• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Water is removed from an alkaline solution used to extract relatively high concentrations of mercaptans from a hydrocarbon stream by stripping the alkaline solution with a hydrocarbon vapor stream. The vapor stream is then admixed with the oxygen-containing off-gas stream of the process to enrich the off-gas stream above its explosive limit.
    公开号:SU1075982A3
    申请号:SU772470242
    申请日:1977-04-08
    公开日:1984-02-23
    发明作者:Джеймс Кристман Уильям
    申请人:Юоп Инк (Фирма)；
    IPC主号:
    专利说明:

    ABOUT
    -h ate
    CO 00G The invention relates to a method for removing mercaptans from a hydrocarbon feedstock. A continuous process is known for removing mercaptans from a hydrocarbon feedstock by extracting the feedstock with an aqueous alkali solution, followed by removing the purified feedstock and the mercaptan alkaline stream from the extraction zone, contacting the latter with phthalocyanium containing catalyst in the oxidation zone to form a stream containing disulfide compounds alkali and water 13. The closest to the proposed technical essence and the achieved result is a method of removing mercaptans from hydrocarbons, boiling from the beginning of boiling to 348 ° C, containing 0.10, 66% by weight of mercaptans by extracting the starting material with an aqueous alkali solution, followed by removing from the extraction zone the purified raw material and the mercaptan containing alkaline stream, contacting the latter with a phthalocyanine catalyst in the oxidation zone to form a stream containing disulfide compounds, alkali and water, dividing it into a first liquid phase containing alkali and water, a second liquid phase containing disulfide compounds and a gaseous phase, oxygen, with the second liquid and gaseous phases being removed from the process by recirculation to the extraction zone of the first liquid phase C2. A disadvantage of the known methods is that they do not allow the water from the alkali solution that is formed during the oxidation of mercaptans to be removed by simply keeping in the presence of air withdrawn from the reaction cycle as a waste stream (tailings). Therefore, the water formed during the oxidation of mercaptan impurities dilutes the alkali solution at a much higher rate than the rate of moisture removal in the case when the concentration of mercaptans in liquefied hydrocarbons exceeds 1000 hours per million. As a result, the alkaline solution gradually loses its effectiveness and becomes unsuitable for further processing of the additional hydrocarbon stream contaminated with mercaptans. The aim of the invention is to increase the efficiency of the process by removing water from the alkaline solution and providing such an oxygen concentration in the exhaust gas stream that is less than the explosive limit of the mixture. The goal is achieved by the method of removing mercaptans from a hydrocarbon feedstock; boiling away from. the beginning of boiling up to containing 0.1-0.66% by weight of mercaptans by extracting the raw material with an aqueous alkali solution, followed by removing the purified raw material and the mercaptan-containing alkaline stream from the extraction zone, contacting the latter with a phthalocyanine catalyst in the oxidation zone to form a stream containing disulfide compounds, alkali and water, dividing it into a first liquid phase containing alkali and water, a second liquid phase containing disulfide compounds, and a gaseous phase containing oxygen, with the output from the process of the second liquid and gaseous phases and recirculation to the extraction zone of the first liquid phase, the first liquid phase ne. By recycling in the amount of 37.7100 vol.%, contacting the countercurrent with the evaporated volatile hydrocarbon at 50-250 ° C and a pressure of 1-21.4 atm, followed by addition of the resulting mixture of volatile hydrocarbon with water to the gaseous phase withdrawn from the process. The method is carried out as follows. ROTOCK hydrocarbon feedstock, for example oil, with a relatively high content of mercaptans, falls into the lower part of the extraction zone. It rises upstream in countercurrent with a substantially mercaptan-free aqueous alkaline stream that enters the extraction zone. The usual process of extracting a liquid with a liquid leads to an almost complete transition of the mercaptans contained in the feed stream to an alkaline stream, and to the formation of a removable mercaptan-containing alkaline stream. Hydrocarbons leave the extraction zone as a treated product stream. The air flow is shifted to the mercaptan alkaline stream, and the resulting mixture enters the oxidation zone. In the oxidation zone, almost all of the mercaptans present in the mixture are oxidized to disulfides. The effluent from the oxidation zone / enters the settling tank which operates as a phase separation zone. Disulfides are released as a separate liquid phase and are removed as a by-product stream. Excess oxygen and nitrogen in the air stream is removed from the sump as a vapor stream. The more dense alkaline aqueous phase is removed as a liquid stream. Part
    The flow enters the upper part of the zones. vapor-liquid contact. A vapor stream rich in volatile hydrocarbons. For example, a combustible gas is supplied to the lower part of the contact zone and flows counter to the liquid. The conditions in the contact zone are maintained to ensure the transfer of water from the liquid to the steam flow. This affects the concentration of alkali in the liquid, which is then removed and mixed with the main part of the liquid stream. The vapor stream containing volatile hydrocarbons and water is removed from the upper part of the contact zone. This vapor stream is then mixed with the vapor stream to obtain an exhaust gas stream in which the concentration of hydrocarbon will exceed the explosive limit of the oxygen-hydrocarbon mixture contained in this stream.
    The oxygen required for the regeneration of the alkaline solution is supplied by mixing air into the mercaptans alkaline solution. However, it is also possible to use other sources of acid. Usually, air is injected in quantities that provide an excess of oxygen compared to its quantity required for oxidation. Then, the alkaline solution and the oxygen pass through the oxidation zone operating as indicated earlier, and the stream leaving the oxidation zone passes further through the phase separation zone. Excess oxygen mixed with the alkaline solution causes an excess of oxygen in the phase separation zone. oxygen. It, together with nitrogen, from the air and some water vapor is removed in the form of a relatively small steam flow. The presence of oxygen gas in any of the streams of this process requires extreme care to prevent the accidental formation of explosive mixtures when the oxygen-containing stream is mixed with hydrocarbons or other flammable substances. Following up This is usually practiced by deliberately mixing such a stream with a stream of volatile hydrocarbons, which leads to the determination of the concentration of C1: and the hydrocarbon is above the explosive limit of the mixture. Thus, the arbitrary addition of hydrocarbons only leads to further enrichment of the flow with hydrocarbons and does not lead to the formation of an explosive mixture. The vapor stream used for this purpose is a combustible gas stream to be burned, and the mixture obtained is used as fuel. When mercaptans are oxidized in
    water is formed as a by-product; With relatively low concentrations of mercaptan in the feed stream, the amount of water vapor leaving the process in the steam flow withdrawn from the phase separation zone usually corresponds to the amount of water produced. However, if the mercaptan concentration exceeds 1000 parts by weight. per million in the feed stream, water begins to collect and dilute the alkaline solution. To maintain the effectiveness of the alkaline solution, excess water should be removed. This is achieved due to the fact that part of the regenerated alkaline solution is withdrawn from the phase separation zone with a stream of volatile hydrocarbons mixed with the waste gas stream from the phase separation zone. Volatile hydrocarbons used in. The vapor-liquid contact zone can be separated and the processed product, if sy -; - stream flow consists of volatile hydrocarbons. Such contacting takes place in the vapor-liquid contact zone, and occurs under conditions that promote the transfer of water and alkaline solution into a vapor stream. Typically, the contact area is a layer of packing, however, it can be in the form of a column containing a series of horizontal plates with tools to improve the conditions of contact or any other suitable devices. This leads to the fact that the vapor stream leaving the contact zone contains both water vapor and volatile hydrocarbons. Here, the term volatile hydrocarbons OTHOCJITCH to hydrocarbons containing less than five carbon atoms in a molecule. At the beginning of the process, there is no need to remove water from the alkaline solution. Therefore, it is preferable not to initiate the operation of the contacting zone until the solution is diluted to some noticeable degree. The contacting step is usually carried out at pressures very close to the pressures existing in the phase separation zone - and in the extraction zone of E1Ov: nor. The pressure in these two zones is usually characterized by an increase in pressure created by the pressure used to recycle the alkaline solution. However, as can be seen from the following examples, the extraction zone can also function under significantly increased pressure. The distance in the contact zone can reach a value of up to 70.32 kg / cm, but it is preferably in the range from 3.52 kg / cm2 to 10.5 kg / cm. The temperature in the contact zone should be maintained in the range from 10 to 121 C and preferably from 38 to 53. The amount of water to be removed can be controlled by changing the temperature or pressure in the contact zone, or the speed of passage of steam through this zone. The most preferred method is to adjust the contact conditions. The volume flow rate of steam required to remove this water depends on the parameters, such as the water content of the incoming steam, the conditions established in the contact zone, the effectiveness of the contact operation and the amount of water to be removed. Preferably, 0.001 to 0.01 mol of gas per each 0.454 kg of alkaline solution to be treated passes through the contact zone. After passing through the vapor-liquid contact zone, the more concentrated portion of the alkaline solution is connected to that portion of the solution that did not pass through the zone. This combined stream is fed further into the extraction zone. It is also possible to contact the entire flow of alkaline solution with a stream of steam. The extraction process can use any of the alkaline reagents that can extract the mercaptans from the feed stream under practical operating conditions, and which can be regenerated using the method described above. Preferred alkaline reagents include an aqueous alkali metal hydroxide solution, for example sodium hydroxide or potassium hydroxide. Sodium hydroxide, commonly referred to as caustic, can be used in concentrations of from 1 to 50 wt.%, With preferred concentrations being in the range of 5-25 wt.%. If desired, some agents can be added to increase the solubility of mercaptans in solution, usually methanol or ethanol is used for these purposes. while other agents can be used, for example phenol, cresol or oleic acid. Suitable hydrocarbons for removing mercaptan in the extraction zone vary from propane-butane mixtures to middle distillates. Flows from gas condensation units in catalytic cracking units, in a fluidized bed, natural or cracked gasolines, jet fuel, diesel fuel, kerosene, and mixtures of these materials fall into this sphere. The method can also be used to remove mercaptans from many solvents, alcohols, aldehydes, etc .. More generally, these materials can be classified as ordinary liquid hydrocarbon compounds with a boiling point below 343 ° C. CONDITIONS created in the extraction zone can vary widely depending on factors such as the nature of the hydrocarbon stream being treated and the content of mercaptan in it, etc. In general, the extraction can be carried out at temperatures above-16s and at a pressure sufficient to ensure in the liquid phase. The temperature in the extraction zone is maintained in the range of from 10 to 121 ° C, and preferably from 27 to 49 ° C. The ratio of the volume of alkaline solution required to the volume of the feed stream will vary depending on the content of mercaptan in the feed stream. Typically, this ratio is from 0.01: 1 to 1: 1, although there may be other ratios. The flow rate of the alkaline solution is typically 2-3% of the flow rate of the liquefied gas and can be up to 20% of the light distillate direct distillate. Optimal extraction in this liquid system is achieved with scrubbing through the openings of from 1.5 to 3.0 m / s. Virtually all extractable mercaptans must pass from the feed stream to an alkaline solution. The catalysts used are metal phthalocyanides, for example cobalt phthalocyanine, vanadium phthalocyanine, etc. The greatest catalytic activity can be obtained by using the polar derivative of the metal phthalocyanine, especially the monosulfonic, disulfonic, trisulfonic and tetrasulfonic derivatives. Oxidation catalysts can be used in soluble form, or in a form capable of forming suspensions in an alkaline solution, or can be applied to a solid carrier material. If the catalyst is present in solution, then it is preferably cobalt or vanadium phthalocyanine disulfonate in concentration. 51000 weight.h. per million. The carrier material must be highly absorbent and able to withstand an alkaline environment. It turned out that both vegetable and animal coals are very suitable for this purpose. The carrier material must be suspended in a fixed bed, which ensures effective circulation of the alkaline solution. Preferably, the phthalocyanites of the metals are cocTaBJiJuiH. 0.1-2.0 wt.% Of the final composition, .-; Example 1. The feed stream is liquefied petroleum gas 129.2 APH, 39, with an average molecular weight of 47.1. The flow rate of the feed stream is 3.44 liters. It is fed to the extraction zone as a liquid under a pressure of 23.2 kg / cm 2 at. A 40 l / min lean alkaline stream containing sodium hydroxide enters the upper part of the extractor at 38 ° C and has a specific gravity of 1.149. The Mercaptan-containing, rich ICOM caustic stream is removed from the extraction zone and its pressure is reduced to 11.6 kg / cm. Then this pot is heated to 51, and a ft.alocyanine catalyst and about 17 mol per hour of air are added to it. The resulting mixture goes up through the oxidation zone containing the compacted layer, to the stream leaving the oxidation zone, an oil stream of 1.4 (5.3 l / min) is mixed in, which serves to promote the separation of disulfide compounds from the alkaline aqueous phase, and enters the zone of division into .phases. The separator used has a diameter of 1.22 m and a tangential path in it is 6.25 m. The liquid stream containing disulfide compounds and oil is removed as a by-product stream - disulfide oil under a pressure of 10.2 kg / cm. A steam flow of about 15.9 moles per hour, which removes about 2.94 kg / h of water vapor as an exhaust gas stream. The flow of the regenerated lean alkaline solution with a specific density of 1.42 is withdrawn from the separation zone at a temperature of about 50, and divides into two parts. The first part (15.1 l / min) is heated to 6b, and enters the upper part of the nozzle of the steam contact zone under a pressure of 0.35 kg / cm. This part of the alkaline solution is in contact with a 15 mol / h power flow of the treated noiocchine material withdrawn from the extraction zone. This steam flow enters the contact zone at 37 and at a pressure of about 0.7 kg / cm. Fluid flow at a rate of 17.74 l / min is withdrawn from the contact at 49 ° C and combined with an alkaline solution that does not fall into this zone, as a result of which a thin alkaline solution is obtained which then enters the extrusion zone. A vapor stream of 18 mol / h containing 29.4 kg / g of water vapor is removed from the contact zone. This vapor stream is combined with the waste gas stream withdrawn from the separation zone into phases and fed to a heater for use as fuel. Example 2. An example illustrates the operation of a method in which all regenerated alkaline solutions pass through a vapor-liquid contact zone. The feed stream in this example consists of lighter hydrocarbons, and in the extraction zone is treated as steam. It is obtained by thermal cracking of asphalt and is intended for use as a combustible gas. Therefore, it is present); various mercaptans and other sulfur compounds at concentrations varying up to 6600 parts by weight. per million, which must be removed in order to make the gas suitable for this purpose. The example also illustrates the use of a portion of the treated liquefied petroleum gas as volatile hydrocarbons used to concentrate the slurry solution. The feed stream contains about G :, 3.7% by volume of hydrogen, 35.9% by volume of methane, 18.1% by volume of ethane, 6.7% by volume of propylene, 10.9% by volume of propane and various other volatile hydrocarbons. It also has a maximum of about 100 rpm. on million water and about 2000 ob.h. per million of carbon dioxide. The feed stream is treated by contacting with an amine solution to remove most of the acid disulfide that is present. However, residual amounts of this material are removed before the feed stream is introduced into the extraction zone. This is done by using sodium hydroxide washing, in which the caustic solution is continuously replaced at a rate of about 7.7 L / min. The feed stream enters the extraction zone at and at a pressure of about 4.08 kg / cm with a flow rate of about 494 mol / h. The alkaline solution, which is also a sodium hydroxide solution, enters the extraction zone at a rate of 6.9 gallons / km / (31.3 L / min) at 40 ° C. Contacting in countercurrent leads to the transition of almost all mercaptans from the feed stream to the alkaline stream. About 71% by volume of these mercaptans contain one carbon atom in the molecule, while about 20.5% by volume have two and about 7% by volume have three carbon atoms per molecule. The resulting purified combustible gas is discharged at an oKO.no speed of 494 mol / h. The mercaptan-containing alkaline solution removed from the extraction zone is heated to 52 sec and mixed with a stream of air entering at a rate of 7 mol / h. The resulting mixture is fed to the oxidation zone under a pressure of about 2.67 kg / cm. A phthalocyanine oxide catalyst is mixed in the system and mixed with a liquid alkaline stream. This leads to the oxidation of mercaptans to disulfides and the formation of water 13 as a side product of the oxidation process. Then, the entire stream coming from the oxidation zone passes through the phase separation zone at a temperature of 52 C under a pressure of about 2.32 kg / cm. The waste gas flow from the exhaust gas to this zone also has a speed of about 6.6 mol / h and contains 18.1 kg / hr steam The average molecular weight of this vapor stream is 28.2. 19.5 L / min of the regenerated alkaline solution with a specific density of about 1.055 is removed from the separation zone to $ aza. under pressure 2.32 kg / cm and heated to a temperature of about. This clean stream then flows into the upper part of the nozzle layer of the vapor-liquid contact zone. At the bottom of the contact zone under a pressure of 0.42 kg / cm and with temperature, the processed feed stream is fed at a rate of 6.4 mol / h. The steam obtained is a vapor stream that can be removed from this zone, has an average molecular weight of 29.8, a temperature of bb, 7c and a flow rate of 7.6 mol / h. This vapor stream is then combined with the effluent gas stream from the separation zone into phases to enrich the stream with hydrocarbons. Liquid alkaline solution is removed at temperature L-. about and pass through the refrigerator. It is then reused in the extraction zone. The known method 121 can be used only for hydrocarbon streams, the content of mercaptans in which does not exceed 1000 ppm. In the case when the concentration of mercaptans is more than 1000 ppm, the alkali solution is gradually diluted, since air; As an oxidizing agent, it is not possible to remove additional water formed during the oxidation of more mercaptans. Concerning the comparison of the amount of water removed from the alkaline solution at the first stages of the process, in the first example the air flow is 2.7 kg / h of water vapor / In addition, 27 kg / h of water is removed from the alkaline solution with the fuel gas stream. With regard to the second example, the waste gas flow contains 1.8 kg / h, and the water content in the outflow from the discharge stream noencxa lj is the difference between the flow rate of the fuel gas supplied and discharged from the contact tower, or 7.6-6 4 mol / h, i.e. is 1.2 mol / h. When multiplied by the average molecular weight of this stream, namely 29.8, the amount of water removed in the concrete tower, which is 9.72 kg / h, is obtained. With such a comparison, the advantages of the proposed method are clearly seen in comparison with the known method.
    权利要求:
    Claims (1)
    [1]
    METHOD FOR REMOVING MERCAPTANS FROM HYDROCARBON RAW MATERIAL, boiling from the beginning of boiling to 348 ° С, containing 0.1-0.66 wt.% Mercaptans by extraction of the feedstock with an aqueous alkali solution, followed by removal of the extraction zone of the purified feedstock and mercaptan-containing alkaline stream, contacting the latter with a phthalocyanine catalyst in the oxidation zone to form a stream containing disulfide compounds, alkali and water, dividing it into a first liquid phase containing alkali and water, a second liquid phase containing dis lphide compounds, and a gaseous phase containing oxygen, with the withdrawal of the second liquid and gaseous phases from the process and recirculation to the extraction zone of the first liquid phase, characterized in that, in order to increase the efficiency of the process, the first liquid phase before recirculation in an amount of 37.7 -100 vol.% Contact countercurrent with an evaporated-volatile hydrocarbon at 50- ~
    250 ° С and a pressure of 1-21.4 atm, followed by the addition of the resulting mixture of volatile hydrocarbon with water to the gaseous phase removed from the process.
    >
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    同族专利:
    公开号 | 公开日
    CA1094005A|1981-01-20|
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    DE2714947A1|1977-10-13|
    US4104155A|1978-08-01|
    BR7702235A|1978-08-08|
    JPS52123404A|1977-10-17|
    DE2714947B2|1980-09-25|
    US4040947A|1977-08-09|
    IT1078031B|1985-05-08|
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    DE2714947C3|1981-06-19|
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    FR2347433A1|1977-11-04|
    FR2347433B1|1982-11-26|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US05/675,081|US4040947A|1976-04-08|1976-04-08|Mercaptan extraction process utilizing a stripped alkaline solution|
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