Method of splitting fractions of crude quinoline bases from coke-chemical production into components

FIELD: chemistry.

SUBSTANCE: invention relates to chemistry and can be used in coke-chemical production when processing coke gas. The method involves using fractions of heavy crude pyridine bases which form during coal carbonisation as raw material, from which pyridine bases are extracted first and the obtained faction of crude quinoline bases is split into components. The fractions of crude quinoline bases are split into components through supercritical preparative chromatography, where the separated mixture is brought into contact with gas in supercritical state, which is simultaneously the mobile phase and adsorbent.

EFFECT: simpler, faster and more reliable separation.

1 dwg

 

The invention relates to chemistry and can be used in the manufacture of coke in the processing of coke oven gas, namely, to obtain pure reason quinoline, isoquinoline, khinolinovykh and other residues from the production of obtaining pyridine bases allocated from formed during the coking of heavy crude pyridine bases.

Crude pyridine bases formed during coking coal is a mixture of heterocyclic compounds of the aromatic series with the General formula CnH2n-5N. Crude pyridine bases include pyridine C5H5N and its homologues, as well as other nitrogen-containing compounds of the main character and a more complex structure, such as quinoline, isoquinoline, heraldin and others (Rehabbed, Ehiagwina, Abilov "Technology of coke production", M.: metallurgy, 1982, s).

The main difficulty in the separation of the components of crude khinolinovykh grounds, which remains the production of obtaining pure pyridine bases, is in the proximity of their physical properties, in particular the boiling point: the difference is measured in degrees. As a consequence, the division into pure components by direct distillation is not feasible.

In practice on an industrial scale for the separation of the crude fraction x is malinovich grounds on a narrower fraction quinoline, of isoquinoline, rinaldina use selective methods, based on differences in their chemical and physical properties, for example different solubilities and melting phosphate salts of these components or adducts with phenyl, cresol and csinalom (Dstatic "Pyridine and quinoline bases", M.: metallurgy, 1973, s). However, these methods do not allow you to get a lump sum of the individual product, i.e. the product is a pure, without impurities. To obtain the product in pure form requires additional purification from impurities, because of the way it was received.

The known method of separation of quinoline and isoquinoline, also used in industry, based on differences in the temperatures of crystallization. Use what isoquinoline and quinoline to form a crystalline water, giving a mixed eutectic (Dstatic "Pyridine and quinoline bases", M.: metallurgy, 1973, s-251). In the example of performing the method, a mixture containing 80% of quinoline and 20% of isoquinoline, with the addition of water 15%, raids!! to minus 30 to minus 35C and the crystals of the hydrate, which is then dehydrated, allocate more than half of the total amount of pure quinoline. The remaining commections a mixture of quinoline and isoquinoline, which contains about 40% of isoquinoline, dehydrated and cooled to minus 20C. the result is e get pure crystals of isoquinoline. Then the isoquinoline is separated in the centrifuge from the mother liquor, which contains 80% quinoline. The mother liquor is returned for re-freezing.

The method allows to obtain in pure form the main components of the fractions. The disadvantage of this method is the inability to extract the main components of the factions, and the impossibility of separation into pure components without phase separation into narrow fractions. Furthermore, the method allows to obtain only two components quinoline bases, namely: quinoline and isoquinoline, which limits its functionality.

There are other ways of selection of isoquinoline and quinoline of the quinoline-isoquinoline" fractions used in industry, using deposition and subsequent fractional crystallization of sulfates of alcohol, the deposition of sulfates in glacial acetic acid and the hydrochloride in anhydrous environment; separation of N-oxides of quinoline and isoquinoline, products join with phenol and 2-naftalina, the deposition of products of accession with calcium chloride, anatropous rectification glycol, complexation with Nickel thiocyanate and a number of other methods (Whichmakes "Pyridine bases, Kiev, 1965, s).

There is a method of separating pure isoquinoline of the quinoline-isoquinoline" faction, in which ispolzuyeca complexation with cobalt chloride. Because isoquinoline forms a more stable, compared with quinoline, complex compounds with a number of salts of heavy metals, including cobalt chloride, Nickel or iron, the method allows to produce a rough separation of quinoline and isoquinoline (Whichmakes "Pyridine bases", Kiev, 1965, s).

The above methods of separation of fractions of crude quinoline bases coke production components allow you to get only two components quinoline bases: quinoline and isoquinoline. In addition, the methods require additional purification of the obtained substances from ancillary reagents. In this case, as in the previous cases, the known methods do not allow to obtain a pure substance during one cycle of separation directly from fractions of crude quinoline bases, bypassing the phase of obtaining narrow fractions of these substances.

Closest to the present invention is used in industry, a way to divide fractions crude quinoline bases coke production components, in accordance with which the heavy base after separating them from the fractions of the resin in the form of sulphate of pyridine and quinoline dehydrate, then separated from the pyridine base. The product remaining after the separation of the fractions pyridine bases - fractions crude quinoline is o reason - subjected to separation by distillation on a narrow faction: quinoline - 90% quinoline, isoquinoline - 90% isohaline, hinolinovy - 90% of rinaldina, Lebedinoye - 90% lepidine. However quinoline fraction boils in the temperature range from 235 to 240C, isoquinoline - from 240 to 244C, rinaldina from 244 to 246C, Lebedinovka from 259 to 263C (Dstatic "Pyridine and quinoline bases", M.: metallurgy, 1973, s).

The disadvantage of this method lies in the difficulty and complexity of implementation, due to the proximity of the temperature of narrow boiling fractions. This leads to the inexpediency of its use on an industrial scale. In addition, the known method does not allow you to get every product is fully allocated, as the boiling temperature close and allocated to the moment the product is placed next to the product close to it by boiling. Moreover, it reduces the purity of the secreted product. In this known method allows you to split a fraction of crude quinoline bases also on the narrow fraction, i.e. the method does not allow you to get during one cycle of the separation of an individual product in a pure form, without impurities directly from fractions of crude quinoline bases, bypassing the phase of obtaining narrow fractions of these substances. In addition, due to the proximity of the boiling points of sostavlyayushchii raw khinolinovykh grounds the method allows to separate components with markedly different boiling point, i.e. the method does not allow a complete separation of the components of the fractions of crude quinoline bases of coke production.

Thus, identified as a result of a patent search methods of separation of fractions of crude quinoline bases coke production components in the implementation does not ensure the achievement of the technical result consists in the possibility to obtain in pure form all of the components contained in the feedstock, in the course of one cycle of division, without additives and with minimal losses, bypassing the phase of obtaining narrow fractions, and complex in execution.

The proposed method for the separation of fractions of crude quinoline bases coke production components solves the problem of creating an appropriate way, which ensures the achievement of the technical result consists in the possibility of obtaining pure, without impurities of all components contained in the feedstock, in the course of one cycle of division, with minimal losses, bypassing the phase of obtaining narrow fractions, and simplifying the technological separation schemes, the expansion of the means for the industrial separation of pure components fra is the crude quinoline bases of coke production.

The essence of the invention is that the inventive method of separation of fractions of crude quinoline bases coke production components, in accordance with which is used as raw material fractions of crude pyridine bases contained in the formed during coking coal fractions of heavy crude pyridine bases from which pre-allocated pyridine bases, what's new is that the division of fractions crude quinoline bases on the components perform by preparative supercritical chromatography.

The technical result is achieved in the following way. Use as raw materials produced during coking coal fractions of heavy crude pyridine bases from which pre-allocated pyridine bases, allows to exclude from the way the operation selection pyridine bases that simplifies the way. In addition, this significant feature dissociates fractions crude quinoline bases of coke production from quinoline bases, obtained by artificial means. This is essential as solving the stated method, the goal of achieving a technical result consists in the possibility to obtain in pure form all of the components contained in the feedstock during one the of Tcl separation, without additives and with minimal losses, bypassing the phase of obtaining narrow fractions, simplifying the technological separation schemes, the expansion of the means for the industrial separation of pure components fractions crude quinoline bases of coke production is relevant in the manufacture of coke.

As was shown above, in practice for the industrial division of fractions of crude quinoline bases coke production on a smaller faction, quinoline, isoquinoline, rinaldina, and to obtain pure substances, use of selective methods, based on differences in their chemical and physical properties, such as differences in boiling points, the differences in the temperatures of crystallization, the differences in the complexation reactions, differences in solubilities and melting phosphate salts of these components or adducts with phenyl, cresol and csinalom etc. However, the patent search division of fractions of crude quinoline bases coke production has not revealed the fact that the use for them industrial separation properties of some substances dissolve in a gaseous substances in supercritical state. Such substances include components and fractions crude quinoline bases coke production is odstv. Authors for the industrial division of fractions of crude quinoline bases coke production components for the first time used the property as a constituent fractions of crude quinoline bases coke production to be dissolved in the gaseous substances in supercritical state. This, in turn, has enabled the application of supercritical preparative chromatography for the industrial division of fractions of crude quinoline bases coke production components. Has not previously been used for the industrial division of fractions of crude quinoline bases coke production on the components of the property constituting fractions crude quinoline bases coke production to be dissolved in the gaseous substances in supercritical and supercritical preparative chromatography and first used to solve this problem the authors.

In the result of a patent search revealed mention of the use of supercritical fluid chromatography for analytical purposes for the study of products of processing of coal (Supercritical fluid chromatography" edited Rsmith, M.: Mir, 1991, p.64, table 4). Supercritical chromatography is called "fluid" (Avishai, Aijin "Adsorption g the gas and liquid chromatography", M.: Chemistry, 1979, p.137). However, preparative chromatography is the allocation of full individual compounds of the mixture. Use it when you need to select from a mixture of many individual compounds, and widespread methods: distillation, extraction, crystallization, etc. do not provide the clarity and completeness of the receiving components (Cigacice, Saurav "preparative gas chromatography): Chemistry, 1972, p.5). The use of supercritical preparative chromatography for separation in full of individual compounds from fractions of crude quinoline bases of coke production is not known.

The possibility of using for the industrial division of fractions of crude quinoline bases coke production components by preparative supercritical chromatography expands the Arsenal of means to obtain pure components of the fractions of crude quinoline bases of coke production.

As mentioned above, preparative gas chromatography provides the allocation of individual compounds from the feedstock. The proposed technical solution for the separation of the feedstock, i.e. for the selection of individual compounds from the feedstock, using gas adsorption temple is tography, in which the separation is based on the difference in adsorbiruyuschee of mixture components on the adsorbent (Cagoldasd, Mshvildisrit "Introduction to gas chromatography): Chemistry, 1990, p.29). As a result of application of preparative chromatography provides the ability to sequentially obtain pure substances from the feedstock as they adsorption of mobile phase without changing the hardware design. This allows the division directly fractions crude quinoline bases, not separating them previously on a narrow faction, as in the prototype, quinoline, isoquinoline, hinolinovy, Lebedinoye. In addition, this allows the separation on the same equipment, without the use of recycling, which simplifies the technological scheme of separation.

Supercritical chromatography (fluid) is an intermediate option between the gas and liquid chromatography. In this case, the mobile phase and the adsorbent is the gas which is in a supercritical state (Cagoldasd, Mshvildisrit "Introduction to gas chromatography): Chemistry, 1990, p.30). Separation of fractions of crude quinoline bases by preparative supercritical chromatography in which the mobile phase to form compounds under normal conditions in a gaseous state, put the m into a supercritical state, gives the possibility of obtaining pure products dividing fractions without additives solvent as the mobile phase at the exit of the mixture from the column of the chromatograph goes to gas and evaporates.

Historically, the industrial division of fractions crude quinoline bases coke production components by preparative supercritical chromatography was not running and was first proposed by the authors of the claimed invention. While the achievement of the claimed technical result is the possibility of obtaining all of the components contained in the raw material during one cycle of separation, pure, without impurities, and with minimal losses, bypassing the phase of obtaining narrow fractions, simplifying the technological separation schemes, the expansion of the means for the industrial separation of pure components fractions crude quinoline bases of coke production in the claimed technical solution is provided due to the high selectivity of separation resulting from the use of the specificity of interactions between components of the feedstock with the adsorbent, which allows to separate compounds with similar properties; high separation efficiency due to the developed surface mass transfer; the possibility of obtaining several components of the feedstock is not orestano of complex multicomponent mixtures during one cycle of division; the selection of the target product with minimal loss and no delay mixture in the separation column; the flexibility of the method and the simplicity of instrumentation, as well as the possibility of complete automation of the whole process.

Thus, from the above it follows that the claimed method of separation of fractions of crude quinoline bases coke production components in the implementation ensures the achievement of the technical result consists in the possibility of obtaining all of the components contained in the feedstock, in the course of one cycle of division, without additives and with minimal losses, bypassing the phase of obtaining narrow fractions, simplifying the technological separation schemes, the expansion of the means for the industrial separation of pure components fractions crude quinoline bases of coke production.

The claimed method of separation of fractions of crude quinoline bases coke production components perform the following way. In is used as raw material produced during coking coal fractions of heavy crude pyridine bases from which pre-allocated pyridine bases. Industrial division of fractions crude quinoline bases on the components perform by supercritical drug who ate chromatography.

For carrying out the proposed method can be used, for example, supercritical chromatograph, with a classic scheme described in the Internet address www.NOVASEP.com. Chromatograph contains a chromatographic column, a device for producing supercritical mobile phase from gaseous compounds, in particular of CO2capacity for partial mixture, input devices in the chromatographic column of the substance in the mobile phase and the partial mixture, the detector output component of the mixture that is installed at the outlet of the column, the cyclones for the collection of selected components of the original mixture. For detection of the output component of the mixture used spectrophotometric detector with diode array.

Through the chromatographic column is passed are listed in the supercritical state CO2and through the input device sample inject a partial mixture, in this case the fraction of crude quinoline bases of coke production, particles which are dissolved in the substance of the mobile phase. In the result of differences in adsorption properties of the substance in the mobile phase and shared components of the mixture at the outlet of the chromatographic column consistently appear its components. The detector determines and fixes the appearance of each component and gives the signal to open the corresponding is iClone to collect the selected substances. Carbon dioxide before it enters the cyclone selected substances at the outlet of the column is evaporated from a mixture of selected substances and carbon dioxide and is collected in a special gazosbornik, and then goes to recycling. As a result, during one cycle of division consistently get all the components of the fractions of crude quinoline bases of coke production in the form of a pure product without impurities and practically without losses.

Industrial applicability of the claimed method confirms the chromatogram (see drawing) separated into its constituent fractions of crude quinoline bases of coke production. Separation of components was performed using the inventive method. As raw materials used waste products the shop getting pribinova grounds LLC NTMK, namely, formed during coking coal fractions of heavy crude pyridine bases from which pre-allocated pyridine base.

The approach to each division individual and specific temperature and pressure in the column pick up each time so that at the output to obtain the maximum yield of a specific or certain substances. When this is taken into account that the valid interval of the temperature in the column is determined, firstly, the critical temperature of the mobile phase, i.e. tempera is Urai, which still retains the characteristics of the translated in the supercritical state gaseous compounds. For example, when using propane as the mobile phase temperature in the column is +110C, carbon dioxide +36C. secondly, the temperature in the column is determined by the properties of the partial substances, namely: the temperature in the column, which is the temperature of separation, must be below the temperature of decomposition of the partial substances, and separating compounds thermally resistant substances, the temperature in the column must ensure their maximum output. At low temperatures the partial decomposition of substances vary the pressure in the column and the selection of the composition of the mobile phase, selecting a mobile phase with a stronger adsorption properties. The pressure in the column is in direct proportion to the length of the column, namely directly proportional to the length of the column. By varying the pressure and temperature in the column can be adjusted retention time of the selected component in the column, and also to focus on the selection of the required components.

In the pilot separation fractions crude quinoline bases was obtained pure products on average up to 4 kg per day.

Below are examples of the separation of mixtures of quinoline bases (bottom residue on the Le rectification isoquinoline faction). As the mobile phase can be used any gas connection, translated in critical condition, not prone to polymerization and non-corrosive and chemically active with respect to the materials used in the equipment, and initial raw material.

Example 1. The separation conditions:

column of 4.6250 mm, 60 A Chromasil;

fluid CO2food + EtOH OFS(95%+5%);

the flow rate of 4 ml/min;

pressure 150 bar; temperature +35C.

The chromatogram showed that under given conditions of separation at the exit of the chromatographic column recorded six pure quinoline bases: quinoline, indole, giraldin, quinoline-7-methyl -, quinoline-4-methyl-and quinoline-2,4-dimethyl, respectively by 3.75 minutes, 4,07 min, 4,33 min, 4,69 min, for a total of 5.21 min, 5,61 minutes

From the chromatogram shows that the obtained separation allows to obtain accurate results, and this confirms that when carrying out the claimed method provides the achievement of the technical result consists in the possibility of obtaining all of the components contained in the raw material during one cycle of division, without additives and with minimal losses, bypassing the phase of obtaining narrow fractions, simplifying the technological separation schemes, the expansion of the means for the industrial separation of pure components FR the functions crude quinoline bases of coke production.

Example selection by preparative supercritical chromatography quinoline and isoquinoline fraction of crude quinoline bases of coke production. The separation was performed on a chromatographic column Cromasil 60, dimensions: a 4.6250 mm; mobile phase CO2to 3.8 ml/min + C2H5HE is 0.2 ml/min; temperature of 36C; pressure 182 kg/cm2. Along the axes X and Y pending in arbitrary units, respectively the time and the detector.

Method of separating fractions of crude quinoline bases coke production components, in accordance with which is used as raw material produced during coking coal fractions of heavy crude pyridine bases from which pre-allocate a pyridine base, after which the thus obtained fraction crude quinoline bases are divided into components, characterized in that the separation of fractions of crude quinoline bases on the components perform by preparative supercritical chromatography, in which a partial mixture is brought into contact with are in critical condition gas, which is at the same time mobile phase and the adsorbent.



 

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