The method of obtaining fibrous ion exchanger


(57) Abstract:

Usage: factories, producing and processing of acrylic fiber with subsequent use of the ion exchanger for the recovery of chemicals from waste water and ventilation gases. The inventive acrylic fiber treated with 10-90% alkaline solution of alkylamine at 70-85oC 30-60 min and Then treated with 10-30% aqueous solution dimethyldodecylamine at 75-85oC 45-60 minutes 2 C.p. f-crystals, 2 tab.

The invention relates to the production of ion-exchange structured fibrous materials and can be used in factories, producing and processing of polyacrylonitrile (PAN) fibers with subsequent application of the resin for trapping reagent from sewage and ventilation gases.

A method of obtaining an ion-exchange PAN-fibers by treating the fibers based on polyacrylonitrile in two stages: first with hydroxylamine concentration of 10-15 g/l 24-60 minutes, and then 20-80% aqueous solution of alkylamine at 70-95oC for 120 min. /1/. As alkylamino use Ethylenediamine, or tetramethylaniline or polyethylenepolyamine (Pepa). At the specified method are, in particular, anyoneor static exchange capacity (SOY) ion exchanger, obtained by processing the probe is in HCl 0.1 N. of 2.0 mEq/g, NO21,06 mg-EQ/g; treated Triethylenetetramine respectively to 5.2 mEq/g, and 2.37 mEq/g with the increase In SOYBEAN sharply decreases the mechanical strength of the fibrous ion exchanger from 15 to 9.5 CN/Tex. Obtained by a known method fibrous ion exchanger has a number of disadvantages, namely: relatively low SOY in HCl 0.1 N. and, accordingly, slobodianiuk ions (NO2). In addition, fibrous ion exchangers obtained by the interaction of the fibers from the an copolymers with amines of a homologous series of Ethylenediamine (including the PET) have relatively high swelling properties depending on the pH of the medium:

pH 4, the swelling properties 80%

pH 12, the swelling properties 190%

pH 1, the swelling properties 100% /2/.

The amount of swelling of the fibers indicates a low chemical resistance of resins obtained by a known method. Such resins can be used only when the pH of the medium is close to neutral.

Closest to the present invention is a method of obtaining fibrous ion exchanger based on a grafted copolymer of polyacrylonitrile with glycidylmethacrylate (GMA), followed by aminating alkylamino /3/.

-I'm partial carboxylation PAN-fibers in an alkaline bath at a pH of 14, temperature 70oC for 60 min, 2nd application of the initiator salts of divalent iron) on the fiber for 30 min followed by washing of the excess salt distilled water for 30 min, 3rd grafting GMA concentration of 7-10% at the 90oC for 15 min and module baths 25, 4th washing the fiber with isopropyl alcohol excess GMA for 30 min, followed by drying for 15 min, 5th amination of grafted fiber 15% solution of diethylamine at 40oC for 60 min followed by washing with distilled water and drying.

The ion exchanger obtained by a specified method, has a relatively high sorption capacity for the bichromate ions (1 g of the resin absorbs up to 108 mg Cr+6that is 2.0 mmol/g), is regenerated with sulfuric acid in countercurrent, does not restore the chromium VI to chromium III. However, as can be seen from the description, obtaining the resin by a known method is difficult because of mnogostadiinost process, which is economically and environmentally profitable.

The technical result of the invention is to develop a method of producing fibrous ion exchanger according to a simplified technological and environmental-friendly production schemes.

The task is questions in the industrial area, as well as saving time, chemicals, water and isopropyl alcohol to rinse the fibers while improving operational characteristics of the obtained resin.

A significant difference of the invention is that the PAN fiber is treated with an alkaline solution of alkylamine, and then an aqueous solution of dimethyldodecylamine (DMEM). Comparative analysis of known and proposed methods of fibrous ion exchanger are given in table. 1. As can be seen from the data in table. 1, the proposed method of producing fibrous ion exchanger significantly technologically simplified (instead of the 5 stages of the proposed two-stage), which reduces processing time and of reagents used and, accordingly, is the most environmentally friendly way. In the proposed method, the ion exchanger after amination pressed, then washed with water, which is returned to the bath amination and subsequent dosage. The second processing stage is DMEM and the first rinsing water is also returned to the working bath with subsequent dosing. Physico-mechanical properties of fiber-resin will depend on the terms of the modification. When the concentration of alkylamine (PEPA), equal to 10% of voloknistoyj characteristics of the resin obtained in 70% concentration of probes, the temperature of processing fiber 85oC for 45 min and subsequent modification laminirovannogo fiber DMEM concentration of 30% at 85oC for 60 min Thus, the proposed method of producing fibrous ion exchanger in contrast to the known environmentally friendly and technologically run on existing hardware. For the purpose of explaining the invention examples.

Example 1. Fibers based on polyacrylonitrile (PAN) is treated with 10% alkaline solution of alkylamine (polyethylenepolyamine PEPA) at a temperature of 80oC, module baths 20 for 60 minutes Exchange capacity (OE) in HCl 0.1 N. was 5.2 mmol/g (mEq/g). Fiber strength of 13.2 CN/Tex. Then pressed from excess reagents and washed with distilled water, the fiber is treated with 10% aqueous solution DMEM at 80oC for 45 min, the module baths 30 OE 0.1 N. HCl is 5.3 mmol/g of Cr+63.0 mmol/g fiber Strength of the resin is equal to 16.0 CN/Tex.

Other examples of fibrous ion exchanger are given in table.2O

1. The method of obtaining fibrous ion exchanger treatment of polyacrylonitrile fibers, characterized in that the treatment is carried out with an alkaline solution of alkylamine, and then water in alkaline solution of alkylamine within 30 to 60 min at 70 85oC, and then 10 to 30% aqueous solution of dimethyldodecylamine within 45 to 60 min at 75 85oC.

3. The method according to p. 1, characterized in that as alkylamine use polyethylenepolyamine, tetraethylenepentaamine, Triethylenetetramine, Diethylenetriamine.


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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.

2 ex

FIELD: sorbents.

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

Abstract // 2293061


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

FIELD: chemistry.

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 90-95C.

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

FIELD: chemistry.

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 350-450C, 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