RU2507153C1 - Method of obtaining active coals from charges of coking production - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: invention relates to method of obtaining active coal. Method includes separation of 1-3 mm fraction from charge for layered high-temperature coking and the following stages: oxidation with air oxygen at temperature 250°C with rate of temperature increase from room to specified temperature 15-20°C/min with keeping at final temperature for 2.5 hours, carbonisation of oxidised raw material with temperature increase with rate 5°C/min to temperature of carbonisation 550-650°C, with keeping at temperature of carbonisation for 60 minutes, and activation of obtained products with water steam to 35-40% burn at temperature 950°C.

EFFECT: providing possibility of obtaining active coals from charges of coking production without introduction of any additional components.

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Description

The invention relates to a method for producing activated carbon from batch coke production used in the production of metallurgical coke using high-temperature layer coking technology without introducing any additional components and can be used to clean gases and liquids.

When preparing the blends for layer-by-layer coking of the coke-chemical production, coking coal grades recommended by GOST 25543-88 are used: DG, G, GZH, GZhO, Zh, KZh, K, KO, KSN, KS, OS, SS, TS in various ratios, as using additives that improve the sintering ability of coal blends, and without. Examples of the preparation of such blends without the use of additives are given in patent RU 2305122 C1, the scientific basis for the preparation of blends is given in the Handbook of Coke Chemist, Kharkov 2010, volume 1, pp. 117 ÷ 120. One of the basic principles of compiling coal charges for coking is to obtain the indicator "sintering" of the charges y = 16 ÷ 18 mm (according to GOST 1186) and the yield of volatile substances from the charge V ^daf = 27 ÷ 28% (according to GOST 7303). These indicators predetermine the proportion of coals of various grades in the preparation of the charges for high-temperature layer coking of coke production.

This invention provides for the production of activated carbon from blends for layer coking of coke production used in the production of metallurgical coke using high-temperature layer coking without the use of additives that improve the sintering ability of coal blends.

A known method of producing activated carbon (see A.S. SU 1836289 A3, class C01B 31/08) from crushed coal raw materials and a resin binder, including mixing crushed coal raw materials and a resin binder, granulating the mixture, carbonizing the granules, and activating them.

To prepare the mixture take:

35% (mass.) Of SS brand coal (GOST 10 355-76),

35% (mass.) Of coal semi-coke of long-flame coal grade D (GOST 10 355-76),

30% (mass.) Of wood chemical resin (TU 13-4000-77-160-84).

This technology for the production of activated carbon is complicated by the need to use a sintering additive, which complicates the manufacturing technology and increases the cost of producing a mixture for producing activated carbons, as well as the use of highly specialized grades of carbon brand CC (y = 0 ÷ 1) and brand D (y = 0 ÷ 4) practically not used in the preparation of coke charges for high-temperature layer coking.

A known method of producing activated carbon (see AS SU 1789505A1, class C01B 31/08) comprising the production of activated carbons from black gas coals of grade G6 (GOST 8162-79) with a volatile content of 39.4%.

The negative side of the known method can be attributed to the use of a highly specialized brand of coals of grade G6, which is little used in the preparation of coke charges (V ^daf = 39.6%).

A known method of producing activated carbon (see and.with. SU 689090 A class C01B 31/08) including the production of activated carbon, including from low-sintering coal grade 2CC with a yield of volatile 17-25%.

This known method is complicated by the need to use a highly specialized brand of coal grade 2CC, little used in the preparation of coke charges (y = 0 ÷ 1).

The aim of the present invention is to provide a technology for producing activated carbon from charges for layer-by-layer coking of the coke production without introducing any additional additives for use both for the needs of the coke production itself, as an example, for purification of its own production and industrial storm water, and for related purposes.

The technical result of the claimed invention is the creation of activated carbon technology from production charges for layered coking of coke production without the introduction of additional additives.

The task is achieved during the preparation of activated carbons from the charges for layered coking of the coke production without the introduction of additional components. At the same time, they use the infrastructure of coke production at the stage of final crushing without making any changes.

Example 1. Take pre-metered and crushed to a degree of fineness - the content of the class is less than 3 mm not less than 75% of the mixture of coals supplied for coking (charge). Then the mixture is sieved with the extraction of fractions 1-3 mm.

Further, all processes are carried out in rotating electric furnaces, or furnaces with heating by flue gases through the wall. The selected fraction is 1-3 mm. subjected to pre-oxidation with atmospheric oxygen in furnace No. 1 (pre-oxidation furnace) at a temperature of 250 ° C with a rate of temperature rise from room temperature to a predetermined 15-20 ° C / min. with exposure at a final temperature for 2.5 hours.

At this temperature exposure, due to oxidation by air oxygen, the mixture loses its sintering properties.

Next, the product is transferred to a rotary kiln No. 2 (carbonization furnace), in which the temperature is raised at a rate of 5 ° C / min to a carbonization temperature of 550 ° C, with exposure to carbonization temperature for 60 minutes, with the removal of combined-gas coking products and obtaining carbonizate - a material with a high carbon content.

A certain heating rate of the carbon-containing material with exposure at a given temperature allows the formation of the primary porosity of the carbonized product, which is opened and developed during activation. At carbonization temperatures (550-650 ° C), volatile substances undergo intense gas generation with the formation of all types of pores in the coal, including transition pores and macropores, which supply the activating agent at the activation stage.

The resulting carbonizate is activated with water vapor. Activation is carried out in furnace No. 3 (activation furnace) at a temperature of 950 ° C with a rate of temperature rise from the carbonization temperature of 10 ° C / min, with holding at a final temperature of 40 minutes. (depending on the achievement of the required value of the burn equal to 35-40%, which is determined by weighing periodically taken samples of grains of a certain volume). In the furnace serves sharp water vapor with a flow rate of 6-7 kg per 1 kg of activated carbon. The latter, upon reaching the required degree of burning, is unloaded from the furnace and cooled to a temperature of less than 40-50 ° C in a special sealed container.

Example 2. The process as in example 1 to the stage of carbonization. Carbonization is carried out in a rotary kiln at a temperature of 600 ° C. The modes after the activation stage are the same as in example 1.

Example 3. The process as in example 1 to the stage of carbonization. Carbonization is carried out in a rotary kiln at a temperature of 650 ° C. The modes after the activation stage are the same as in example 1.

Example 4. The process to as in example 1 at the stage of pre-oxidation, then heating to 650 ° C at a rate of 2.5 ° C / min. Temperature exposure at 650 ° C and further through the activation stage - as in example No. 1.

Example 5. The process to as in example 1 at the stage of pre-oxidation, then heating to 650 ° C at a rate of 7.5 ° C / min. Temperature exposure at 650 ° C and further through the activation stage - as in example No. 1.

The characteristics of the obtained activated carbons from the blends for high-temperature layer coking of coke production are given in the table:

Example No. V _SH2O , cm ³ / g V _SC6H6 ,
cm ³ / g V _SCCL4 , cm ³ / g V _ΣH2O , cm ³ / g V _ΣH2O
V _SC6H6 V _SH2O -
V _SC6H6 +
V _SCCL4 Example 1 0,0714 0.0198 1.65-10 ^-3 0.537 0.466 0,050 Example 2 0,0540 0,0380 2.22-10 ^-3 0.397 0.343 0.014 Example 3 0,0755 0,0309 2.38-10 ^-3 0.287 0.212 0,042 Example 4 0,0711 0,0202 2.62-10 ^-3 0.314 0.243 0,048 Example 5 0,0630 0,0298 2.20-10 ^-3 0.328 0.265 0,031

The compositions of the charges used for the preparation of activated carbons given in the examples:

Example No. 1: GWF 5.2%, GW 19.2%, W 17.8%, KO 26.2%, KS 28.0%, KSN 3.6%.

Example No. 2: GJ 13.9%, W 31.6%, KO 3.1%, KS 44.4%, OS 7%.

Example No. 3: W 48.5%, KS 18.1%, OS 33.4%.

Example No. 4: GF 8%, GF 12.4%, W 31.3%, KO 18.5%, KS 14.3%, OS 14.0%, T 1.5%.

Example No. 5: GF 19.8%, W 31.4%, KO 31.8%, OS 17.0%.

Where coal grades are given in accordance with GOST 25543-88, namely:

GZhO - gas fat lean; GG - gas fatty; F - bold;

KO - coke lean; KS - slightly coking coke; SPF-coke low-caking low-metamorphosed; OS - lean sintering; T is skinny.

The adsorption capacity of the obtained activated carbons for petroleum products obtained from the prototype is 80-90% of that of the industrially produced brands of activated carbons on a coal base (AG-3) and wood based (BAU).

Claims (1)

A method for producing activated carbon on a coal-based basis, including the separation of a 1-3 mm fraction from a charge for high-temperature layer coking (raw materials) and sequentially performed operations of oxidation with atmospheric oxygen at a temperature of 250 ° C at a rate of temperature rise from room temperature to a predetermined 15-20 ° C / min with exposure at a final temperature for 2.5 h, carbonization of oxidized raw materials by raising the temperature at a rate of 5 ° C / min to a temperature of 550-650 ° C with holding at this temperature for 60 min, activating the resulting product water vapor to burn 35–35% at a temperature of 950 ° C with a rate of temperature rise from the carbonization temperature to the activation temperature of 10 ° C / min with holding at a final temperature of 40 min.