The method of obtaining the resulting carboxylic cation exchangers

 

(57) Abstract:

Usage: getting the chromatographic material for the separation, purification and analysis. The inventive copolymerization of (meth)acrylic acid with meta - or para-divinylbenzene or mixtures thereof at a mass ratio of 1 3 in aqueous medium in the presence of a suspension stabilizer mixture of water-soluble starch and dynamite glycerin in their mass ratio of 3 to 1. table 1.

The invention relates to a technology for chromatographic materials used for the selection of chemical compounds in biological systems, chemical, pharmaceutical and food industries.

For preparative selection trudnoreshaemyh amides and amino acids from plant and animal tissues cation requires a specific structure, i.e. with the strict location of the substituents on its surface, a certain porosity and stitching. Structure and properties of ion exchangers depend on the method and conditions of its receipt.

A method of obtaining carboxylic cation exchangers with large granules (particle diameter of 200-2000 μm) emulsion copolymerization of acrylic esters, methacrylic acids and Smoot is Rasa magnesium chloride. The disadvantage of this method is the large amount of spherical granules, the instability of the chemical composition of the copolymer and high hydrophobicity, interfering in the conduct of chromatographic work on the separation of amino acids, peptides and protein fragments.

Closest to the proposed method is the method of obtaining the resulting carboxylic cation exchange resin emulsion copolymerization MAC or AK with technical DVB in the aquatic environment rich in inorganic salts in the presence of a stabilizer of emulsions of polyvinyl alcohol.

Practice chromatographic analysis of natural chemicals shows that when using column chromatography cation requires a specific structure.

In a known manner it is impossible to obtain a carboxyl cation of the desired structure due to the fact that in the polymerization process using technical DVB, which has no permanent staff.

The proposed method allows to obtain the carboxylic cation exchange resin of a specific structure with regularly spaced substituents on its surface, a certain porosity and stitching.

The aim of the invention aastu by chromatography amides and acids.

This objective is achieved in that the carboxylic cation exchangers receive the suspension copolymerization with meta-DVB or a pair of DVB at mass ratio of 1:3 in the presence of a mixture of soluble starch and dynamite glycerin at a mass ratio of 3:1.

The time of completion of polymerization ranges from 2-2 .5 hours depending on which isomer of DVB used in the process.

P R I m e R 1. In triggerlevel glass flask (reactor) with a capacity of 1.5 liters, equipped with a reflux condenser, stirrer type hedgehog with 64 sharp glass needle, thermometer and a socket for the supply of nitrogen, purified from oxygen, make 450 ml of a saturated solution of sodium chloride in demineralized water. There also contribute 3 g of soluble starch (refined by repeated washing with demineralized water and 15 ml of dynamite glycerine. With vigorous stirring (1500 rpm) and heated reactor in a water bath to 80aboutSince there is a complete dissolution of the starch. In the resulting dispersed environment make a mixture of monomers consisting of MACS (50 g), para-DVB (5 g) and benzoyl peroxide (1 g). Bring the temperature of the reaction mass to 88about(In nitrogen atmosphere) and incubated for 2 h at scorodonia 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, believe that the reaction is complete and the reaction mass cooled to 50-60aboutWith transferred into a 3-liter flask, filled dinheirosaurus water to separate from powdered material (particles with a diameter of 0.1-2 μm). Defending against dust lasts for 10 h, after which the supernatant together with the pulverized material is decanted, and the residue is re-weighed into a 3-liter flask with diaminotoluenes water and allow to settle for 10 h at room temperature to separate the residue from the pulverized material. The precipitate was separated from the mother liquor on a Buechner funnel and washed sequentially with demineralised water (I ml), isopropyl alcohol (g ml) and acetone (CH ml). After this white spherical carboxylic cation exchange resin is transferred into a vacuum drying oven and dried. Get 52,3 dry spherical cation (br93.1 from theoretical). The static exchange capacity of the cation exchange resin in sodium ion is equal to 11.2 mEq/g

For chromatographic works selected fraction of the cation exchange resin with a particle diameter of 12 2 μm hydrodynamic method of Hamilton in the conical flask dimensions: length 86 cm diameter (at the widest part) 22 see Flask nourish Domingo on this way of cation exchange resin. This faction balance in 100 ml of 1 N. hydrochloric acid and applied to a glass chromatographic column 0,h cm to a height of 15 see Then a cation exchange resin in the column was washed with demineralized water (20 ml) and it in turn contribute to 0.05 mg of one of the amides or amino acids (aspartic or glutamic) and column elute demineralized water under pressure of 20 kg/cm2the analyzer T-339. A mixture of asparagine, glutamine, aspartic and glutamic acids is considered to be the most difficult separation processes chromatography of all amino acids and therefore was chosen as a suitable test for chromatographic quality of the resulting carboxylic cation exchangers. For detection of amines and amino acids in the eluate used an improved reagent ninhydrin.

At the end of the first chromatogram (i.e., after the release of the 4th component) in the same chromatographic column make any of the above components, without having to regenerate the cation exchange resin in it, as it is recommended for amino acid analyzer and the chromatography is carried out in the mode prescribed for the analyzer T-339.

The results of chromatography of 4-component mixture by cation exchange resin (for the numbering of the examples given in the table.

ry, 3 g of starch and 15 ml of dynamite glycerine. The mixture of monomers consists of 50 g MACK, 5 g of meta-DVB and 1 g of peroxide bentolila. The copolymerization reaction and processing of the obtained copolymer are as in example 1. Get a 51.3 g of dry white cation (about 92.3% of theory) having a static exchange capacity is 10.8 mEq/g and a particle diameter of 1-20 μm. Chromatographic properties 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, 50 g MACK, 2.5 g of para-DVB, 2.5 g of meta-DVB and 1 g of benzoyl peroxide. The copolymerization reaction is carried out in the conditions of example 1. Get copolymer with a particle diameter of 1 to 14 μm, the static exchange capacity of 11.1 mEq/G. of the dry Weight of white cation 50,8, Chromatographic properties shown in the table.

P R I m e R 4. In the reactor described in example 1, make 450 ml of demineralized water, saturated sodium chloride, 50 g of POPPY and 12 g technical DVB, and 1 g of benzoyl peroxide. According to gas-liquid chromatography (GLC) on the device "Chrome 4" technical DVB has the following composition, para-DVB 17,2; meta-DVB 28,9; paradisvanessa 11,6; Metalinvest 38,6; partitives 1.1 metatheatrical 1,3; naphthalene 1,2; other PR static exchange capacity of 9.8 EQ-g and a particle diameter of 1 to 18 μm. Properties listed in the table.

P R I m e R 5. In the reactor described in example 1, make 450 ml of demineralized water, saturated sodium chloride, 50 g MACK, 1,25 g of para-DVB, 3.75 g of meta-DVB (ratio of meta-DVB: para-DVB 3:1) and 1 g of benzoyl peroxide. The copolymerization reaction and processing of the obtained copolymer are as in example 1. Particle diameter of the copolymer is in the range 0.6 to 18 μm, the static exchange capacity of 11.2 mEq/g Obtained 50,3 g of dry cation exchanger, the chromatographic properties of which are given in the table.

P R I m e R 6. In the reactor described in example 1, make 450 ml of demineralized water, saturated sodium chloride, 3 g of soluble starch and 15 ml of dynamite glycerine. At a temperature of 80aboutWith all the starch is dissolved in the dispersion medium. To the resulting solution was added a mixture of monomers consisting of 50 g MACK, 2.5 g of para-DVB, 7,5 meta-DVB (ratio of meta-DVB para-DVB 3:1) and 1 g of benzoyl peroxide. The copolymerization reaction and processing of the obtained copolymer are as in example 1. The cation exchange resin has a particle diameter of 1-20 μm, the static exchange capacity of 10.4 mEq/g of Chromatographic properties summarized in table (N 7).

P R I m e R 7. In the reactor described in example 1, make 450 ml DRI temperature 80aboutWith all the starch is dissolved in the dispersion medium. To the resulting solution was added a mixture of monomers consisting of 50 g MACK, 0.75 g of para-DVB, 2.25 g of meta-DVB (ratio of meta-DVB: para-DVB 3: 1) and 1 g of benzoyl peroxide. The copolymerization reaction and handling of the copolymer are as in example 1. Get a 51.2 g of a white fine-grained cation exchange resin with a particle diameter of 1-20 μm, the static exchange capacity of 10.2 mEq. , Chromatographic properties summarized in table (N 8).

The METHOD of OBTAINING the RESULTING CARBOXYLIC CATION exchange resin emulsion copolymerization of (meth)acrylic acid with divinylbenzene in an aqueous medium in the presence of an emulsion stabilizer, characterized in that, in order to give the cation of high resolution chromatography amides and their aminocyclo, as divinylbenzene use meta-or paragovernmental or their mixture at a mass ratio of 1:3 respectively, and as a stabilizer of the emulsion mixture of water-soluble starch and dynamite glycerin at a mass ratio of 1:3.

 

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