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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EFFECT: optimized manufacture conditions.

2 ex

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2 cl, 1 tbl, 2 ex

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18 cl, 5 tbl, 16 ex

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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

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2 cl, 2 tbl, 30 ex

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EFFECT: improved preparing method.

1 tbl, 8 ex

Abstract // 2293061

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7 cl, 9 tbl, 9 ex

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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.

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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

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