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1. WO1992015385 - BUTADIENE ACRYLONITRILE POLYMERIC COATING AND CHROMATOGRAPHIC PACKING MATERIAL

Publication Number WO/1992/015385
Publication Date 17.09.1992
International Application No. PCT/US1992/001822
International Filing Date 04.03.1992
Chapter 2 Demand Filed 05.10.1992
IPC
B01J 20/32 2006.01
BPERFORMING OPERATIONS; TRANSPORTING
01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
30Processes for preparing, regenerating or reactivating
32Impregnating or coating
CPC
B01D 15/325
BPERFORMING OPERATIONS; TRANSPORTING
01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
DSEPARATION
15Separating processes involving the treatment of liquids with solid sorbents
08Selective adsorption, e.g. chromatography
26characterised by the separation mechanism
32Bonded phase chromatography
325Reversed phase
B01J 20/286
BPERFORMING OPERATIONS; TRANSPORTING
01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
281Sorbents specially adapted for preparative, analytical or investigative chromatography
286Phases chemically bonded to a substrate, e.g. to silica or to polymers
B01J 20/287
BPERFORMING OPERATIONS; TRANSPORTING
01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
281Sorbents specially adapted for preparative, analytical or investigative chromatography
286Phases chemically bonded to a substrate, e.g. to silica or to polymers
287Non-polar phases; Reversed phases
B01J 20/3204
BPERFORMING OPERATIONS; TRANSPORTING
01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
30Processes for preparing, regenerating, or reactivating
32Impregnating or coating ; ; Solid sorbent compositions obtained from processes involving impregnating or coating
3202characterised by the carrier, support or substrate used for impregnation or coating
3204Inorganic carriers, supports or substrates
B01J 20/327
BPERFORMING OPERATIONS; TRANSPORTING
01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
30Processes for preparing, regenerating, or reactivating
32Impregnating or coating ; ; Solid sorbent compositions obtained from processes involving impregnating or coating
3231characterised by the coating or impregnating layer
3242Layers with a functional group, e.g. an affinity material, a ligand, a reactant or a complexing group
3268Macromolecular compounds
327Polymers obtained by reactions involving only carbon to carbon unsaturated bonds
B01J 20/3276
BPERFORMING OPERATIONS; TRANSPORTING
01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
30Processes for preparing, regenerating, or reactivating
32Impregnating or coating ; ; Solid sorbent compositions obtained from processes involving impregnating or coating
3231characterised by the coating or impregnating layer
3242Layers with a functional group, e.g. an affinity material, a ligand, a reactant or a complexing group
3268Macromolecular compounds
3276Copolymers
Applicants
  • SIMON, Ethan, S. [US]/[US]
  • HOLLAND, Kevin, B. [US]/[US]
  • McCLANAHAN, Christopher [US]/[US]
Inventors
  • SIMON, Ethan, S.
  • HOLLAND, Kevin, B.
  • McCLANAHAN, Christopher
Agents
  • PARKER, Sheldon, H.
Priority Data
664,34404.03.1991US
664,36604.03.1991US
Publication Language English (EN)
Filing Language English (EN)
Designated States
Title
(EN) BUTADIENE ACRYLONITRILE POLYMERIC COATING AND CHROMATOGRAPHIC PACKING MATERIAL
(FR) REVETEMENT POLYMERE EN BUTADIENE ACRYLONITRILE ET MATERIAU DE REMPLISSAGE CHROMATOGRAPHIQUE
Abstract
(EN)
A chromatographic packing material includes a coated support material which is a chromatographically suitable substrate. An immobilized butadiene acrylonitrile polymer coating is provided on the substrate. The copolymer can be crosslinked by gamma radiation, or by means of a crosslinking agent such as dicumyl peroxide. The support material can be silica, alumina, diatomaceous earth, zeolite, porous glass or carbon, but preferably is spherical lamellar shaped crystals of aluminum hydroxide. The aluminum hydroxide crystals are bonded together at a central core and extend radially outwardly from a central core with a particle density ranging from 0.3 to 2.5 g/cm3 and a diameter of 2 to 150 microns. The organic materials are separated by providing a bed of packing material selected from the group consisting of silica and alumina, diatomaceous earth, zeolite and porous glass with a polymeric coating being bonded thereto. Organic materials are introduced to the bed, and an eluting fluid is added. The fluid and one of the organic materials are removed from bed, and the materials are then separated and removed from the fluid. A chromatographic packing material is disclosed comprising a coated support material which is a chromatographically suitable substrate, with an uniform immobilized functionalized coating. A chromatographic column is disclosed having a stationary phase with a suitable substrate coated support material and an uniform immobilized functionalized coating. A stationary phase for reversed-phase liquid chromatography consisting of a crosslinked, polybutadiene-coated, macroporous, alumina substrate is disclosed wherein the micropores have a diameter predominantely in the range of 50 to 1000 Angstroms, and the alumina substrate is so occludingly coated with polybutadiene that the integrity of the stationary phase is not adversely affected by extended exposure to liquid environments having a pH of 12. The method for preparing a stationary phase for liquid chromatography by occludingly coating onto a macroporous alumina substrate having micropores of a diameter predominantely in the range of 90 to 500 Angstroms, an unsaturated polybutadiene oligomer having pendant vinyl groups and a molecular weight less than 50,000 Daltons. The polybutadiene oligomer is partially crosslinked to the substrate to provide a polybutadiene coating having pendant vinyl groups. The hydrophobicity of the polybutadiene coating is increased by providing alkyl groups onto said polybutadiene coating, so that the retention time of o-xylene is increased by at least 30 % over retention time of a stationary phase coated with polybutadiene having 18 mole percent vinyl groups per butadiene unit.
(FR)
Un matériau de remplissage chromatographique comporte un matériau de support revêtu qui est un substrat se prêtant à des applications chromatographiques. Un revêtement polymère en butadiène acrylonitrile immobilisé est prévu sur le substrat. Le copolymère peut être réticulé par rayonnement gamma, ou bien au moyen d'un agent de réticulation tel que du peroxyde de dicumyle. Le matériau de support peut être de la silice, de l'alumine, de la diatomite, de la zéolite, du verre ou du carbone poreux, mais de préférence est constitué de cristaux lamellaires sphériques d'hydroxyde d'aluminium. Ces cristaux d'hydroxyde d'aluminium sont liés ensemble au niveau d'un noyau central et s'étendent radialement vers l'extérieur depuis un noyau central avec une masse volumique particulaire comprise entre 0,3 et 2,5 g/cm3 et un diamètre de 2 à 150 microns. Les matières organiques sont séparées par réalisation d'un lit de matériau de remplissage choisi dans le groupe composé de silice et d'alumine, de diatomite, de zéolite et de verre poreux, un revêtement polymère étant adhérisé à ce matériau. Des matières organiques sont introduites dans le lit, et un fluide éluant est ajouté. Le fluide et l'une des matières organiques sont éliminés du lit, et les matières sont ensuite séparées et éliminées du fluide. Est décrit un matériau de remplissage chromatographique comprenant un matériau de support revêtu qui est un substrat se prêtant à des applications chromatographiques, avec un revêtement fonctionnalisé immobilisé homogène. Est décrite une colonne chromatographique possédant une phase fixe avec un substrat approprié constitué d'un matériau de support revêtu, et un revêtement fonctionnalisé immobilisé homogène. Est décrite une phase fixe pour chromatographie liquide à phase inversée, constituée d'un substrat d'alumine macroporeux réticulé et revêtu de polybutadiène, dans laquelle les micropores présentent un diamètre principalement dans la plage de 50 à 1000 Å, et le substrat d'alumine est revêtu de manière si occlusive avec du polybutadiène que l'intégrité de la phase fixe n'est pas affectée par une exposition prolongée à des environnements liquides présentant un pH de 12. Est également décrit un procédé pour préparer une phase liquide pour chromatographie liquide en déposant de manière occlusive, sur un substrat d'alumine macroporeux présentant des micropores d'un diamètre principalement dans la plage de 90 à 500 Å, un oligomère de polybutadiène insaturé possédant des groupes vinyle pendants et un poids moléculaire inférieur à 50.000 Daltons. L'olygomère de polybutadiène est partiellement réticulé au substrat pour former un revêtement de polybutadiène présentant des groupes vinyle pendants. L'hydrophobie du revêtement de polybutadiène est accrue par l'adjonction de groupes alkyle, de sorte que le temps de rétention du o-xylène est accru d'au moins 30 % par rapport au temps de rétention d'une phase fixe revêtue de polybutadiène présentant 18 moles pour cent de groupes vinyle par unité de butadiène.
Also published as
EP1992907763
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