Class Codes: B01J 20/261 obtained by reactions only involving carbon to carbon unsaturated bonds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds per se C08F
• CPC Class Codes: B01J 20/28042 Shaped bodies; Monolithic structures
• CPC Class Codes: B01J 20/28052 Several layers of identical or different sorbents stacked in a housing, e.g. in a column
• CPC Class Codes: B01J 20/283 based on silica
• CPC Class Codes: B01J 20/285 based on polymers
• CPC Class Codes: B01J 2219/00162 controlling the pressure
• CPC Class Codes: B01J 2220/54 Sorbents specially adapted for analytical or investigative chromatography
• CPC Class Codes: B01J 2220/58 Use in a single column
• CPC Class Codes: B01J 2220/82 Shaped bodies, e.g. monoliths, plugs, tubes, continuous beds
• CPC Class Codes: B01J 39/26 Cation exchangers for chromatographic processes
• CPC Class Codes: B01J 41/20 Anion exchangers for chromatographic processes
• CPC Class Codes: B01J 8/0005 Catalytic processes under superatmospheric pressure non-catalytic processes B01J3/00
• CPC Class Codes: G01N 2030/522 pressure
• CPC Class Codes: G01N 2030/525 surface properties, e.g. porosity
• CPC Class Codes: G01N 2030/528 Monolithic sorbent material
• CPC Class Codes: G01N 2030/567 coating
• CPC Class Codes: G01N 30/30 : of temperature
• CPC Class Codes: G01N 30/52 : Physical parameters
• CPC Class Codes: G01N 30/54 : Temperature
• CPC Class Codes: G01N 30/56 : Packing methods or coating methods
• CPC Class Codes: G01N 30/6091 : Cartridges
• CPC Class Codes: Y10T 29/49604 : Filter

Abstract

Permeable polymeric monolithic materials are prepared in a plastic column casing. In one embodiment, the permeable polymeric monolithic materials are polymerized by the application of heat from an external source starting at a low temperature such as 40 degrees centigrade, depending on the mixture and size of the column, and continuing at a higher temperature, such as 60 degrees centigrade. The temperature at the start of the polymerization is low enough so as not to cause exothermal run-away conditions and to avoid high heat of reaction that would prevent a substantially constant temperature across the cross-section of the column. The higher temperature is used after sufficient monomer depletion has occurred and steric interference has increased so the polymerization reaction is sufficiently slow to avoid heat of reaction generation high enough to cause significant reduction in the homogeneousness of the pore sizes.

Claims

1. A method of making a monolithic chromatography column, said method comprising the steps of

(a) adding a polymerization mixture containing a porogen to a chamber,

(b) polymerizing the polymerization mixture in the chamber to form a monolithic chromatography polymer plug in the shape of a chromatography column, at least part of said polymerizing being performed by applying sufficient pressure to the polymerization mixture to prevent wall channel openings in said polymerized monolithic polymer plug and while heating the polymerization mixture at a controlled elevated temperature, and said polymerization is performed under temperature-time moderating conditions, whereby temperature gradients are controlled to prevent substantial cross sectional variations in the monolithic polymer plug, and

(c) washing the polymer plug to remove the porogen.

2. The method of claim 1 in which the monolithic polymer plug is formed in a chromatography column.

3. The method of claim 1 in which the monolithic polymer plug is formed in a capillary tube column.

4. The method of claim 1 in which polymerizing is performed under a pressure of at least 80 psi during at least part of said polymerizing.

5. The method of claim 1 in which polymerizing is performed under a pressure of at least 150 psi during at least part of said polymerizing.

6. The method of claim 1 in which polymerizing is performed under a pressure of at least 180 psi during at least part of said polymerizing.

7. The method of claim 1 in which the pressure is applied in intervals of increasing pressures.

8. The method of claim 1 in which said pressure is sufficient to prevent voids from being formed inside the polymer plug.

9. The method of claim 1 in which said controlled elevated temperature is increased gradually during polymerization by controlling the temperature on the outside of the chamber.