Carbon sorbent with antibacterial properties and method for preparing it
FIELD: medicine, pharmaceutics.
SUBSTANCE: group of inventions refers to a method for preparing a carbon sorbent with the antibacterial properties, and to the carbon sorbent with the antibacterial properties prepared by this method. The declared method involves impregnation of the carbon hemosorbent granules in an initiator solution in N-vinylpyrrolidone at pH 7.0-7.5 and a residual pressure of 15-20 mm Hg. The hemosorbent : initiator solution in N-vinylpyrrolidone ratio is 1:1.4-2.0. Then the temperature is raised to 65-75°C, kept at that temperature for 0.5-8 hours in an inert medium and washed in water from the residual monomer at room temperature.
EFFECT: carbon sorbent with the antibacterial properties prepared by the specified method represents the round granules, contains polyvinylpyrrolidone in an amount of 4,5-5,5% and is characterised by a specific surface adsorption of less than 50 m2/g and total pore volume of less than 0,30 cm3/g.
2 cl, 2 tbl, 1 dwg, 7 ex
The invention relates to a process for the production of carbon sorbents with antibacterial properties based on porous carbon adsorbents and is intended for use in medicine and veterinary medicine.
The development of effective materials with antibacterial properties, is still an urgent task. One of the most effective methods of efferent therapy for the treatment of infectious diseases is the application sorption (vulnerable) is a method of removing toxic components through the wound or inflammation. When applying sorbent cleans the wound of the content or purulent cavity and accelerates the transport of certain substances from the blood and their subsequent sorption.
It is known that carbon materials exhibit high sorption capacity against bacteria and bacterial toxins.
The manifestation of the sorption capacity of activated carbon relative to the staphylococcal toxin was found in the works Can, Vffsekvua, Vinaccia and others (Kaplina NN. [and others] a Method of increasing the sorption capacity of activated carbon relative to the staphylococcal toxin // Laboratory work. 1979. No. 9. S). Also found that the nature and amount of adsorption of bacterial cells depends on the pore volume of the carbon sorbent (Cove is lenko GA [and other] // Carbon materials as adsorbents for biologically active substances and bacterial cells. 1999. T. No. 6. S-795).
Known carbon materials SUMS-1 (based on mineral media Al2O3) and SKN-1K, SKN-4M (synthetic polymers), can absorb from the lymph cells of Staphylococcus aureus (strain Wood 46"), pneumococcus, Streptococcus (Samsonov C.V. Comparative efficiency of sorption of bacteria and bacterial toxins carbon and carbon-mineral sorbents // Bulletin of physiology and pathology of respiration. 2008. VIP. P.48-50). According to the results of carbon-mineral sorbent SMS-1 was besieged on its surface the largest number of investigated pantropic microorganisms that due to the presence on its surface of various chemical nature centers: polar and non-polar. Largely this sorbent was deposited aureus, somewhat less pneumococcus and Streptococcus.
To improve the antibacterial properties of carbon hemosorbent SUMS-1 on its surface adsorbing antibacterial and antimicrobial drug metronidazole (the active substance: 1-(b-oxyethyl)-2-methyl-5-nitroimidazol) (RF patents №№2121842, 2127595, 2144797). This drug is active against Trichomonas vaginalis, Gardnerella vaginalis, Giardia intestinalis, Entamoeba histolytica, obligate Ana is one bacteria: Bacteroides spp. (including Bacteroides fragilis, Bacteroides distasonis, Bacteroides ovatus, Bacteroides thetaiotaomicron, Bacteroides vulgatus), Fusobacterium spp., Veillonela spp.; some gram-positive bacteria: Eubacterium spp., Clostridium spp., Peptococcus spp., Peptostreptococcus spp. and Helicobacter pylori.
The effect of this drug have not been investigated against pathogenic bacterial pathogens of sepsis. In addition, the use of metronidazole are the contraindications: hypersensitivity, impaired hematopoiesis, active disease of the Central nervous system, as well as a significant number of side effects.
Thus, to increase the effectiveness of antibacterial properties of carbon sorbents, you must use the modifier is a drug active against pathogenic microflora wide spectrum, but not its negative effects on the body.
It is known that polymers based on N-vinylpyrrolidone (VP) are widely used as hydrophilic non-toxic materials in medicine and biology. They are approved for use in contact with the biological environment of a living organism and can perform a variety of functions as part of medical supplies (Chernikova E.V., Terpugova PS, Filippov A.N. Controlled radical polymerization of N-vinylpyrrolidone and N-minilatinname under conditions of reversible chain transfer mechanism accession is their fragmentation. // Russian journal of applied chemistry. 2009. T. No. 10. S-1737). Polymers based on EAP is used for modification of anionic surfactants having a high bactericidal activity (Afinogenov G., Panarin E.F. Antimicrobial polymers. Saint-Petersburg: Hippocrates, 1993, 263 C.). A number of copolymers of VP with the ionic comonomers has its own antimicrobial activity, immunostimulating and immunomodulating effects. For removal of toxic substances from the body usually use poly-N-vinyl pyrrolidone (PVP) with a molecular weight of 10000-15000.
Low molecular weight PVP is widely used as an auxiliary substance for the creation of different dosage forms, which have antibacterial effects (RF patents №№2281773, 2279278); when you create eye films in ophthalmology (patent No. 2286170); as a solubilizer when creating a disinfectant (patent No. 2308292); a biologically active substance and the amendment in wound dressings (patent No. 2331444); as conjugate when creating antibacterial medicines (patent No. 2371447); as a stabilizer in antiviral drug (patent No. 2438697); as an immunomodulator in the preparations for the prevention and treatment respiratory and gastro-intestinal infectious diseases of bacterial and viral etiology of farm animals (patent No. 2286171) is so
It is known the use of PVP in the composition of ointments for the treatment of infected wounds with a content of up to 5.5% (patents No. 2146127, 2233652). According to research Vinylicious and others (Vinmalva, Vasilenko, Yahatanishi. The influence of polyvinylpyrrolidone on microbial cells // Journal of Microbiology. 1987. # 4. P.9-11) PVP starts to show antibacterial properties at a concentration in solution of about 1.0%.
Application of PVP on the surface of the carbon sorbent can improve its detoxification properties due to migration of PVP macromolecules in the biological fluid. The additional positive effect of the increase of wettability of the carbon material due to freeze-drying of the surface and lower surface energy.
Closest to the proposed sorbent is mesoporous carbon hemosorbent the Spa (scientific production Association-1, which consists of granules of size 0.5-1.0 mm, characterized by a high chemical purity (carbon content not less than 99,5%) and specific adsorption surface 300-400 m2/g (Technical conditions TU 9398-002-71069834-2004 carbon Hemosorbent in saline solution sterile Spa (scientific production Association-1; advertising Avenue Spa (scientific production Association-1 Institute of hydrocarbons processing SB RAS, 2011).
Closest to the proposed method of obtaining carbon sorbent having aetsa method of modifying carbon sorbent by impregnation of the granules of carbon hemosorbent aqueous solution of aminocaproic acid with a concentration of 5-20% when the ratio hemosorbent:the solution of the modifying acid 1:10-1:20 for 2-4 hours at a temperature of 25-90°C, Department of hemosorbent from the impregnating solution, drying the impregnated hemosorbent at 105°C to constant weight, the process of polycondensation deposited on the surface of hemosorbent aminocaproic acid in an inert environment at a temperature of 120-350°C for 0.25 to 6 hours under stirring, boiling in distilled water for 1-3 hours and drying the obtained product in air at room temperature (patent RF №2440844).
The aim of the invention is to develop a carbon sorbent with antibacterial properties.
The proposed method of obtaining carbon sorbent with antibacterial properties includes impregnation of the granules of carbon hemosorbent solution modifier and drying of the product and differs in that the impregnation of the pellets of 0.2-1.0% solution of the initiator in N-vinyl pyrrolidone at pH 7,0-7,5, a residual pressure of 15-20 mm Hg and the ratio hemosorbent:initiator solution in N-vinyl pyrrolidone 1:1,4-2,0 within 15-30 minutes, followed by rise in temperature up to 65-75°C., holding at that temperature for 0.5-8 hours in an inert atmosphere and washed in water from the residual monomer at room temperature for 0.5 to 2 hours.
The proposed carbon sorbent with antibacterial properties is a gr is duly rounded, contains polyvinylpyrrolidone in the amount of 4.5-5.5 percent, is characterized by specific adsorption surface is less than 50 m2/g and total pore volume less than 0.30 cm3/year
Distinctive features of this invention are:
- use as source material carbon hemosorbent developed specific adsorption surface 300-400 m2/g and a total pore volume of at least 0.4 cm3/g;
- surface modification of carbon hemosorbent initiator solution in N-vinyl pyrrolidone, followed by curing the applied substance.
The inoculation process is carried out in several stages:
- impregnation of the granules of carbon hemosorbent initiator solution in N-vinyl pyrrolidone with a concentration of 0.2-1.0% at pH 7.0 and 7.5, the residual pressure of 15-20 mm Hg and the ratio hemosorbent:initiator solution in N-vinyl pyrrolidone 1:1,4-2,0 within 15-30 minutes.
- curing the applied N-vinylpyrrolidone, why spend the rise of temperature 65-75°C and maintained granules at this temperature for 0.5-8 hours in an inert atmosphere;
- washing pellets from residual monomer in water at room temperature for 0.5-2 hours;
- drying the washed product at room temperature for 18-24 hours with the production of carbon sorbent with antibacterial properties.
modificirovanie carbon hemosorbent the proposed method modifier - monomer N-vinyl pyrrolidone - with its subsequent polymerization changes the chemical nature of the surface of the carbon matrix, and its porous structure. The results illustrating the changes of the parameters of porous structure and chemical composition of the samples of the carbon sorbent, obtained on the prototype and in the modification of N-vinylpyrrolidone followed by polymerization, in accordance with examples of the present invention, are shown in table 1.
Determination of physico-chemical characteristics of samples of the original and modified carbon sorbent was carried out by standard methods used in the study of porous materials: basic textural characteristics - specific adsorption surface area, total pore volume and the pore size was determined by isothermal adsorption-desorption of nitrogen obtained with the device "Gemini 2380 (USA). The calculation of adsorption specific surface area was carried out according to the BET equation. The topography and the surface morphology of the samples of the carbon sorbent was studied using scanning electron microscopy with electron microscope "JSM - 6460 LV" ("JEOL", Japan). X-ray microanalysis of the surface of the samples was performed by energy dispersive spectrometer EDAX ("EDAX", Japan)equipped with a Si (Li) detector with energy the economic resolution of 130 eV. IR spectra were recorded on a spectrometer NICOLET 5700 company Thermo Fisher Scientific with a resolution of 4 cm-1and the number of accumulation spectra 32. Spectra are presented after processing in the software package ORIGIN (base line correction and smoothing). Measurement by x-ray photoelectron spectroscopy was carried out on the device ES-300 Kratos Analytical with the use of Mg-anode (hv=1253.6 eV). The amount deposited on the surface of hemosorbent polymer PVP was determined by the method of differential thermal analysis for the weight loss that was observed in thermograms in the temperature range of 330 to 340°C.
Figure 1 shows the data of thermogravimetric (TGA) and differential thermal (DTA) analyses of samples of the prototype (a) and carbon sorbents in example 3(b) and example 7(b).
Studies were conducted on the device DTG-60H of SHIMADZU (Japan), which writes the same thermal curves: the temperature T and DTA, TG. The accuracy of temperature was 1°C, and the weight change of 0.1%. The shooting took place in an atmosphere of air, in the temperature range from room temperature up to 1000°C, weighed sample was 10 mg, the speed of temperature rise of 10°/min
The presence of the monomer (N-vinylpyrrolidone) was determined by the results of the analysis of the composition of the wash water modified sorbents by NMR With13spectrometer "Adance-400". In the presence of VP in the composition of the wash water on the NMR spectra were recorded peaks, characteristic for the EAP.
To study the antibacterial properties of modified samples of carbon hemosorbent in the Central research laboratory of the Omsk state medical Academy conducted biomedical research (bench tests).
Use the gram-positive test organisms (Staphylococcus aureus, Staphylococcus aureus) and gram-negative test organisms (Pseudomonas aeruginosa, Escherichia coli; Klebsiella pneumoniae, Klebsiella pneumonia, Escherichia coli, Escherichia coli). In addition, we examined the mixture of the tested crops, which were prepared by mixing equal volumes of the prepared working concentration of microbial cells. The original breeding with a concentration of 0.5 units on Mac to Parlando using a Densitometer, the mixing of cultures, suspensions sorbent culture was performed on a shaker for "Vortex". Working dilution cultures to experience - 1×103CFU in 1 ml Sorption cells conduct of physiological solution with a concentration of microbial cells 1×103CFU/ml
For evaluation of antibacterial action of carbon sorbents used the method of direct seeding on a nutrient medium. As the nutrient medium is selected mastopathy agar.
Quantitatively the definition of microorganisms was performed by counting bacterial colonies on two Petri dishes with a diameter of 90 mm, find the mean and multiplying by the rate of breeding, to calculate the number of bacteria in 1 g per 1 ml of sample. The control were sown working dilutions of the tested crops.
Sterilization sorbents before the bench of biomedical tests carried out with saturated steam at a gauge pressure of 0.11±0.02 MPa and a temperature of (12±1)°C in the autoclave.
To illustrate the invention the following examples.
Example 1 (the prototype)
To hemosorbent (0.5 ml) was added 1 ml of microbial suspension (test microorganisms) and incubated for days with periodic manual shaking within the first 30 min of contact (to remove air bubbles). Have three parallel tests for each type of bacterial cells and a mixture of microorganisms.
The supernatant in the amount of 100 µl inoculated on agar plates with culture medium after 24 h of contact with the sorbent. Sown in Petri dishes incubated for 18-20 hours at 37°C in a thermostat. Conduct the counting of grown colonies stencil visually in 5 fields on 1 cm2and count on the size of the Cup. The result judged by the number of colony forming units on the surface of the agar in comparison with the control.
Carbon hemosorbent showed antibacterial activity against the test microorganisms Staphylococcs aureus: the number of bacterial cells after contact with hemosorbent decreased from 1x10 3up to 30 CFU/ml (300 to 11 colonies on the Cup). The concentration of gram-negative bacteria after contact with the carbon hemosorbent comparable to the concentration in the control samples.
A portion of hemosorbent (1.0 g) is poured into the three-neck flask, tightly closed and connected to a vacuum pump with a vacuum of not less than 15 mm Hg and maintained at room temperature for 1 hour. Next, prepared with 0.5% solution of initiator (DINITROL azabicycloalkanes acid - DINIZ) in the EAP impregnated insulated sample for 15 minutes at a ratio of hemosorbent:initiator solution in N-vinyl pyrrolidone 1:1,4. Then the vacuum pump is shut off, the flask serves inert gas (argon), raise the temperature to 75°C and maintained within 0.3 hours. After modifying the sample sorbent is removed from the flask and conduct washing with distilled water at room temperature for 0.5 hour, after which the sample is dried at room temperature for 24 hours.
A portion of hemosorbent impregnated with a 1% solution of the initiator in the EAP at a ratio hemosorbent:solution 1:1.5 and conduct the polymerization at a temperature of 68°C for 2 hours followed by washing and drying.
Spend the adsorption of bacterial cells according to example 1.
It is established that carbon sorbent the possession is t antibacterial activity against the studied test-microorganisms - after interaction of the modified sorbent with pathogenic microbial growth on the Petri dishes were missing.
A portion of hemosorbent impregnated with 0.1% solution of the initiator in the EAP at a ratio hemosorbent:solution 1:1.2 and conduct the polymerization at a temperature of 85°C for 4 hours followed by washing and drying.
A portion of hemosorbent impregnated with a 1.5% solution of the initiator in the EAP at a ratio hemosorbent:solution 1:1.6 and conduct the polymerization at a temperature of 50°C for 8 hours followed by washing and drying.
A portion of hemosorbent impregnated with a 0.7% solution of the initiator in the EAP at a ratio hemosorbent:solution 1:1.4 and conduct the polymerization at a temperature of 68°C for 2 hours followed by washing and drying.
A portion of hemosorbent impregnated with 0.8% of a solution of the initiator in the EAP at a ratio hemosorbent:solution 1:2 and conduct the polymerization at 70°C for 6 hours followed by washing and drying.
Analysis of physico-chemical characteristics of samples carbon sorbent has allowed to establish the effect of the modification on the parameters of the porous structure and chemical composition (table 1). In the process of modifying the fully closed micropores in ~2 times lower volume of mesopores. The shielding of the carbon surface and the polymer film PVP reduces its value in ~2-3 times (from 394 to 32 m 2/g), reduced total pore volume from 0,630 cm3/g to 0,208 cm3/so In this case, the larger the amount of the modifier into the porous structure, the lower the value of specific surface area and total pore volume. The nitrogen content in the composition of the sorbent increases from 0 to 3.52% for the modified samples.
As follows from the examples and table 1, the reduction in the number of modifying solution leads to a reduction in the content of PVP, sorbirovannogo on the surface of hemosorbent and, consequently, to a smaller change of texture: the pore volume and specific surface area. The decrease in the concentration of the initiator in modifying the formulation leads to incomplete curing the applied monomer and the presence of EP on the surface of the modified hemosorbent even at the time of polymerization for 4 hours and subsequent washing. The increase in the content of the initiator to 1.5% also reduces the amount of polymer on the surface of hemosorbent. Lowering the temperature of polymerization of up to 50°C almost no leads to polymerization of the EAP, texture indices are practically does not decrease the amount of PVP at the time of polymerization for 8 hours is 1.0%.
To remove PVP carbon sorbent samples were kept in saline solution (0.15 M NaCl) in static conditions at room temperature for 24 hours. Next, the samples were dried at anatoy temperature and analyzed: investigated the adsorption properties by adsorption of nitrogen-determination of specific surface value (S BET), determined the content of total nitrogen (table 1). Aqueous solutions after contact with the carbon sorbent samples were analyzed by NMR to identify them in PVP.
It was found that after contact with saline solution for 24 hours, the specific surface is increased, and the nitrogen content of this naturally decreases. The results obtained indicate migration caused to PVP in a physiological solution.
The results of the study of antimicrobial properties of modified samples of carbon hemosorbent presented in table 2. In the control crop germ concentration was 1×103CFU/ml After exposure to the investigated carbon sorbents was found that the sample of carbon hemosorbent (prototype) exhibits antibacterial properties against gram-positive bacterial (Staphylococcus aureus, Staphylococcus aureus). Sample carbon sorbent modified EAP with subsequent polymerization, according to the poster of medical tests, exhibits antibacterial properties against gram-positive and against gram-negative bacteria. After contact of the sorbent with pathogenic microflora growth of colonies of bacterial cells on the Petri dish was missing.
Thus, whom the Lex physico-chemical methods are installed, the process of modifying the carbon hemosorbent N-vinyl pyrrolidone proceeds with the formation of the polymer poly-N-vinylpyrrolidone, which is able to migrate in a biological environment (physiological solution), leading to the manifestation of the antibacterial properties of the obtained carbon sorbent.
The proposed carbon sorbent with antibacterial properties is a promising material for vulnerable (application medicine).
|Example 1 (prototype)||Example 3|
|Concentration, CFU/ml||Growth in the Cup||The concentration of CFU/ml||Growth in the Cup||Concentration, CFU/ml||Growth in the Cup|
|1||Pseudomonas aeruginosa||1·103||drain height, 30 colonies||1·103||comparable to the control||0||growth no|
|2||Staphylococcus aureus||1·103||drain height, 300 colonies||~30||11 colonies||0||growth no|
|3||Escherichia coli||1·103||drain height, 300 colonies||1·103||comparable to the control||0||growth no|
|4||Klebsiella pneumoniae||1·103||drain height, 300 colonies||1·103||comparable to the control||0||growth no|
|5||The mix of cultures||1·103||drain height, 300 colonies||1·103||comparable to pin Olam||0||growth no|
1. The method of obtaining carbon sorbent with antibacterial properties, including impregnation of the granules of carbon hemosorbent solution modifier and drying of the product, characterized in that the impregnation of the pellets of 0.2-1.0% solution of the initiator in N-vinyl pyrrolidone at pH 7,0-7,5, a residual pressure of 15-20 mm Hg and the ratio hemosorbent:initiator solution in N-vinyl pyrrolidone 1:1,4-2,0 within 15-30 min, followed by rise in temperature up to 65-75°C., holding at that temperature for 0.5 to 8 hours in an inert atmosphere and washed in water from the residual monomer at room temperature for 0.5 to 2 hours
2. Carbon sorbent with antibacterial properties in the form of granules rounded, characterized in that the method according to claim 1, contains polyvinylpyrrolidone in the amount of 4.5-5.5 percent, is characterized by specific adsorption surface is less than 50 m2/g and total pore volume less than 0.30 cm3/,
SUBSTANCE: invention relates to production of activated carbon. Disclosed is a method of forming activated carbon from microcrystalline cellulose, involving: converting microcrystalline cellulose powder into microcrystalline cellulose granules by mixing microcrystalline cellulose powder with water and extrusion to obtain spherical granules. The method involves carbonisation the microcrystalline cellulose to obtain carbonised microcrystalline cellulose and activation of the carbonised microcrystalline cellulose to obtain activated carbon. Disclosed also is a method of making a smoking article filter which contains the obtained activated carbon granules, and a method of making a smoking article having said filter.
EFFECT: invention provides an optimum porous structure of activated carbon used in smoking article filters.
9 cl, 2 dwg
SUBSTANCE: invention relates to a method for carbonisation and activation of carbon material and an externally heated revolving furnace for realising said method. The revolving furnace has an inlet and a discharge side, with an inclination downwards towards the discharge side, annular partition walls lying along the furnace for controlling movement of the material and hoisting boards between the partition walls for mixing the material and parts which raise the material upwards and force the raised material to fall in stages into the lower part of the revolving body. The method involves feeding material into the discharge end of the furnace. The material is fed into the furnace in an atmosphere of water vapour or carbon dioxide, essentially free from oxygen. Temperature which is sufficient for drying or removing the solvent from the material without carbonisation is maintained in the first zone of the furnace. Temperature maintained in the second zone lying downstream from the first zone is sufficient for carbonisation of the material, and the temperature maintained in the third zone lying downstream from the second zone is sufficient for activation of the carbonised material.
EFFECT: obtained activated carbon is in form of granules with low content of fine coal, having both a mesoporous/microporous structure and a highly active surface.
16 cl, 7 dwg, 1 tbl
FIELD: medicine, pharmaceutics.
SUBSTANCE: claimed group of inventions relates to adsorbent, which contains porous carbonic material, which is produced from vegetable raw material, which has content of silicon (Si) not less, than 5 wt %, and which has value of specific surface area, determined by nitrogen method BET, not less than 10 m2/g, content of silicon not less than 1 wt %, and volume of pores determined by BJH method and MP method, not less, than 0.1 cm3/g. Said adsorbent is applied for adsorption of organic substance, which has average molecular weight from 1×102 to 5×102 and suitable for: medical and per oral application. Also claimed are medication applied in case of renal failure and functional nutrition, which contain claimed porous carbonic material.
EFFECT: invention ensures adsorbent with high adsorption ability.
5 cl, 26 tbl, 9 dwg, 6 ex
FIELD: medicine, pharmaceutics.
SUBSTANCE: declared group of inventions which refers to an adsorbent, a mask with adsorbent and an absorbent layer for organic substance adsorption, an adsorbent for allergen adsorption, an adsorbent to be used in medicine and an oral adsorbent. Said adsorbents, mask and adsorbent layer contains a porous carbon material comprising spherical pores having average diameter of 1×10-9 to 1×10-5 and regularly spaced (in an orderly fashion) with a surface area of the material making more than 3x102 m2/g.
EFFECT: invention provides preparing the adsorbents with high adsorbent ability.
37 cl, 4 dwg, 20 tbl, 7 ex
SUBSTANCE: invention relates to methods of producing activated carbon. The carbon precursor material in form of fibre with diameter of 7-20 mcm is coated with a phosphorus-based chemical solution and activated. Activated carbon can also be formed by coating an immature carbon precursor with a chemical solution which chemically reacts with carbon, followed by carbonisation of the obtained material and physical activation of the material during at least part of the carbonisation operation. In another version, activated carbon can be formed by coating carbon or a carbon precursor with iron and nickel nanoparticles and carbonisation. If the carbon is a carbon precursor, subsequent catalytic activation in air and inert gas, and physical activation in steam or carbon dioxide gas is carried out. If the carbon is not a carbon precursor, catalytic activation and physical activation of the chemically pre-activated carbon is carried out after coating with nanoparticles.
EFFECT: invention enables to obtain activated carbon, having controlled mesoporosity.
15 cl, 18 dwg, 6 tbl, 11 ex
SUBSTANCE: invention relates to production of adsorption-activated carbon products. An article with a given shape, made from texolitem, is filled with activated carbon with particle size of 0.5-1.5 mm and subjected to carbonisation while raising temperature at a rate of 4-12°C/min to 850-870°C in the medium of carbon dioxide gas. The product is held at final temperature for 25-35 minutes and activated with steam at 820-840°C until development of maximum sorption pore volume of 0.25-0.50 cm3/g.
EFFECT: high adsorption capacity of the obtained carbon products and low power consumption during production thereof.
SUBSTANCE: method includes stages of combined flow formation from mainly or fully unmixable heated flows of polymerised liquid initial substance and liquid disperse medium and processing of combined flow of polymerised liquid initial substance by dispersion, in dispersion medium in form of drops. Mixing and dispersion of combined flow are carried out in joined with tube statistic mixer during short, in comparison with polymerisation duration, time, to eliminate unintended increase of viscosity and/or precipitation of agglomerated materials. After that, polymerisation of drops in laminar flow of dispersion medium at specified temperature of polymerisation until separate solid granules, incapable of agglomeration are formed, and separation of said granules from dispersion medium are carried out.
EFFECT: method and device in accordance with invention make it possible to obtain granules with relatively equal size, and eliminate undesirable accumulation of polymer aggregates.
25 cl, 7 dwg
SUBSTANCE: invention relates to a method of producing a carbon sorbent used for extracting rare metals, particularly gold cyanide from aqueous alkaline solutions. The method involves treatment of activated carbon with a polymer with amino groups. Activated charcoal is treated using polyhexamethylene guanidine hydrochloride in form of an aqueous solution. After treatment, alkali is added while stirring and the solution is separated from the carbon. The carbon is saturated with ammonia solution, phenol and formalin. The mixture is held while boiling for 1-5 hours and the carbon separated from the solution is dried at 150-160°C.
EFFECT: obtaining a carbon composition with high strength and anion-exchange capacity from readily available and cheap charcoal.
1 tbl, 5 ex
FIELD: process engineering.
SUBSTANCE: invention relates to production sorbents intended for entrapping radioactive isotopes. Proposed method comprises preparing impregnation solution that contains triethylendiamine and potassium or barium iodide, impregnating active carbon grains with said solution, aging and thermal treatment. Carbon with grain size of 1.5-3.5 mm, volume of micro pores of 0.35-0.60 cm3/g, volume of transfer pores of 0.15-0.35 cm3/g, is used. Impregnation is performed dispensing impregnation solution. Total volume of impregnation solution makes 0.82-1.00 of total volume of pores of active carbon.
EFFECT: higher degree of entrapment of radionuclides of iodide-131 and methyl iodide-131.
3 cl, 3 ex
SUBSTANCE: invention relates to decontamination of wastes. Spent activated carbon undergoes thermal treatment with water vapour. The water vapour is split into two streams, part of which is fed into a plasmatron. The low-temperature vapour plasma obtained in the plasmatron is fed into a container where, upon mixture with the remaining part of the water vapour, a high-temperature jet of reaction gas at temperature 1000-1200°C is obtained. The activated carbon is blown with the obtained reaction gas. 1.3-1.5 kg of water vapour is spent on 1 kg of activated carbon. A gaseous mixture containing H2 and CO is obtained from decontamination of the spent carbon.
EFFECT: possibility of obtaining a valuable product in form of a gaseous mixture containing H2 and CO during decontamination of spent activated carbon.
SUBSTANCE: invention relates to analytical chemistry. Disclosed is a complexing sorbent which is obtained by impregnating the surface of cellulose filters with organic complexing reagents selected from thiophene-2-carbaldehyde thiosemicarbazone or 5-nitrothiophene-2-carbaldehyde thiosemicarbazone. The sorbent is efficient for concentrating heavy metals from solutions for subsequent X-ray fluorescence determination.
EFFECT: obtaining a sorbent having high sorption capacity for a wide range of aliovalent ions and capacity for both individual and group extraction of heavy metals.
3 cl, 2 tbl, 2 dwg
SUBSTANCE: invention can be used for improvement of membrane and sorption technologies, in water preparation, in elaboration of technologies for utilisation of ions of heavy metals from water solutions and sewage waters. Method of modification of cellulose-based sorbents includes their successive treatment with solutions of oxidiser, hydroxylamine hydrochloride, hydrogen peroxide and sodium hydroxide with washing with water after each stage. Interaction of sorbents with oxydiser is realised with microwave irradiation with power 300 W, with frequency 2.45 GHz and temperature 25-55°C for 5-15 minutes in solution with concentration 0.1-0.3 M at pH 2.5-4.5 and module solution/sorbent 15-50. Treatment with hydroxylamine hydrochloride is carried out with 0.3-1 M water solution at pH 3-5, module solution/sorbent 15-50 for 40-60 min. treatment with hydrogen peroxide id performed with its 30% solution at pH 5-7 for 30-60 min at room temperature and module solution/sorbent 15-50. Treatment with sodium hydroxide solution is carried out at pH 8-9 for 5 min at room temperature. As oxidiser preferably used is sodium metaperiodate, periodic acid or sodium hypochlorite, and as sorbents - cotton or wood cellulose, short flax fibre or sawdust.
EFFECT: invention makes it possible to increase degree of extraction of ions of heavy metals from solutions with concentration of metal ions to 1,5 mmol/l by 13-15% and reduce sorption time to 1-20 min.
2 cl, 1 tbl, 5 ex
SUBSTANCE: surface is treated with a dispersed polymer-containing composite material, followed by regeneration or recycling of the spent product. The polymer used is a linear polymer with an unlimited degree of swelling in an oil product - latex of natural rubber or butadiene-styrene rubber, deposited on inert filler. The inert filler used is material with high specific surface area - vermiculite or oxidised graphite, obtained by foaming the starting component immediately before depositing the polymer on it. The filler is treated with the polymer at low pressure ranging from 0.9 atm to 1·10-4 atm. Sorbent is obtained in the apparatus directly at oil or oil product spill site.
EFFECT: high efficiency of the method of cleaning surfaces by increasing sorption capacity of the sorbent, reduced cost of transporting the sorbent.
2 cl, 3 ex
SUBSTANCE: inventions can be used in apparatus for purifying natural and waste water. The sorbent catalyst is obtained from schungite III which is ground to particle size 3-5 mm with carbon content of about 30%. After washing with water, the schungite is flooded with a solution consisting of a mixture of 5% HCl and 5% H2O2 solutions in ratio: 5% HCl - 50%, 5% H2O2 - 50%, and held in that solution for 8 hours. The schungite is then rewashed with water and dried at temperature of 105°C.
EFFECT: obtained sorbent catalyst has high sorption and catalytic properties and its use provides high efficiency and cost-effectiveness of the process of purifying natural and waste water.
2 cl, 1 tbl, 1 ex
FIELD: process engineering.
SUBSTANCE: invention relates to sorption technologies. Carbon sorbent represents a matrix of activated charcoal impregnated with inorganic acid. Said sorbent is produced by adding inorganic acid to substances selected from the following family without heating: wood, manure compost, peat-moss, straw, municipal hard wastes containing manure, litter materials, nutshell, coir fiber, coal or oil coke. Ammonia is absorbed from gas flow on prepared sorbent.
EFFECT: efficient sorbent, cheap raw stock, simple process.
19 cl, 1 dwg, 7 tbl
SUBSTANCE: invention relates to applied ecology and can be used to purify industrial waste water from phenols, suspended substances and surfactants, heavy metal ions and oil products. The method of producing sorbtion material involves treating sawdust with 4.5-5.5% orthophosphoric acid solution, washing with distilled water, mixing bentonite clay, water and treated sawdust in ratio of 1:2:2, drying the obtained mixture at temperature 80-85°C, grinding to obtain a 3-15 mm fraction and heat treatment at temperature 90-95°C.
EFFECT: invention enables to obtain an effective sorbent with high mechanical strength.
1 tbl, 1 ex
FIELD: process engineering.
SUBSTANCE: invention relates to molecular sieve with hydrophobic coating used in electronic hardware components. Sieve comprises particles sized to 1000 nm or less with their surface coated by silane of general formula SiR1R2R3R4, where radicals R1R2R3R4 feature definite structure. Proposed method consists in processing alumophosphates or silicoalumophosphates by said silanes. Invention covers compositions and apparatuses containing said molecular sieves.
EFFECT: efficient trapping of gas molecules, good dispersion in organic compounds.
21 cl, 10 dwg, 6 ex
SUBSTANCE: present invention relates to aggregated zeolite adsorbents based on X and LSX zeolites. The adsorbent contains zeolite X powder, substituted with at least 90% barium ions only or barium and potassium ions, where in exchangeable sites occupied by potassium, representing up to 1/3 of exchangeable sites occupied by barium and potassium ions, there are additional alkali or alkali-earth ions other than barium and potassium, as well as zeolite LSX powder substituted with at least 90% barium ions only or barium and potassium ions, where in exchangeable sites occupied by potassium, possibly representing up to 1/3 exchangeable sites occupied by barium and potassium ions, there are possibly additional alkali or alkali-earth ions other than barium and potassium, and also binder in an amount equal to or less than 20% of the total weight of the agglomerated zeolite adsorbent. The obtained adsorbents are efficient in separating C8 aromatic isomers, particularly xylenes, separating sugars, separating polyatomic alcohols, separating isomers of substituted toluenes, separating cresols and separating dichlorobenzenes.
EFFECT: higher efficiency.
16 cl, 1 dwg, 5 tbl, 10 ex
SUBSTANCE: invention relates to agglomerated zeolite adsorbents. Disclosed is a powdered zeolite X based adsorbent with low content of silicon dioxide and containing barium or barium and calcium in an exchange complex. Disclosed also is a method of obtaining an agglomerated zeolite adsorbent, in which a mixture of zeolite clay and a silicon dioxide source is formed, treated with sodium hydroxide, washed and subjected to ion exchange. The adsorbent is recommended for use when separating sugar, alcohols containing several substituted hydrogen atoms, isomers of substituted toluene, cresols or when extracting paraxylene of very high purity.
EFFECT: invention enables to obtain an agglomerated adsorbent with small crystals and high mechanical strength.
22 cl, 7 tbl, 9 ex
FIELD: processing procedures.
SUBSTANCE: invention can be used in analytic chemistry for sorption concentration and successive determination of heavy metals in water solutions. The procedure for production of sorption material consists in impregnation of surface of a cellulose filter with an analytic reagent wherein thio-semi-carbazone of picoline aldehyde is used as such. Impregnation is carried out with conditioning cellulose material in solution of the reagent in ethanol containing 2.5 % of cetyl alcohol with successive extraction and drying in air. Produced cellulose material is applied for sorption-roentgen-fluorescent analytic determination of heavy metals in water solutions. Metals are extracted with cellulose material for roentgen-fluorescent determination at pH 7.5-10.5, preferably, at pH 10.0.
EFFECT: simple and safe procedure for production of sorption cellulose material used for efficient concentration of heavy metals with successive determination of each of them separately and in whole.
4 cl, 2 tbl, 2 ex
FIELD: process engineering.
SUBSTANCE: invention relates to method of producing active sorbents. Proposed method comprises mixing the powder of zeolite or silica gel or combination thereof with polymer solution to form obtained composition to final product of preset geometry. Solution of ethylene fluorine derivatives (that of Teflon) in ketone is fed for mixing with powder. Forming is performed by electrostatic spinning in air at 25°-50°C. After forming, thermal treatment is conducted in vacuum at 70-120°C.
EFFECT: high kinetic parameters of sorbate mass transfer, sorption capacity and modulus of elasticity.
3 cl, 8 ex, 1 tbl, 2 dwg