Method of processing acid sludge

FIELD: chemistry.

SUBSTANCE: invention relates to a method of processing acid sludge, wherein sulphuric acid is removed by mixing the acid sludge with distilled water in ratio of 1:6 by volume at 20°C and atmospheric pressure and mixing the aqueous solution of the acid sludge with aqueous ammonia solution in ratio of 7:1.9 by volume.

EFFECT: lower power consumption during neutralisation, low consumption of auxiliary materials and number of process operations.

1 dwg, 1 tbl

 

The invention relates to the field of chemistry, in particular to the processing of the acid tars.

Acid tars are large-tonnage trudnookislyaemymi waste oil refining industry. They are formed when cleaning oils (transformer, capacitor, medical, perfume and other) concentrated sulfuric acid or oleum. Acid tars are highly viscous resinous mass containing a variety of organic compounds, free sulphuric acid and water and are a valuable secondary material resources at the disposal of acid tars possible to obtain surface-active substances, demulsifier for oil-water emulsions of the reaction products of neutralization, as well as liquid fuels, coke, bitumen.

There is a method of processing sour tar by heating to 45-85°C due to the combustion gases of combustion, the mixture is heated acidic residue in the dryer-granulator with soot, which previously from aqueous solution caused the neutralizing agent is a hydroxide, or carbonate salts of alkali or alkaline earth metal I-II group of the Periodic system of elements. The neutralization process is carried out at 45-85°C for 4-10 min [1].

A modification of this method is neutralized with the use of synthetic fatty acids. The way p is rerabotka acidic tars includes the selection of a product from cyclohydrolase pond, the heating is to a temperature of 40-85°C, mixing with the composition to neutralize on the basis of hydroxide and carbonate salts of alkali and alkaline earth metals of groups I-II of the Periodic system of elements and neutral oil.

Hydroxide and carbonate salts are pre-dispersed in the presence of 0.3-0.7 wt.% synthetic fatty acid fraction C6-C22to the degree of dispersion (particle size) of 25-50 μm. At a temperature of 40-85°C and time 6-8 hours spend neutralization process with subsequent separation of the mixture of liquid and solid phase, removing water from the liquid phase in blogospherical, heated by the hot flue gases, pumping of the liquid phase - neutral oil in reservoir storage, and disposal of solid phase [2].

The disadvantages of these methods are the high energy consumption during heating, a large number of technological operations, the cost of auxiliary materials.

Closest to the present invention is a method of processing an acidic tars [3], which includes clearing of sulfuric acid and thermal cracking of the oily component at 400-550°C in the presence of gosatomnazdor ammonia at a ratio of tar:ammonia = 1:(0.05 to 0.1) by weight. The acidic tars from sulfuric acid comprises a mixture of acid sludge with water in a ratio of 1:6 by weight and heating the mixture up to 95-98°C when the permanent stirring until slightly alkaline reaction (pH 8), the separation of sulfuric acid from the oily fraction of the component, the neutralization of the sulfuric acid solution of 25%aqueous ammonia solution.

The disadvantage of this method is the increased energy consumption during heating.

The objective of the invention is the reduction of energy consumption during neutralization, the cost of auxiliary materials and the number of technological operations.

The problem is solved as follows. A method of processing an acidic tars includes a mixture of distilled water and the neutralization of free sulfuric acid aqueous solution of ammonia. Cleaning from sulfuric acid by mixing the acid tar distilled water in the ratio of 1:6 by volume at 20°C and atmospheric pressure, the process of neutralizing free sulfuric acid by mixing an aqueous solution of acid tar with a water solution of ammonia in the ratio of 7:1,9 volume.

The processing of the acid tar by the present method is carried out in two stages. The first stage is the dilution of acid tar water to reduce viscosity and a small increase of the pH of the medium, which leads to some decrease of corrosivity of the mixture. In the second stage is added a solution of ammonia water (GOST 3760-79, wt. the proportion of ammonia is not less than 25%) to neutralize the free sulfuric acid is you.

First acidic tar was mixed with distilled water (pH 5,95) in the ratio 1:6 (for the experiment was taken in 10 ml of tar and 60 ml of distilled water), the mixture was cooled to room temperature. The pH of the mixture was 1.74.

For neutralization of free sulfuric acid was added ammonia, closing the flask with a stopper, then cooled the mixture to room temperature, and then measured the pH of a solution on a laboratory pH meter. The results of the pH measurements are shown on the graph (figure 1).

From the graph it is seen that a sharp change in pH is observed when adding 19 ml of ammonia: adding 18 ml of pH amounted to USD 3.84, and in 19 ml sharply increased to 9,89 (this experiment was repeated 3 times). Adding 19 and 20 ml of ammonia color of the mixture became lighter, tinted orange (the end of the neutralization process is determined by the color change of the reaction mass and increase the pH of the medium up to 8-9).

When disposing of acid tars possible to obtain surface-active substances from the reaction products of neutralization. The production of surface-active substances on the basis of acid tars based on the high surface activity of sulfonic acids and sulfonates, are part of them. Sulphonate surfactant find wide industrial application as dispersing agents, emulsifiers, demulsifiers, defoamers, smace is atela etc.

As one of the indicators of the effectiveness of surface-active substances are pennoobrazovaniem and foam standing, the resulting solutions were tested for these properties.

This was collected in 0.5 ml of solution was diluted with distilled water in an amount of 5 ml, shook, measured the height of the foam (the foam height for all samples was 2-2,5 cm) and the time at which the foam fell over the entire surface. The results are shown in the table.

Results for foam standing
The amount of added ammonia, mlThe time decay of the foam, min
1610
1712,27
1823,01
19.25,36
2027,10

From the data shown in figure 1 and in the table it is seen that the optimum is to neutralize the solution acidic tar ammonia water in the amount of 1.9 share.

Thus, the inventive method compared to the prototype allows to achieve a slightly alkaline reaction (pH≈8) without heating, and thus the claim is ucit from the production process heating, that also reduces energy consumption during processing of the acid tars. In addition, the resulting reaction products can be used in the oil industry as a surfactant.

Sources of information

1. Patent No. 2186086 RF, C10G 17/10, C10G 19/02, 2002.

2. Patent No. 2183655, C10G 17/10, C10G 19/02, 2002.

3. Patent No. 2179571 RF, C10G 17/10, C10G 55/04, 2002.

A method of processing an acidic tars, including mixing with distilled water and the neutralization of free sulfuric acid aqueous solution of ammonia, characterized in that the cleaning from sulfuric acid by mixing the acid tar distilled water in the ratio of 1:6 by volume at 20°C and atmospheric pressure and mixing an aqueous solution of acid tar with a water solution of ammonia in the ratio of 7:1,9 volume.



 

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Method of refining // 2235753
The invention relates to the technology of oil processing for receipt of petroleum products

FIELD: crude oil treatment.

SUBSTANCE: invention relates to freeing crude oil, gas condensates, and fractions thereof from hydrogen sulfide using neutralization reagents. Cruse oil is purified by treating starting material with 10-45% aqueous solution of alkali metal pyrosulfite or hydrosulfite, or nitrite, or ammonium hydrosulfite taken on the basis of at least 1 mole pyrosulfite or 2 mole hydrosulfite, o5 1 mole nitrite per 1 mole hydrogen sulfide. Process is conducted in presence of alkaline caprolactam production effluent taken in amounts 3 to 15 g per 1 g hydrogen sulfide at 10 to 80°C.

EFFECT: enhanced process efficiency and extended application area for alkaline caprolactam production effluent.

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