Production procedure of petroleum coke with low content of sulphur oxides in combustion gases

FIELD: oil and gas industry.

SUBSTANCE: invention is related to the production procedure of petroleum coke with a low content of sulphur oxides in combustion gases, which is based on usage of substances binding sulphur. High-sulphur petroleum coke is saturated with an aqueous dispersion of shale-based substance binding sulphur, stirred up thoroughly to a paste-like state, water is evaporated at a temperature of 120-150°C up to the permanent weight and then cooled down.

EFFECT: reducing the sulphur oxide content in combustion gases.

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The invention relates to methods of producing coal products, particularly petroleum coke, with a lower content of sulfur oxides in flue gases of combustion through the introduction of additives, connecting sulfur.

The known method (application WO 01/25373 A1, 12.04.2001, C10L 9/10) the coal production with lower sulphur content, which consists in grinding coal into powder form with a particle size of 20÷80 mesh, mixing it with slaked lime, the addition of water so that the humidity was 10-30%. on the total weight of the granules, premises powder, hydrated lime and water in a container and heated to a temperature of 149÷205°C in an open container to reduce the moisture content of less than 10% vol.

There is a method of binding in coal production (in particular, in brown coal) sulfur in solid residues of combustion, based on the use of substances that bind sulfur, mainly CaO or MgO, with crushed and sometimes pre-dried brown coal and the substance that binds the sulfur is mixed to a state in which a substance in a mixture is dispersed in the form of (DE 3319086, C10L 10/04, 06.12.84).

The disadvantage is the inability to achieve an optimal combustion conditions. It should also be noted that suitable inert from the point of view of binding sulfur flammable substances by themselves are not amenable to either very bad p is Dauda briquetting. Even chopping the whole mixture is achieved by means of the mixer, which may be technically difficult.

There is a method of linking parts of sulfur from coal production (coal or mixtures of coal and lignite), in which coal or a mixture of brown and black coal is mixed with a substance that binds sulfur, to a state in which this substance is in the final mixture is present in finely dispersed form (DE 3326826, C10L 10/04, 14.02.85).

The disadvantage is that when a large number of additives, binding the sulfur emissions sulfur oxide is quite high.

This technical solution adopted for the prototype. However, the prototype has the same disadvantages as the analogues, namely, the emission of sulfur dioxide, though a small percentage occurs. The disadvantage of this method is the high cost of the proposed additions, connecting sulfur oxides in the combustion gases.

The objective of the invention is to develop a method of producing petroleum coke with achievement of the following technical result is a decrease in the content of sulfur oxides in flue gases of combustion.

The problem is solved in that in a method of producing petroleum coke with a lower content of sulfur oxides in flue gases of combustion, based on the use of substances that bind sulfur, according to the invention Vysokoe the NISTO petroleum coke impregnated with the aqueous dispersion of the substance, connecting sulfur, carefully mix to a paste-like state, water is evaporated at a temperature of 120-150°C to constant weight and cooled, the substance that binds sulfur, use slate, shale semi-coke or oil shale ash.

The method is performed by the following sequence of actions: high-sulphur petroleum coke and oil shale, shale semicoke or shale ash is pulverized in a ball mill until a particle size of less than 1.3 mm; prepare a water dispersion of shale, shale semicoke or oil shale ash content of the substances to 20% wt. To stabilize the dispersion Pets introduction of stabilizers. Next, perform a mixture of petroleum coke and freshly prepared aqueous dispersion of shale, shale semicoke or oil shale ash for at least 1 h of High-sulphur petroleum coke charge / mass ratio of from 0.5:1.0 to 1.0:1.0 aqueous dispersion of shale, shale semicoke or oil shale ash. The obtained carbon paste is evaporated to dryness at a temperature of 120-150°C to constant weight and cooled.

For more uniform distribution of the additive slate, shale semicoke or oil shale ash in petroleum coke is recommended that the introduction of additives in several successive stages, to the final content of the additive in the sample coke was from 5 to 15% wt.; each placenta is the one stage of introduction of the additive in the sample is accompanied by stirring, evaporation of water and cooling.

The selection of the slate and its products - shale semi-coke and oil shale ash as a basis for impregnating material due to the presence in their composition of active substances (oxides of alkaline earth metals), which are in the process of burning coke to form a stable chemical compound with grey, passing into the slag. Due to the transfer of organic sulfur in sustainable mineral compound, the amount of sulfur oxides in flue gases of combustion is reduced.

Impregnation sour coke aqueous dispersion of shale, shale semi-coke and ash can reduce the sulfur content in the combustion gases, and the described method allows to obtain eco-friendly energy fuel.

Examples of implementation of the method

Example 1. 4 porcelain crucible with a glass rod for each) weigh the sample of petroleum coke NovoKuibyshev refinery, previously crushed in a ball mill and sieved through a sieve with a particle size of less than 1.3 mm, the sulfur content of 5.8 wt.%, the release of volatile substances 8% wt.; later in the crucibles impose a 10% aqueous dispersion of the Baltic shale deposits whose characteristics are presented in table 1; mix thoroughly with a glass rod until a paste-like state for at least 10 minutes; water is evaporated when the tempo is the atur 120-150°C to constant weight; then the crucible is cooled and transferred to a desiccator; after stabilization of the mass of the crucible is weighed.

The introduction of additives, following the sequence of operations described above is carried out before until the gain introduced supplements to the original sample will be not less than: for Cup No. 1 - 2% wt.; for crucible No. 2 - 4% wt.; for crucible No. 3 - 6% wt.; for crucible No. 4 - 8% wt. The results for the reduction of sulfur in the flue gases of combustion are presented in table 3.

Example 2. The described method of obtaining coal products with a reduced content of sulfur oxides in flue gases of combustion are conducted in accordance with all the conditions of example 1, except that as substances that bind sulfur, the use of oil shale semi-coke prepared by the carbonization of oil shale at a temperature of 520°C. the Results for the reduction of sulfur in the flue gases of combustion are presented in table 3.

Example 3. The described method of obtaining coal products with a reduced content of sulfur oxides in flue gases of combustion are conducted in accordance with all the conditions of example 1, except that as substances that bind sulfur, use the shale ash obtained by burning oil shale at a temperature of 850°C until complete digestion, the characteristics of fly ash are presented in table 2. The results for the reduction of sulfur in the flue gases of combustion are presented in table 3.

The figure shows the change of the output of sulfur from combustion products in terms of the mass of coke with different concentrations of additives in the coke.

Data show that impregnation sour coke considered additives can reduce the sulfur content in the combustion gases, and is most effective with the use of supplements based on oil shale. When his involvement in raw materials in the amount of 8.6% wt. the sulfur content in the combustion gases is reduced from 5.8% wt. to 0.8 wt.%. in terms of the mass of coke In the case of the introduction in Cox supplements based on shale semicoke is the residual product of processing oil shale in the amount of 9 wt.%. the sulphur emissions are reduced to 2.2 wt.%. in terms of the mass of coke. Add oil shale ash in the amount of 9.5% wt. reduces the sulfur content in the combustion gases is to 2.9 wt.%. in terms of the mass of coke. The sulfur content in the combustion gases of the original coke NovoKuibyshev refinery without additives was 5.8% wt.

The emission reduction efficiency of sulfur oxides from gases of combustion of coke with various additives shown in table 4.

As can be seen from table 4 presents the data, the maximum reduction in emissions of sulfur oxides from the combustion gases is achieved by the inclusion of the additive on the basis of slate: at 5% wt. efficiency is 32.8% Rel., with 9 wt.%. - 86,0% Rel. In the impregnation sour coke water di is the Persia shale semi-coke and ash oil shale in an amount of 5 wt.%. efficiency is 22.4% Rel. 17.2% Rel. accordingly, when 9% wt. accordingly, a 58.6% Rel. and 46.6% of Rel.

The efficiency of oil shale semi-coke and ash slate can be explained by the reduction of the effect of transport of the active compounds of the alkaline earth metal to the burning surface, which carry out allocated hydrocarbons slate, as well as content in the composition of the char and ash mineral sulfur - sulfate and, as a consequence, a lower content of the active substance.

In the process of burning coke can happen phenomena contributing to the strengthening of active actions of the components in the composition of the slate, which lead to better communication of the investigated coke with the active substance and reduction of sulfur compounds in the gases of combustion.

Conducted a study on the combustion (oxidation) of the original high-sulfur coke and coke saturated aqueous dispersion of oil shale and shale semicoke, showed higher reactivity to oxygen and a higher burning rate. This fact will allow us to judge that under the same conditions in the furnace part of the energy furnaces burning impregnated coke samples with the addition of slate and shale semicoke is more complete than the original coke, which will increase the overall efficiency of the furnace.

Table 1
Characterization of oil shale in the Baltic deposits
Options
The moisture content W, % wt.Ash A, % wt.Sulfur S,% wt.The coking Fisher yield on the dry shale, % wt.Fractional composition of oil, wt.%
Paragenetically waterResinThe chargasNC - 200°C200-360°C>360°C
2,350,81,80,921,071,86,3163450

Table 2
The chemical composition of the ash oil shale
SiO2/td> Al2O3TiO2CaOMgOFe2O3Cr2O3MnOSO3Na2OK2O
25,66,60,430,72,35,00,010,032,60,40,8

the 7.43
Table 3
Reducing the sulphur content of the gases of combustion of high-sulfur coke with various additives
Options
View SupplementThe mass of coke, gWeight of the additive, gThe content of the additive, wt.%The release of sulfur from the gases of combustion, % wt. coke
Without additives- --5,80
Slate (example 1)7,160,212,954,94
7,200,335,183,78
7,130,537,471,81
7,170,628,580,81
Shale semi-coke (example 2)6,990,162,365,52
6,970,395,644,17
6,980,497,033,32
7,000,649,142,15
Oil shale ash (example 3)7,150,192,68the ceiling of 5.60
0,45the 6.064,50
7,240,506,954,00
7,000,679,602,90

Table 4
The emission reduction efficiency of sulfur oxides from the combustion gases, % Rel.
Options
View Supplementat 5% wt. supplementswith 9 wt.%. supplements
Slate (example 1)32,886,0
Shale semi-coke (example 2)22,458,6
Oil shale ash (example 3)17,246,6

1. The method of obtaining petroleum coke with a lower content of sulfur oxides in flue gases of combustion, based on the use of substances that bind sulfur, characterized in that the high-sulphur petroleum coke impregnated with water is Oh dispersion of the substance, linking the sulfur-based slate, carefully mix to a paste-like state, water is evaporated at a temperature of 120-150°C to constant weight and cooled.

2. The method according to p. 1, characterized in that as substances that bind sulfur, use the slate.

3. The method according to p. 1, characterized in that as substances that bind sulfur, use of oil shale semi-coke.

4. The method according to p. 1, characterized in that as substances that bind sulfur, use of oil shale ash.

5. The method according to p. 1, characterized in that use high-sulfur petroleum coke with a particle size of less than 1.3 mm

6. The method according to p. 1, characterized in that the high-sulphur petroleum coke charge / mass ratio of from 0.5:1.0 to 1.0:1.0 aqueous dispersion of the substance that binds the sulfur-based slate.



 

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