Methods of increasing quantity of mesopores in microporous coal

FIELD: chemistry.

SUBSTANCE: invention can be used in obtaining adsorbents in substances for smoking and filters for tobacco smoke trapping. Granules of microporous activated coal of vegetable origin are submerged into solution of alkali earth or alkali metal, shaken, filtered with the following drying of filtered coal. Microporous coal, processed with salt, can be activated with vapour, for instance, in argon, for 1-10 h. Obtained coal has volume of micropores at least 0.4 cm3/g and volume of mesopores at least 0.3 cm3/g.

EFFECT: invention provides improved capability of coal to filter tobacco smoke.

18 cl, 4 dwg, 4 tbl, 2 ex

 

The invention relates to a method of preparing mesoporous carbon materials, mainly for use as adsorbents in the media for Smoking and filters to trap the smoke.

It is well known introduction porous carbon materials in funds for area and filters to trap the smoke to reduce the content of some materials in the smoke. Porous carbon materials can be prepared in a variety of ways. Physical properties of porous carbon materials, including shape and size of particles, the size distribution of particles in the sample, the coefficient of abrasion particles, the pore size distribution pore size and surface area, vary widely in accordance with the method of their preparation. These changes significantly affect the characteristics or the suitability of the material to perform the functions of the adsorbent in different environments.

As a rule, the larger the surface area of a porous material, so it is more efficient adsorption. Surface area of porous materials evaluated by measuring changes in the volume of nitrogen adsorbed material with a partial pressure of nitrogen at a constant temperature. Analysis of the results using mathematical models created by Brunauer, Emmett and Teller, gave the measure, known as the surface area by BET.

The pore distribution in which Ariston coal material also affects its adsorption characteristics. In accordance with the terminology used by specialists, the pores in the adsorption material called ”micropores”, if the size of the pores of diameter less than 2 nm (2×10-9m), and ”mesopores”, if the pore size is in the range from 2 to 50 nm. Pores called ”macropores”, if the pore size exceeds 50 nm. Pores having diameters greater than 500 nm, typically small Vliyaniye on the adsorption capacity of porous materials. Therefore, for practical purposes, the pores having diameters in the range from 50 to 500 nm, more typically from 50 to 300 nm, or from 50 to 200 nm, are classified as macropores.

The relative amounts of micropores, mesopores and macropores in a porous material is evaluated using the well known technique of nitrogen adsorption and mercury porosimetry. Mercury porosimetry used to estimate the amount of macro - and mesopores; the adsorption of nitrogen is used to assess the amount of micro - and mesopores using the so-called mathematical model of bjh's. However, as theoretical basis for these different estimates, the amount obtained by these two methods cannot be directly compared with each other.

British patent No. 2395650 compares the influence of several carbon materials with different volumes of micropores and mesopores in the aroma of tobacco smoke, containing flavouring agents, such as menthol. Argue that coal mater what Aly volume of micropores is not more than 0.3 cm 3/g and mesopores of at least 0.25 cm3/g adsorb less menthol than materials with other distributions of pore sizes, and therefore are considered more appropriate for use in filters flavored cigarettes.

International publication No. WO 03/059096 discloses cigarettes, including tobacco wiring and filtering component having a cavity filled with granular coal in the form of balls with a spherical shape with a diameter of from 0.2 to 0.7 mm, the surface area according to BET in the range of 1000-1600 m2/g and the prevailing distribution of pore sizes in the range of micropores and small mesopores.

International publication No. WO 2006/103404 discloses a porous carbon material suitable for introduction into the filters to trap the smoke, having a surface area according to BET of at least 800 m2/g and a pore structure that includes mesopores and micropores. Pore volume (measured by nitrogen adsorption) is at least 0.9 cm3/g, and from 15 to 65% of the pore volume falls in the mesopores. The pore structure of the material provides bulk density, generally less than 0.5 g/cm3. This material is produced by buglarian and activation of organic resins.

Carbon materials are treated to increase their surface area by using a process known as activation. Activated charcoal receive steam Ilyinichna activation. For example, activation can be performed by heating the coal treated with phosphoric acid or zinc chloride, or by heating the coal with steam or carbon dioxide. For activation of coal sometimes need additional stage modification of air, which comprises heating the coal in the air. The activation process removes material from the inner surface of coal particles, which leads to the reduction of mass, the mass loss is proportional to the period of treatment.

Activated carbon plant-based, for example, charcoal from coconut shell, currently more and more used in a growing number of filters for cigarettes. In the case of charcoal from coconut preferred steam activation. The process of steam activation is preferably carried out in two stages. First, the coconut shell is turned into charcoal using process buglarian. Charcoal from coconut shell is then activated by reaction with steam at a temperature of 900-1100°C in a controlled atmosphere. The reaction of steam and charcoal flows on the inner surface area with the formation of a larger number of centers for adsorption. The temperature at which flows activation, is of great importance. Below 900°C, the reaction is too slow, which is uneconomical. At temperatures above 1100°C, the reaction proceeds on the outer surface of drives the century of coal, which leads to his loss. Activated carbon from coconut has a variety of useful properties that make it attractive for the introduction of filters for cigarettes. It includes a large number of micropores. However, it is desirable that the adsorbent used in the means for the area included high levels of mesopores to enhance their ability to adsorb components of smoke.

Therefore, the present invention is the addition of mesopores to microporous coal based plant materials to improve its adsorption properties and characteristics when used in filters for cigarettes. In particular, the object of the present invention is to offer a way to provide mesoporous carbon, which is more effective at removing the components of cigarette smoke than traditional activated carbon from coconut, or equivalent adsorption materials.

Another objective of the present invention is a method of adding the mesopores to a porous carbon materials to provide adsorbents, which are particularly effective in reducing the content of one or more components of tobacco smoke. The method should be simple, cost-effective and to obtain reproducible results. It should be noted that there are few pic the scale introduction of mesopores in the coal plant or mineral origin, such as coal from coconuts.

In accordance with the first aspect of the present invention proposes a method of introduction of mesopores in the microporous coal, including the processing of microporous coal salt, alkaline earth metal, such as calcium nitrate (Ca(NO3)2), or a salt of an alkali metal. Microporous coal is preferably a microporous charcoal from coconut, for example, microporous activated carbon from coconut.

In one embodiment of the invention the method proposed in the invention, includes three stages. The first stage involves the dispersion of a salt of alkaline earth metal or alkali metal microporous coal. The second stage involves adding the mesopores using activation with water vapor (steam). The third stage involves the removal of metal from mesoporous coal acid, such as hydrochloric acid.

In the first stage salt, alkaline earth metal or alkali metal preferably is dispersed in a granular microporous carbon. In one embodiment of the invention the coal is immersed in the salt solution with subsequent shaking of the mixture over a period of time, such as from 1 to 24 hours. After dipping and shaking the coal is removed by filtration and dried.

In h is the local version of the salt of the alkali earth metal include Ca(NO 3)2. More precisely, 2M solution of Ca(NO3)2add to granular microporous coal. The mixture is then shaken for a period of time up to 12 hours. The exact period of time shaking the mixture depends on coal, but, as a rule, it is from 2 to a maximum of 12 hours. The mixture is then filtered and dried without the use of distilled water.

Salt of the alkaline earth or alkali metal used in the proposed invention, is preferably soluble in water and it is added to the granular coal in the form of a solution. Salt Ca(NO3)2soluble in water, having a solubility 121,2 g/100 ml at room temperature that, apparently, is favorable for the proposed in the present invention method. It is also safe, relatively inexpensive and gives excellent results, making it ideal for use in the methods proposed in the present invention. You can use CaCO3although this salt is poorly soluble in water. Generally, the preferred salts of alkaline earth and alkali metal hydroxide, carbonate and nitrate anions. Calcium is a suitable cation.

In the second stage are activated to obtain the mesopores by extracts of granulated coal in water vapour. In an alternative embodiment, the image is etenia to activate the use of carbon dioxide. Preferably as a carrier gas used argon, which is passed through the water to generate steam. Alternative gases-storage media include, for example, nitrogen. The activation is preferably performed at a temperature in the range from about 800 to about 900°C. and more preferably at about 850°C. the Ideal flow of carrier gas depends on the number of activated coal. For example, 500 mg of coal, saturated Ca(NO3)2offer a flow rate of at least 100 ml/min

The gas flow rate and temperature are selected to give a granular coal desired properties of the mesoporous material. The activation period of the coal also affects the properties of the coal and its adsorption capacity. The influence of the activation period of the coal is illustrated in the following example 2. In a preferred variant of the invention, the activation is conducted for a time from 1 to 10 hours, more preferably from 3 to 7 hours. The longer the period of activation, the greater is formed of mesopores. However, it should be noted that the activation within 10 hours or more may result in the loss of granular coal its structural integrity and its transformation into a powder. Obviously this is undesirable, and thus in one embodiment of the present invention stage activation not spend more than within 0 hours and preferably not more than 9 hours.

At the third stage granular activated charcoal process for removing metal, for example, calcium, if used as salts of alkaline earth metal Ca(NO3)2or CaCO3. The treatment is carried out using a solvent, for example, acids, such as HCl. In one embodiment of the invention using 1 M HCl solution for washing granulated charcoal for 2 hours. Then granulated charcoal is filtered and dried.

Preferred properties of the obtained carbon material include, for example (using the definition of IPAC micropores, mesopores or macropores), micropore volume of at least 0.4 cm3/g, the volume of mesopores of at least 0.1 cm3/g and preferably at least 0.3 cm3/g and a particle size in the range from 250 to 1500 μm. Coal particles with these properties show excellent adsorption capacity.

The source material used in the proposed invention the method is preferably microporous coal based on vegetable raw materials. This coal preferably has a granular form. Activated carbon from coconut readily available and widely used. It can be prepared by known processes, activation of natural coal. For example, granulated charcoal from coconut is Rehob with her you can handle at 383 K for 2 hours in vacuum to prepare a suitable starting material for the proposed invention. Alternatively, the microporous activated carbon from coconut can be purchased, for example, Jacobi Carbons.

Methods in accordance with the present invention offer the use of any activated charcoal as source material. Preferred properties of the activated carbon starting material include a total pore volume from 0.1 to 0.8 cm3/g, the volume of mesopores from 0 to 0.4 cm3/g, micropore volume from 0.1 to 0.5 cm3/g, surface area (BET) of from 800 to 1200 m2/g, the width of the pores of 0.5 to 0.8 nm and a particle size of from 30 to 60 mesh.

In accordance with the second aspect of the present invention offers a mesoporous carbon, obtained by the method in accordance with the first aspect of the present invention. Mesoporous coal preferably is of vegetable origin.

Preferably, the methods in accordance with the present invention provide a porous carbon material having a BET surface of at least 800 m2/g, a density of not more than 0.5 g/cm3, porous structure, comprising mesopores and micropores, and a pore volume (measured by nitrogen adsorption) of at least 0.9 cm3/year

Porous carbon materials obtained in accordance with the proposed invention means preferably have a bulk density less than 0.5 g/cm3 . Typical upper range values of the densities of the carbon material in the present invention are 0.45 g/cm3, 0.40 g/cm3and 0.35 g/cm3. Preferably, the bulk density of the coal material proposed in the present invention, is in the range from 0.5 to 0.2 g/cm3.

Coal submissions to the invention are characterized by a greater degree of its porous structure than the density.

Thus, mesoporous carbon-in accordance with the second aspect of the present invention has a surface area according to BET of at least 800 m2/g, the porous structure comprising mesopores and micropores, and a pore volume (measured by nitrogen adsorption) of at least 0.9 cm3/g, from which from 15 to 65% mesopores.

The preferred porous carbon materials proposed in the invention are also characterized by a porous structure in which the pore volume (measured by nitrogen adsorption) at least is 1.0 cm3/g but less than 20% of the pore volume accounted for by pores with a size of 2-10 nm. Usually less than 15% and often less than 10% of the total pore volume accounted for by pores with a size of 2-10 nm.

Density and porous structure of a porous carbon material are closely linked. In General, the coal samples of materials prepared with the COI is whether the way presented in the invention, more than the total amount of micro-, meso - and macropores, the lower the density, because the pores increase the volume of this material without increasing its weight. In addition, as the density decreases, an increasing proportion of macro - and mesopores against the micropores. That is, in General, the lower the density of the coal material offered in the invention, the greater the proportion of mesopores and macropores in the volume of pores in comparison with the share of micropores. However, the correlation between density and pore volume determined by nitrogen adsorption, is not accurate. Therefore, some carbon materials proposed in the invention, having a porous structure as defined in any of the preceding two paragraphs, may have a density greater than 0.5 g/cm3for example, to 0.52, 0.55, which, of 0.60 or 0.65 g/cm3. On the contrary, some carbon materials proposed in the invention can have a density less than 0.5 g/cm3and porous structure, in which less than 15% (for example, 12%, 10% or 5%) of the total volume of mesopores and micropores have to mesopores.

The lack of complete correlation between density and micro - and mesoporous structure arises from the fact that the technique of adsorption of nitrogen, used to estimate the distribution of pore sizes, typically not used for the measurement of pore sizes larger than about 50 nm. Therefore, the total pore volume of the material the material, estimated ways on the basis of nitrogen adsorption, corresponds to the total volume of micropores and mesopores. This technique does not show the volume of macropores material. Thus, when the coal materials proposed in the invention have a low density and a relatively small fraction of mesopores, determined by nitrogen adsorption, low density attributed to the relatively high pore volume in the range of macropores adjacent to the range of mesopores, i.e. in the range from 50 to 500 nm. When the volume of pores in the range of macropores is assessed through a mercury porosimetry, the results obtained when using this technique do not correspond to those obtained when using the technique of adsorption of nitrogen. Therefore, it is difficult to accurately estimate the pore volume of material in the full range of pore sizes from 2 to 500 nm.

Surface area according to BET the preferred porous carbon materials proposed in the invention is at least 800 m2/g and preferably at least 1000 m2/, Typical values of surface area by BET offer in the invention of the carbon materials comprise about 1000, 1100, 1200, 1250 and 1300 m2/, Most preferred porous carbon materials with surface area by BET up to 1250 m2/g, for example, 1000-1250 m2/year

Proposed in the invention, carbon materials preferably have a pore volume (about enemy adsorption of nitrogen) of at least 0.95 g/cm 3and preferably at least 1 g/cm3. Carbon materials with a pore volume of at least 1.1 cm3/g is particularly suitable as adsorbent tobacco smoke. Typical values of pore volume of coal materials amount to 1.15 cm3/g, 1.2 cm3/g, 1.25 cm3/g and 1.3 cm3/, As a rule, the total pore volume is in the range from 1.1 to 2.0 cm3/year Proposed in the invention, carbon materials with pore volume significantly higher than 2.1 cm3/g, for example, 2.2 or 2.3 cm3/g, have a low density and therefore more difficult to be processed in the equipment for manufacture of cigarettes. For this reason, such a carbon material is less favorable for use in cigarettes or filters to trap the smoke.

In the preferred coal materials proposed in the present invention, at least 30%, but preferably not more than 65% of the pore volume (as estimated by nitrogen adsorption) are in the mesopores. Typical minimum values of the volume of mesopores in percent of the total volume of micropores and mesopores coal materials proposed in the invention, comprise 35%, 40% or 45%. Typical maximum values of these quantities equal to 65%, 60% and 55%. Preferably, the volume of mesopores proposed in the invention of the coal material is in the range of 35-55% of the total volume of mesopores and micropores.

In accordance stratim aspect of the present invention offers a means for Smoking, includes material for Smoking, and mesoporous carbon material obtained using the method corresponding to the first aspect of the present invention.

In accordance with the fourth aspect of the present invention proposes a filter to trap the smoke, including mesoporous carbon material obtained using the method corresponding to the first aspect of the present invention.

Example 1

Granular activated carbon from coconut (0.5 ml/g of micropore volume, 0 is the volume of mesopores) was immersed in 100 ml solutions of Ca(NO3)2with a concentration of 2 mol/l at room temperature for one day after the preliminary degassing at 10 MPa and 383 K for 2 hours. Then after drying at 383 K in one day was obtained impregnated coal. Impregnated charcoal activated with steam at 1123 K for 1 hour in a stream of argon at 400 ml/min Activated samples were soaked in 1 mol/l hydrochloric acid solution was mixed for 4 hours and then washed with deionized water to remove residual chemical agent.

Adsorption isotherms of nitrogen obtained coal at 77 K showed hysteresis, indicating the presence of mesopores. The amount added of mesopores amounted to 0.20 ml/g, which is enough to influence the adsorption characteristics of triacetin. Size doba is certain to coal mesopores was approximately 15 nm.

Below are the structural parameters of mesoporous carbon:

surface area by BET (m2/g)1200
micropore volume (ml/g)0,41
the volume of mesopores (ml/g)0,20
the average micropore width (nm)0,72
burning (%)27,5

Table 1 shows the results of comparing the mesoporous carbon according to the invention, prepared as described in example 1, with the control, namely activated (microporous) charcoal from coconut. In the cavity of the filter control cigarettes were introduced 60 mg of coal. For control used 60 mg commercially available microporous carbon from coconut and a hollow cavity. The percentage decrease was attributed to the cigarette with a hollow cavity (i.e. not containing carbon).

Smoking is conducted under the terms of the ISO (international organization for standardization), i.e., the puff volume of 35 cm3a duration of two seconds every minute. All experiments were performed at 22°C and 60% relative humidity, and cigarettes were kondicionirovanie prior to the rhenium at 22°C and 60% relative humidity for three weeks.

Table 1
% DecreaseTest 1Test 2Control coal
Acetaldehyde303527
Acetone424832
Acrolein475435
Butyric aldehyde374730
CROTONALDEHYDE405335
Formaldehyde373626
Methyl ethyl ketone405033
Propionic aldehyde404431
HCN404415
1,3-Butadiene5225
Acrylonitrile5635
Benzene6031
Isoprene6335
Toluene6026

From the data presented in table 1, shows that the mesoporous carbon, obtained by the method presented in this invention is able to provide a greater reduction in the content of components in smoke than the control coal (microporous charcoal from coconut). Therefore, mesoporous coal more effective as an adsorbent when it is turned on in the tool area than the well-known activated carbon.

Example 2

10 g of granulated charcoal from coconut pre-heated at 383 K for 2 hours in vacuum. Then 1 genagricola coal was loaded in 10 ml of 2M solution of Ca(NO 3)2. The mixture was shaken for 12 hours, after which it was filtered and dried.

Then 500 mg samples of activated charcoal in argon and water vapour at 1123 K in a flow of argon with a flow rate of 100 ml/min Samples activated for 1, 3, 5, 7 and 10 hours. Then the activated samples were soaked in 50 ml of 1 M hydrochloric acid for 2 hours. Finally, samples were washed with deionized water, filtered and dried.

Adsorption isotherms of nitrogen obtained coal, shown in Fig.1, showed that the presence of mesopores in the resulting angle is increased over the time during which it was held stage activation. The inventors noted that coal obtained after activation of the pre-heated for 10 hours of coal, easily turned into a powder that has allowed to assume its instability.

In Fig.2 shows the changes in the micropores and mesopores of coal after activation during different periods of time. The volumes are then shown on the graph were determined curve αs. This analysis requires non-porous, chemically similar to the reference material and the use of disordered carbon black (404).

Table 2 presents the structural properties of activated carbon.

Table 2
The activation time0 hours1 hour3 hours5 hours7 hours10 hours
Total pore volume (cm3/g)Sch,400,480,820,961,072,05
The volume of mesopores (cm3/g)*0,020,120,350,510,561,51
The volume of mesopores (cm3/g)**0,030,130,350,520,671,56
Micropore volume (cm3/g)*0,370,360,470,450,510,54
Micropore volume (cm3/g)**0,370,340,47 0,440,400,49
S. S. A. (m2/g) BET9759551260122413921436
S. S. A.(m2/g)αs9889381206116612471328
The width of the pores (nm)0,770,820,880,881,260,96.
*define the chart data register (DR)
**defined by the diagram αs

S. S. A. specific surface area

The data in table 2 show that the more time activate impregnated coal, the greater the volume of mesopores. The method presented in the invention also leads to an increase in the volume of micropores. The source material has almost no mesopores.

In tables 3 and 4 show the results of the evaluation of mesoporous carbon from coconut obtained in PR is as 2, with 60 mg of mesoporous carbon, is included in the cavity of the cigarette. These results were achieved using the same methodology as in example 1.

The data shown in table 4, also shown in Fig.3 and 4.

The data in tables 3 and 4 show the adsorption of different chemicals control coal EcoSorb® CX and coal, prepared in accordance with the method shown in example 2, and activated for 1, 3, 5 and 7 hours. EcoSorb® CX is a premium grade activated carbon based on coconut shell production Jacobi Carbons used for removal of organic compounds from a gaseous phase.

Table 3
Measurement (μg/cigarette)Empty cavityControl coal1 hour3 hours5 hours7 hours
Acetone27013795,470,1to 49.943,4
Acrolein68,432,25 of 21.91711,710,6
Acrylonitrile11,44,02,21,81,91,3*
Benzene35,715,56,84,0*4,2*4,0*
1,3-Butadieneof 40.322,712,89,4the 9.77,4
Butyric aldehyde36,118,712,28,575,945,42
CROTONALDEHYDE20,47,31a 3.872,171,281,21
Formaldehyde61,0533,7 27,625,620,819,1
Isopreneof 225.680,4of 21.220,8*21,6*20,9*
Methyl ethyl ketone6830,71811,56,985,39
Propionic aldehydeof 45.724,151813,910,69,38
Toluene37,123,318,2*18,1*18,8*18,2*
*where the outputs were less than the value used in the Limit of Quantification, and therefore quantitative indicators of some substances that are defined during the analysis, go to the plateau.

Table 4
Reduction (%)Control coal1 hour3 hours5 hours7 hours
Acetaldehyde3037434753
Acetone4965748284
Acrolein5368758385
Acrylonitrile6581848488*
Benzene578189*88*89*
1,3-Butadiene4468777682
Reduction (%)Control coal1 hour3 hours5 hours7 hours
Butyric aldehyde4866768485
CROTONALDEHYDE6481899494
Formaldehyde4555586669
Isoprene649191*90*91*
Methyl ethyl ketone5574839092
Propionic aldehyde47 61707779
Toluene3751*51*49*51*
* Reduction based on the values of Limit of Quantification

From the data presented in tables 3 and 4, it follows that the mesoporous carbon, obtained by the method presented in the invention is able to provide a greater reduction in components of the smoke than the control coal (microporous charcoal from coconut). Therefore, mesoporous coal more effective as an adsorbent for inclusion in the tool area than the well-known activated carbon.

The data presented in tables 1, 3 and 4 show that mesoporous carbon, prepared in accordance with the invention method, suitable for use as adsorbent in the media for Smoking and filters to trap the smoke and is more effective at removing some components of smoke than the traditionally used microporous charcoal from coconut.

1. The method of introduction of mesopores in the microporous coal, including the processing of microporous granules of coal salt, alkaline earth or alkaline IU is Alla, in which microporous charcoal is activated carbon of vegetable origin.

2. The method according to p. 1, in which the microporous charcoal is activated charcoal from coconut.

3. The method according to p. 1, in which the salt of the alkaline earth metal is calcium nitrate.

4. The method according to p. 1, in which the salt of the alkaline earth or alkali metal dispersed on microporous coal dipping coal in the salt solution.

5. The method according to p. 4, in which shake the mixture of coal and salt solution.

6. The method according to p. 4, in which a mixture of coal and salt solution is then filtered and dried coal.

7. The method according to p. 1, in which the method includes the activation of microporous coal, processed salt.

8. The method according to p. 7, in which activation is a steam activation or activation with water vapor.

9. The method according to p. 8, in which the activation is carried out in argon.

10. The method according to p. 8 or 9, in which the activation is carried out in the period of time from 1 to 10 hours.

11. The method according to any of the p. 7, in which the activated carbon is treated to remove metal.

12. The method according to p. 11, in which the coal is washed with acid to remove metal.

13. Mesoporous carbon, obtained by the method according to any of paragraphs.1-12.

14. Tool for Smoking, including material for area and mesoporous carbon, obtained by the method according to any of paragraphs.1-12.

15. Filter is to trap the smoke, containing mesoporous carbon, obtained by the method according to any of paragraphs.1-12.

16. The method according to p. 1, in which the mesoporous carbon has a micropore volume of at least 0.4 cm3/g and the volume of mesopores of at least 0.3 cm3/year

17. Mesoporous carbon, p. 13, in which the mesoporous carbon has a micropore volume of at least 0.4 cm3/g and the volume of mesopores of at least 0.3 cm3/year

18. A filter for trapping smoke under item 15, in which the mesoporous carbon has a micropore volume of at least 0.4 cm3/g and the volume of mesopores of at least 0.3 cm3/,



 

Same patents:

FIELD: chemistry.

SUBSTANCE: invention relates to the synthesis of carbon materials, used for hydrogen separation. A carbon molecular sieve is obtained from anthracite or hard coal. Raw material is subjected to oxidation with air oxygen. Oxidation is carried out with heating the raw material from 100 to 450°C in a descending air flow, which is supplied at a rate of 0.5-15 m/sec.

EFFECT: invention provides obtaining a selective adsorbent for the separation of hydrogen with reduction of costs.

3 cl, 2 tbl

FIELD: chemistry.

SUBSTANCE: thermal stability of thermally activated cellulose-based coal is increased by influencing it with halogen and/or a halogen-containing substance, containing bromine, chlorine, fluoride, iodine, ammonium bromide, other nitrogen-containing salts of halogens or calcium bromide. The said thermally activated coal contains approximately from 5 to 20 wt % of halogen relative to the total weight of the thermally activated coal, subjected to the impact of halogen and/or the halogen-containing substance. Such a processed cellulose-based coal is suitable for application in processes of reducing the content of harmful substances in flue gases, in particular in flue gases, the temperature of which is in the range approximately from 100°C to 420°C.

EFFECT: increased stability.

5 cl, 5 dwg, 1 tbl

FIELD: chemistry.

SUBSTANCE: claimed is production method, which includes raw material crushing, drying, introduction of chemical activating agent, activation, washing and drying of final product. As raw material used is wood or technical lignin or peat. Potassium or sodium hydroxide is used as chemical activating agent. Drying is carried out at temperature 280-600°C. Activation is realized in atmosphere of steam gases with increase of temperature to 550-800°C. washing is carried out in three stages at temperature 70-90°C. At the first stage washing is performed with water, then with hydrochloric acid and at the last stage with water.

EFFECT: increase of adsorption ability of activated coal by iodine, and by methylene blue.

3 ex

FIELD: chemistry.

SUBSTANCE: process of obtaining granulated porous carbon material consists of two stages. At the first stage soot is mixed with petroleum pitch and solvent, after which obtained mixture is granulated, granules are stabilised in gas medium at temperature not higher than 250°C, subjected to carbonisation at 600-1200°C and cooled. Product, obtained at first stage, possesses narrow distribution of pores. At the second stage product, obtained at first stage, is crushed to particle size smaller than 1 mm, mixed with petroleum pitch and solvent, mixture is granulated. Obtained granules are subjected to stabilisation and carbonisation under the same conditions as at the first stage.

EFFECT: providing possibility of obtaining porous carbon material, characterized by bimodal distribution of pores and low soot content.

1 dwg, 1 tbl, 5 ex

FIELD: chemistry.

SUBSTANCE: method of obtaining granular activated carbon includes milling a coal raw material, mixing it with a resin binding agent and doping additive, granulation of the composition, cooling the granules, carbonisation and steam-gas activation. As the doping additive into the carbon-resin composition introduced is tristrimethylsiloxyphenylsilane.

EFFECT: invention makes it possible to obtain granulated activated carbon with the high absorption ability, recommended for the extraction from sewage and return waters of flotation factories of residues of flotation agents, such as potassium xanthogenate.

3 ex

FIELD: chemistry.

SUBSTANCE: method of obtaining a carbon cation exchanger includes processing of activated carbon with a mixture of ammonia and hydrazine, taken in a ratio of 1:(2-2.5). The process is realised at a temperature of 350-450°C.

EFFECT: obtaining the carbon cation exchanger with improved properties.

1 tbl, 3 ex

FIELD: process engineering.

SUBSTANCE: invention relates to production of charcoal sorbent to be used for production of active coals and carbon sorbents used in agriculture. Carbon-bearing stock (saw dust with initial moisture content of 10-30%) is carbonized at 450-600°C.Carbonised matter is activated by steam-gas mix at 650-800°C and cooled in thin bed to 20-30° at temperature decreased rate of 10°C/min. Obtained charcoal sorbent is subjected to additional activation for air oxygen oxidation.

EFFECT: invention allows production of charcoal sorbent that features iodine absorption capacity of 30-41% that complies with GOST requirements to DAK-grade ground active coal; continuous carbonisation-activation in one apparatus, porous structure of sorbents, required adsorption properties.

2 ex

FIELD: chemistry.

SUBSTANCE: modification process includes washing with distilled water, heating to 200°C in an air atmosphere for 2 hours and treating with hydrochloric acid solution with concentration of 0.1 mol/dm3.

EFFECT: high dimethylamine sorption capacity of the carbon and increasing dimethylamine extraction by 35% on average.

3 tbl, 3 ex

FIELD: nanotechnology.

SUBSTANCE: invention is directed at obtaining functionalised carbon nanotubes having good compatibility with polymeric matrices. The carbon nanotubes are subjected to processing in hydrogen peroxide vapour at a temperature of from 80°C to 160°C for 1-100 hours. The processing may be carried out in a unit with fluidised bed of the carbon nanomaterial.

EFFECT: method is characterised by high efficiency, lack of toxic oxidation products, low consumption of reagents, can be easily scaled.

2 cl, 2 dwg, 4 tbl, 4 ex

FIELD: chemistry.

SUBSTANCE: disclosed is a method of producing activated charcoal, which comprises crushing rapeseed straw into 1-10 cm pieces, carbonising the straw in an inert atmosphere at temperature of 450-500°C while raising temperature at a rate of 1-20°C/min and holding at final temperature for 30-60 minutes. Activation is then carried out with steam at temperature of 820-850°C, which is fed at a rate of 3-5 kg per kg of the carbonised product. Resorcinol capacity is 0.0030-0.0050 mg/g and hydroquinone capacity is 0.0040-0.0050 mg/g.

EFFECT: obtaining powdered activated charcoal with high adsorption capacity for polyphenols.

3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to molecularly imprinted polymers selective for at least one tobacco specific nitrosamine (TSNA), the polymer being obtained using materials comprising a TSNA or a structural analogue thereof, a neutral functional group-containing monomer selected from a group comprising 2-hydroxyethylmethacrylate (HEMA), acrylamide, methacrylamide, glycerol monoacrylate and glycerol monomethacrylate, and a hydrophobic cross-linking agent. The invention also describes a method of producing a molecularly imprinted polymer, a smoking article, a tobacco smoke filter and a kit for detecting, quantitative determination and separation of nitrosamines contained in a sample, which include a molecularly imprinted polymer, a method of reducing content of at least one TSNA in a tobacco product and a method of producing tobacco material.

EFFECT: obtaining molecularly imprinted polymers which are selective for nitroso-containing compounds.

25 cl, 18 dwg, 8 ex

FIELD: tobacco industry.

SUBSTANCE: filtering tip contains a filtering zone including a filtering material and aromatic vegetal particles improving smoke characteristics, dispersed inside the filtering material and chosen from among mint, peppermint, basil, oregano, rosemary, sage, thyme, lavender, hepatica and bergamot. The smoking product contains the filtering tip consisting of one filtering zone segment with ingrained aromatic vegetal particles improving smoke characteristics and one segment of common filtering material, the tip constantly connected to the tobacco core. According to the filtering tip production method, one performs uniform sprinkling of a corresponding quantity of aromatic vegetal particles improving smoke characteristics onto a strap moving edgewise on a mechanical support before the strap shaping in the filtering tip.

EFFECT: production of a filtering tip improving characteristics of tobacco smoke during smoking products usage.

35 cl

FIELD: technological processes.

SUBSTANCE: invention relates to a composite material with higher force of adhesion made of at least one polymer and at least one compound selected from silicon dioxide and activated coal, at the same time the specified composite material has the following: average particle size of at least 100 mcm, porous volume (Vd1), formed by pores with diameter from 3.6 to 1000 nm, of at least 0.2 cm3/g, force of adhesion such that content of particles in it with size of less than 100 mcm, produced under air pressure of 2 bar, makes less than 1.5 vol. %, is preferably equal to 0.0%. Also a method to produce a composite material is described, as well as its usage as a liquid medium carrier, a catalyst carrier, an additive or for filtration of liquid or gas, in particular, in cigarette filters.

EFFECT: invention provides for high properties of hazardous components reduction in filtered medium.

33 cl, 2 tbl, 5 ex

FIELD: tobacco industry.

SUBSTANCE: invention relates to a cigarette filter containing a natural vegetal material and to a cigarette containing such filter. According to the invention the filter is filled with a natural vegetal material milled into specified size particles; alternatively, the vegetal material is distributed on the filter made of a fibre material. The vegetal material is represented by recovered tobacco leaves, in milled form after drying and in the form of granules.

EFFECT: invention ensures uniform delivery of the natural aroma typical of the plant to the smoker and significantly reduces the cigarette smell and offensive breath by way of neutralisation of the smell typical of a cigarette.

12 cl, 8 dwg, 3 tbl, 4 ex

FIELD: tobacco industry.

SUBSTANCE: cigarette filter and its versions are designed to soften taste when smoking. The cigarette filter comprises a filtering plug, having a cylindrical body of a wrap, and a filtering material arranged in a cylindrical body. Wrapping of the filtering plug is formed from highly strong and highly permeable paper, longitudinal rigidity of which makes 30 or more, when measured in accordance with the standard JIS P8143, and air permeability makes 1000 units of Coresta or more. Versions are related to a cigarette filter, comprising multiple filtering plugs, which uses highly strong and highly permeable paper as wrapping for a filtering plug to wrap a filtering material and/or as a shaping paper that connects multiple filtering plugs. The invention also relates to a cigarette with a filter.

EFFECT: improved quality of cigarettes by increasing ventilation ratio, providing of possibility of fresh air supply for a higher dissolution of smoke inhaled by a smoker and reduction of a cigarette prime cost.

17 cl, 9 dwg, 4 ex

FIELD: food industry.

SUBSTANCE: smoking product has an outer surface and multiple fragile microcapsules arranged on the outer surface. The microcapsules are capable to be manually destroyed by the consumer for releasing the flavouring agent which is incapsulated in them.

EFFECT: invention ensures possibility to impart an intensified olfactory sensation to the consumer (without change of taste-and-flavouring and other properties of the main smoke flow produced during the smoking product combustion).

8 cl, 4 dwg

FIELD: food industry.

SUBSTANCE: cigarette filter contains filtering core made from bunch of fibers through which cigarette smoke goes, fine powder with high surface area coefficient that is mixed and distributed in bunch of fibers, and double-stranded DNA molecula attached to the outer surface of fine powder with high surface area coefficient. Herewith harmful substances such as benzo[a]pyrene contained in cigarette smoke are removed by intercalation (implementation) in double-stranded DNA molecula.

EFFECT: creation of cigarette filter that does not deteriorate distinctive cigarette aroma and filter breathability when smoking and effectively removes harmful substances.

6 cl, 5 dwg, 2 tbl, 4 ex

FIELD: food industry.

SUBSTANCE: filtering material for tobacco smoke is developed for smoking products. The material is produced by dissolving chitosan in acetic acid solution with the acid content from approximately 0.1% to approximately 10%. The obtained solution containing chitosan in the amount from approximately 0.1% to approximately 20% is filtered and dripped into precipitating solution containing sodium hydroxide from approximately 1 mole to approximately 5 moles, thus producing gel granules. Then the gel granules are washed and suspended in a cross-linking solution during from approximately 1 hour to approximately 24 hours to produce cross-linked granules. The above cross-linking solution contains from approximately 0.1% to approximately 50% of the cross-linking compound which is glutaraldehyde or glyoxal. The cross-linked granules are washed and dried producing porous granules of cross-linked chitosan polymer. Another version implies that the obtained chitosan solution as stated above containing chitosan in the amount from approximately 0.1% to approximately 20% is cooled down below the standard room temperature in order to be precipitated. The above precipitating solution contains sodium hydroxide, water and methanol. Chitosan solution is dripped to the above precipitating solution producing gel granules. The precipitating solution contains gel granules. The said gel granules are washed and suspended in the cross-linking solution as stated above.

EFFECT: ensuring selective removal of hydrocyanic acid, aldehydes, heavy metals and sulphides from tobacco smoke gaseous phase.

6 cl, 7 ex

FIELD: tobacco goods.

SUBSTANCE: filter contains activated charcoal, in which volume of pores of maximum of 0.3 cm3/g (N2) is provided with pores of diameter of less than 2 nm (micropores), and (a) volume of pores of at least 0.25 cm3/g (N2) is provided with pores of diameter from 2 to 50 nm (mesopores) and/or (b) volume of pores of at least 0.12 cm3/g (Hg) is provided with pores of diameter from 7 to 50 nm (larger mesopores).

EFFECT: filter provides satisfactory filtration of steam phase and presentation of aroma in the presence of volatile.

21 cl, 2 tbl

FIELD: tobacco industry.

SUBSTANCE: cigarette sorbent is composed of, wt %: carbon 28.0-36.0, potassium 1.2-2.6, aluminum 2.6-3.3, manganese 0.05-4.7, titanium 0.22-0.4, calcium 0.13-0.17, silicon 18.0-24.0, sodium 0.2-0.51, and oxygen 30.0-38.6. Preparation of sorbent involves preliminarily crushing schungite to predetermined size and separating fraction having required granulometric composition, which fraction is further modified by chemical activation consisting in boiling the fraction in 15-35% sodium hydroxide solution for 30 to 180 min followed by filtration of modified schungite, washing with distilled water to pH 7-10, drying at 104-106°C, and recrushing.

EFFECT: increased catalytic activity.

5 cl, 1 dwg, 2 tbl, 5 ex

FIELD: tobacco industry.

SUBSTANCE: invention relates to smoke-generating compositions for electronic devices imitating tobacco smoking, to a method for such smoke-generating composition production as well as to the electronic device cartridge and the electronic device proper. The composition contains water and/or ethanol, flavouring agents and/or nicotine, glycerine and/or polypropylene glycol with molecular weight from 425 to 1025. Polypropylene glycol is mixed with the other components of the smoke-generating composition. The cartridge contains the smoke-generating composition. The electronic device (such as an electronic cigarette) includes a cartridge containing the smoke-generating composition.

EFFECT: invention enables reduction of the probability of the smoke-generating compound leakage from the cartridge or electronic device (electronic cigarette) prevention undesired penetration of the smoke-generating compound into the oral cavity.

4 cl, 2 tbl, 2 dwg

Up!