The method of obtaining the ion exchange sorbent
(57) Abstract:Use: production of ion exchangers for the removal of coloured organic substances from water and mud. The inventive condensation of phenol, formaldehyde and hexamethylenetetramine in sulfuric acid medium in the presence of the transducer of ethylene glycol at 60 - 75°C, at a molar ratio of phenol: formaldehyde: hexamethylenetetramine: sulfuric acid: ethylene glycol, equal 1 : (0,6 - 2,0) : (0,06 - 0,24) : (0,4 - 1,9) : (2,4 - 5,7) of cured polycondensate extracted with water, ethylene glycol and sulfuric acid. After evaporation of the solution the last return in the process. Formaldehyde is used in the form of paraformaldehyde or trioxane. 2 C.p. f-crystals, 1 table. The invention relates to the field of chemical technology and can be used in the production of anion exchange resins, which are used to remove colored organic compounds from natural water (humic acid), from various hydrolysates chemical and microbiological origin.A known method of producing ionosorbed by condensation of metaphenylenediamine, resorcinol and formaldehyde in hydrochloric acid medium in the presence of large amounts of water. Ionosorbed Oblonsky strength, there is no true porosity, moisture reduction during storage leads to deterioration of quality.To impart porosity, increase the mechanical strength of the sorbent and its capacity for colored organic compounds, a method for sorbent condensation of phenol and formaldehyde in the environment of ethylene glycol at pH 7-8. In the second stage of the process is administered aliphatic amine containing a primary amino group. Having good porosity (0.4 to 1.2 cm3/g), the sorbent provides a high sorption capacity in static conditions (0.7 to 1.5 mg/ml). When testing in dynamic conditions, the sorbent shows a lack of implementation capacity specified in static conditions.Closest to the claimed is a method of producing anion exchange resins, which are co-condensation of phenol and hexamethylenetetramine, an aqueous solution of formaldehyde at 90-95aboutWith sulfate in the environment in two stages. In the first stage, carry out the condensation at a molar ratio of phenol:formaldehyde: hexamethylenetetramine: sulfuric acid: mineral salt: water= 0,095-1: (1,75-1,8):(0,37-0,38):(0,60-0,63):(0,35-0,65): (8,0-8,5) within 2 h, at the second stage, increasing the molar content of the acid up to 1,90-1,95. As mineral and the organic layers) is used to increase acidity in three times.Obtained in this way anion exchange resin has a low porosity of 0.2-0.3 cm3/g, which is a specified way to improve it is not possible. Insufficient capacity of the anion on humus gamestm (0.6 mg/ml) in case of insufficient chemical resistance. When using water commodity resins obtained solution containing sulfuric acid, sodium chloride or potassium, formaldehyde, ammonium sulfate. This solution is almost impossible to return to the process cycle. Regeneration is the process of evaporation allows to obtain a solution containing sulfuric acid, sodium sulfate or potassium, ammonium sulfate. Such a solution cannot be reused. In addition, receive the condensate water containing hydrochloric acid, methylamine. This condensate reuse can only 1-2 times.The aim of the invention is to increase the porosity of the sorbent, chemical stability in contact with the solutions, and the capacity of organic matter humus nature, and other colored compounds). Additionally achieves the important goal of creating zero waste.This goal is achieved by the fact that expose cocondensate phenol and hexamethylenetetramine, formaldehyde in sulfuric acid medium at Navo, the condensation is carried out at a temperature of 60-75aboutAnd formaldehyde is used in the form of low molecular weight polymers of formaldehyde is paraformaldehyde or trioxane. The condensation is carried out at a lower relative pH of the medium in one stage, with the following molar ratio of phenol: formaldehyde: hexamethylenetetramine:sulfuric acid:ethylene glycol= 1: (0,6-2,0): (0,06-0,24):(0,6-1,9):(3,8-5,7), moreover, to ensure the waste products of the technological process glycol and sulfuric acid is extracted from the finished resin with water, and after evaporation of the resulting solution back into the process.The invention is illustrated by the following examples.P R I m e R 1. In a reactor equipped with a jacket for heating and cooling, a stirrer, a thermocouple, load of 4.7 mol (291,4 wt.h.) of ethylene glycol, 0.15 mol (21 wt.h.) hexamethylenetetramine (urotropine), 1 mol (94 wt.h.) phenol, 1.3 mol (137 wt.h.) 93% sulfuric acid, 1.3 mol in terms of formaldehyde (39 wt.h.) trioxane or paraformaldehyde. The temperature of the reaction mass was raised to 67aboutC. At this temperature and stirring maintain the reaction mass 90 minutes, then poured into a pan and placed in a heat chamber, magneticone resin. Spend the extraction of water from the resin of ethylene glycol and sulfuric acid. The yield of tar 376 g with a humidity of 70%. A solution of ethylene glycol and sulfuric acid evaporated and return to the stage of condensation, taking into account when calculating the amount of the glycol and acid.Information on examples 2-3 are summarized in the table that presents the test results of the properties of the obtained sorbent. Examples 4-13 tably serve as a control.The proposed method, the sorbent can be the porosity of the product is 0.5-1.2 cm3/g, the minimum content of organic matter in the treated water, which indicates a high chemical stability and selectivity of sorption, the number purified from organic substances water 800-1000 about/about.the resin. You can create a waste-free manufacturing process through the use of one stripped off the solution after extraction from the pores of the resin of ethylene glycol and sulfuric acid.In receipt of sorbent used products:
the synthetic phenol, GOST 23519-79,
ethylene glycol, GOST 19710-83,
trioxane symmetric, THE 6-05-211-1420-86,
paraformaldehyde, THE 6-05-930-78,
urotropine (hexamethylenetetramine technical), GOST 1381-73,
acid is ncacii by heating phenol, formaldehyde, hexamethylenetetramine in the presence of sulfuric acid and pore-forming with subsequent thermotherapies of the polycondensation product, characterized in that, to increase porosity, chemical resistance and capacity of the sorbent for organic substances as blowing agent used ethylene glycol, the condensation is carried out at 60 - 75oC and a molar ratio of phenol: formaldehyde : hexamethylenetetramine: sulfuric acid: ethylene glycol 1 : 0,6 - 2,0 : 0,06 - 0,24 : 0,4 - 1,9 : 2,4 - 5,7, then from the fully cured polycondensate extracted with water, ethylene glycol and sulfuric acid.2. The method according to p. 1, characterized in that use formaldehyde as paraformaldehyde or trioxane.3. The method according to p. 1, characterized in that the extracted water solution of ethylene glycol and sulfuric acid is evaporated and returned to the process.
SUBSTANCE: method of producing liquid resin essentially consisting of phenol-formaldehyde and phenol-formaldehyde-amine condensates, having water dilution at 20°C at least equal to 1000% and content of free formaldehyde of at most 0.1% of the total weight of the liquid, involves reaction of phenol with formaldehyde in molar ratio formaldehyde/phenol greater than 1 in the presence of a basic catalyst, cooling the reaction mixture and adding amine to said reaction mixture during cooling, which reacts with the free formaldehyde and phenol according to a Mannich reaction. Cooling is stopped the moment amine is added and the reaction mixture is held at addition temperature for a period of time varying from 10 to 120 minutes. After cooling, acid is added in amount which is sufficient to achieve pH value of the resin less than 7.
EFFECT: obtaining and using liquid phenol resin with low content of free formaldehyde.
17 cl, 3 ex
SUBSTANCE: liquid resin essentially consists of phenol-formaldehyde and phenol-formaldehyde-amine condensates and has water dilution at 20°C at least equal to 1000%. The resin contains 0.3% or less free formaldehyde and 0.5% or less free phenol, where said content is expressed with respect to total weight of the liquid.
EFFECT: obtaining and using liquid phenol resin with low content of free formaldehyde and free phenol.
17 cl, 3 ex
SUBSTANCE: invention relates to a water-soluble resin composition, a method of producing such a resin composition, use of the resin composition as binding material for non-woven fibre material, particularly insulation materials, and a method of producing such insulation material. The water-soluble resin composition contains a resin which is a product of reaction of aldehyde, preferably selected from a group including formaldehyde and (lower alkyl (C1-C4)) mono- or di-aldehydes or formaldehyde precursors, which can form formaldehyde directly in the resin composition, and a hydroxyl-aromatic compound selected from a group including substituted and unsubstituted mono- or polycyclic phenols, preferably from phenol, said composition further containing: an amino compound containing 2-6 amino groups, which is selected from a group comprising urea, dicyandiamide and melamine, and where the amino compound can also be a mixture of two or more different amino compounds; and a sugar alcohol. The resin has initial molar ratio of aldehyde to the hydroxyl-aromatic compound from 2.3 to 5.5; the ratio of the resin to the amino compound plus the sugar alcohol ranges from 45:55 to 70:30 pts.wt; the ratio of the amino compound to the resin lies between 20:80 and 50:50 pts.wt; and the ratio of the sugar alcohol to the resin plus the amino compound lies between 5:95 and 30:70 pts.wt. The sugar alcohol has a boiling point higher than the setting point of the resin.
EFFECT: obtaining a resin composition having well preserved water-solubility and without ammonia, reduced phenol and formaldehyde emissions during hardening and preservation of mechanical properties of the hardened resin, particularly wet strength.
16 cl, 2 tbl, 6 ex
SUBSTANCE: invention relates to a liquid phenol resin for addition to a gluing composition for mineral fibres, which primarily contains phenol-formaldehyde condensates and phenol-formaldehyde-glycine condensates. The invention also relates to a method of producing said resin, a gluing composition containing the resin and to insulating materials based on mineral fibres glued with said gluing composition.
EFFECT: improved resin properties.
16 cl, 2 tbl, 9 ex
SUBSTANCE: described curable compositions comprise a polybenzoxazine component, a polyamine component, and a fluoropolymer component. The fluoropolymer component used is selected from fluoroolefin (co) polymers, perfluoroolefin (co) polymers, (co) polymers of perfluoroalkylvinylethers and (co) perfor alkoxyvinyl ether polymers.
EFFECT: invention provides protection against corrosion of substrates under the influence of high temperatures.
14 cl, 3 tbl, 3 ex
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