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EP0043074A2 Expired / Lapsed EP ⏱️ 0.0 years remaining

High speed liquid chromatographic packing and process for production thereof

Assignee: Asahi Kasei Corp
•
Filing: 1981-06-23
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Granted: —
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Expires: 2001-06-23
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Abstract

Abstract A granular crosslinked copolymer suitable as a high speed liquid chromatographic packing and especially as a gel permeation chromatographic packing is disclosed. In a preferred embodiment of the invention the packing is a copolymer essentially consisting of (I) units of at least one vinyl alcohol, (II) units of at least one vinyl ester of a carboxylic acid and (III) units of at least one crosslinking monomer having an isocyanurate ring, the ratio of the units (I) to the units (II) in the copolymer being within the range satisfying the following equation: aboutabout 0.8 wherein a and b are molar ratios of the units (I) and (II), respectively, in the total units (I), (II) and (III) of the copolymer, and a process for preparing the same by suspension polymerization is disclosed.

Inventors

  • 👤 Yuzo Yanagihara
  • 👤 Kohji Noguchi
  • 👤 Makoto Honda

Bibliographic Details

Application Number —
Jurisdiction EP
Data Source google_patents
Last Synchronized 2026-11-01 19:13
CPC Classifications
B; B01; B01J; B01J20/00; B01J20/281; B01J20/282; B01J20/285; B01D; B01D15/00; B01D15/08; B01D15/26; B01D15/34; B01J20/28; B01J20/28014; B01J20/28047; B01J20/28054; B01J20/28057; C; C08; C08F; C08F8/00; C08F8/12

Claims Analysis

Total Claims: 26
Claim 1
Independent Claim 96 words
A totally porous packing for high speed liquid chromatography comprising a granular crosslinked copolymer essentially consisting of (I) units of at least one vinyl alcohol, (II) units of at least one vinyl ester of a carboxylic acid and (IIi) units of at least one crosslinking monomer having an isocyanurate ring, the ratio of the units (I) to the units (II) in the copolymer being within the range satisfying the following equation: wherein a and b are molar ratios of the units (I) and (II), respectively, in the total units (I), (II) and (III) of the copolymer.
Claim 2
Dependent Claim 96 words
A totally porous packing for high speed liquid chromatography comprising a granular crosslinked copolymer essentially consisting of (I) units of at least one vinyl alcohol, (II) units of at least one vinyl ester of a carboxylic acid and (IIi) units of at least one crosslinking monomer having an isocyanurate ring, the ratio of the units (I) to the units (II) in the copolymer being within the range satisfying the following equation: wherein a and b are molar ratios of the units (I) and (II), respectively, in the total units (I), (II) and (III) of the copolymer.
Claim 3
Dependent Claim 27 words
The packing of Claim 1, wherein the ratio of the units (I) to the units (II) in the copolymer is within the range satisfying the following equation:
Claim 4
Dependent Claim 57 words
The packing of Claim 1, wherein the ratio of the units (I), (II) and (III) in the copolymer is within the range satisfying the following equation: wherein a and b are the same as defined above, and c is the molar ratio of the units (III) in the total units (I), (II) and (III) of the copolymer.
Claim 5
Dependent Claim 35 words
The packing of Claim 1 or Claim 3, wherein the units of the vinyl ester of a carboxylic acid are those of the vinyl ester of a carboxylic acid having 2 to 5 carbon atoms.
Claim 6
Dependent Claim 31 words
The packing of Claim 4, wherein the vinyl ester of the carboxylic acid is selected from the group consisting of vinyl acetate, vinyl propionate, vinyl butyrate, vinyl valerate and vinyl pivalate.
Claim 7
Dependent Claim 16 words
The packing of Claim 5, wherein the vinyl ester of the carboxylic acid is vinyl acetate.
Claim 8
Dependent Claim 16 words
The packing of Claim 5, wherein the vinyl ester of the carboxylic acid is vinyl propionate.
Claim 9
Dependent Claim 58 words
The packing of Claim 1 or Claim 3, wherein the units of the crosslinking monomer having an isocyanurate ring are those of the crosslinking monomer having the formula: wherein R 1 , R 2 and R 3 may be the same or different and are selected from the group consisting of -CH 2 -CH=CH 2 , -CH-C≡CH and
Claim 10
Dependent Claim 12 words
The packing of Claim 8, wherein the crosslinking monomer is triallyl isocyanurate.
Claim 11
Dependent Claim 57 words
A packing of Claim 3, wherein the ratio of the units (I), (II) and (III) is within the range satisfying the following equation: wherein a, b and c are the same as defined above, and the exclusive molecular weight for polyethylene glycol or dextran is in the range of about 10 3 to about 10 5 .
Claim 12
Dependent Claim 57 words
A packing of Claim 3, wherein the ratio of the units (I), (II) and (III) is within the range satisfying the following equation: wherein a, b and c are the same as defined above, and the exclusive molecular weight for polyethylene glycol or dextran is in the range of about 10 5 to about 10 8 .
Claim 13
Dependent Claim 17 words
The packing of Claim 1 having a water regain of about 0.5 to about 2.0 g.water/g.dry gel.
Claim 14
Dependent Claim 21 words
The packing of Claim 12, wherein the water regain is in the range of about 0.8 to about 2.0 g·water/g·dry gel.
Claim 15
Dependent Claim 21 words
The packing of Claim 1, wherein the copolymer has a weight average particle diameter of about 5 to about 20 µm.
Claim 16
Dependent Claim 21 words
The packing of Claim 14, wherein the copolymer has a weight average particle diameter of about 5 to about 12 µm.
Claim 17
Dependent Claim 107 words
A process for producing a packing for high speed liquid chromatography, which comprises subjecting a monomer mixture of at least one vinyl ester of a carboxylic acid having 2 to 5 carbon atoms and at least one crosslinking monomer having the formula: wherein R 1 , R 2 and R 3 may be the same or different and are selected from the groups consisting of -CH 2 -CH=CH 2 , -CH-C≡CH and to suspension polymerization and subjecting to the resulting granular copolymer to ester exchange reaction or saponification to such an extent that the ester exchange ratio or the saponification ratio is about 0.4 to about 0.8.
Claim 18
Dependent Claim 107 words
A process for producing a packing for high speed liquid chromatography, which comprises subjecting a monomer mixture of at least one vinyl ester of a carboxylic acid having 2 to 5 carbon atoms and at least one crosslinking monomer having the formula: wherein R 1 , R 2 and R 3 may be the same or different and are selected from the groups consisting of -CH 2 -CH=CH 2 , -CH-C≡CH and to suspension polymerization and subjecting to the resulting granular copolymer to ester exchange reaction or saponification to such an extent that the ester exchange ratio or the saponification ratio is about 0.4 to about 0.8.
Claim 19
Dependent Claim 21 words
17, The process of Claim 16, wherein the ester exchange ratio or the saponification ratio is about 0.45 to about 0,75,
Claim 20
Dependent Claim 30 words
18, The process of Claim 16, wherein the mol ratio of the vinyl ester of the carboxylic acid to the crosslinking monomer is 1 to about 0.08 - about 0.22.
Claim 21
Dependent Claim 29 words
The process of Claim 18, wherein the mol ratio of the vinyl ester of the carboxylic acid to the crosslinking monomer is 1 to about 0.11 - about 0.16.
Claim 22
Dependent Claim 29 words
The process of Claim 18, wherein the mol ratio of the vinyl ester of the carboxylic acid to the crosslinking monomer is 1 to about 0.12 - about 0.18.
Claim 23
Dependent Claim 31 words
The process of Claim 16, wherein the vinyl ester of the carboxylic acid is selected from the group consisting of vinyl acetate, vinyl propionate, vinyl butyrate, vinyl valerate and vinyl pivalate.
Claim 24
Dependent Claim 15 words
The process of Claim'21, wherein the vinyl ester of the carboxylic acid is vinyl acetate.
Claim 25
Dependent Claim 16 words
The process of Claim 21, wherein the vinyl ester of the carboxylic acid is vinyl propionate.
Claim 26
Dependent Claim 12 words
The process of Claim 16, wherein the crosslinking monomer is triallyl isocyanurate.

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