• 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:
    A relatively nonvolatile, high molecular weight sulfur solvent produced by activating a dialkyl disulfide oil by the addition of a relatively high molecular weight predominantly aliphatic amine (e.g., a N-alkyl-1,3-propane diamine) and optionally further increasing the molecular weight by the addition of elemental sulfur. Such a sulfur solvent is particularly useful in sustaining a liquid phase at bottomhole conditions for high temperature, high pressure sour gas.
    公开号:SU1058517A3
    申请号:SU813238648
    申请日:1981-01-28
    公开日:1983-11-30
    发明作者:П.Шарп Шелби；Ярбороф Лаймэн
    申请人:Стандарт Ойл Компани (Фирма)；
    IPC主号:
    专利说明:

    01
    00 SP
    This invention relates to methods for dissolving elemental sulfur deposits in wells produced during the extraction of sour gas from deep-seated deposits at high temperatures and pressures. As is known, when the temperature is behind the boil is 121 ° C and at the bottomhole pressure of about 4000 r Si (280 atm) during operation, problems associated with the removal of sulfur deposits can occur. Problems associated with sulfur deposition and accumulation in wells of high-sulfur gas result in the clogging of formations, pipes are cut in various ways using different types of solvents, for example aromatic hydrocarbons such as benzene, toluene, calcine, naphthane, and also a kindling siougl. The closest to the proposed technical essence and the achieved result is a method of removing sulfur deposits in wells by treating them with solvents, using as a mixture of dialkyl disulfide of type R - 5 -SR, where R is an alkyl group, with a low aliphatic amine C 12 And the latter is introduced into the solvent in an amount of not more than 10% by weight of the dialk disulfide. The prepared mixture is kept for 3090 days before being pumped into the well or camouflage. C2 3. A disadvantage of the known methods is that the solvents used lose their effectiveness when operating under conditions of high temperatures and pressures, since under these conditions they are not able to exist in the liquid phase. The purpose of the invention is to enable the process to be carried out at high temperatures and pressures. This goal is achieved by the fact that, according to the proposed method, the treatment of wells and commutations is carried out with a solvent, containing dialkyl disulfide and high molecular weight fatty amine in an amount of 30 wt. h per 100 weight. dialkyl disulfide The solvent is inserted in such a way as to maintain the liquid phase at the bottom of the well. In the main embodiment of this invention, the sulfur solvent is injected into the bottom zone and the well is shut off and the operation is suspended to allow the solvent to be absorbed and to remove sulfur deposits. In another embodiment of the invention, a small but effective amount of sulfur solvent is continuously injected into the bottomhole zone and production string during operation in order to remove sulfur deposits and inhibit or prevent the formation of further sulfur deposits. In another, the third case, the presence of sulfur deposits is monitored and, as necessary for a particular well, continuous injection is interleaved with the absorption method. In all cases, a liquid sulfur solvent in the bottom hole conditions is obtained by introducing a fatty amine into dialkyl disulfide before injecting it into the high sulfur gas well. . Thus, the purpose of the invention is to provide a fatty amine-activated sulfur dialkyl disulfide solvent, and the solvent volatility can be provided in accordance with the requirements for each sour high-sulfur gas treated well in such a way that after injecting small amounts of solvent, the sulfur dissolving liquid will be C5 as a liquid phases in severe downhole conditions; and also in the utilization of this liquid gas to dissolve sulfur in gas wells with sour gas at high temperature and under high pressure to remove and prevent the formation of sulfur deposits, resulting in lower bleedings. It has been found that when using a relatively high molecular weight amine (fatty amine) for the dialkyl disulfide, a heavy dialkid disulfide oil activated with the amine is obtained, which can be in the liquid phase under the conditions of the bottom of the well in the case of 1 sulphurous. gas. This heavy oil was found to be sulfur solvent when used in wells with all-syphonic gas. The fatty amine x # 4 is believed to bind to the dialkyl disulfide to form the required high grade compound with a concomitant low volatility. Consequently, the liquid phase exists at high temperatures and high pressures in the extraction of sour gas even when using “small amounts of this solvent. By adjusting the amount of fatty amine, the degree of volatility can be adjusted to fit the needs of a particular gas well while ensuring the presence of a liquid phase under conditions of a well. Sulfur solvent can be crawled in several ways with the provision of two key features. First, the main component is selected from the class of compounds or mixtures of compounds — dialcldisulfides; and secondly, a sufficient amount of fatty amine is introduced into the dialkid disulfide before it and the well in order to reduce the volatility of the resulting amine-activated dialkyl disulfide so that under the well conditions it is in the form of a liquid phase, Dialkysdisulfida (alky / sisulfida), suitable as starting materials for obtaining improved sulfur solvent, can be considered as compounds in a key pairing of a pair of alkyl radicals, (R and), bonded to a disulfide base according to the formula RR-5-R .. The individual dialkyl disulfide includes such compounds as dimethyl disulfide, diethyl disulfide, dioctyl disulfide, di-tertiary tetra decyl disulfide and the like. Suitable materials are a mixture of aliphatic disulfides, in which the aliphatic group contains about 2-11 carbon atoms, for example (CjHyS), () 2, etc., usually these sulfide mixtures are obtained as a product of the Merox process. Such mixtures of disulfides are obtained by first contacting a stream of petroleum refractory carbon containing aliphatic mercaptans with a solution of caustic to obtain the corresponding sodium salts of mercaptans. The latter are then converted to dialkyl cisulfides by air oxidation with simultaneous regeneration of the caustic. The addition of a high molecular weight aliphatic amine (fatty amna) to dialkyl disulfide oil to obtain a high molecular weight relatively nonvolatile sulfur to dissolve sulfur according to the invention is somewhat similar to the known titration of dialkyl disulfide lower amine to obtain solvent solvents. However, the compositions obtained by known methods / are unable to remain in the liquid phase under the conditions typical for the gas wells in question, whereas the proposed compositions may exist in the liquid phase under the same conditions. Such a difference in the phase state is a consequence of the differences in the compositions made during the preparation of the dialkyl disulfide feed activated by the amine (in addition to an extremely molecular gminus with an excess of 12 atoms in the aliphatic half). In addition, the amine is introduced into the dialkyl disulfide at a concentration that significantly exceeds the level of the previously used concentrations. High molecular weight amines or fatty amines are, in principle, long-chain alkylamines, which are usually synthesized from fatty acids that contain an alkyl group containing 12 or more carbon atoms. Commercially available fatty C1mines may contain mixtures of alkyls with different chain lengths, since they are derived from naturally occurring fatty acids. Often this leads to an excess of substances with an even number of carbon atoms and the presence of unsaturation, for example, as is the case in oleic, palmitic and similar structures. However, any aliphatic rhythm, preferably in the form of simple substances with an even or odd amount of carbon, or in a mixture of these substances, is considered a suitable high molecular weight amine for the purposes of the invention. These fatty amines are preferably wax-like solids or semi-melted substances, low melting point at temperatures characteristic of the gas wells in question. Increasing the molecular weight to reduce volatility is critical to achieving the desired liquid phase under the conditions of high temperature and pressure occurring at the wellhead. In cases where the LIQUID amine is liquid at room temperatures (i.e., fatty amines with alkyl chains preferably at the lower end of the allowable range, for example, reaching), it may be necessary to add elemental sulfur to the activated amine dialkyl disulfide the required high molecular weight heavy oil, which is able to exist as a phase, forming a liquid film, under stringent conditions characteristic of the case in question. A subclass of fatty amines, especially suitable for use in the present invention, is represented by M-alkyl-1,3-propane diami; Although it is known to use lower alkylamines to activate a dialkyl disulfide, the alkylamines being most preferred, it has been found that any aliphatic amine can be introduced into dialkyl disulfide (as a result of which a chemical reaction takes place, which seems to be common to all aliphatic amines and dialkyl disulfides. This assumption is partly based on the fact that, in accordance with the invention, the fatty amines, when added to the dialkyl disulfide, significantly change the phase behavior at high temperatures and pressures due to chemical bonding and partly due to experimental evidence regarding the control of the aliphatic amine vapor pressure. during the activation of the dialkyl ciculide amine (using an amine whose vapor pressure can be measured, for example, diethylamine). It has been noted / that when controlling the vapor pressure of diethylamine during the activation period of the Merox mixture at low concentrations, the vapor pressure first increases when heated and then drops to a very low value, indicating that the amine chemically reacted with dialkyl disulfide. When repeating this technique with gradually increasing amount of amine, it is noted that 2 mol of dialkyl sulfide per 1 mol of amine nitrogen is the upper stoichiometric amount of amine that can be introduced by an amine-activated dialkyl disulfide Under the conditions described and using aliphatic amines with the lowest molecular weight and dialkyl sulfides is the upper stoichiometric ratio roughly corresponds to 10 weight. % amine. When implementing the proposed method, a significant amount of the liquid phase is observed at high temperatures and pressures up to 50% of the stoichiometric amount of fatty amines. When using meroxssi 50% stoichiometric amount correspond to approximately 3040% weight. including high molecular weight amine per 100 wt. dialkyl disulfide depending on the specific molecular weight of the amine. In addition, a necessary phase is observed under wellhead conditions with amine concentrations 10 times higher than the lowest values (300 parts by weight per 100 parts by weight of dialkyl disulfide), which is higher than the stoichiometry. An example. To confirm the presence of a film necessary for the formation of a LIQUID film, at high temperatures and pressures, a series of phase distribution experiments were performed in a PVT cell of variable volume. Table 1 presents the data related to the preparation of activated fatty amines of dialkyl disulfide oils, some of which were used in the photoelectric distribution experiments. Table 1
    When five activated amines of dialkyl disulfide oils are given in Table 1, the amount of fresh dialkyl disulfide oil, as indicated in the second column, is placed in a 500 ml reaction bottle, to which the appropriate amount of fatty amine is then added in the amount indicated in the third column. Due to the lack of volume in the reaction flask, 500 ml of the weight of the reagents in samples 4 and 5 are halved. The specific pure disulfide oil is a sbb of a merox mixture of dialkyl disulfides, which are produced at the Warren Petroleum facility in Beyton, consisting of: (I) N-alkyl-1, 3-propane diamine (RNHCH2CH2CH2NH) 2, where the alkyl group (R) is: It is made of solid fat with an average carbon number of about 18, the trade name is Duotneen 1. (2) Mepokc is a disulfide oil produced by the Warren-Petroleum Company at the Beyton facility. ; The composition of the Merox mixture is given in table 2.
    Diethyl bisulfide Dipropyl disulfide Dibutild isu.t1fid. Dipentyldisulfide dihexyldisulfide Diheptyldis ulf cd
    A particular fatty amine used to activate the dialkyldisulfide mixture is N-alkyl1, 3-propanediamine, supplied by the Chicago Ermeik of under the trade name Duomee.nT. This fat gshin is described as
    350
    Tabliya2
    13.44
    16,15
    33.26
    29.97
    6.62
    0.56
    N-solid fat-1, 3-propanediamine of the general formula J NHCHjCfl-NHj.
    The composition of a typical mixture of alkyl proteins (in the above formula and some typical properties of this fatty amine are presented in Table 3.
    That blitz 3
    0.841
    32
    195 In preparing various samples, Table 1 selected three different relative amounts of fatty amine per 100 g of dialkyl disulfide oil to reflect the amount, below the stoichiometric, stoichiometric amount and excess versus the stoichiometric amount. Since the particular amine used had two nitrogen and since each of them was apparently chemically active to promote dialkidisulfyl oils, whereby this reaction was described as a reaction involving 2 moles of dialkyl disulfide per mole of asoTci in the amine, samples 1, 2 and 3 show what can be expected at approximately 1/3 of the stoichiometric amount of amine, samples 4 and 5 represent an excess of more than 6 times the amount of amine versus stoichiometry and sample b stoichiometric amount. Samples 1-4 are further investigated by the addition of pulverized elemental sulfur. In order to confirm the solution of the composition with respect to sulfur for freshly prepared Merox solutions, the appropriate amounts of sulfur dispersed sulfur are added to the solution with no trace. The dissolution of sulfur is carried out in a confused manner by heating with occasional shaking. After cooling to room temperature, the weight of the wet sulfuric acid is measured, given in Table 1. The data in the last three columns of Table 1 show that activated by dialing dialkyl disulfide oil acts as a solvent for sulfur. The properties of the solvent solvents are extremely close to what was previously known in relation to the promotion of the solubility of sulfur by dialkyl disulfides by using low molecular weight molecules. To confirm the presence of a liquid phase at high temperatures and pressures typical of wellhead conditions, samples 5 and 6 of tables. 1 to select for the presence of a dry gas in a high-pressure PVT cell with variable volume. Initially, the MAN cell was charged with 2.83 cm 3 of active Ciognep T disulfide oil (sample 5) at a pressure of 1500 {105 Ata) and a temperature (32.2 ° C) and 6.346 gm of gas having a composition of Tg1bl.4. TABLE 41 Component T This particular composition corresponds to 3.35 barrels of activated aminel dialkyl disulfide oil introduced 1 into a gas well per million standard cubic feet of dry gas withdrawn from the well / 5.7-10-l / nm ) The MMSCF gadget is maintained at 30lP (149 ° Cj, changing the volume so that the pressure in the gull changes from about 5000 to 15000 (from 350 to 1050 atm). The total cell volume and the volume of the liquid phase in the cells registered yiOT. at various pressures. Then the temperature of the PVT cell is raised to 352 T () and the volume is again; are formed in such a way that the pressure changes from about 5000 to 11000 (from 350 to 770 atm) and then again to 5000 ps-ia. Table 5 shows the results of phase distribution tests for activated JDuomeen T dialkyl disulfide oil with dry gas at a temperature of Curves 301 and 352 ° F (149 i), 149 rJ) uomeen T / 5 in dialkyl disulfide oil. An additional series of experiments was performed using 5.72 cm of activated Duomeen. T dialkyl disulfide (sample 5) loaded in a PVT cell at I500peic ((105 ata) and 95 F () together with 6.346 g-mol of gas from .1. The composition used in this series of experiments corresponds to 6.78 b The temperature under MMSCF is kept ), while the pressure varies from about 2,700 to 13,000 (from 189 to 910 atm). From tab. 5 it follows that there are at least two different signs depending on the formulations used: the total gas to liquid ratio; the relative amount of commune to disulfide in relation to the sulfur used to make the polysulfide oil.
    As indicated in the third column of Table 5, a significant amount of the liquid phase is present in the entire pressure range under all experimental conditions. It follows that nonTable 5
    bypassing the liquid phase exists at the wellhead. The fifth column shows the ratio of the bulk volume at the indicated temperature and pressure: 1 per volume of the amine-activated dialkyl disulfide. These data are of practical interest for calculating the processing of an industrial well in that they qualitatively reflect the relative volume of the liquid phase remaining at different pressures (depths) in the well when 3.5 and B, 78 barrels are injected into the well ( 1 ba of 159 l) oil per 1 MMSCF (0.028) of selected dry gas. The second phase distribution experiment was carried out using activated Duomeen T dialkyl disulfides of sample b in Table 1. The PVT cell is loaded with 3.10 cm of sample b at 1600 psf (112 atm) and 100 ° F (C8c) together with 6.901 g-mol of dry gas, and its composition is given in table 6. Table 6 Component Mol. % 3, 38b of oil / MMSC 2.874 1308.58 1.40.11 5.054 796.01 7.040 621.59 9.017 530.62 O oils / mm S 1242.07 2.4 3.044 0.16 0.11 O These are specific the composition corresponds to 3.38 barrels of oil / MMSCF gas (0.0193 l / nm). The PVT cell is maintained at 351 ° F (177 ° C) as the volume changes so that the pressure in the cell varies from about 2800 to 9000 psi (from 196 to 630 atm). The test is terminated at a pressure of 9000 psia (630 ata) due to the disappearance of the liquid phase under these conditions. At the same time, a second series of experiments was carried out with an increased concentration of the activated amine of dialkyl disulfide. In the second series of experiments, sample 6 with a volume of 6.20 cm was used, which was introduced into a cell at 160 psiot (112 at) and 105 F (38 ° C), together with 6,091 g-mol of dry gas from table 6. This composition corresponds to 6.75bbP oil / MMSCF gas | (0.0385 l / nm) ;-). And in this case, the temperature is maintained at 351 f (), while the pressure varies from about 3,000 to 15,000 psia (from 210 to 1050 atm). Table 7 presents the results of experiments on phase determination for activated Daomeen. TS dialkyl disulfide, oily hC oil with dry gas at 1 ° 7 ° C) i 45.1 g l) uomeenf 100 g of diysyl disulfide. Table 7a (0.0193 l / nm) 0.45l 0.419 0.226 O ase 0.387
    A sample study showed that at 3.38 bc / mmbCP (0.0198 l / nm) the liquid phase is present up to a pressure of about 15,000 psioi
    (1050 ata), whereas in the study of sample 6 of the liquid phase at 3.38
    Kommersant / MM 5CF (0.0193 l / nm), upon reaching a pressure of 9000 paid (630 atm) no. The practical significance of this observation is that the composition of 3.38 barrels of sample 6 (i.e., approximately the stoichiometric amount of amine activator) in one MM of gas has an upper pressure limit, the height of which the liquid phase cannot exist. Therefore, it is impossible to expect that the composition of 3.38 barrels of sample 6 per MM 5CF gas will be effective as a corrosion inhibitor or corrosion inhibitor carrier when it is introduced into a dry gas well at a depth corresponding to a pressure above 9000 psia. However, this does not mean that the composition of sample b is ineffective for the purposes of this invention. The second series of experiments with the corresponding injection of 6.75 Å of the MMSCF (0.0385 l / nm) clearly indicates the presence of a significant amount of the liquid phase in the entire pressure range from 3000 to 15000f sici (from 210 to 1050 atm).
    Thus, the use of a fatty amine to activate dialkyl disulfide oil produces formulations that exist in the liquid phase under high temperature and high pressure conditions that occur in deep dry gas wells. Consequently, the injection of such a liquid-phase sulfur solvent into the well leads to the removal of sulfur deposits and to the suppression of its further deposits. In addition, significant volumes of the liquid phase can be maintained in the downhole conditions with very high dry gas intakes when injecting up to 3-4 barrels of oil per million standard cubic feet of dry gas to be extracted. So
    Thus, the use of a fatty amine to activate dialkyl disulfide oil significantly reduces the volatility of the resulting activated ciMHHCM dialkyl disulfide oil, so that this oil will exist in the liquid phase when injected into deep wells of hot cjocoro gas.
    When comparing data relating to the 3.38Fw / MMSCF series in Table 7 with the results of the 6.75 CC / MM5CF series, it can be concluded that increasing the amount of amine-activated dialkyl disulfide oil not only increases the amount of liquid phase present, but also expands . pressure range at which a liquid phase is needed; , towards higher pressures. In this way, increasing the amount of injected activated tire of dialkyl disulfide oil will provide a protective film as pressure increases.
    Comparison of the data in Table 5 with the data in Table 7 shows that with an excess of fatty acid activator (as compared with the stoichiometric amount), the possibility of increasing the required liquid phase is further increased. It was found that an additional reduction in the volatility of the activated amines of dialkyl disulfide, and thus the additional guarantee of the presence of the liquid phase, can be achieved by 1 preliminary activation of the dialkyl disulfide solvent with dissolved elemental sulfur. Tlfvid motl, with this technique, an amine-activated dialkyl disulfide oil is produced, which exhibits extremely low volatility under the conditions at the wellhead.
    In practice, the injection of sulfur dissolving compositions according to the inventive method can be carried out by any known method in oil production to introduce additives into bottomhole fluids.
    权利要求:
    Claims (2)
    [1]
    1. METHOD FOR REMOVING ELEMENTARY SULFUR DEPOSITS IN WELLS by introducing into them a solvent containing dialkyl disulfide and an amine, characterized in that, in order to enable the process to be carried out at high temperature and pressure, a high molecular weight amine C ^ -C is used as an amine ^ and enter it in an amount of pb at least 30 weight, - h. per 100 weight. including dialkyl disulfide.
    [2]
    2. The method according to claim 1, characterized in that the solvent is introduced into the well in such a way as to maintain the presence of a liquid phase at the bottom of the well.
    Joint venture
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    公开号 | 公开日
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    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US06/043,517|US4290900A|1979-05-29|1979-05-29|Method and composition for removing elemental sulfur from high temperature, high pressure wells and flow lines|
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