EP0207784A2
Expired / Lapsed
EP
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Packing material for liquid chromatography
Assignee: Shiseido Co Ltd
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Filing: 1986-07-01
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Granted: —
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Expires: 2006-07-01
Abstract
Abstract A packing material for liquid chromatography, comprising particles having a silicone polymer film coated on substantially the entire surface thereof, the packing material being produced by a process comprising the steps of: (a) bringing at least one silicone compound having the general formula (I): wherein R 1 , R 2 , and R 3 represent, independently, a hydrocarbon residue having 1 to 10 carbon atoms, which may be substituted with at least one halogen atom, R 4 , R 5 , and R 6 represent, independently, hydrogen ora hydrocarbon residue having 1 to 10 carbon atoms, which may be substituted with at least one halogen atom, a is zero or an integer of 1 or more, b is zero or an integer of 1 or more, c is zero or 2, and a + b + c is 3 to 300, into contact with particles, whereby the silicone compound is polymerized on substantially the entire surface of the particles, and (b) crosslinking unreacted Si-H groups in the presence of a catalyst, or (c) carrying out an addition reaction of a vinyl compound having up to 40 carbon atoms to unreacted Si-H groups.
Inventors
- 👤 Yutaka Ohtsu
- 👤 Motokiyo Nakano
- 👤 Taketoshi Kanda
- 👤 Osamu Shirota
- 👤 Hiroshi Fukui
- 👤 Okitsugu Nakata
- 👤 Isao Tanaka
- 👤 Junichi Koyama
Bibliographic Details
Application Number
—
Jurisdiction
EP
Data Source
google_patents
Last Synchronized
2026-11-09 04:44
CPC Classifications
B; B01; B01J; B01J20/00; B01J20/281; B01J20/286; B01J20/02; B01J20/10; B01J20/103; B01J20/28; B01J20/28002; B01J20/28004; B01J20/28054; B01J20/28078; B01J20/30; B01J20/32; B01J20/3202; B01J20/3204; B01J20/3231; B01J20/3242; B01J20/3268; B01J20/327; B01J20/3272; B01J20/328; B01J20/3282; B01J20/3291; B01J20/3293; B01J2220/00; B01J2220/50; B01J2220/54; B01J2220/58; Y; Y10; Y10T; Y10T428/00; Y10T428/29; Y10T428/2982; Y10T428/2991; Y10T428/2993; Y10T428/2995
Claims Analysis
Total Claims: 19
Claim 1
Independent Claim
172 words
A packing material for liquid chromatography, comprising particles having a silicone polymer film coated on substantially the entire surface thereof, said packing material being produced by a process comprising the steps of: (a) bringing at least one silicone compound having the general formula (I): wherein R 1 , R 2 , and R 3 represent, independently, a hydrocarbon residue having 1 to 10 carbon atoms, which may be substituted with at least one halogen atom, R 4 , R 5 , and R 6 represent, independently, hydrogen or a hydrocarbon residue having 1 to 10 carbon atoms, which may be substituted with at least one halogen atom, a is zero or an integer of 1 or more, b is zero or an integer of 1 or more, c is zero or 2, and a + b + c is 3 to 300, into contact with particles, whereby the silicone compound is polymerized on substantially the entire surface of the particles, and (b) crosslinking unreacted Si-H groups in the presence of a catalyst.
Claim 2
Dependent Claim
172 words
A packing material for liquid chromatography, comprising particles having a silicone polymer film coated on substantially the entire surface thereof, said packing material being produced by a process comprising the steps of: (a) bringing at least one silicone compound having the general formula (I): wherein R 1 , R 2 , and R 3 represent, independently, a hydrocarbon residue having 1 to 10 carbon atoms, which may be substituted with at least one halogen atom, R 4 , R 5 , and R 6 represent, independently, hydrogen or a hydrocarbon residue having 1 to 10 carbon atoms, which may be substituted with at least one halogen atom, a is zero or an integer of 1 or more, b is zero or an integer of 1 or more, c is zero or 2, and a + b + c is 3 to 300, into contact with particles, whereby the silicone compound is polymerized on substantially the entire surface of the particles, and (b) crosslinking unreacted Si-H groups in the presence of a catalyst.
Claim 3
Dependent Claim
38 words
A packing material for liquid chromatography produced by a process according to claim 1, further comprising the step of: (c) trimethylsilylating Si-OH groups formed slightly in said step (b) with an agent capable of providing a trimethylsilyl group.
Claim 4
Dependent Claim
64 words
A packing material for liquid chromatography produced by a process according to claim 1, wherein the silicone compound having the general formula (I) is brought into contact with particles having an average 0 particle size of 3 - 1000 µm and pores of 30 - 1000 A, selected from a group consisting of silica gel, alumina, glass bead, zeolite, hydroxyapatite, graphite and composite particles.
Claim 5
Dependent Claim
37 words
A packing material for liquid chromatography produced by a process according to claim 1, wherein, in step (a), a silicone compound having the general formula (I) in a vapor phase is brought into contact with the particles.
Claim 6
Dependent Claim
30 words
A packing material for liquid chromatography produced by a process according to claim 1, wherein, in step (b), an alkaline, alkyl metal or alkylamine catalyst is used as the catalyst.
Claim 7
Dependent Claim
33 words
A packing material for liquid chromatography produced by a process according to claim 1, comprising particles having the silicone polymer film coated 0 thereon to a thickness of 3 A to 30 A.
Claim 8
Dependent Claim
75 words
A packing material for liquid chromatography, comprising particles having a silicone polymer film coated on substantially the entire surface thereof, said silicone polymer having the general formula (II) wherein R represents a hydrocarbon residue having 1 to 10 carbon atoms, which may be substituted with at least one halogen atom, t is an integer for making a weight-average molecular weight of the polymer more than 150,000, and x and y have the following relationships: and
Claim 9
Dependent Claim
75 words
A packing material for liquid chromatography, comprising particles having a silicone polymer film coated on substantially the entire surface thereof, said silicone polymer having the general formula (II) wherein R represents a hydrocarbon residue having 1 to 10 carbon atoms, which may be substituted with at least one halogen atom, t is an integer for making a weight-average molecular weight of the polymer more than 150,000, and x and y have the following relationships: and
Claim 10
Dependent Claim
174 words
A packing material for liquid chromatography, comprising particles having a silicone polymer film coated on substantially the entire surface thereof, said packing material being produced by a process comprising the steps of: (a) bringing at least one silicone compound having the general formula ( I ): wherein R 1 , R 2 , and R 3 represent, independently, a hydrocarbon residue having 1 to 10 carbon atoms, R 4 , R 5 , and R 6 represent, independently, hydrogen or a hydrocarbon residue having 1 to 10 carbon atoms, which may be substituted with at least one halogen atom, a is zero or an in teger of 1 or more, b is zero or an integer of 1 or more, c is zero or 2, and a + b + c is 3 to 300, into contact with particles, whereby the silicone compound is polymerized on substantially the entire surface of the particles, and (b) carrying out an addition reaction of a vinyl compound having up to 40 carbon atoms to unreacted Si-H groups.
Claim 11
Dependent Claim
174 words
A packing material for liquid chromatography, comprising particles having a silicone polymer film coated on substantially the entire surface thereof, said packing material being produced by a process comprising the steps of: (a) bringing at least one silicone compound having the general formula ( I ): wherein R 1 , R 2 , and R 3 represent, independently, a hydrocarbon residue having 1 to 10 carbon atoms, R 4 , R 5 , and R 6 represent, independently, hydrogen or a hydrocarbon residue having 1 to 10 carbon atoms, which may be substituted with at least one halogen atom, a is zero or an in teger of 1 or more, b is zero or an integer of 1 or more, c is zero or 2, and a + b + c is 3 to 300, into contact with particles, whereby the silicone compound is polymerized on substantially the entire surface of the particles, and (b) carrying out an addition reaction of a vinyl compound having up to 40 carbon atoms to unreacted Si-H groups.
Claim 12
Dependent Claim
30 words
A packing material for liquid chromatography produced by a process according to claim 8, further comprising the step of: (c) crosslinking unreacted Si-H groups in the presence of a catalyst.
Claim 13
Dependent Claim
38 words
A packing material for liquid chromatography produced by a process according to claim 9, further comprising the step of: (d) trimethylsilylating Si-OH groups formed slightly in said step (c) with an agent capable of providing a trimethylsilyl group.
Claim 14
Dependent Claim
65 words
A packing material for liquid chromatography produced by a process according to claim 8, wherein the silicone compound having the general formula (I) is brought into contact with particles having an average 0 particle size of 3 - 1000 µm and pores of 30 - 1000 A, and selected from a group consisting of silica gel, alumina, glass bead, zeolite, hydroxyapatite, graphite and composite particles.
Claim 15
Dependent Claim
37 words
A packing material for liquid chromatography produced by a process according to claim 8, wherein, in step (a), a silicone compound having the general formula (I) in a vapor phase is brought into contact with the particles.
Claim 16
Dependent Claim
121 words
A packing material for liquid chromatography produced by a process according to claim 8, wherein, in step (b), a vinyl compound having the general formula (III): wherein R 8 and R 9 represent, independently, a hydrogen atom, an alkyl group having 1 to 40 carbon atoms, a cycloalkyl or cycloalkenyl group having 4 to 8 carbon atoms, or an aryl group which may be substituted by one or more alkyl groups having 1 to 20 carbon atoms, and wherein said alkyl, cycloalkyl or cycloalkenyl group, or aryl group optionally substituted by one or more alkyl groups may be substituted by one or more halogen atoms, hydroxyl, carboxyl, amino, cyano, alkoxycarbonyl, aryloxycarbonyl and/or sulfonic acid groups, is used as the vinyl compound.
Claim 17
Dependent Claim
30 words
A packing material for liquid chromatography produced by a process according to claim 9, wherein, in step (c), an alkaline, alkyl metal or alkylamine catalyst is used as the catalyst.
Claim 18
Dependent Claim
89 words
A packing material for liquid chromatography, comprising particles having a silicone polymer film coated on substantially the entire surface thereof, said silicone polymer having the general formula (IV): wherein R 1 represents a hydrocarbon residue having 1 to 10 carbon atoms, which may be substituted with at least one halogen atom, R 7 represents a hydrocarbon residue having up to 42 carbon atoms, u is an integer for making a weight-average molecular weight of the polymer more than 150,000, and x', y' and z have the following relationships: and
Claim 19
Dependent Claim
89 words
A packing material for liquid chromatography, comprising particles having a silicone polymer film coated on substantially the entire surface thereof, said silicone polymer having the general formula (IV): wherein R 1 represents a hydrocarbon residue having 1 to 10 carbon atoms, which may be substituted with at least one halogen atom, R 7 represents a hydrocarbon residue having up to 42 carbon atoms, u is an integer for making a weight-average molecular weight of the polymer more than 150,000, and x', y' and z have the following relationships: and
References Cited (Backward Citations)
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