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US4338404A Expired / Lapsed US ⏱️ 0.0 years remaining

Gel permeation chromatographic packing and process for producing same utilizing suspension polymerization

Assignee: Asahi Kasei Corp
•
Filing: 1981-01-26
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Granted: 1982-07-06
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Expires: 2001-01-26
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Abstract

Abstract A novel granular crosslinked copolymer suitable as a high speed liquid chromatograph packing and especially as a gel permeation chromatograph packing is disclosed. In a preferred embodiment of the invention the packing is a copolymer of styrene and divinylbenzene having a volume average particle diameter of about 2 to 50 μm, an exclusive molecular weight for a polystyrene being from about 500 to 20,000, and the weight % (X) of divinylbenzene units based on the entire monomeric units of the copolymer and the gradient (α) of the calibration curve of the polystyrene are defined by the region bounded by and including the following three lines in rectangular coordinates (α, X) ##EQU1## α=2.5 X=35 and a process for preparing the same by suspension polymerization in the presence of an initiator having specific half-life properties is disclosed.

Inventors

  • 👤 Yasuyuki Tanaka
  • 👤 Junichi Takeda
  • 👤 Kohji Noguchi

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-02 15:42
CPC Classifications
B; B01; B01J; B01J20/00; B01J20/22; C; C08; C08F; C08F212/00; C08F212/02; C08F212/04; C08F212/06

Claims Analysis

Total Claims: 16
Claim 1
Independent Claim 236 words
A packing for high speed liquid chromatography prepared by the process which comprises suspending in water a mixture consisting of 65 to 90 parts by weight of at least one monovinylbenzene, 35 to 10 parts by weight of at least one polyvinylbenzene, the total amount of the monovinylbenzene and polyvinylbenzene being 100 parts by weight, and 30 to 200 parts by weight of a solvent capable of dissolving polystyrene, and free radical-polymerizing the monovinylbenzene and the polyvinylbenzene in suspension, said polymerizaton being carried out in the presence of 0.1 to 5.0 parts by weight of at least one free radical polymerization initiator having a half-life period of about 2 to 60 minutes at 70° C., and in such a manner that at least until the polymerization conversion reaches 50%, the polymerization is effected at a temperature at which the half-life period of the polymerization initiator is in the range of about 5 to 120 minutes to thereby provide a microporous, granular cross-linked monovinylbenzene-polyvinylbenzene copolymer having a volume average particle diameter of about 2 to 50 micrometers, an exclusive molecular weight for polystyrene of about 500 to 20,000, and the weight percent (X) of polyvinylbenzene units based on the total monomeric units in the copolymer and the gradient (α) of the calibration curve of the polystyrene are defined by the region bounded by and including the following three lines in rectangular coordinates (α, X): ##EQU11## α=2.5 X=35.
Claim 2
Dependent Claim 236 words
A packing for high speed liquid chromatography prepared by the process which comprises suspending in water a mixture consisting of 65 to 90 parts by weight of at least one monovinylbenzene, 35 to 10 parts by weight of at least one polyvinylbenzene, the total amount of the monovinylbenzene and polyvinylbenzene being 100 parts by weight, and 30 to 200 parts by weight of a solvent capable of dissolving polystyrene, and free radical-polymerizing the monovinylbenzene and the polyvinylbenzene in suspension, said polymerizaton being carried out in the presence of 0.1 to 5.0 parts by weight of at least one free radical polymerization initiator having a half-life period of about 2 to 60 minutes at 70° C., and in such a manner that at least until the polymerization conversion reaches 50%, the polymerization is effected at a temperature at which the half-life period of the polymerization initiator is in the range of about 5 to 120 minutes to thereby provide a microporous, granular cross-linked monovinylbenzene-polyvinylbenzene copolymer having a volume average particle diameter of about 2 to 50 micrometers, an exclusive molecular weight for polystyrene of about 500 to 20,000, and the weight percent (X) of polyvinylbenzene units based on the total monomeric units in the copolymer and the gradient (α) of the calibration curve of the polystyrene are defined by the region bounded by and including the following three lines in rectangular coordinates (α, X): ##EQU11## α=2.5 X=35.
Claim 3
Dependent Claim 14 words
The packing of claim 1 wherein the polymerization initiator is 2,2'-azobis(2,4-dimethylvaleronitrile) or diisopropyl peroxydicarbonate.
Claim 4
Dependent Claim 34 words
The packing of claim 1 wherein the polymerization initiator is 2,2'-azobis(2,4-dimethylvaleronitrile) and at least until the polymerization conversion reaches 50%, the polymerization is carried out at a temperature of about 65° to 85° C.
Claim 5
Dependent Claim 35 words
The packing of claim 1 wherein the polymerization initiator is diisopropyl peroxydicarbonate and at least until the polymerization conversation reaches 50%, the polymerization is carried out at a temperature of about 60° to 80° C.
Claim 6
Dependent Claim 21 words
The packing of claim 1 wherein said at least one monovinylbenzene is styrene and said at least one polyvinylbenzene is divinylbenzene.
Claim 7
Dependent Claim 25 words
The packing of claim 1 wherein said polymerization initiator is selected from the group consisting of 2,2'-azobis(4-methoxy-2,4-dimethylvaleronitrile), 2,2'-azobis(2,4-dimethylvaleronitrile), isobutyryl peroxide, diisopropyl peroxydicarbonate, and di-2-ethylhexyl peroxydicarbonate.
Claim 8
Dependent Claim 34 words
The packing of claim 1 wherein the weight % (X) and the gradient (α) are defined by the region bounded by and including the following three lines in rectangular coordinates (α,X): ##EQU12## α=3 X=27.
Claim 9
Dependent Claim 35 words
The packing of claim 1, wherein the weight % (X) and the gradient (α) are defined by the region bounded by and including the following four lines in rectangular coordinates (α,X): ##EQU13## α=4.4 X=27 X=35.
Claim 10
Dependent Claim 20 words
The packing of claim 1, wherein said copolymer has a volume average particle diameter of about 5 to 30 μm.
Claim 11
Dependent Claim 16 words
The packing of claim 1, wherein said exclusive molecular weight is from about 1,500 to 12,000.
Claim 12
Dependent Claim 15 words
The packing of claim 1 having a toluene regain of about 0.5 to 2.5 m/g.
Claim 13
Dependent Claim 12 words
The packing of claim 1, wherein said copolymer is a styrene-divinylbenzene-based copolymer.
Claim 14
Dependent Claim 65 words
The packing of claim 1 wherein said mixture suspended in water consists of about 65 to 80 parts by weight of at least one monovinylbenzene, about 35 to 20 parts by weight of at least one polyvinylbenzene, the total amount of the monovinylbenzene and the polyvinylbenzene being 100 parts by weight, and 80 to 150 parts by weight of the solvent capable of dissolving polystyrene.
Claim 15
Dependent Claim 14 words
The packing of claim 1 wherein the solvent capable of dissolving polystyrene is toluene.
Claim 16
Dependent Claim 32 words
The packing of claim 1 wherein said polymerization initiator having a half-life of 2 to 60 minutes at 70° C. makes up at least 60% by weight of the total polymerization initiator.

References Cited (Backward Citations)

US3326875A Cited
US3322695A Cited
US4174430A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1985-07-05 1986-01-04 1986-07-06 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1989-07-05 1990-01-04 1990-07-06 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1993-07-05 1994-01-04 1994-07-06 $7700.00 Window Closed / Lapsed

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