EP0143423A2
Expired / Lapsed
EP
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Polyethylenimide bound chromatographic packing
Assignee: Avantor Performance Materials LLC
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Filing: 1984-11-20
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Granted: —
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Expires: 2004-11-20
Abstract
Abstract The reaction product of silica gel or controlled pore glass and polyethyleniminopropyl trimethoxy silane suitable for use as chromatographic column packing.
Inventors
- 👤 Hugh E. Ramsden
Bibliographic Details
Application Number
—
Jurisdiction
EP
Data Source
google_patents
Last Synchronized
2026-11-01 17:40
CPC Classifications
B; B01; B01D; B01D15/00; B01D15/08; B01J; B01J39/00; B01J39/26; B01J20/00; B01J20/22; B01J20/26; B01J20/281; B01J20/286; B01J20/30; B01J20/32; B01J20/3231; B01J20/3242; B01J20/3268; B01J20/3272; B01J41/00; B01J41/20
Claims Analysis
Total Claims: 24
Claim 1
Independent Claim
86 words
The covalently bound, non-crosslinked polyethylenimine reaction product of particulate silica gel having an average particle diameter of from about 3 to about 70 microns and an average pore size of from about 50 to about 1000 Angstrom units, or particulate controlled pore glass having an average particle diameter of from about 37 to about 177 microns and an average pore size of from about 40 to about 1000 Angstrom units, with polyethyleniminopropyl trimethoxy silane having an average molecular weight of from about 400 to about 1800.
Claim 2
Dependent Claim
86 words
The covalently bound, non-crosslinked polyethylenimine reaction product of particulate silica gel having an average particle diameter of from about 3 to about 70 microns and an average pore size of from about 50 to about 1000 Angstrom units, or particulate controlled pore glass having an average particle diameter of from about 37 to about 177 microns and an average pore size of from about 40 to about 1000 Angstrom units, with polyethyleniminopropyl trimethoxy silane having an average molecular weight of from about 400 to about 1800.
Claim 3
Dependent Claim
61 words
A covalently bound, non-crosslinked polyethylenimine chromatographic column packing consisting essentially of the reaction product of particulate silica gel having an average particle diameter of from about 3 to about 70 microns and an average pore size of from about 50 to about 1000 Angstrom units with polyethyleniminopropyl trimethoxy silane having an average molecular weight of from about 400 to about 1800.
Claim 4
Dependent Claim
61 words
A covalently bound, non-crosslinked polyethylenimine chromatographic column packing consisting essentially of the reaction product of particulate silica gel having an average particle diameter of from about 3 to about 70 microns and an average pore size of from about 50 to about 1000 Angstrom units with polyethyleniminopropyl trimethoxy silane having an average molecular weight of from about 400 to about 1800.
Claim 5
Dependent Claim
54 words
The packing of Claim 2 wherein the particulate silica gel has an average particle diameter of from about 5 to about 40 microns and an average pore size of from about 50 to about 330 Angstrom units and the polyethyleniminopropyl trimethoxy silane has an average molecular weight of from about 400 to about 600.
Claim 6
Dependent Claim
42 words
The packing of Claim 2 wherein the particulate silica gel has an average particle diameter of about 40-62 microns and an average pore size of about 420 Angstrom units and the polyethyleniminopropyl trimethoxy silane has an average molecular weight of about 1000.
Claim 7
Dependent Claim
39 words
The reaction product of Claim 1 which is converted to a weakly acidic carboxylated product containing from about 0.3 to to about 1.2 carboxyl milliequivalent per gram by reaction with a dibasic acid anhydride in an inert organic solvent.
Claim 8
Dependent Claim
33 words
The reaction product of Claim 1 which is converted to a weakly acidic carboxylated product containing about 0.8 carboxyl milliequivalent per gram by reaction with succinic acid anhydride in an inert organic solvent.
Claim 9
Independent Claim
161 words
A method for preparing a covalently bound, non-crosslinked polyethylenimine chromatographic column packing which comprises: a. reacting particulate silica gel having an average particle diameter of from about 3 to about 70 microns and an average pore size of about 50 to about 1000 Angstrom units, or particulate controlled pore glass having an average particle diameter of from about 37 to about 177 microns and an average pore size of from about 40 to about 1000 Angstrom units, in an inert organic solvent slurry with a lower alkanolic solution of polyethyleniminopropyl trimethoxy silane having an average molecular weight of from about 400 to about 1800, said reaction being conducted at ambient to refluxing temperature for about 2 to about 50 hours; b. recovering the resultant solid fraction from the reaction mixture; and c. heating said solid fraction at a temperature and for a time sufficient to dry and complet- ly bond the silane to the respective silica gel or controlled pore glass.
Claim 10
Independent Claim
161 words
A method for preparing a covalently bound, non-crosslinked polyethylenimine chromatographic column packing which comprises: a. reacting particulate silica gel having an average particle diameter of from about 3 to about 70 microns and an average pore size of about 50 to about 1000 Angstrom units, or particulate controlled pore glass having an average particle diameter of from about 37 to about 177 microns and an average pore size of from about 40 to about 1000 Angstrom units, in an inert organic solvent slurry with a lower alkanolic solution of polyethyleniminopropyl trimethoxy silane having an average molecular weight of from about 400 to about 1800, said reaction being conducted at ambient to refluxing temperature for about 2 to about 50 hours; b. recovering the resultant solid fraction from the reaction mixture; and c. heating said solid fraction at a temperature and for a time sufficient to dry and complet- ly bond the silane to the respective silica gel or controlled pore glass.
Claim 11
Independent Claim
124 words
A method for preparing a covalently bound, non-crosslinked polyethylenimine chromatographic column packing which comprises: a. reacting particulate silica gel having an average particle diameter of from about 3 to about 70 microns and an average pore size of about 50 to about 1000 Angstrom units in an inert organic solvent slurry with a lower alkanolic solution of polyethyleniminopropyl trimethoxy silane having an average molecular weight of from about 400 to about 1800, said reaction being conducted at ambient to refluxing temperature for about 2 to about 50 hours; b. recovering the resultant solid fraction from the reaction mixture; and c. heating said solid fraction at a temperature and for a time sufficient to dry and complet- ly bond the silane to the silica gel.
Claim 12
Independent Claim
124 words
A method for preparing a covalently bound, non-crosslinked polyethylenimine chromatographic column packing which comprises: a. reacting particulate silica gel having an average particle diameter of from about 3 to about 70 microns and an average pore size of about 50 to about 1000 Angstrom units in an inert organic solvent slurry with a lower alkanolic solution of polyethyleniminopropyl trimethoxy silane having an average molecular weight of from about 400 to about 1800, said reaction being conducted at ambient to refluxing temperature for about 2 to about 50 hours; b. recovering the resultant solid fraction from the reaction mixture; and c. heating said solid fraction at a temperature and for a time sufficient to dry and complet- ly bond the silane to the silica gel.
Claim 13
Dependent Claim
18 words
The method of Claim 8 wherein heating step c is conducted at about 40-120°C for about 1-4 hours.
Claim 14
Independent Claim
198 words
A method for preparing a covalently bound, non-crosslinked polyethylenimine chromatographic column packing which comprises: a. reacting particulate silica gel having an average particle diameter of from about 3 to about 70 microns and an average pore size of about 50 to about 1000 Angstrom units, or particulate controlled pore glass having an average particle diameter of from about 37 to about 177 microns and an average pore size of from about 40 to about 1000 Angstrom units, in an inert organic solvent slurry with a lower alkanolic solution of polyethyleniminopropyl trimethoxy silane having an average molecular weight of from about 400 to about 1800, said reaction being conducted at ambient to refluxing temperature for about 2 to about 50 hours; b. recovering the resultant solid fraction from the reaction mixture; c. heating said solid fraction at a temperature and for a time sufficient to dry and complet- ly bond the silane to the respective silica gel or controlled pore glass; and d. converting the resultant covalently bound, non-crosslinked product to a weakly acidic carboxylated product containing from about 0.3 to about 1.2 carboxyl milliequivalent per gram by reaction with a dibasic acid anhydride in an inert organic solvent.
Claim 15
Independent Claim
198 words
A method for preparing a covalently bound, non-crosslinked polyethylenimine chromatographic column packing which comprises: a. reacting particulate silica gel having an average particle diameter of from about 3 to about 70 microns and an average pore size of about 50 to about 1000 Angstrom units, or particulate controlled pore glass having an average particle diameter of from about 37 to about 177 microns and an average pore size of from about 40 to about 1000 Angstrom units, in an inert organic solvent slurry with a lower alkanolic solution of polyethyleniminopropyl trimethoxy silane having an average molecular weight of from about 400 to about 1800, said reaction being conducted at ambient to refluxing temperature for about 2 to about 50 hours; b. recovering the resultant solid fraction from the reaction mixture; c. heating said solid fraction at a temperature and for a time sufficient to dry and complet- ly bond the silane to the respective silica gel or controlled pore glass; and d. converting the resultant covalently bound, non-crosslinked product to a weakly acidic carboxylated product containing from about 0.3 to about 1.2 carboxyl milliequivalent per gram by reaction with a dibasic acid anhydride in an inert organic solvent.
Claim 16
Dependent Claim
94 words
A chromatographic column suitable for liquid chromatography packed with covalently bound, non-crosslinked polyethylenimine reaction product of particulate silica gel having an average particle diameter of from about 3 to about 70 microns and an average pore size of from about 50 to about 1000 Angstrom units, or particulate controlled pore glass having an average particle diameter of from about 37 to about 177 microns and an average pore size of from about 40 to about 1000 Angstrom units, with polyethyleniminopropyl trimethoxy silane having an average molecular weight of from about 400 to about 1800.
Claim 17
Dependent Claim
94 words
A chromatographic column suitable for liquid chromatography packed with covalently bound, non-crosslinked polyethylenimine reaction product of particulate silica gel having an average particle diameter of from about 3 to about 70 microns and an average pore size of from about 50 to about 1000 Angstrom units, or particulate controlled pore glass having an average particle diameter of from about 37 to about 177 microns and an average pore size of from about 40 to about 1000 Angstrom units, with polyethyleniminopropyl trimethoxy silane having an average molecular weight of from about 400 to about 1800.
Claim 18
Dependent Claim
62 words
A chromatographic column suitable for liquid chromatography packed with covalently bound, non-crosslinked polyethylenimine reaction product of particulate silica gel having an average particle diameter of from about 3 to about 70 microns and an average pore size of from about 50 to about 1000 Angstrom units with polyethyleniminopropyl trimethoxy silane having an average molecular weight of from about 400 to about 1800.
Claim 19
Dependent Claim
62 words
A chromatographic column suitable for liquid chromatography packed with covalently bound, non-crosslinked polyethylenimine reaction product of particulate silica gel having an average particle diameter of from about 3 to about 70 microns and an average pore size of from about 50 to about 1000 Angstrom units with polyethyleniminopropyl trimethoxy silane having an average molecular weight of from about 400 to about 1800.
Claim 20
Dependent Claim
62 words
A chromatographic column suitable for liquid chromatography packed with covalently bound, non-crosslinked polyethylenimine reaction product of particulate silica gel having an average particle diameter of from about 5 to about 40 microns and an average pore size of from about 50 to about 300 Angstrom units with polyethyleniminopropyl trimethoxy silane having an average molecular weight of from about 400 to about 600.
Claim 21
Dependent Claim
62 words
A chromatographic column suitable for liquid chromatography packed with covalently bound, non-crosslinked polyethylenimine reaction product of particulate silica gel having an average particle diameter of from about 5 to about 40 microns and an average pore size of from about 50 to about 300 Angstrom units with polyethyleniminopropyl trimethoxy silane having an average molecular weight of from about 400 to about 600.
Claim 22
Dependent Claim
50 words
A chromatographic column suitable for liquid chromatography packed with covalently bound, non-crosslinked polyethylenimine reaction product of particulate silica gel having an average particle diameter of about 40-62 microns and an average pore size of about 420 Angstrom units with polyethyleniminopropyl trimethoxy silane having an average molecular weight of about 1000.
Claim 23
Dependent Claim
50 words
A chromatographic column suitable for liquid chromatography packed with covalently bound, non-crosslinked polyethylenimine reaction product of particulate silica gel having an average particle diameter of about 40-62 microns and an average pore size of about 420 Angstrom units with polyethyleniminopropyl trimethoxy silane having an average molecular weight of about 1000.
Claim 24
Dependent Claim
17 words
. 15. A chromatographic column suitable for liquid chromatography packed with the carboxylated product of Claim 5.
References Cited (Backward Citations)
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