US3795313A
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Chromatographic packing with chemically bonded organic stationary phases
Assignee: EIDP Inc
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Filing: 1972-10-25
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Granted: 1974-03-05
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Expires: 1992-10-25
Abstract
Abstract A process for making a chromatographic packing having a polymeric stationary phase in which molecules having the formula WHEREIN R3'' is a hydroxyl, or an aliphatic or aromatic hydrocarbon monovalent radical, and R4 is a monovalent aliphatic or aromatic hydrocarbon radical, are partially prepolymerized, chemically bonded to a polyvalent metal-containing substrate, the metal having a valence of 3-5, and futher polymerized. The polymeric stationary phase has a repeating unit of the formula WHEREIN A is -O- or a monovalent aliphatic or aromatic hydrocarbon radical, and is chemically bonded to the surface of the substrate by an LINKAGE, WHERE SILICON IS PART OF A REPEATING UNIT.
Inventors
- 👤 J Kirkland
- 👤 P Yates
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 16:37
CPC Classifications
C; C08; C08G; C08G83/00; C08G83/001; B; B01; B01J; B01J20/00; B01J20/02; B01J20/10; B01J20/103; B01J20/28; B01J20/28002; B01J20/28004; B01J20/28054; B01J20/28057; B01J20/281; B01J20/286; B01J20/288; B01J20/30; B01J20/32; B01J20/3202; B01J20/3204; B01J20/3214; B01J20/3217; B01J20/3231; B01J20/3242; B01J20/3268; B01J20/3272; B01J20/328; B01J20/3282; B01J41/00; B01J41/20; C08G65/00; C08G65/02; C08G65/04; C08G65/22; B01J2220/00; B01J2220/50; B01J2220/54; B01J2220/58; B01J2220/80; B01J2220/84; B01J2220/86
Claims Analysis
Total Claims: 25
Claim 1
Independent Claim
33 words
The process of producing an improved chromatographic packing with a chemically-bonded polymolecular stationary phase comprising: a. heating a solution of a polymerizable compound in a substantially non-aqueous solvent, said compound having the formula
Claim 2
Dependent Claim
38 words
The process of producing an improved chromatographic packing with a chemically-bonded polymolecular stationary phase comprising: a. contacting the surface of a silica-containing substrate with a solution of a polymerizable compound in a solvent, said compound having the formula
Claim 3
Dependent Claim
40 words
The process of claim 2 wherein prior to heating said solution of said polymerizable compound, said polymerizable compound is formed by heating a solution of a reagent compound dissolved in said substantially non-aqueous solvent, said reagent compound having the formula
Claim 4
Dependent Claim
12 words
The process of claim 4 wherein said non-aqueous solvent is an ether.
Claim 5
Dependent Claim
12 words
The process of claim 5 wherein said ether is tetrahydrofuran or dioxane.
Claim 6
Dependent Claim
13 words
The process of claim 6 wherein said substrate comprises silica particles or gel.
Claim 7
Dependent Claim
39 words
The process of claim 7 wherein prior to heating said solution whereby polymerization of said polymerizable compound is at least initiated, the pH of said solution is adjusted to a value within the range of about 3 to 6.
Claim 8
Dependent Claim
18 words
The process of claim 8 wherein acEtic acid is added to adjust the pH to within said range.
Claim 9
Dependent Claim
12 words
The process of claim 8 wherein R1 and R2 are the same.
Claim 10
Dependent Claim
14 words
The process of claim 10 wherein R3 is the same as R1 and R2.
Claim 11
Dependent Claim
21 words
The process of claim 4 wherein R1 and R2 are selected from the group consisting of -OCH3, -OC2H5, -OC2H4OCH3, and -OOCCH3.
Claim 12
Dependent Claim
30 words
The process of claim 8 wherein said compound is selected from the group consisting of gamma-glycidoxypropyltrimethoxysilane, beta-(3,4-epoxycyclohexyl)-ethyltrimethoxysilane, gamma-aminopropyl triethoxysilane, N-beta-(aminoethylgamma-amino)-propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, methyltriethoxysilane, phenyltriethoxysilane, amyltriethoxysilane, methyltrimethoxysilane, diphenyldiethoxysilane, 3-chloropropyl-trimethoxysilane, beta-cyanoethyltriethoxysilane, and beta-cyanoethyl-methyldiethoxysilane.
Claim 13
Dependent Claim
46 words
The process of claim 4 wherein R1, R2 and R3 of a first portion of said reagent compound are alkoxyl, and R1 and R2 of a second portion of said reagent compound are alkoxyl and R3 of said second portion is neither a hydroxyl nor alkoxyl.
Claim 14
Dependent Claim
17 words
The process of claim 2 wherein subsequent to said further heating, said R1 is further chemically reacted.
Claim 15
Dependent Claim
43 words
An improved chromatographic packing comprising a polyvalent metal-containing substrate and a stationary phase, said stationary phase comprising a polymer being sufficiently porous to allow penetration by a carrier fluid and the material contained therein, said polymer having the repeating unit of the formula
Claim 16
Dependent Claim
10 words
The packing of claim 16 wherein said metal is silicon.
Claim 17
Dependent Claim
9 words
The packing of claim 17 wherein A is -O-.
Claim 18
Dependent Claim
15 words
The packing of claim 17 wherein A is a monovalent aliphatic or aromatic hydrocarbon radical.
Claim 19
Dependent Claim
15 words
The packing of claim 17 wherein said stationary phase comprises at least two copolymerized portions.
Claim 20
Dependent Claim
31 words
The packing of claim 20 wherein A in the first of said portions is -O-, and A in thhe second of said portions is a monovalent aliphatic or aromatic hydrocarbon radical.
Claim 21
Dependent Claim
14 words
The packing of claim 16 wherein said substrate comprises silica gel or silica-containing particles.
Claim 22
Dependent Claim
29 words
The packing of claim 22 wherein A is -O- and R is selected from the group consisting of gamma-glycidoxypropyl, beta-(3,4-epoxycyclohexyl)-ethyl, gamma-aminopropyl, N-beta-(aminoethyl-gamma-amino)-propyl, gamma-methacryloxypropyl, methyl, phenyl, amyl, 3-chloropropyl, and beta-cyanoethyl.
Claim 23
Dependent Claim
17 words
The packing of claim 22 wherein A is methyl or phenyl and R is phenyl or beta-cyanoethyl.
Claim 24
Dependent Claim
21 words
The packing of claim 16 wherein said stationary phase has an average thickness of about from 50 A* to 2,000 A*.
Claim 25
Dependent Claim
20 words
The packing of claim 16 wherein said polymer comprises 25 to 65 percent of the volume of said stationary phase.
References Cited (Backward Citations)
US3500616A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1977-03-04 | 1977-09-03 | 1978-03-05 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1981-03-04 | 1981-09-03 | 1982-03-05 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1985-03-04 | 1985-09-03 | 1986-03-05 | $7700.00 | Window Closed / Lapsed |