SU1281559A1 - Method for removing sulfides from gases and liquid hydrocarbons - Google Patents

Abstract

The invention relates to methods for the purification of gases and liquid hydrocarbons from sulfur compounds and can be used in the oil refining industry and petrochemical industry. The aim of the invention is to increase the degree of purification of hydrocarbon feedstock from sulfur compounds. The method of purification of gases and liquid hydrocarbons from sulfur compounds is carried out by adsorption by the flask, activated alkali and containing 14, wt.% Iron oxide. The method allows to achieve a degree of purification in dimethyl sulfide up to -50%, and in ethyl mercaptan up to 100 wt.%. 3 tab. C /) C

Description

The invention relates to methods for purifying hydrocarbon gases, paraffin hydrocarbons or gasoline fraction from organic sulfur compounds, namely sulphide and mercaptans, and can be used in refining, petrochemical industries.

The purpose of the invention is to increase the degree of purification of hydrocarbon feedstock from sulfur compounds.

Example 1. The flask was charged with the initial flask and a 5% solution of sodium hydroxide (NaOH) in the ratio of 1:10, the treatment was carried out at the boiling solution for 2 hours. Then the flask was washed to neutral with water, dried on water Noah bath to air-dry state.

The flask is charged with an alkali-treated flask and 1N. a solution of ferric chloride in the ratio of sorbent:: a solution of 1: 6. The activation is carried out at the boiling point of the solution for 2 hours, followed by keeping in air for 2 days. Then, the sorbent is washed from C1 ions and dried in a water bath to an air-dry state. The resulting adsorbent is subjected to heat treatment at 200-300 C.

The boundary values of the content of iron oxides in the alkali-treated flask are listed in Table. one.

The flask is charged with 2 g of activated alkali and ferric chloride and 50 ml of n-hexane containing ethyl mercaptan. The mixture is vigorously stirred at room temperature. The initial and purified n-hexane is analyzed for the content of mercaptan sulfur by potentiometric titration.

The results of the experiment are given in Table. 2. (. For comparison, data are given on the purification of n-hexane from ethyl mercaptan under the conditions described above: the initial bed, flask, activated with ferric chloride, and the flask, activated with sodium hydroxide).

The process of cleaning gases and liquid hydrocarbons from sulfur compounds is carried out at a pressure of 0-24 atm, the activation temperature of the flask is 200-300 s.

Example 2: The method is carried out analogously to Example 1 with the only difference that 2 g of activated alkali and jelly chloride are charged into the flask.

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for flasks and 50 ml of n-hexane containing dimethyl sulfide. The mixture is vigorously stirred at room temperature. The initial and purified n-hexane is analyzed for sulfide sulfur content by potentiometric titration.

The results of the experiment are given in table. 2 (for comparison, the data on the purification of n-hexane from dimethyl sulfide under the conditions described above are given by flask base, flask activated with ferric chloride and flask activated with sodium hydroxide).

EXAMPLE 3 The method is carried out as in example 1, but 2 g of activated alkali and ferric chloride ferric chloride and 50 ml of naphtha gasoline containing sulphide, mercaptan and disulfide sulfur are charged into the flask. The mixture is vigorously stirred at room temperature.

The initial and purified gasoline is analyzed for the content of sulfide, mercaptan and disulfide sulfur by potentiometric titration.

The results of the experiment are given in table. 3 (for comparison, data are given on the purification of straight gasoline from organic sulfur compounds under the conditions described above: initial bed, flask, activated ferric chloride, flask, activated hydroxy)

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Analysis of the degree of purification of paraffin hydrocarbons or gasoline fraction from organic sulfur compounds showed that the effect obtained in the proposed method of purification of gases and liquid hydrocarbons from sulfur compounds using flask after alkali-salt treatment is significantly higher (the degree of purification is 3.8 times for mercaptans. and 2 times for sulphides) as compared with the known method. I

A flask with a high content of iron oxy50 (15.88 wt.%) Compared to a once worked flask (14.69 May,%) is obtained by treating it twice with 1N. ferric chloride solution. Optimum content

55 iron oxides in the flask in the proposed method is justified by the fact that in a single treatment of the flask 1n. iron chloride solution receive flask with an iron oxide content of 14.69%

and the maximum degree of purification from mercaptans and sulphides (respectively, 100 and 50%), double treatment with the same salt solution leads to an increase in the content of iron oxides in flask to 15.58%, to a decrease in the activity of the sample (degree of purification, respectively, 84.61 % and 46.87%, which is valid).

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Based on these data, the optimum content of iron oxides in the flask is 14.69-15.58 wt.%.

EXAMPLE 4 Natural gas, containing 300-500 mg / m of mercaptan sulfur and 20-50 mg / m of hydrogen sulfide, at a speed of 3 (gas consumption is determined by a rheometer and a gas meter) is fed to an adsorber (diameter 31, 4 mm, height 400 mm), filled with activated flask, prepared analogously to example 1. The height of the flask layer in the adsorber is 150 mm. The adsorption process is carried out at 20-50 ° C, pressure 49-50 kg / cm. For proskokuyu concentration of the accepted concentration on mercaptans 36 mg / m, for hydrogen sulfide 10 mg / m. Source and purified gas

The method of purification of gases and liquid hydrocarbons from sulfur compounds by adsorption by their flask, activated alkali, characterized in that, in order to increase the

analyzed for the content of mercaptan purification, using flask, owl and hydrogen sulfide sulfur by potentiometric titration.

holding 14,69-15,58 wt.% iron oxide.

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The results of the experiment are given in table. 4 (for comparison, data on the purification of natural gas from mercaptan sulfur and hydrogen sulphide under the conditions described above is given by the source, the residue, treated with sodium hydroxide, the flask, activated with ferric chloride).

The data table. 4 shows that the proposed method makes it possible to increase the capacity of mercaptan sulfur by 3 times in comparison with the known. . The optimal content of iron oxides in the flask in the proposed method 5 is justified by the fact that a further increase (more than 15.58 wt.%) Of the amount of iron oxides in the flask is impractical because it leads to blocking of the active centers, closure of the pores and a sharp decrease in the degree of sulfur removal.

Claims (1)

Invention Formula The method of purification of gases and liquid hydrocarbons from sulfur compounds by adsorption to them by flask, activated alkali, characterized in that, in order to increase the degree of purification, they use a flask containing 14.69-15.58% by weight of iron oxide. Table 1 Nekhodka 2.12 82.91 5.97 0.34 2.72 0.25 0.7U 1.20 0.29 1.33 Hydroxide on three 51st Chloride Fe (t) tH. Gidroksip On 52-ny n once ovabakna I n, FeClj Na hydroxide 5X- and twice processed 1 n. FeCl 2.94 68.12 12.04 0.74 4.5z 0.33 1.47 1.75 1.73 2.14 0.58 3.18 3.18 2.15 84.55 5.94 0.28 2.96 0.22 0.21 0.70 0.15 1.10 0.09 14,69 14,694.92 61.47 11.16 0.7314.32 0.37 0.60 1.45 0.43 7.36 0.50 15.58 15.58 4.06 62.15 10.02 0.70 15.13 0.45 0.54 1.53 0.62 2.80 0.49 Re ob- Not ob- 4.58 disrupted wife 5.8 Not about- 3.63 outward "but 14,69 6.75 15.58 5.20 4.86 25.00 26.15 203 3.18. 28.12 41.54 205 9.20 11.02 40.62 75.38 141 43.02 80.0 194 14,69 50.00 100.0 219 Processed with 5% sodium hydroxide solution and twice treated with 1N. ferric chloride (Fe) solution. 15.58 46.87 84.61 208 0.417 0,692 51.0 Table 2 0.403 0.468 43., 7 0,304 0,660 48,5 0.504 0.685 50.2 0.420 0.691 51.8 0.435 0.713 52.7 16, 20 45.10 82.0 Processed with 5% sodium hydroxide solution and twice treated with 2n. ferric chloride solution () Initial 16.75 2.97 45.10 80.0 185 0.390 0.680 50.8 18.75 23.08 130 0.345 0.612 32.0 Initial 0.0840.081 3.57 0.060 0.2850.257 9.82 0.560 0.1500, 1.33 0.040 52-nyu solution hydroxide sodium 0.084 0.076 9.52 0.160 0.285 0.248 (2.98 0.740 0.150 0.145 3.33 0.100 Obravoina 1 n, solution of ferric chloride (Fe), containing zhe- aesa oxides 3.18 wt.X 0.084 0.074 11.90 0.200 0.285 0.23t 18.9 1.080 0.130 0.140 6.67 0.200 198 0.388 0.677 50.5 Treated with 1–5 × 5 m sodium hydroxide solution and once compressed with 1 n. ferric chloride solution (containing oxides of iron Leaa and, 69MASL 0.084 0.031 63.0 1.060 0.28S G.208 27.02 1.140 0.1500.130 13.33 0.400 Processed with 5X-sodium solution of sodium hydroxide and twice treated with 1 and, with chlorine iron (Fe) solution, containing iron oxides 15.58 mas.10.084 0.036 57.14 0.960 0.2850.214 24.91 1.420 0.1500.135 10 00 0,300 Initial 500 Treated with 50% sodium hydroxide solution (known) Continuation of table 3 Table4 0.11 50 0,00085 0.15 50 0,0043 Processed 1 and. ferric chloride (Fe) solution containing iron oxides 3.18% by weight Processed with 5% sodium hydroxide solution and once treated with 1N. ferric chloride solution (), containing iron oxides 14.69 wt.% Processed with 5% sodium hydroxide solution and twice treated with 1 and. ferric chloride (Fe) solution containing iron oxides 15.58 wt.% 0.17 50 0,0087 0.45 .50 0.098 0.40 50 0.080