Formed coke obtaining method

FIELD: oil and gas industry.

SUBSTANCE: method for production of formed coke of carbon-containing material includes stages of oil semi-coke heating, pressure moulding with obtainment of green mouldings and their further cocking. Oil semi-coke is heated up to 350-400°C, at that oil semi-coke with carbon-to-hydrogen atomic ratio within range of (1.3-1.7) or oil semi-coke with carbon-to-hydrogen atomic ratio more than 1.7 is used with addition of sintering additives. After the heating stage before moulding the heated oil semi-coke is hold within 10-20 s.

EFFECT: invention allows improving quality of mouldings, simplifying the method and increasing technology stability and reliability, reducing energy costs and expanding sources of raw materials.

3 cl, 2 dwg, 1 tbl, 4 ex


The invention relates to a method of obtaining a lump formed coke petroleum coke and can be used in the coke and oil refining industries, as well as in non-ferrous metallurgy.

A method of obtaining a molded coke on AU of the USSR №1798364 from petroleum coke breeze faction 0-8 mm with the release of volatile substances 11-15%, which includes stages of heating to 460-500°C., molding the resulting mass under pressure in damp forming a predetermined shape and size and coking them to a predetermined temperature.

As outlined in the known way by speakers of the USSR №1798364 examples, the method determines a low quality of the formed coke - forming, have low technological value due to stresses arising declared in the description of the operating modes.

The disadvantage of this method are:

- limited resources by grade (use for a method of screening oil semi-coke trivia - fraction 0-8 mm and volatile - 11-15%), while the currently available oil semi-coke with volatile up to 30%. In addition, up to 30% oil semi-coke fines volatile in the range of from 11 to 15% have a low sintering properties and, therefore, will not always be suitable on its physico-chemical properties for the production is odstv formed coke of high quality;

- complex technology, the method, due to the fact that in the known method perform high-speed heating, which leads to the necessity of using more complex and expensive technologies, and, consequently, to increased operational costs. The complexity of the technology, the method is also due to the following. When heating oil polyoxo to 460-500°With loss of sintering properties as at 400°C is observed hardening plastic mass in plastometer GOST 1186-87 (for particles of petroleum coke 0-1,6 mm), and according to GOST 13324-94 to a particle size of 0-0,2 mm curing occurs at 400-460°C. Particles of larger size are transferred in a plastic state, and then otverzhdajutsja at lower temperatures. Thus plastic properties of petroleum coke during pressing in the temperature range of 460-500°C lost and good forming it doesn't work;

- the impossibility of using a constant technology for implementing the method, due to the volatility of raw material quality, because with the same values of volatile substances the char may have a sintering properties and may not possess them, which leads to the impossibility of implementation of the known method is, as stated in the formula.

Long-term studies of the authors in the field technologist the ical application of coke showed coccobello and their strength for the basic metallurgical processes mine ore smelting non-ferrous metals, including mining smelting of oxidized Nickel ores must have a lot 260-350,

Lower the size of the briquettes and grinding during pyrolysis lead to a large waste of coke, the formation of large amounts of carbon monoxide (CO), deterioration of process performance and environmental degradation due to incomplete combustion and emissions increase, decrease economic indicators shaft melting, as well as to accelerated depreciation of technological equipment.

Decades of research has shown that a large number of samples neftegazovoi things with the release of volatile substances 11-15% have no sintering properties or have very low rates of baking and therefore not suitable in an individual used to produce coke. The results of these studies are shown in Table 1 (samples are samples of petroleum coke from different manufacturers).

Table 1
No. sampleWa, %Ad, %vdaf, %RI, % The quality of coke, %The output of lump coke, %
40,490,09 11,080----
70,190,1117,495425,254,779,3to 89.5
90,24 0,1615,042--16,484,2

13 0,220,0113,410----


Wa- humidity, %;

Ad- ash content, %;

Vdaf- volatile content, %;

RI - index Horns, % (baking);

CRI - reactivity coke;

CSR coke strength after reaction with carbon dioxide;

CBS - strength coke cold.

As seen in the information table, when the value of the volatile content in the range from 11 to 16% petroleum coke may have a sintering properties and may not possess such properties. Application for obtaining formulano the coke from the various oil polyoxo common technology, based only on the criteria of the content of volatile matter in petroleum coke, will lead to that obtained from various petroleum polyoxo molded coke will be of variable quality.

Also research has shown that the curing of petroleum coke occurs at temperatures around 400°C (GOST 1186-87) for the layer of particles up to 1.5 mm (in close range 380-400°C will be the consolidation of larger particles of 1.5-8.0 mm) and at 450°C (GOST 13324-94) for particles smaller than 0.2 mm, after which the material becomes unsuitable for molding.

The technical result achieved by the claimed invention is the reduction of energy consumption in the production of formed coke, simplification method of producing molded coke, improving the stability and reliability of the technology, the expansion of raw materials.

The claimed technical result is achieved in that in the method of obtaining a formed coke from carbonaceous material containing petroleum coke, including the stage of heating petroleum coke, molding under pressure to get crude molds and their subsequent carbonization, according to the invention, the heating of the oil coke is carried out until the temperature of 350-400°C, used oil coke, characterized by the atomic ratio of carbon to hydrogen in the range (1.3 to 1.7) or use the Ute petroleum coke, characterized by atomic ratio of carbon to hydrogen over 1.7 with the addition of sintering additives.

With this in mind, the most effective temperature for an effective process of plasticizing and molding of the plastic mass from the oil polyoxo are a temperature of 350-400°C.

It is after the heating stage before the stage of molding to exercise restraint heated petroleum coke within 10-20 seconds.

It is advisable that the heating rate during coking was (1-3) deg/min

Suitable molding be carried out at pressures above 3 kg/cm2.

The proposed solution was created by the authors due to the fact that they pointed out that when the same values of volatile substances petroleum coke in some cases had sintering properties, and in other cases, the sintering properties were missing.

The authors faced the problem to establish which characteristics of the original petroleum coke depends on its sintering property.

It is known (Shizunai "Production, improvement and use of petroleum coke", M., ed. Chemistry, 1973, page 97), which is the process of coking petroleum coke is affected by various factors, including the chemical composition of the raw material; inlet temperature of the secondary raw material into the reactor; the duration of stay in the project for a product in the reactor and other

The most informative, according to the authors, is the chemical composition of raw materials. The chemical composition of petroleum coke characterizes the atomic ratio of carbon to hydrogen.

This ratio characterizes the degree of buglarian in the coking process, but also reflects the possibility of formation of plastic masses (as suggested by the authors - and the formation of resinous substances in the petroleum coke).

The authors have conducted numerous experiments, which showed that there is a direct relationship between the atomic ratio of carbon to hydrogen and sintering properties of petroleum coke in the temperature range from 350 to 400°C.

The atomic ratios of carbon to hydrogen to oil polyoxo increase with increasing temperature of pyrolysis of the particulate petroleum coke. This reflects buglarian (i.e. accumulation of C-C-bonds) and is primarily due to the loss of hydrogen (hydrogen-containing complexes), including low molecular weight resins While the authors noted that the atomic ratio of carbon to hydrogen in the range (1.3 to 1.7) obtaining the formed coke is only possible from such petroleum coke, because at this ratio of carbon to hydrogen petroleum coke has good coking properties.

When the atomic ratio of carbon to hydrogen over 1.7 oil polyoxometalate moderate sintering or no caking. In this case, to obtain a formed coke requires the use of sintering additives.

Determination of the atomic ratio of carbon to hydrogen is carried out simply by burning samples (GOST 2408.1-95, ISO 625-75) and determine the products of combustion of carbon and hydrogen.

Defining the pre as a source of petroleum coke by atomic ratio of carbon to hydrogen has a choice of technology for production of formed coke, namely, if the atomic ratio of carbon to hydrogen of less than 1.7, then the original petroleum coke is not necessary to add sintering additives, such as the char has sufficient sintering properties to obtain high-quality molds. If the atomic ratio of carbon to hydrogen in the source of the petroleum coke is more than 1.7, in this case, the receiving quality of the molds is possible only with the addition of sintering additives. As sintering additives may use any known additives, their choice is determined by the ability of the manufacturer and is not crucial for the proposed method.

The inventive method allows to obtain new criteria for evaluation of sintering properties of petroleum coke and selection, according to these criteria the technology of production of formed coke. This allows AEC to improve the quality of the molds, because precluded when the original petroleum coke having a volatile content in the range, which should be observed sintering properties, actually does not possess such properties.

Knowing in advance of sintering properties of the original petroleum coke, simplified choice molding technology of petroleum coke, the quality of the final product.

After the heating stage, it is advisable to withstand hot oil coke within 10-20 seconds. This exposure will allow to accumulate in the oil coke required number plastifitsirujushchie substances and to create conditions for pressing all types of presses (as molding will require lower pressure). The main requirement for presses in this case will only requirement facilities pressing. From observations of the destruction of coal when heated, it is established that the exposure time affects the output of the degradation products. Increasing the exposure time at 400°C leads to the highest yield of tar, it is possible to assume that the relatively high molecular weight (heavy liquid products) do not have time to leave Kokshetau mass and are the main material for the formation of a plastic mass, and then coke.

Thus, it is possible with a sufficient degree of confidence that the low values of atomic relations of carbon in which Dorado (1.7) oil polyoxo indicate the possibility of formation of significant quantities of resin (low molecular weight) products, remove from volatile substances, and education plastic mass of the high-molecular compound is not removed from Kokshetau mass and which is the basis formed by the pyrolysis coke.

Suitable gumming molds to behave in a certain mode, in order to preserve their integrity. The initial temperature calcination of 350-400°C. the heating Rate - (1-3) deg/min Heating of the coking is carried out until the temperature of 700-1000°C. the Molding is carried out at low pressures - greater than 3 kg/cm2.

The inventive method can be used to obtain a molded coke immediately given size, but you can get molded coke large size. I.e. formed into large pieces, such as "bar", "cakes", which then, when the pyrolysis is divided into separately as a result of thermal stresses.

The inventive method is simple, allows to obtain high-quality molded Cox; preliminary analysis of petroleum coke does not require complex special equipment.

Figure 1 shows a plot of the logarithm of the atomic relations s/N petroleum coke from the temperature of the subsequent pyrolysis of the research results.

Figure 2 shows a plot of the logarithm of the index Horns from atomic ratio of carbon to hydrogen according to the results of research.

zavisimosti atomic relations C/s temperature (figure 1) subsequent pyrolysis char, obtained by slow coking of heavy petroleum residues in the subsequent pyrolysis, shows that when heated to 400°C not observed any noticeable changes. If further heating is observed buglarian char (accumulation C-C-bonds), resulting in a linear increase in the logarithm of N with increasing temperature. This dependence upon pyrolysis char from high-sulfur heavy oil residue is observed in the interval from 400 to 1400°C. at higher temperatures there is a smooth linear dependence of the logarithm of the s/N on temperature, due to the graphitization process, i.e. the change in the structure of coke. Thus, at temperatures from 400°C to 1400°C is observed carbonization char at temperatures above 1400°C is the gravity of coke.

Thus, in figure 1 at temperatures close to 400°C, there is a point of inflection dependencies, due to changes occurring processes.

Existing representations of the mechanism of formation of petroleum coke from oil residues similar to the mechanism of formation of coke from coals and associated with changes in the elemental composition and accumulation of C-C linkages due to the loss of volatile low-molecular light connections, which is reflected by the increase in atomic relations s/N (figure 1). During slow coking n is franich residues depending on the attained temperature of the obtained oil polyoxo changing volatile content and sintering properties of the char. There is an unstable relationship between the volatile content of the char and its sintering. There is a stronger dependence of sintering properties polyoxo from atomic relations s/N, as more informative value that expresses the degree of buglarian char, and the presence of high molecular weight, having a sintering properties of the compounds (figure 2).

The inventive method is illustrated by the following examples.

Example 1.

5 kg of petroleum coke in size 0-10 mm, characterized by a content in the organic part: With°=90,05%, N°=5,08%, atomic ratio s/N=1,48, Vdaf=15,03%, JR=55 (where Vdaf- the release of volatile substances, JR - index Horns,° C-mass fraction of carbon in the organic mass of petroleum coke, N° C - mass fraction of hydrogen in the organic mass of petroleum coke) was heated up to 400°C, was kept heated for 15 seconds and were molded separately weighing 370 g under a pressure of 5 kgf/cm2and then pyrolyzable - first with a heating rate of 1°C/min up to 700°C, and then, with a heating rate 3°C/min up to 1000°C.

Was obtained molded coke with lots of molds 314-320 g and an apparent density of 1.51 g/cm3. Molded coke has high strength, can withstand without failure for more than 10 drops from a height of 1.8 m and a indicators P10=3,4%, A25 (P,P)=96,6% (, a10, A25, P and P - durable and the local indicators of coke in the tests according to GOST 9521-74, where P10 is output in percent of class less than 10 mm, A25 - output in percent of class less than 25 mm, P output in percent of class less than 40 mm, B output in percent of class less than 60 mm).

Molded coke compared with metallurgical coke layer coking virtually no dropouts small classes, and with Stoker firing (when used in shaft furnaces non-ferrous metallurgy upon receipt of Nickel, copper and others) has a higher efficiency of the chemical potential. Therefore, it can be expected that the total relative effect of reducing the flow rate of the formed coke compared to coal coke larger than 40 mm will reach about 25%.

Example 2.

2.5 kg of petroleum coke with the size of 0-10 mm, characterized by a content of C°=87,66%, N°=5.25%, and the atomic ratio s/N=1,39, Vdaf=18,21%, JR=72 and 1.5 kg of petroleum coke with a particle size of 0,0.3 mm with the release of volatile substances Vdaf=1,5% (With°=93,0%, N°=0,45%, atomic ratio s/N=17,22, JR=0) were mixed and heated in a laboratory rotary furnace for 10 minutes to a temperature of 400°C and were molded separately weighing 350 g, and then pyrolyzable speeds ranging from 1.0 to 3.5°C/min up to 1000°C. the obtained molded coke has a high strength, low ash content (up to 2%), low reactivity and strength a10 - 4,5%, P - 95,5%.

Obtained the molding (molded coke) on properties suitable for mining smelting of oxidized Nickel ores and other ores of non-ferrous metals.

Example 3.

5 kg of petroleum coke with a particle size of 0-5,0 mm, characterized by a content of C°=89,25%, N°=4,81%, atomic ratio s/N=1,55, Vdaf=16.3%, and JR=25, was heated for 5 minutes in a rotating laboratory furnace to a temperature of 360°C and after exposure for 10 seconds, were formed separately in the form of a biconvex lens diameter 60 mm weight 100 g, and then pyrolyzable initially with a speed of 1.5°C/min to a temperature of 700°C and then speed up to 4°C/min up to 1000°C. the Obtained solid molded coke with lots of separateness 83-84, Obtained molded coke can withstand more than 10 drops from a height of 1.8 m without failure and has strength characteristics A10 - 5,3%, P - 94,7%.

Such a coke suitable for the calcination of limestone in shaft furnaces of various industries.

Example 4.

Petroleum coke of example 1 is heated to 360°C., and then molded using a screw or hydraulic press at specific pressure of 30 kgf/cm2in the form of logs, which pyrolized at a speed of 1.0°C/min up to 700°C, and then up to 1000°C with a speed of up to 5°C/min, it Turns out lumpy durable molded coke with a developed surface, and a high gas permeability. The resulting coke is in the process of calcination up to 1000°C decomposes (as a result of thermal stresses) into pieces with a size of 80-100 mm, which is suitable for process use is isawanya in shaft furnace with Stoker firing.

1. A method of obtaining a formed coke from carbon-containing material, comprising the stage of heating petroleum coke, forming the source of heated material under pressure to get crude molds and their subsequent carbonization, characterized in that use carbon-containing material containing petroleum coke, heating oil coke is carried out until the temperature of 350-400°C, used oil coke, characterized by the atomic ratio of carbon to hydrogen in the range (1.3 to 1.7), or use petroleum coke, which is characterized by the atomic ratio of carbon to hydrogen over 1.7 with the addition of sintering additives, after heating stage before the stage of forming exercise restraint heated petroleum coke within 10-20 seconds.

2. A method of obtaining a formed coke according to claim 1, characterized in that the heating rate during coking is (1-3) deg/min

3. A method of obtaining a formed coke according to claim 1, characterized in that the molding is carried out at pressures above 3 kg/cm2.


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3 cl, 2 tbl

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2 tbl

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