The way to obtain ultra-fine spherical carboxylic cation exchangers for microcolumn chromatography

 

(57) Abstract:

Usage: for cleaning and analysis of chemical compounds in biological systems, chemical, pharmaceutical and food industry, medicine and agriculture. The inventive method to obtain ultra-fine particles are spherical carboxylic cation exchangers for microcolumn chromatography by aqueous emulsion copolymerization MAC or AK with a mixture of pure steam and metasomal divinylbenzene, in the ratio of 3 : 1, in the presence of initiator-saturated solution of the salt of the mineral acid and the emulsion stabilizer is a mixture of starch with alkylglycerol with the length of the carbon chain alkyl residue from C8to C12taken in a mass ratio of 1 : 0.4 to 1. table 1.

The invention relates to a technology for chromatographic materials used for studying the chemical composition of biological objects in the chemical, pharmaceutical and food industries.

Sorbents for microcolumn chromatography must be mechanically strong to withstand the high pressure in the analysis, homogeneous chemical and granulometric composition. Most often used for this purpose careernet-active substances, used as a stabilizer emulsion copolymerization process, as well as from the presence in solution of inorganic electrolytes.

A method of obtaining granular cation exchange resin suspension copolymerization of a mixture of styrene and technical divinylbenzene and acrylic monomers (ethyl(meth)acrylate, (meth)acrylic acid) [1] the Copolymerization is conducted in aqueous medium, in a stream of nitrogen at 80aboutC for 8 hours as a stabilizer of emulsions using polyvinyl alcohol or carboxymethyl cellulose, taken in an amount of 0.1-5% by weight of monomers. Get krupnogalechny the cation exchange resin with a particle diameter of 0.1 to 1.0 mm

The disadvantage of this method is the large amount of spherical granules and the long duration of the copolymerization reaction.

There is also known a method of obtaining a carboxylic cation exchangers with a large grain (particle diameter of about 2000 μm) of methacrylic (MAC) or acrylic (AK) acids and technical divinylbenzene (so-DVB) [2] According to this method, the copolymerization reaction is conducted in aqueous environment saturated inorganic salt (potassium chloride, sodium sulfate and other), and as a stabilizer of emulsions used ethylene glycol. The reaction is carried out by tre the second method is the large size of the obtained particles (up to 2000 µm) and long duration of the copolymerization reaction.

Closest to the present invention is a method of obtaining a coarse carboxylic cation exchange resin emulsion copolymerization MAC or AK with tons of DVB in the aquatic environment rich in inorganic salts and poly(meth)acrylic acid [3] as a stabilizer of emulsions used polyvinyl alcohol. The copolymerization reaction by this method are under intensive stirring (800 rpm) with three-temperature mode: the start of the reaction is held at 70aboutC (1 h), the main process at the 90aboutC (1 h) and copolymerizate under 100about(9 hours).

The disadvantage of this method is that in the copolymerization use of polyvinyl alcohol as a stabilizer of the emulsion, which is due to the high viscosity is not possible to obtain particles with a diameter of 1-10 μm, and the use of technical divinylbenzene is not possible to obtain a cation exchange resin with regular structural stitching due to the volatile chemical composition of divinylbenzene. Practice chromatographic analysis shows that the microcolumn chromatography cation requires a certain faction, strict structural stitching and high purity chemical composition.

Known methods is izlagaemogo method is getting very fine spherical carboxylic cation exchange resin of a specific structure with high resolution.

This objective is achieved in that in the known method carboxylic cation exchangers receive emulsion copolymerization of a mixture of monomers in the aqueous phase, saturated inorganic salt. As a stabilizer of emulsions using ethylene glycol and polyvinyl alcohol. The difference is that as an emulsion stabilizer in the proposed method uses a mixture of starch and alkylglycerol with long chain alkyl residue from C8to C12that allows to obtain spherical carboxyl ativity with particle diameters of 0.1-10 μm, and as a cross-linking agent is used para - or meta-DVB or mixtures thereof. Carboxylic cation exchangers obtained by the proposed method is well reproduced from batch to batch and have high chromatographic characteristics.

Comparative analysis of the proposed technical solution with the prototype shows that the inventive method differs from the known fact that the process of emulsion copolymerization AK or MAK are in a saturated aqueous solution of sodium chloride in the presence of stabilizers in emulsion a mixture of starch and alkylglycerol with pure DVB isomers or their well-defined mixtures. Thus, C is olymerization monomers are in the aqueous phase, saturated inorganic salt in the presence of ethylene glycol, it is not possible to obtain a carboxyl cation of the desired diameter, which are obtained in the proposed technical solution. This allows to make a conclusion about its compliance with the criterion of "Significant differences".

High chromatographic characteristics and reproducibility of carboxylic cation exchangers is that the copolymerization AK or MAK are in a saturated aqueous solution of sodium chloride in the presence of certain selected ratio of stabilizers in emulsion a mixture of water-soluble starch and alkylglycerol, and as a crosslinking agent, we take a pure DVB isomers or their mixtures in strictly defined proportions.

The time of completion of the copolymerization reaction is 2-2,5 hours In a mixture of monomers do not add styrene and other hydrocarbons, insoluble in water, which gives the target cation the possibility of using them in microcolumn chromatography.

P R I m e R 1. In triggerlevel flask (reactor) capacity 1.5 liters, equipped with a reflux condenser, stirrer type "hedgehog", a thermometer and a socket for the supply of nitrogen, purified from oxygen, make 450 ml of demineralized water, saturated with chloride in the reactor make a mixture of monomers of the POPPY (50 g), para-DVB (1,25 d), meta-DVB (3.75 g) and benzoyl peroxide (1 g). The copolymerization reaction are in nitrogen atmosphere with vigorous stirring (2000-2200 rpm) at a temperature of 88aboutWith over 2 hours Of completion of the polymerization process are judged according to the settling velocity of spherical particles of the copolymer in water under an optical microscope. If the copolymer particles with a diameter of 10 microns sink in water for 2-3 minutes, consider that the reaction was completed and cooled to 50-60aboutWith the reaction mass is transferred to a 3 liter flask with demineralized water to separate from powdered material (particles with diameter less than 0.1 microns). Defending against dust lasts for 10 h, after which the supernatant together with the pulverized material is decanted and the operation is repeated. The precipitate was separated from the mother liquor and washed on the filter SCHOTT consistently demineralized water (2 x 100 ml), isopropyl alcohol (2 x 50 ml) and acetone (2 x 50 ml). After this white spherical fine carboxylic cation exchange resin is dried in a vacuum Cabinet. The weight of the dry product of 46.8 g, static exchange capacity is 11.6 mEq/g of Chromatographic properties shown in the table.

P R I m m e R 2. In the reactor described in example 1, make 450 ml demineralizovannoj starch in the reactor make a mixture of monomers, consisting of 50 g MACK, 1,25 g of para-DVB, 3.75 g of meta-DVB and 1 g of benzoyl peroxide. The copolymerization reaction and handling of the copolymer are as in example 1. Receive and 47.5 g of dry fine-grained cation exchange resin with a particle diameter of 0.1 to 10 μm, the static exchange capacity of 11.6 mEq/g of Chromatographic properties of the cation is shown in the table.

P R I m e R 3. In the reactor described in example 1, make 450 ml of demineralized water, saturated sodium chloride, 3 g of soluble starch, 0.4 g of dodecylguanidine. After complete dissolution of starch in the reactor make a mixture of monomers consisting of 50 g AK, 1,25 g of para-DVB, 3.75 g of meta-DVB and 1 g of benzoyl peroxide. The copolymerization reaction and handling of the copolymer are as in example 1. Get to 47.1 g of dry fine-grained cation exchange resin with a particle diameter of 0.1 to 10 μm, the static exchange capacity of 11.4 mEq/g of Chromatographic properties of the cation is shown in the table.

The WAY to OBTAIN ultra-FINE SPHERICAL CARBOXYLIC CATION exchangers FOR MICROCOLUMN CHROMATOGRAPHY by aqueous emulsion copolymerization of methacrylic acid or acrylic acid with divinylbenzene in the presence of the initiator of a saturated solution of salt of mineral acid and emulsion stabilizer, oti carbon chain alkyl residue from C8to C12taken in the mass ratio 1 0.4 to 1, and as co monomer, a mixture of pure steam and metasomal divinylbenzene, in the ratio of 3 to 1, respectively.

 

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