The method of obtaining macrosector of the anion
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.
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%.
FIELD: sanitary and hygienic facilities.
SUBSTANCE: invention relates to technology of manufacturing chemisorption materials for use in municipal hygiene sphere. Method consists in treatment of chemisorption carboxyl-containing material in Na form with 0.5-1.0% aqueous acid solution, e.g. hydrochloric acid solution, at modulus (ratio of weight of chemisorption material to acid solution volume) 1:30 and treatment time 0.5-1.0 h to transfer material into H-form. Chemisorbent is then washed with softened water to pH 5-6, after which material in H-form is treated for 0.5-1.0 h with 0.5-1.0% potassium hydroxide solution, modulus 1:30. At the expiration of treatment time, material is washed with softened water to pH 5.0-6.5. Presence of three-dimensional lattice, both during treatment time of chemisorption material in the form of fibers or nonwoven material and upon use of products from this material, prevents dissolution of polymer in water or in aqueous solution of acid or potassium hydroxide. Owing to filtration, chemisorbent entraps in water heavy metal ions contained therein and water is saturated with potassium ions so that chemisorption material acquires at least 4 mmol/g of carboxyl groups in K-form.
EFFECT: optimized manufacture conditions.
SUBSTANCE: invention relates to technology for preparing sorbents with fibrous structure by using waste of industrial manufacture. Method involves treatment of fibrous matrix from waste of tanning leather chips with polyelectolyte an aqueous solution obtained by alkaline hydrolysis of polyacrylonitrile or copolymer based on thereof. Prepared sorbent shows the improved capacity for extraction of different components from different aqueous media.
EFFECT: improved preparing method, improved and valuable properties of sorbent.
2 cl, 1 tbl, 2 ex
FIELD: polymer materials.
SUBSTANCE: invention relates to manufacture of ion-exchange fibers with special properties, which can be used as sorbent or as a sorbent constituent for cleaning liquid media, largely natural and waste waters. Method consists in performing alkali hydrolysis of polyacrylonitrile fiber in presence of hydrazine at elevated temperature completed by treatment of fiber with active agent causing degradation of chromophore groups of fiber. Alternatively, ion-exchange fiber is manufactured via alkali hydrolysis of polyacrylonitrile fiber in presence of hydrazine at elevated temperature, hydrolysis reaction being effected in concentrated solution of salt of alkali metal with weak acid followed by treatment of fiber with active agent as above.
EFFECT: improved characteristics of fiber at lower consumption of reagents and stabilized manufacturing process to provide ion-exchange fiber with desired number of chelating sorption groups due to appropriate balance of acid and basic groups resulting from hydrolysis.
18 cl, 5 tbl, 16 ex
FIELD: waste water and gas emission treatment.
SUBSTANCE: invention relates to methods for preparing catalytic materials to clean waste waters and gas emissions via removal of organic and inorganic components by liquid-phase oxidation process. Method comprises consecutive treatment of knitted cloth with hot alkali solution containing 14-42 g/L hydroxylamine chloride and an aqueous solution of variable-valence metal salts. In the first stage, treatment is carried out with modifying hydroxylamine chloride and ethylenediamine-containing solution wherein molar ratio of polyacrylonitrile unit number to ethylenediamine ranges from 2 to 10 and solution pH is 6-9. Treatment temperature is 95-105°C and treatment time 1-1.6 h. In the second stage, treatment with aqueous solution of variable-valence metal salts is carried out for 0.5 to 2 h.
EFFECT: simplified manufacture technology, reduced expenses on reagents, and reduced process time without loss in the firmness of fixation of variable-valence metal salts on cloth.
2 tbl, 21 ex
FIELD: catalysts for waste water and emission gas treatment.
SUBSTANCE: invention relates to technology of removing organic and inorganic components from waste waters and emission gases via liquid-phase oxidation, in particular, to preparing textile-supported polymer catalyst consisting of polyacrylonitrile monothreads and complex threads. Knitted cloth is treated with modifying solution at 106 to 150°C for 10 to 30 min when ratio of amounts of polyacrylonitrile units to amount of chlorine-containing hydrazine salt equal to 20-30 and the same to chlorine-containing hydroxylamine salt 10-15, pH of solution being 6-9. After that, cloth is treated with transition metal salts for 1.0-2.0 h until content of metal on catalyst achieves 0.81-1.2 mmol/g. Treatment is followed by washing with desalted water.
EFFECT: simplified catalyst preparation technology and intensified preparation process.
2 cl, 2 tbl, 30 ex
FIELD: chemical technology, resins.
SUBSTANCE: invention relates to a method for preparing polyhalide strong-basic anion-exchange resins of gel and macroporous structure designated for disinfection of water in closed ecological objects, domestic drinking water and water from non-checked sources. Polyhalide anion-exchange resins is prepared from strong-basic quaternary ammonium anion-exchange resins in chloride form by their iodination with J2 solution in KJ at stirring, thermostatic control and washing out. Iodination is carried out with triiodide solution on conditioned strong-basic anion-exchange resins in chloride form in the content of strong-basic groups 80%, not less, in the mole ratio anion-exchange resin : triiodide = 1.0:(1.1-1.5). Ready product is kept at 20-55°C additionally. Invention provides preparing polyhalide anion-exchange resins characterizing by high resource in water disinfection and in simultaneous reducing iodine release in disinfecting water in retention of high disinfecting indices.
EFFECT: improved preparing method.
1 tbl, 8 ex
FIELD: ION-EXCHANGE MATERIALS.
SUBSTANCE: invention relates to a process of preparing gel-like cationites for use in treatment and purification processes. Gel-like cationites are prepared by inoculating-incoming process wherein (a) aqueous suspension of microcapsulated cross-linked styrene polymer in the form of granules and containing cross-linking agent is provided as inoculating polymer; (b) inoculating polymer is left to swell in monomer mixture composed of vinyl monomer, cross-linking agent, and radical initiator, namely peracid aliphatic ester; (c) monomer mixture is polymerized in inoculating polymer; and (d)resulting copolymer is functionalized via sulfatization. Process is characterized by that, in step (a), content of cross-linking agent in cross-linked styrene copolymer amounts to 3.5-7 wt % and inoculum-to-income ratio in step (b) amounts to 1:(0.25-1.5).
EFFECT: enabled preparation of gel-like cationites having high osmotic and mechanic stabilities as well as improved oxidation resistance.
7 cl, 9 tbl, 9 ex
FIELD: chemical technology.
SUBSTANCE: invention relates to technology for preparing chemosorption materials possessing high protective properties with respect to ammonia vapors that can be used for using in filtering protective devices. Method involves impregnation of nonwoven activated fabric made of hydrocellulose fibers in an aqueous solution containing zinc chloride and nickel chloride. Also, this solution contains 1,2,3-propanetriol (glycerol) as a modifying agent taken in the amount 0.5-1.0% of the total amount of the prepared solution.
EFFECT: improved preparing method.
1 tbl, 1 ex
SUBSTANCE: invention can be used for extracting metal ions, purifying waste and industrial solutions from toxic metal ions. The method of obtaining anion-exchange fibre material involves reacting activated polyacrylonitrile fibre nitron and 30-70 wt % modifying agent - mixture of diethanolamine with 10-30 wt % hexamethylenediamine in an aqueous 5% solution of dimethylformamide. Nitron is activated in a 3-6% aqueous alkaline solution for 3-5 minutes at 90-95°C.
EFFECT: invention makes it easier to obtain fibrous anionite and can be used for effective purification waste water from leather industry and electroplating plants from chromium (VI) ions, and for concentrating and separating chromates from industrial solutions.
1 tbl, 4 ex
SUBSTANCE: composition is meant for producing cation-exchange fibre material used in water treatment processes and treatment of industrial sewage. The composition is also used to soften and desalinate water, in production of synthetic detergents, in the paint industry and industry of polymer materials. The composition consists of paraphenol sulphonic acid and formalin. The composition additionally contains filler - basalt wool. The basalt wool is first heat treated for 1 hour at temperature 350-450°C, followed by microwave treatment at 180 or 750 W for 30 s. Content of components is as follows, wt %: paraphenol sulphonic acid 50-55.8, formalin 40.9-35.1; basalt wool 9.1. The composition enables synthesis of cation-exchange fibre material with improved properties, particularly lower oxidation number of the filtrate, higher specific volume of the cationite, as well as high dynamic exchange capacity and high osmotic stability of the cationite.
EFFECT: composition enables synthesis of cation-exchange fibre material with improved properties.
1 tbl, 4 ex