The purification method of crude oil, gas condensate and their fractions from mercaptans and hydrogen sulfide

 

(57) Abstract:

The invention relates to petrochemistry, in particular to methods of refining oil, gas condensate and their fractions from mercaptans and hydrogen sulfide. How are the processing of raw materials organic reagent, which is used as dioxazine patterns

where R is alkyl, aryl, oxyalkyl, alkylaryl group; or mixtures thereof, previously entering into the composition of the reagent tertiary amines N (R')3where R' - alkyl, aryl, oxyalkyl group; in an amount of 0.01 to 0.05 wt.%. The reagent charge in the amount of 0.25 to 0.05 to 1 mol of mercaptan sulfur and hydrogen sulfide. Processing of raw materials is carried out at 10-40°C. the Invention allows to increase the degree of purification of raw materials and reduces reagent consumption. 2 C.p. f-crystals, 1 table.

The invention relates to petrochemistry, in particular to methods of refining oil, gas condensate and their fractions from mercaptans and hydrogen sulfide, and can be used in oil, gas, refining, petrochemical and other industries to neutralize corrosive and highly toxic low molecular weight mercaptans and hydrogen sulfide production, preparation, storage and processing of sulfur crude oil, condensates and f is - and/or nitrogen-containing organic reagents-anhydrides, inorganic salts of carboxylic acids, peroxide, diazo-propylenecarbonate, dimethylacetal-in primary forms, taken in a molar ratio of the hydrogen sulfide in the range (1-50):1, (UK application No. 2185994, 2185995, 2186590, 1987).

The main disadvantages of the known methods that prevent their wider application in industry, are not sufficiently high degree of purification, and high consumption of scarce reagents. The technical essence and the achieved result closest to the proposed invention is a method of purification of oil, gas condensate and their fractions from mercaptans and hydrogen sulfide by treatment of the feedstock with an organic reagent, which use metasomatically, diethanolamine, metadataelement or mixtures thereof (patent RF №2121492, 1995).

The method includes the processing of raw materials by ethanolammonium, diethanolammonium, metadataelement or mixtures thereof, taken in an amount of 0.3 to 2 mol per 1 mol of mercaptan sulfur and hydrogen sulfide. The processing of the feedstock is carried out at 20 to 80°C.

The main disadvantage of this method is not sufficiently high degree of purification of the raw materials from methyl and ethyl mercaptan. In the prototype control of the methyl - and ethyl mercaptan is out of line. As shown by the study authors, this method does not allow objective control for small values of the content of mercaptans. Using the chromatographic method using flame photometric detector according to GOST R-95 revealed that the residual concentration of methyl - and ethyl mercaptan after treatment by a known method does not allow to achieve 20 ppm, i.e., does not provide requirements for the content according to GOST R-2002 Oil. General technical conditions", which was introduced in the last time. In connection with the tightening of requirements for environmental and industrial safety in the oil and gas industry. Another significant disadvantage of this method is the processing of raw materials reagent and a significant consumption of the reagent.

The above disadvantage significantly reduces the efficiency of the process as a whole and prevents its widespread use in industry for sweetening raw material to ensure its safe storage, transportation and processing.

The technical objective is to create a method of cleaning oil products that can improve the efficiency of the process as a whole.

Technical results and processing of raw materials.

The technical result is achieved by processing the feedstock with an organic reagent, which use dioxazine patterns

where R is alkyl, aryl, oxyalkyl, alkylaryl group; or mixtures thereof, previously entering into the composition of the reagent tertiary amines N(R')3where R' - alkyl, aryl, oxyalkyl group; in an amount of 0.01 to 0.05%. Preferably take aqueous solutions of the reagent in the amount of 0.25-0.5 mol per 1 mol of mercaptan sulfur and hydrogen sulfide. In addition, processing of raw materials is preferably carried out at a temperature of 10 to 40°C.

The novelty of the proposed method is to use dioxazine in a mixture with tertiary amines in the above optimal molar ratio in aqueous solution as a chemical reagent - catalyst efficiency low molecular weight mercaptans and hydrogen sulfide, with the processing of raw materials is carried out at a temperature range of 10-40°C.-Known technical solutions containing the distinguishing features of the claimed method, namely the use of alkyl-, dialkyl, oxyalkyl substituted dioxazine or mixtures thereof in the presence of tertiary amines for cleaning oil, gas condensate and their fractions from mercaptans, zerowatt the efficiency of the process as a whole.

We offer the molar ratio of 0.25-0.5) 1 mol of hydrogen sulfide and mercaptan sulfur associated with the stoichiometry of the flowing neutralization reactions of mercaptans, hydrogen sulfide with the formation of non-volatile, stable, non-corrosive, soluble in liquid hydrocarbons, nitrogen - and hydrogen sulfide-containing organic compounds (diazinon) is optimal, since the molar ratio less than (0.25 to 0.5:1) significantly reduced the degree of purification of raw materials from low molecular weight mercaptans, hydrogen sulfide and not achieved a satisfactory degree of purification of oil, gas condensate and its fractions, and reduced chemical consumption. Increase their molar ratio is more than 0.5 mol per 1 mol of mercaptan and hydrogen sulfide sulfur already does not lead to further significant improvements in the purification of raw materials from mercaptans and hydrogen sulfide and causes the excessive reagent.

The feasibility of using the above dioxazines in a mixture with tertiary amines is due to the catalytic action of the latter in response interaction dioxazine with mercaptans. It is necessary to specify the use of 1-hydroxy-2-(perhydro-1,3,5 dioxazine-5 yl) ethane for neutralization of hydrogen sulfide from gases (Patino the degree of purification of gases from mercaptans thus low, not more than 30%, and the degree of purification of oil and condensate - no more than 20-25%, which does not allow to speak about the practical possibility of using free dioxazine for these purposes in the oil and gas industry. Introduction in the reaction medium tertiary amines with concentration (0.01 to 0.05%) in relation to dioxazine allows to increase the degree of purification. At lower concentration the catalytic effect is not sufficient to ensure the necessary degree of purification of raw materials from mercaptans, increasing the concentration of more than 0.05% is not advisable, because, does not lead to further increase in the purity of raw materials.

Preferably the process of refining oil and gas with an aqueous solution of dioxazine, with a concentration of 10-50%. The use of aqueous solutions is appropriate, since the concentration of the reagent above 50%, the viscosity of the worsening in the terms of processing of raw materials. Concentration below 10% inappropriate, because it does not lead to further improvement of the conditions of processing of raw materials (contact materials by mixing).

The preferred carrying out of the cleaning process in the proposed temperature range (10-40°C) is appropriate, because at temperatures below 10°C reduced / min net is AET to proceed with high speed at a temperature of 20°C). The temperature rise above 40°With economically impractical because of the increased energy consumption for carrying out the cleaning process (preheating of the feedstock).

The proposed method has been tested in laboratory conditions. Below are examples of the implementation of this method.

Example 1. 200 ml of Tengiz oil (180 g) containing 0,08% mercaptan sulfur, which according to chromatographic analysis method (GOST R-95) the mercaptan contains 148 ppm (wt.) and ethyl mercaptan 192 ppm (wt.) and hydrogen sulfide 10 ppm, were placed in a reaction flask equipped with a mechanical stirrer and reflux condenser. Then the flask was injected 0.7 ml of a 50% aqueous solution of dioxazine 1-hydroxy-2-(perhydro-1,3,5-dioxazine-5-yl)ethane containing 0.01% of tributylamine. The molar ratio of mercaptan and hydrogen sulfide sulfur:dioxazine in the reaction mixture is 1:0.5 in. The mixture was intensively stirred at a temperature of 40°C and atmospheric pressure for 20 minutes After mixing, immediately conducted a quantitative analysis of the purified oil content of mercaptan sulfur and hydrogen sulfide. The residual concentration of mercaptans to 5.2 ppm, the mercaptan to 8.2 ppm, hydrogen sulfide was not detected, which corresponds to the degree Octoberfest, reduced toxicity and corrosiveness, sufficient for safe storage, preparation and processing of these raw materials.

Example 2. Cleaning Tengiz oil was carried out similarly to example 1 using 1,4 ml of 25% aqueous solution of 1-hydroxy-2-(perhydro-1,3,5-dioxazine-5-yl)ethane containing 0.015% tributylamine, in a molar ratio of mercaptan and hydrogen sulphide sulphur: dioxazine in the reaction mixture is 1:0.5 in. The degree of purification from methyl and ethyl mercaptan is, respectively, 98% and 96%, the hydrogen sulfide in the treated oil was not found.

Example 3. Cleaning Tengiz oil was carried out similarly to example 1 using 3.5 ml of 10% aqueous solution of 1-hydroxy-2-(perhydro-1,3,5-dioxazine-5-yl)ethane containing 0.05% tributylamine, the molar ratio of mercaptan and hydrogen sulphide sulphur: dioxazine in the reaction mixture is 1:0.5 in. The degree of purification from methyl and ethyl mercaptan, respectively, 99,3 and 98.4%, the hydrogen sulfide in the treated oil was not found.

Example 4. Cleaning Tengiz oil was carried out similarly to example 1, using 0.4 ml of 50% aqueous solution of 1-hydroxy-2-(perhydro-1,3,5-dioxazine-5-yl)ethane containing 0.01% triethanolamine, moogo 1:0,3. The degree of purification from methyl and ethyl mercaptan are, respectively, 68,2 and 60.1%, the hydrogen sulfide in the treated oil is missing.

Example 5. Cleaning Tengiz oil was carried out similarly to example 1, using 1 ml of a 50% aqueous solution of 1-hydroxy-2-(perhydro-1,3,5-dioxazine-5-yl)ethane, containing 0.02% triethanolamine, in a molar ratio of mercaptan and hydrogen sulphide sulphur: dioxazine in the reaction mixture above the stoichiometric 1:0.75 in. The degree of purification from methyl and ethyl mercaptan is, respectively, and 99,5 99,0%, hydrogen sulfide was not detected.

Example 6. Cleaning Tengiz oil was carried out similarly to example 1, using 0.25 ml of a 50% aqueous solution of 1,2-bis-(perhydro-1,3,5-dioxazine-5-yl)ethane containing 0.01% triethylamine, in a molar ratio of mercaptan and hydrogen sulphide sulphur:dioxazine in the reaction medium at a ratio of 1:0.25 in. The degree of purification from mercaptans is 95.2% of the ethyl mercaptan 94.6% of the hydrogen sulfide in the treated oil was not found.

Example 7. Cleaning heavy high carbon oil (oil fields of Tatarstan), containing 0,148% mercaptan sulfur, 5 ppm of methylmercaptan, 70 ppm ethyl mercaptan and 250 ppm of hydrogen sulfide was carried out similarly to example 1 and the n, in a molar ratio of mercaptan and hydrogen sulphide sulphur: doxepin in the reaction mixture 1:0,5. The degree of purification from methyl and ethyl mercaptan are, respectively, 96,0 and 92.0%, a residual amount of hydrogen sulfide to 2.8 ppm.

Example 8. Cleaning heavy high carbon oil (oil fields of Tatarstan) in composition, similar to that shown in example 7, was performed using 0,85 ml of 10% aqueous solution of 1,2-bis-(perhydro-1,3,5-dioxazine-5-yl)ethane containing 0.015% Tripropylamine, in a molar ratio of mercaptan sulfur and hydrogen: dioxazine in the reaction medium 1:0,55. Mercaptan in the treated sample is not detected, the hydrogen sulfide content of 3.2 ppm, the mercaptan to 5.8 ppm, which 1 corresponds to the degree of purification, respectively 98,9 and 91,7%.

Example 9. Cleaning the Astrakhan gas condensate containing of 0.20 wt.% markatanova sulfur, 83 ppm H2S, 636 ppm of mailmarketing and 438 ppm ethyl mercaptan was performed using a 50% aqueous solution of dioxazine 1,2-bis-(perhydro-1,3,5-dioxazine-5-yl)ethane containing 0.01% of N-methyldiethanolamine, the molar ratio of mercaptan and hydrogen sulphide sulphur: dioxazine in the reaction mixture 1:0.6mm. The degree of purification from mercaptan - 99,2%, hydrogen sulfide - 98, 25 ppm of methylmercaptan, 39 ppm ethyl mercaptan was carried out similarly to example 1 using 25% aqueous solution of methylpregna-(1,3,5-dioxazine) containing 0.05% tributylamine, in a molar ratio of mercaptan and hydrogen sulphide sulphur: dioxazine in the reaction mixture of 1:0,5. The degree of purification from methyl and ethyl mercaptan, respectively 92.3 per cent, of ethyl mercaptan to 96.3%, from sulfide 98%.

Example 11. Cleaning of thermal cracking gasoline containing 9 ppm H2S, methylmercaptan 14 ppm and 533 ppm ethyl mercaptan was carried out similarly to example 1 using 10% aqueous solution of methylpregna-1,3,5-dioxazine containing 0,042 triethanolamine, in a molar ratio of mercaptan and hydrogen sulphide sulphur:dioxazine 1:0,65. The degree of purification of ethyl mercaptan is 98.7%. Hydrogen sulfide and methyl mercaptan in the treated gasoline are in trace quantities.

Example 12. Cleaning straight-run fractions NK-350°With the Astrakhan gas condensate containing of 0.18 wt.% mercaptan sulfur, in which 470 ppm of methylmercaptan, 140 ppm ethyl mercaptan and 6 ppm of hydrogen sulfide was carried out similarly to example 1 with the control of a 10% aqueous solution of 1,2-bis-(perhydro-1,3,5-dioxazine-5-yl)ethane containing 0.015% dimethylethylamine, begging the TCI inputs was 5 min, the degree of purification from methylmercaptan 95,9%, from ethyl mercaptan is 95.2%. The hydrogen sulfide in the treated condensate is absent.

Example 13. Cleaning Astrakhan condensate composition and the content of hydrogen sulfide and mercaptans, which are defined chromatographic (GOST R-95), and the content of total mercaptan sulfur potentiometric method (GOST 17323-71) spend 20% aqueous solution of 1,2-bis-(1,3,5-perhydro-dioxazine-5-yl)ethane. The latter contains 0.01% dimethylphenylamine, and the molar ratio of mercaptan and hydrogen sulfide sulfur dioxazine 1:0,5. The results of the experiments are summarized in table. The degree of purification of raw materials from methylmercaptan 96.8 per cent, of hydrogen sulfide to 100%. The removal of mercaptan according to the potentiometric titration, i.e., the degree of purification of the total mercaptan sulfur is 89%. Laboratory results are presented in the table.

Example 14. Cleaning a broad fraction of light hydrocarbons, C2-C5(NGL) Astrakhan gas condensate feedstock (50 g) containing 0.05% mercaptan sulfur in the sampler container at a pressure of 1.5 MPa by intensive shaking for 10 min, treated 0,12 ml of 50% aqueous solution of 1-hydroxy-2-(perhydro-1,3,5-dioxazine-5-yl)ethane, the soda, the mixture is 1:0,58. The temperature of the reaction mixture 20°C. After shaking were used to define the content of mercaptan sulfur in purified NGL what was otdovali the contents of the sampler container with an inert gas in the absorption flask, followed by quantitative analysis of mercaptan sulfur in solution by potentiometric titration. Detected trace amounts of mercaptans in purified raw materials.

Comparative experiment showed that when cleaning the specified Astrakhan condensate in a known manner (prototype) with a ratio of the mercaptan and hydrogen sulfide sulfur: reagent 1:1 the degree of purification from mercaptans is 52% and hydrogen sulfide from the 90%. The degree of purification from methylmercaptan is 88% and ethyl mercaptan 85,8%, this leads to the fact that the residual content of methyl - and ethyl mercaptan and hydrogen sulfide is higher than required by GOST R-2002, i.e., the known method does not provide environmental and industrial safety of storage, transportation and processing of raw materials.

The data presented in examples 1-14, suggest that cleaning up the oil condensate and fractions of the proposed method in comparison with the known (prototype) allows to increase the degree by their content is normalized according to GOST R-2002) from 88 to 98-99%, ethyl mercaptan with 85,8 up to 98-99%, of hydrogen sulfide from 90 to 100%. The content of total mercaptan sulfur increases from 71 to 89%.

In addition, the process of the proposed method, in comparison with known allows you to clean when the molar ratio of mercaptan and hydrogen sulfide sulfur to reagent 1:0.25 to 0.5, i.e. 2-4 times to reduce the neutralizing agent. In addition, reducing the time of processing.

The above advantages of the proposed method allows to increase the efficiency of the purification process of crude oil, gas condensate and its fractions in General, by comparison with the known method.

1. The purification method of crude oil, gas condensate and their fractions from mercaptans and hydrogen sulfide by treatment of the feedstock with an organic reagent, characterized in that the organic reagent used dioxazine patterns

where R is alkyl, oxaalkyl, alkylaryl group;

or mixtures thereof, previously entering into the composition of the reagent tertiary amines N (R')3in an amount of 0.01 to 0.05 wt.%, where R' - alkyl, aryl, oxyalkyl.

2. The method according to p. 1, characterized in that dioxazine take in the amount of 0.25-0.5 mol per 1 mol of mercaptan and served the/P>

 

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