The method of obtaining macrosector of the anion

 

(57) Abstract:

The invention relates to a method for macrosector of the anion exchange resin is a crosslinked copolymer with aminoalkenes groups, which can be used in the chemical, nutritional and microbiological industry for the purification of solutions of biologically active substances. The method of producing resin includes the interaction of nitrogen-containing vinyl acrylic monomer - N-dimethylaminoethylmethacrylate with ehtilenvinilacetata in a molar ratio of 1:0.5 to 1. Etilenglikolevykh used as a crosslinking agent. The concentration of the starting components in the reaction mixture is 30-47%. The copolymerization is carried out in aqueous DMF (dimethylformamide) with a concentration of 85-95%. The invention allows to generate the anion exchange resin with high selectivity and capacity for large organic ions, and high mechanical strength. 1 PL.

The invention relates to the chemistry of macromolecular compounds, namely, to obtain crosslinked copolymers curing type having anionoobmennika group.

Such cross-linked copolymers can be used as anion exchangers in the chemical, food and mikrobiologichne anion exchange resin by copolymerization of styrene with short-chained cross-linking agent, for example, divinylbenzene, followed by chlorotoluene and aminating (USSR author's certificate No. 1571050, IPC C 08 F 212/14, 8/32, C 08 J 5/20, publishing, 1990).

The drawbacks of such anion exchange resin is a low permeability to large organic ions, in particular ballast substances responsible for the pigmentation of solutions of natural origin.

A known method of producing anion exchange resin based on crosslinked copolymers of styrene with divinylbenzene, obtained in the presence of an inert solvent, in which the soluble Monomeric mixture, and the resulting copolymer does not swell, while the subsequent stage of chlorotoluene and amination similar to the synthesis of anion exchange resin of the gel structure (patent RF №2080338, IPC C 08 J 5/20, C 08 F 212/14, 8/52//(C 08 F 212/14, 212:36) publishing, 1997).

Such anion exchange resins adsorb large organic ions, however, a significant disadvantage is the low reversibility of sorption. The anion exchange resin with short-chained cross-linking agents irreversibly “poisoned” organic substances.

Known methods for producing anion exchange resin synthesized by copolymerization monovinyl compounds containing anionic groups, long-chain bifunctional sexualmente used hydroxyethylacrylate, or hydroxyethylmethacrylate (U.S. patent No. 4251634, 4281233), or di-, tri-, Tetra(meth)acrylates of pentaerythritol (RF patent No. 2057763), or bis-(n-vinylbenzyl)-alkanes (K. P. Pamukova, N. M.Ezhova, L. N. Kalyuzhnaya, and other high-Molecular compounds, 1977, 19B, No. 8, S. 617-620. “Net copolymers of styrene and bis-(n-vinylphenol)alkanes”).

These anion permeable to large organic ions at a satisfactory reversibility their sorption.

Closest to the claimed is a method of producing anion exchange resin, which is implemented by the copolymerization of N-dimethylaminopropylamine with hexahydro-1,3,5-tracelistener and N,N-alkylenediamine (N,N-ethylenemethacrylic and N,N-hexamethylenetetramine) in water and 50% formamide at a molar ratio of monomers 5-20:1 and the concentration of the Monomeric mixture of 20-30% (article: K. P. Pamukova, A. A. Demin, G. C. Samsonov and other high-Molecular compounds. Series A. 1995, volume 37, No. 10, S. 1644-1648; K. P. Pamukova, E. S. Nikiforov, A. A. Dyomin. Journal of applied chemistry. 2000, volume 73, No. 4, S. 631-633).

However, major drawbacks of these anion exchange resins is their low mechanical strength, the high cost of the starting monomers, the lack of industrial production of the monomers detelnosti and capacity in relation to large organic ions with a molecular weight of up to 50 thousand daltons; full reversibility of sorption and high mechanical strength.

The invention is characterized by the following combination of characteristics:

conduct radical copolymerization of vinyl monomer containing - N(CH3)2groups with a bifunctional cross-linking agent in salvatorem solvent;

as a vinyl monomer using N-dimethylaminoethylmethacrylate (DMEM);

as a cross-linking agent (crossagency) take etilenglikolevykh (DMAG);

the ratio of the vinyl monomer:crossiant is 1:0.5 to 1.0;

as the solvent used 85-95% dimethylformamide (DMF);

the concentration of monomers in the solvent is 30-47%.

Analysis of the known level of science and technology has shown a lack of information about the synthesis macrosector of the anion on the basis of N-dimethylaminoethylmethacrylate and etilenglikolevykh.

For a better understanding of the essence of the proposed method are examples of specific performance.

Example 1.

to 69.9 g (of 0.45 mole) of dimethylaminoethylmethacrylate and 91 g (0,46 mole) of etilenglikolevykh to 190.5 dissolved in ml of 95% dimethylformamide, to which basisa block copolymer is cooled, extract, pulverized and extracted with isopropanol, and then treated with 1H. HCL solution and washed with water from the excess acid. The yield of dry product 160 g (95%).

The swelling ratio of CL--forms in the water is equal to 2.7.

Capacity for CL-ion is equal to 2.3 mEq/g

Bulk density equal to 0.68 g/cm3.

Examples 2-4 are made in terms of experience, presented in example 1, but differ in the content of water in dimethylformamide. All data presented in the table.

Example 5 performed in the experience presented in example 1, but the content etilenglikolevykh reduced in 2 times.

Example 6 performed in the experience presented in example 1, but the content etilenglikolevykh reduced 4 times. With reduced content of etilenglikolevykh 4 times formed wysokonapieciowe anion, is not suitable for use.

Examples 7, 8, 9, and 10 were made in the conditions of experiment 1, but the concentration of the mixture of monomers ranges from 60 to 25%.

In accordance with the claimed method in examples 1-3 managed to get sorbent - resin with a capacity of 2.3 to 2.4 mEq/g, with high electoral capacity for large organic ieproxy sorbent.

The declared value of dimethylaminoethylmethacrylate to etilenglikolevykh: 1:0.5 to 1. The reduction of this ratio to 1:0.25, the results vysokomarochnogo of the anion, is not suitable for use in columns (example 6).

The stated concentration of dimethylformamide 85-95%. By reducing it to 80% of the formed anion exchange resin with low bulk weight (example 4), fragile, crumbling to powder.

The concentration of monomers in the solvent claimed in the range of 30-47%. When the concentration of the monomer is less than 30% (example 9) anion exchange resin is obtained mechanically fragile, and when the concentration of the monomers in the solvent is more than 47% (examples 7, 8) is formed of resin, do not have significant capacity in relation to large organic ions.

The method of producing resin by copolymerization of nitrogen-containing vinyl acrylic monomer with a bifunctional cross-linking agent in the environment solvotrode solvent in the presence of a radical initiator by heating, characterized in that as the nitrogen-containing vinyl acrylic monomer used N-dimethylaminoethylmethacrylate, as cross-linking agent - etilenglikolevykh when their concentration Enamide with the concentration of 85-95%.



 

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