Method and composition for reduction of ferric sulfide deposits in pipe lines (versions)

FIELD: reduction of ferric sulfide deposits in pipe lines.

SUBSTANCE: proposed method consists in bringing the inner surfaces of pipe in contact with composition prepared from aqueous solution containing the compounds given in formula (I): , where X is anion whose valence "n" is selected from definite group and at least one amine selected from group including alkyl amines, dialkyl amines, alkylen diamines, cycloalkyl amines or their conjugates with acids. According to another version, use is made of composition containing tris(hydroxymnethyl) phosphine, at least one amine or its conjugate with acid and solvent. In presence of composition, fast complexation takes place; as a result, ferric sulfide deposits are dissolved and are removed from pipe.

EFFECT: possibility of using safe, available and inexpensive materials ensuring deposition of polymers.

72 cl, 1 tbl

 

The technical field to which the invention relates.

This invention relates to methods and compositions to reduce or remove deposits of iron sulfide inside or on the pipes, in particular pipelines.

The level of technology

Hydrogen sulfide (H2S) is the reactive nature of the impurity in the liquid obtained, for example, in the processing of oil or gas. Corrosion properties of hydrogen sulfide usually lead to accumulation of iron sulfide particles, which are easily captured by hydrocarbons and glycols, salts and other impurities, forming intractable deposits on the surfaces of pipes, for example in pipelines. The formation of such deposits is a serious problem in the oil and gas industry due to the fact that the pipelines must be cleaned by physical methods. In addition, deposits of iron sulfide may reduce the accuracy in assessing the structural integrity of the pipeline, which is determined by using devices known as "smart pigs to clean the pipes" (smart pigs).

There is a limited set of methods to reduce or remove deposits of iron sulfide in the pipeline. For example, in U.S. patent No. 5820766 Gevertz et al. describe the application of inorganic bromato or Yumatov for oxidation of the captured fluid flow sulphides to TBE the DOI elemental sulfur, you want to collect by mechanical means and remove from the pipeline. A byproduct of such mechanical cleaning is sludge, which can ignite and must be disposed of in a special landfill disposal. In U.S. patent No. 4370236 Ferguson describes the method, which consists in the removal of iron sulfide from the gas stream by flushing the flow of the mixture of hydrocarbon and water. The resulting aqueous phase containing soluble iron sulfide, and iron sulfide in the form of particles, which are removed at the further stages of physical and chemical treatments. See, for example, U.S. patent No. 6153100.

Another approach, based on General chemical principles, is to solubilize the iron sulfide in the water. Ions of iron (II) and (III) generally form a relatively water-insoluble compounds in the neutral pH value. Such iron compounds begin to precipitate from aqueous solution at pH 5 or more. For example, iron (II) precipitates from neutral solutions at pH 7 and hydroxide is oxidized to iron (III) in the presence of oxygen. Thus, the usual method of turning water-insoluble compounds of iron (II) and (III) a water-soluble compound is in the handling solids aqueous mixture in the presence of a strong inorganic acid to reduce the pH of the dissolution of iron compounds. However, in the case of sulfide iron (II), when using this method results in the release of hydrogen sulphide, and if it is secreted in sufficient quantities (>437 cm3/l at 0° (C), the solution is the release of toxic gas. Another disadvantage of the method is the use of strong inorganic acids for cleaning pipelines, as most pipes are made of steel or iron, which are sensitive to the action of strong acids, thus there is corrosion, erosion and pitting (pitting). Moreover, when such action results in the release flammable and explosive hydrogen gas.

Another approach to the removal of iron sulfide is described in PCT publication WO 02/08127, which is to use aqueous compositions of Tris(hydroxymethyl)phosphine, or a corresponding salt of phosphonium (common name CGMP) at pH below or significantly below neutral. However, in the publication '127 PCT indicated that the use of CGMP at pH, which is required for the rapid formation of a complex of iron sulfide, lead to problems, including the formation of insoluble polymer, if TGMP mixed with ammonia as coreagent, and oxylene CGMP to nekompleksuyushego oxide Tris(hydroxymethyl)phosphine. To solve such problems in the publication '127 indicated, is that the iron sulfide can form a chelate complex with aminocarbonyl acids or aminophosphonate acids, included in compositions containing CGMP. According to literature data, using CGMP in the absence of ammonium or ammonia, there is a slight synergistic effect of dissolution of iron sulfide. However, due to the fact that the acid coreagent are expensive, their use is impractical, especially if to remove deposits of iron sulfide must use a significant amount of these reagents.

Thus, until the present time there is a need to develop more effective ways to remove deposits of iron sulfide in comparison with the known in the prior art methods, and in the way you need to use safe, readily available and inexpensive materials that require minimal machining and eliminate associated with chemical reactions problems such as precipitation of the polymers.

Disclosure of inventions

To solve the above-mentioned and other objectives of the present invention developed the songs that get the process comprising mixing at least one compound of the formula I

with at least one amine or ammonium derivative in the presence of an aqueous solvent. In formula I, X represents an is he, the valency of which is equal to n, i.e. the number of people cations of phosphonium. The pH value of the aqueous solvent is preferably adjusted to from about 4.5 to about 10, more preferably from about 6 to about 9. Even more preferably the pH is about 8.

According to another aspect of the invention, a method of reducing the level of iron sulfide in the tubes (ducts). According to the method of the present invention provide a communication pipe with the above composition, with the formation of the second composition, and then remove the second piece of pipe. This approach is based in part on the unexpected discovery of rapid solubilization of iron sulfide in the composition.

Another aspect of the present invention relates to compositions containing Tris(hydroxymethyl)phosphine (TRIS)at least one amine or ammonium derivative and a solvent.

In the present invention has also developed a way to reduce the level of iron sulfide in the pipes, which consists in contacting the tube with the above-mentioned composition based on TRIS, forming a second composition, which is then removed from the pipe.

The present invention can be used to clean many types of pipes, such as pipes dry gas and the treated liquid is th. Moreover, the invention includes a continuous feed compositions of the present invention, and periodic flow, i.e. stepwise process.

In one variant embodiment of the invention the anion X in the formula I is monoanions, gianina or trainina. Thus, acceptable anions choose their group, including, but not limited to, chloride, bromide, iodide, lower alkylcarboxylic, bisulfite, bisulfate, hydrocarboncontent, dihydrophosphate, nitrate, hexaflurophosphate, sulfate, sulfite, monohydratefast and phosphate. Preferred anions include chloride and sulfate, and the preferred compounds of formula I, thus, are chloride, tetrakis(hydroxymethyl)phosphonium sulfate and tetrakis(hydroxymethyl)phosphonium.

In particular, in the present invention preferably use amines, which include, without limitation, ammonia, alkylamines followed, diallylamine, alkylenediamine and cyclooctylamine. Also effective are the conjugates of such amines with acids. The preferred amine is ammonia or alkylamine. More preferably the amine is ammonia or methylamine. A preferred conjugate is ammonium chloride.

In a typical case, the present invention includes the use of a solvent. In more detail, in the case of a composition with the person, in using the compounds of formula I, the solvent is an aqueous solvent. Preferred solvents include, without limitation, water and alcohols. The solvent may also include two or more solvents such as water and alcohol. The preferred alcohol is methanol.

According to the present invention the relative amounts and concentrations of the compounds of formula I and TRIS, as well as amine and ammonium derivative can be varied within a wide range. In one aspect of the invention, the amount of the compounds of formula I or TRIS is in the range from about 1% to about 90% (wt./wt.), preferably 5% (wt./wt.) and more preferably 1% (wt./wt.). In another aspect of the invention, the amount of amine or ammonium derivative can vary from approximately 0.05% to approximately 2.0% (wt./wt.). All these quantities are given in the calculation of the total mass of the composition. The relative amounts of components in compositions calculated by the molar ratio of phosphorus to nitrogen. For compositions that contain one or more compounds of the formula I, the aforementioned ratio is calculated on the molar amount of phosphorus contained in ions of phosphonium formula I. For songs instead of the compounds of formula I include TRIS, the molar ratio of the calculated is to see just based on the molar amount of TRIS. In both types of compositions, the molar ratio of phosphorus to nitrogen may range from about 1:1 to about 15:1. The molar ratio is preferably from about 1.5:1 to about 8:1. The most preferred molar ratio is approximately 2.5:1.

The implementation of the invention

The present invention relates to an effective reduction of the level of iron sulfide in the pipes, such as pipes for the treated liquid or gas. The iron sulfide may be present in the gas stream or, for example, on the surface of the pipe of the pipeline. The tube containing the iron sulfide or its deposits, can be contacted with the composition according to the present invention, the iron sulfide forms a soluble complex, which is easily removed from the pipe. The invention is carried out at a pH close to neutral, and therefore, the machining conditions are not corrosive to pipelines and other types of pipes.

Composition

The compositions of the present invention are especially effective in the complexation and solubilization of iron sulfide. According to one aspect of the present invention this result is easily achieved using one or more compounds of formula I in a mixture with at least one amine or Ammon the emergency derivative. The anion X compensates for one or more

cations of phosphonium. Usually n in formula I is 1, 2 or 3. Thus, X means monoanion, dianion or trunion respectively. Although as X, you can use any of the available anions, X is preferably chosen so that the compounds of formula I were soluble in water, alcohols or their mixtures. Therefore, appropriate monoanion include halides such as chloride, bromide and iodide. You can also use the lowest alkylcarboxylic, where the term "lower alkyl" means a straight or branched C1-C6alkyl group. Examples of lower alkylcarboxylic include methylcarbazole (e.g., acetate), ethylcarboxylate, propyl - and isopropylcarbonate. Other monoanionic include sulfur-containing anions, such as bisulfite, bisulfate and hydrocarboncontent. Hydrocarboncontent are anions of the formula RS(O)2O-, where R is lower alkyl or aryl group. Examples gidrokarbokantno include, without limitation, methylsulfonate, bansilalpet, para-toluensulfonate and isomers cellsurface. Other suitable monoanionic include nitrate and hexaphosphate. The dianions X include sulfate, sulfite and monohydratefast. Suitable trainina is phosphate

The compounds of formula I are produced by a number of firms or can be obtained by synthesis according to known methods. For example, first of all, the preferred compounds of formula I, sulfate, tetrakis(hydroxymethyl)phosphonium and chloride tetrakis(hydroxymethyl)phosphonium produced a number of companies such as Rhodia (Cranberry, NJ), and Nippon Industries (Tokyo, Japan) and Cytec Industries (Mobile, AL). Sulfate, tetrakis(hydroxymethyl)phosphonium usually comes in the form of an aqueous acid solution with a pH in the range from 1 to 4. Other compounds of formula I containing various anions X, can be obtained directly by the known reaction between phosphine and formaldehyde in the presence of an aqueous solution of the acid HX, as described, for example, Katz et al. in U.S. patent No. 4044055. Amine or ammonium derivative, which is mixed with one or more compounds of formula I, selected from various amines and their conjugates with acids. If the amine or its conjugate acid is a solid reagent, preferably, but not necessarily, they must be soluble in the solvent used in the composition according to the present invention. Similarly, if the amine or its conjugate acid are liquid, they should preferably be mixed with the solvent. One of the suitable amine is ammonia.

Primary amines, such as alkylamines followed, first of all, are effective and in practice of the present invention. Examples of bonds alkylamines include, but are not limited to, methylamine, ethylamine, n - and Isopropylamine and n - and tert-butylamine. Other examples of primary amines include alkylenediamine, such as 1,2-diaminoethane and 1,3-diaminopropane. Other examples of primary amines include cyclooctylamine, such as cyclopropylamine, cyclobutylamine, cyclopentylamine and cyclohexylamine.

You can also use ammonium derivatives of these amines. Ammonium derivative is the conjugate acid of the amine. The conjugate acid of the amine obtained directly by adding acid to the specified amine. Suitable acids include inorganic acids such as HCl, HBr, HI and phosphoric acid, and organic acids such as carboxylic acids. Thus, in the present invention included a lot ammonium derivatives. The preferred ammonium derivatives include ammonium chloride, ammonium nitrate, chloride, methylamine and chloride of ethylamine.

In accordance with one alternative embodiment of the present invention composition was prepared by mixing suitable amounts of at least one of the compounds of formula I and at least one amine or ammonium derivative in the presence of an aqueous solvent. The order of addition of reactants may vary, but predpochtitel the NYM is the addition of the amine or ammonium derivative to a solution of the compounds of formula I, pH of which is adjusted, as described below. The most preferred solvents include water and alcohol. In another embodiment, it is possible to use a mixture of water and alcohol. Examples of alcohols include methanol, ethanol and isopropanol.

In preferred embodiments, embodiments of the present invention, the amount of the compounds of formula I is about 5% (wt./wt.) or even 1% (wt./wt.), calculated on the total weight of the composition. An appropriate amount of amine or ammonium derivative is in the range from about 0.05% (wt./wt.) up to approximately 2.0% (wt./wt.), calculated on the total weight of the composition.

The pH value of the mixture described above, bring on the choice up to the value in the range of from about 4.5 to about 10. In another embodiment, the solid compounds of formula I can be dissolved or diluted aqueous solutions of the solvent, the pH of which is brought to a value of from about 4.5 to about 10. In another case, to bring the pH to the required size, add the appropriate acid or base. Suitable acids include hydrochloric and sulfuric acid. Suitable bases include the hydroxides of sodium and potassium, and organic bases such as triethylamine.

In variants of the embodiment of the present invention, using a commercial aqueous solutions of sulphate of those is rakis(hydroxymethyl)phosphonium, the pH value should be increased. the pH increase when adding to the mixture a suitable base. The pH value can be maintained by using a buffer solution. For example, 0.1 mol of acetic acid is dissolved in 0.5 l of water and the pH of the solution was adjusted to 5 by adding 2.0 M solution of sodium hydroxide, the mixture is then diluted with water to a volume of approximately 1 l, re-adjusting the pH to 5 with sodium hydroxide and finally bring the solution volume to 1 L. In another embodiment, it is possible to use sodium acetate or potassium and acetic acid so that the total number of acetate ions from any source amounted to 0.1 mol, dilute the resulting solution to approximately 1 l, to bring the pH to 5 with acetic acid and dilute the solution exactly to 1.0 L. you Can also use other buffer solutions such as phosphate and citrate, within the above range of pH. In addition, as buffer substances can be used nailexpo acid. Examples of acids include nitryltriacetic acid (NTU) and Ethylenediamine-N,N,N',N'-tetraoxo acid (EDTU).

As indicated above, the present invention mainly describes the complexation of iron sulfide in a wide range of pH. The inventors have discovered that the degree of complexation of iron sulfide increases with increasing pH. Thus the om, the pH is preferably from about 6 to about 9 and most preferably about 8. For example, in laboratory experiments have shown that when using an aqueous solution of 0.015 M FeSO4, 0.03 M MH4+and 0.06 M sulfate tetrakis(hydroxymethyl)phosphonium, pH 4.5, which is supported with buffer solution, the degree of complexation of iron sulfide is 0.5 h at 22°C. using similar solution with a pH of approximately 5.0 degree of complexation decreases to 0.01 hours In this case, the term "degree of complex formation" means the time required to increase the absorption of the solution at 500 nm to 1.0.

Without going into the details of any theory or principle, the inventors believe that the compounds of formula I, above all, in aqueous solutions at high pH form of Tris(hydroxymethyl)phosphine (TRIS). Suitable method of obtaining TRIS is bringing the pH of an aqueous solution of sulfate tetrakis(hydroxymethyl)phosphonium up to 8 by adding sodium hydroxide or potassium, with 95% of the phosphorus in the resulting solution is in the form of water-soluble TRIS. The specified transformation described in the art, see Kasparov et al., Journal of General chemistry, 32, (1962), 553. TRIS can be synthesized by the interaction of phosphine, forms the of legido and tetrachloroplatinate potassium, see U.S. patent No. 3030421, Reuter et al. Tris(hydroxymethyl)phosphine is produced, for example, the firm Strem Chemicals, Inc. (Newburyport, MA).

In another variant embodiment of the present invention a composition comprising TRIS, get partially using unexpected discoveries, which consisted in the fact that the products of reaction of TRIS and at least one amine or ammonium derivative, are effective absorbers of iron sulfide in the pipes. According to the present invention the amine or ammonium derivative, as described above, is mixed with TRIS in a solvent to form solution. When using ammonium derivative in an aqueous solvent, it is preferred, but optional, is to increase the pH of the solution.

The composition may be obtained in two main ways. In one variant embodiment of the present invention, first prepare the TRIS of the aqueous solution of the compounds of formula I, such as the sulfate or chloride, tetrakis(hydroxymethyl)phosphonium, according to the method described above. The resulting solution, which contains TRIS, mixed directly with the amine or ammonium derivative, or with their solutions to produce the composition. In another variant embodiment of the present invention, a solution of pure TRIS in the solvent can be mixed with the amine or ammonium derivative. The preferred amine t is aetsa ammonia or a primary amine, such as methylamine or ethylamine. Most preferred is methylamine. Preferred are solvents which dissolve TRIS. Preferred solvents are polar solvents, such as alcohols or water-alcohol mixture.

In preferred embodiments, embodiments of the present invention, the content of TRIS in the composition is from about 5% (wt./wt.) or even 1% (wt./wt.), calculated on the total weight of the composition. A sufficient amount of amine or ammonium derivative is in the range from approximately 0.05 to approximately 2.0% (wt./wt.), calculated on the total weight of the composition.

The methods and compositions of the present invention are effective in the range of relative amounts of compounds of the formula I or TRIS and amine or ammonium derivative. The molar ratio of phosphorus in the composition of the phosphonium ions of formula I or composition TRIS to nitrogen in the composition of the amine or ammonium derivative can vary in the range from about 1:1 to about 15:1. The preferred molar ratio is from about 1.5:1 to about 8:1, even more preferred molar ratio is approximately 2.5:1.

If the amine is ammonia or if ammonium is derived ammonium salt (for example, NH4Cl), then x is de determine the optimum ratio can be observed the formation of a polymer precipitate. However, even under optimal relations residue that completely dissolves with the formation of the composition, which is characterized by low, but the obvious ability to dissolve iron sulfide. In another embodiment, the precipitate can be completely avoided by using a higher molar ratio of phosphorus/nitrogen, compared to the optimum value without any negative effect on the ability of removing iron sulfide. In addition, the use of primary amines, as described above, does not lead to the formation of a polymer precipitate and, therefore, is an unexpected advantage in comparison with known compositions described in the art, the use of which is observed sediment. Moreover, if the ammonia and alkylamine use at the same time, decreases the probability of formation of a precipitate in the presence of ammonia in the range of pH according to the present invention, the formation of solutions, which are also effective in the dissolution of iron sulfide. Thus, the compositions of the present invention, including alkylamines followed, have the advantage of complexation of iron sulfide associated with the flow of water captured by the ammonia.

The compositions of the present from which briteney optionally include one or more additives, which provide compositions for a variety of pipe types, in which the removal of deposits of iron sulfide is a significant problem. Additives include surfactants, biocides, such as glutaric aldehyde and 2,2-dibromo-3-nitrilopropionamide (DBNPA), water dispersants, demulsifiers, scale inhibitors deposits, corrosion inhibitors, defoamers, oxygen scavengers, such as diethylhydroxylamine (DEG) and flocculants.

Surfactants include anionic, amphoteric, cationic and nonionic surfactants, which typically contain a hydrophilic residue and hydrophobic substituents, such as alkyl, alkenyl, cycloalkyl, cycloalkenyl, aryl, alkaryl, arylalkyl and polyarylene group containing from 6 to 24, preferably from 10 to 20 and more preferably from 12 to 18 carbon atoms. Hydrophobic substituents also include polymeric fragments, such as polysiloxane and polyoxypropylene. Examples of anionic surfactants include poorly water-soluble sulfonic acid salt or complex monetary sulfuric acid, such as alkylbenzenesulfonate, alkyl sulphates, sulphates alilovic esters, reincorporate, alkanesulfonyl, alkylphenolate, sulfates alkylphenolic esters, sulfate alkylamidoamines, sulfates alkylamidoamines and alpha califoirnia acids or the corresponding esters containing from 6 to 24 atoms in the of Lerida.

Other examples of anionic surfactants include Soaps, such as linoleates, alkalemia esters of carboxylic, palmitate, resinate, oleates and stearates, and alkylsulfonate, such as di-2-ethylhexylphthalate and vexillologist sodium, acultural, isethionate, sulfosuccinate alilovic esters, acylcarnitine and alkylsulfonate. Anionic surfactants may include anionic phosphate ester, alkylphosphonate, alkylamino or aminomethylphosphonate. Each of these surfactants typically contains at least one hydrophobic Deputy, described above. The ester-containing surfactants include one or more of gliterring, oxyethylene, oxypropylene and oxybutylene groups.

Although the preferred anionic surfactants are sodium salts, produced by other firms salts include salts of lithium, potassium, calcium and magnesium, and ammonium salts of monoethanolamine, diethanolamine, triethanolamine, lower alkylamines followed, alkyl - and hydroxyacetone.

Nonionic surfactants include tertiary acetylenic glycols, polyethoxysiloxane alcohols, polyethoxysiloxane mercaptans, polyethoxysiloxane carboxylic acid, polyethoxysiloxane amines, polyethoxysiloxane hydroxyalkylated, polyethoxysiloxane ALKYLPHENOLS, polyethoxysiloxane glycerolipid or propoxycarbonyl or mixed ethoxylated and ProPak lirovannye derivatives. Polymeric nonionic surfactants include block copolymers of polyoxypropylene and polyethylene, and copolymers of polyoxyethylene and polyoxyethylene or polyoxyethylene and polyoxypropylene.

Amphoteric surfactants include any water-soluble surfactant comprising a hydrophobic residue, such as With6-20alkyl or alkenylphenol group, and a hydrophilic residue, containing the amino group or Quaternary ammonium group and a carboxylate, sulfate or sulfonic acid. Examples of amphoteric surfactants include betaines or imidazolidine. Other examples include sulfates of alkylamidoamines, sulfobetaine and Quaternary amino or imidazolinones acids and their salts. Other suitable surfactants include zwitterionic surfactants, such as N-alkyltin and carboxylates amidoamines. Specific examples include, without limitation, 2-alkilirovanie tall oil, 1-aminoalkylsilane tall oil, 1-carboxymethylation and 2-alkilirovanie coconut oil and N-carboxymethyl-2-(hydroxyalkyl)imidazolin.

The cationic surfactant used in the present invention include alkylammonium salt containing at least 8, preferably from 10 to 30 and more preferably from 12 to 24 aliphatic carbon atoms. Above all, preferred cationic surfactants are three - and tetraalkylammonium salt. Usually, Katie the major surfactants include one or two aliphatic chain, each of which contains from 8 to 20 carbon atoms, and two or three short alkyl groups, each of which contains from 1 to 4 carbon atoms. Specific examples include salts of didecyldimethyl-ammonium and salt benzalconia containing 1 long and 2 short alkyl groups. Other cationic surfactants include salts of N-alkylpyridine, in which the alkyl group contains from 8 to 22 and preferably 10 to 20 carbon atoms. As cationic surfactants can also use salt ascaridiasis-ammonium. Each alkyl group contains from 1 to 4 aliphatic carbon atoms, and alarilla group, such as alkyl benzene group contains from 8 to 22 carbon atoms.

Another class of cationic surfactants include salts alkylimidazole, such as salt alkylmethacrylamide. Examples include the salts alkylmethacrylamide, salt alkylbenzyldimethylammonium and salts of 2-alkyl-1-alkylmethacrylamide. As the cationic surfactant use certain amidoamine. Get them in the interaction of fatty acids, complex ester, glycerides, or their amide-forming derivative with di - or polyamines. Examples of polyamines include Ethylenediamine and Diethylenetriamine.

Cationic surfactants include anion, which may be any anion, which increases the solubility of the surfactant in water. Under adamie anions include, without limitation, the anion X in the formula I, described above.

The above surfactants include their perfluorinated derivatives. First of all, the preferred surfactants of this type include the perfluorinated alkyl sulphates and salts of perfluorinated Quaternary ammonium.

As the surfactant of the present invention preferably uses surfactants used as wetting agents. Wetting agents reduce the surface tension between water and a hydrophobic solid surface, such as the inner surface of the pipe.

The amount of surfactant in the composition can vary over a wide range. Typically, the ratio of the surfactant to the weight of the compounds of formula I or TRIS is from about 50:1 to about 1:200, preferably from about 20:1 to about 1:100 and most preferably from about 10:1 to about 1:50. First of all, the preferred ratio is from about 2:1 to about 1:15.

Inhibitors of the formation of deposits and corrosion, used in the present invention include, without limitation, phosphonates, such as 1-hydroxyethane-1,1-diphosphonate, primality, polyacrylates, polymethacrylates, polyphosphates, esters of phosphates, soluble zinc salts, nitrates, sulfites, benzoate, tannin, ligninsulfonate, b is striatal, mercaptobenzo-thiazoline, imidazoline, resin-based Quaternary ammonium compounds.

An example of a class of flocculants include polyacrylamide dispersers. Defoamers include acetylindole, silicones and their polyethoxysiloxane derivatives. Examples of biocides include compounds of tin and isothiazolone.

The compositions of the present invention can also include surfactants bioenergy, such as described in U.S. patent No. 4778813. Examples of surfactants of bioinert include poly[hydroxyethylene(dimethylimino)ethylene(dimethylimino)methylenchlorid], poly[hydroxyethylene(dimethylamino)-2-hydroxypropyl(dimethylimino)methylenchlorid] dichloride and N-[3-(dimethylammonio)-propyl]-N-[3-(ethyleneterephthalate)propyl] urea.

Another class of surfactant BioInitiative includes hydrotropes, which, at a concentration of about 1% or higher, increase the solubility of poorly and moderately water-soluble substances. Examples of hydrotropes include water-soluble ethers of glycol, such as onomatology ether of diethylene glycol. Other hydrotropes include lower alkylarylsulfonate sodium, potassium and ammonium.

The content present in the compositions of the present invention is not surfactants of bioinert may be approximately less than 50%, preferably approximately less than 20%, more preferably approximately less than 10% naibolee preferably approximately less than 5% (wt./wt.), in calculating the masses of the compounds of formula I or TRIS in the composition.

The above additives are preferably mixed with the previously obtained compositions of the present invention. For example, the compound of formula I or TRIS are mixed with the amine or ammonium derivative, as described above. Then one or more additives added to the resulting composition. Additives can be added in the form of pure compounds or commercial preparations such as aqueous solutions. The compositions of the present invention can be obtained in advance and stored until use. The composition is characterized by a moderate sensitivity to oxygen. Therefore, preferably, but not necessarily, to blow out the composition with an inert gas and stored in an atmosphere of inert gas, such as nitrogen. The composition can be stored in an atmosphere of inert gas or in sealed and almost completely filled containers to minimize the amount of air in the upper part of the container.

Method of reducing iron sulfide

The methods of the present invention are extremely effective in solubilization of iron sulfide. This result is achieved by contacting the pipe containing the iron sulfide, with a composition of the present invention with the formation of the second composition, which then removes the h pipe.

Methods applicable to various pipes, contaminated or clogged by deposits of iron sulfide. In the present invention the term "tube" includes any container, which can supply water, gas or other fluid. Examples of such pipes include, without limitation, pipelines, valves, filters, filtration units, tanks, equipment for warehouses. Of particular importance are the pipelines for the oil and gas industry, which is pumped dry gas, chemically treated liquid, or both types of products. Thus, the main advantage of the present invention in this case is that the pH of the compositions is introduced into the pipeline, it is possible to regulate and control that facilitates handling, maintenance of pipelines and remove songs. The present invention relates to water treatment and water systems such as water tanks, contaminated with iron sulfide. In this context, the removal of iron sulfide reduces the tendency to clogging of the filter device by iron sulfide and, therefore, reduce the need for standard treatment with a strong mineral acids, which usually lead to the simultaneous effect on iron pipes and other systems made from iron. The composition is according to the present invention serves in the pipe by any method or combination of methods, necessary to ensure contact with deposits of iron sulfide. Songs can be submitted in continuous or batch mode, i.e. portions, for example, in operating the pipeline or the pipeline. In another embodiment, the periodic filing is effective for disabled pipelines, for which for some time have not performed maintenance for cleaning. Industrial methods include pipe cleaning scrapers (ruffs), which is effective for the treatment of pipelines. Songs can even be entered in the pipe after cleaning scraper for removal of iron sulfide. In addition, the composition can be used for further processing of such pipelines to maintain low levels of iron sulfide.

Despite the fact that the application of any specific composition of the present invention is effective for removing iron sulfide of the pipes, the optimal molar ratio of phosphorus to iron for this composition is approximately 5:1. The optimal molar ratio in some way may depend on the amine or ammonium derivative contained in the composition, and the ratio can easily be determined by standard experiments. For example, the most effective compositions based on TRIS and ammonia which are composition with a molar ratio of phosphorus to iron 4:1, the formation of solutions from pink to bright red, depending on the concentration of sulphide of iron chelation. The ratio of phosphorus to iron 5,1:1 is most effective for compositions based on TRIS and methylamine, usually forming complexes of iron sulfide, whose color ranges from pink-orange to dark orange-brown, depending on the concentration of sulphide of iron chelation. You can use a molar ratio that is different from the optimum ratio, with sufficient efficiency, while complexation and dissolution of iron sulfide occur with lower speed. In any case, once formed solutions solubilizing iron sulfide, their color quickly changed to light yellow during the slow oxidation of iron in the air, however, the solution remains homogeneous.

Examples

The following examples are provided to illustrate the present invention. It should be understood, however, that the invention is not limited to the specific conditions or details described in these examples.

Example 1. Compositions containing sulfate, tetrakis(hydroxymethyl)phosphonium (TGFS) and ammonium chloride

A. Solfataras(hydroxymethyl)phosphonium (TGFS) used in a commercial product - 5-90 wt.%-aqueous solution, pH which varies in the range of less than 4. If you use the following methods get 1000 g of 5%aqueous compositions, which are capable of forming a complex with iron sulfide. Mix 66.6 g of 75 wt.%-aqueous solution TGFS (in water) and 0.5 g of ammonium chloride and then diluted with 90 g of water and stirred. To increase the pH to approximately 6.5 add a sufficient amount of 30 wt.% an aqueous solution of sodium hydroxide or potassium. The total weight of the product was adjusted with water to 1000 g and then measure the pH. If necessary, after dilution the pH of the mixture can again be brought to the required size.

In this example, water can be substituted for methanol in varying amounts to form solutions with a water content of from 0% to 95% depending on the total relative amounts of TGFS and water solutions. You can get more concentrated compositions by simple restriction of water or alcohol used to dilute the reaction solution.

B. Compositions for industrial use are as follows. Twenty-six (26) gallons (98,4 l) 75%aqueous sulfate solution tetrakis(hydroxymethyl)phosphonium diluted with deionized water to a final volume of approximately 380 gallons (1438,4 l). The obtained acidic solution was adjusted to a pH of 7.7 with 40%aqueous potassium hydroxide solution and the volume brought ionizirovannoi water to 390 gallons (1476,3 l). After thorough mixing, add 0,47 lbs (0.21 kg) of ammonium chloride and the mixture was dissolved under vigorous stirring. The pH value was adjusted to 7.7 with a small amount of a 40%aqueous solution of potassium hydroxide. The resulting composition is stored in a almost completely filled closed containers, by choice, in an atmosphere of nitrogen.

Example 2. Compositions containing sulfate, tetrakis(hydroxymethyl)phosphonium (TGFS) and methylamine

5 wt.%-percent composition was prepared according to the method described in example 1: 1) mix of 6.66 g of 75 wt.%-aqueous sulfate solution tetrakis(hydroxymethyl)phosphonium water, the volume of the solution was adjusted to 90 ml, 2) add concentrated (12 M) solution of potassium hydroxide, forming a TRIS (95%conversion) at pH of 7.7, 3) dilute with water to 100 ml, 4) add to 0.263 g of methylamine and 5) mix. The molar ratio of TRIS/amine in the mixture is 2.6:1.

Example 3. Determination of the optimal ratio reagents/iron

This example shows how the relative molar amount of TRIS and source of Amina affect the optimal complexation of iron (II). In this method of analysis as a convenient standard source of iron choose a water-soluble compound of iron (II) sulfate heptahydrate iron (II). TRIS get the General method is ke, described in examples 1 and 2.

The complex formed by the interaction TRIS, ammonia and iron (II), characterized by a maximum absorption in the region of 490 nm. To determine the optimum ratio of reactants measure the absorption of various compositions complexing components. The optimal molar ratio of components (TRIS, ammonia, iron (II)) is 20:8:5.

Similar studies using methylamine showed that forms a complex with maximum absorption at 473 nm, and the optimum molar ratio (TRIS, methylamine, iron(II)) is 26:10:5.

Example 4. Complex formation of insoluble iron sulfide

Sulfide iron (II) precipitated from aqueous solution by mixing soluble compounds of iron (II) and soluble sulfide in equimolar ratio and in sufficient quantity to exceed the magnitude of the solubility of iron sulfide (II). In this example, the combination of 1.65 ml 0,172 M solution of iron sulfate heptahydrate (II) and 1.65 ml 0,172 M solution of nonahydrate of sodium sulfide in solution (final volume of 50.0 ml) leads to the precipitation of 25 mg of iron sulfide (II) black or to the formation of a dispersion containing approximately 500 mg of sulfide iron (II) in 1 l of solution.

A. Complexation of iron sulfide in dispersion

20 ml of 5 wt.%-Noah aqueous composition obtained as described the ANO in example 2, mixed with 25 mg of iron sulfide in water (final volume 50 ml). The calculated ratio of TRIS/methylamine is 26:10. Sulfide iron (II) is dissolved in 22°with an initial speed of approximately 1800 million-1/h (ppm/hr) to about 33 million-1/h to exhaustion song, or iron sulfide. In another embodiment, a 20 ml aqueous compositions obtained as described in example 1, is mixed with a dispersion of iron sulfide. All the iron sulfide is dissolved within 30 min, which is confirmed by the steady increase in the absorbance of a solution at approximately 500 nm.

B. Complexation deposits of iron sulfide on the filter

The variance of the sulphide of iron (II), obtained as described above, filtered through a fabric filter in the vacuum. Fabric with withheld by iron sulfide is placed in 50 ml of 0.1 M citrate buffer solution in water at pH 5 and 20 ml of the composition obtained as described in example 1 and shaken. The residue is completely removed from the fabric in less than 20 h, during which the absorption of the surrounding solution at 500 nm increased.

Example 5. the pH Dependence of the formation of compositions for complexation of iron (II)

This example demonstrates that the compositions and methods of the present invention, in which sulfate is used tetrakis-(hydroxymethyl)phosphonium (TGFS), are pH-dependent.

For each of the second value, presented in the following table, use the original solution containing FeSO4(0,015 M), NH4+(0,030 M), CGFS (0,06 M), and phosphate buffer solution (0.1 M) at 22°C. Source solutions are practically colorless. 0.1 M phosphate buffer solution used to stabilize the pH at which carry out each test.

Table
pHTime (h), which is required to achieve the magnitude of the absorption at 500 nm to 1.0
1,2 (in the absence of buffer solution)The speed is too low for detection
2,68 (in the presence of buffer solution)26
2,82 (in the presence of buffer solution)12,5
2,97 (in the presence of buffer solution)3,5
4,54 (in the presence of buffer solution)0,5
4,96 (in the presence of buffer solution)0,01

The results obtained indicate that the complexation of iron sulfide occurs at a higher rate in the presence of compositions containing TGFS at high pH value. At pH above 5, the rate of complex formation is constantly increasing, and the example is, at pH 7.5 full complexation occurs within a few seconds.

Example 6. The cleaning cycle using scrapers

In this experiment illustrates an example pipeline cleaning, containing deposits of iron sulfide, using the composition and method according to the present invention.

Scraper launch in the pipeline in a pipeline. The trumpet introduce a sufficient amount of the aqueous composition obtained in example 1. The trumpet runs the second scraper to between two scrapers formed the liquid column, which covers the walls of the pipe circumference. Set of two scrapers in motion with a speed of 6 miles per hour, depending on the adjustment of the pressure used to move pigs. The trumpet runs the third scraper with the carrier fluid for additional clean from any residual solids. To determine the need for additional cleaning, you can take samples from the receiver scrapers.

Example 7. The way to clean without the use of scrapers

This method is required if the pipeline is too contaminated sediment iron sulfide or if the pipeline is not equipped with receivers scrapers and node startup scrapers. In this case, the pipeline is required to install the vessels to partition or boot is definitely type. The aqueous composition of the present invention is administered as a continuous flow in the upper portion of the tube toward the deposition of iron sulfide. Record the flow rate and pressure, and, if possible, take samples. Continuous flow of the composition through the pipeline there is the removal of deposits of iron sulfide.

Example 8. Periodic method using scrapers

In the pipeline periodically injected aqueous composition obtained in example 1, by gravity or by using the internal pressure in the pipeline. Then after processing the stream water composition in the pipeline launch scraper for promotion solution along the pipeline. For greatest efficiency, scraper advance with a speed of 6 miles per hour. During the processing of selected samples from the pig receiver to determine the need for additional cleaning scraper. All the used volume of the composition is determined taking into account the length, internal diameter and degree of contamination of pipes, dust, sludge or sediments. Type scraper chosen depending on the degree of contamination of sediments in the pipeline.

Although the present invention is described and illustrated with the preferred embodiment variants of the invention and preferred methods of its use, the invention is not limited is specified by options since modifications and changes of the invention, which is included in the scope of the invention as set out in the accompanying claims.

1. Method of reducing iron sulfide in the pipe, characterized in that the implement contacts the inner surface of the pipe with the first composition obtained by mixing at least one compound of formula (I)

with at least one amine selected from the group including alkylamines followed, diallylamine, alkylenediamine, cyclooctylamine or their conjugates with acids, in the presence of aqueous solvent, where x is the anion with a valency of n, which is chosen from the group comprising bromide, iodide, lower alkylcarboxylic, bisulfite, bisulfate, hydrocarboncontent, dihydrogen phosphate, nitrate, hexaflurophosphate, sulfite, monohydrogenphosphate and phosphate, with the contacts to get the second composition, which is then removed from the pipe.

2. The method according to claim 1, characterized in that the said tube is a pipeline dry gas.

3. The method according to claim 1, characterized in that said pipe is a pipe for the treated liquids.

4. The method according to claim 1, characterized in that said tube continuously served the specified composition.

5. The method according to claim 1, the best of the decomposing those that said tube periodically submit the specified composition.

6. The method according to claim 1, characterized in that the said amine or its conjugate acid selected from the group including bonds alkylamines and their conjugates with acids.

7. The method according to claim 6, characterized in that the said amine is a methylamine.

8. The method according to claim 1, characterized in that the said amine or its conjugate acid selected from the group including methylamine, ethylamine, Propylamine, Isopropylamine, butylamine, tertbutylamine, 1,2-diaminoethane, 1,3-diaminopropane, cyclopropylamine, cyclobutylamine, cyclopentylamine, cyclohexylamine and their conjugates with acids.

9. The method according to claim 1, characterized in that the molar ratio of phosphorus to nitrogen in the above-mentioned Amina or its conjugate acid without taking into account the nitrogen content of the composition X is from about 1:1 to about 15:1.

10. The method according to claim 9, characterized in that the said molar ratio is from about 1.5:1 to about 8:1.

11. The method according to claim 10, characterized in that the said molar ratio is approximately 2.5:1.

12. The method according to claim 1, wherein the said solvent is water or a mixture containing water and alcohol.

13. The method according to item 12, wherein the said alcohol is methanol.

14. The method according to item 12, otlichuy is the, that the said solvent is water.

15. The method according to item 12, characterized in that the pH value of the above-mentioned solvent is from about 4.5 to about 10.

16. The method according to item 15, wherein the pH of the solvent is from about 6 to about 9.

17. The method according to item 16, characterized in that the pH value of the solvent is approximately 8.

18. The method according to claim 1, characterized in that the amount of the aforementioned compounds of formula I is from 1 to 90%, based on the weight of the composition.

19. The method according to p, characterized in that the amount of the compounds of formula I is 5% based on the weight of the composition.

20. The method according to claim 19, characterized in that the amount of the compounds of formula I is 1% per weight of the composition.

21. The method according to claim 1, characterized in that the number mentioned amine or its conjugate acid is from 0.05 to 2.0% based on the weight of the composition.

22. Method of reducing iron sulfide in the pipe, characterized in that exercise contacting the pipe with a composition comprising Tris(hydroxymethyl)phosphine and at least one amine or its conjugate acid, and the solvent, and the resulting second composition is then removed from the pipe.

23. The method according to item 22, wherein said pipe is a t unaproved dry gas.

24. The method according to item 22, wherein said pipe is a pipe for the treated liquids.

25. The method according to item 22, wherein said composition is continuously fed to the pipe.

26. The method according to item 22, wherein said composition is periodically fed to the pipe.

27. The method according to item 22, characterized in that the said amine or its conjugate acid is chosen from the group comprising ammonia, alkylamines followed, diallylamine, alkylenediamine, cyclooctylamine and their conjugates with acids.

28. The method according to item 27, characterized in that the said amine or its conjugate acid is chosen from the group comprising ammonia, alkylamines followed and their conjugates with acids.

29. The method according to p, characterized in that the said amine or its conjugate acid is chosen from the group comprising ammonia, methylamine and ammonium chloride.

30. The method according to p, characterized in that the said amine or its conjugate acid selected from the group including methylamine, ethylamine, Propylamine, Isopropylamine, butylamine, tert-butylamine, 1,2-diaminoethane, 1,3-diaminopropane, cyclopropylamine, cyclobutylamine, cyclopentylamine, cyclohexylamine and their conjugates with acids.

31. The method according to item 22, wherein the molar ratio of Tris(hydroxymethyl)phosphine to the amine or its conjugate acid is priblizitelen is 1:1 to about 15:1.

32. The method according to p, characterized in that the said molar ratio is from about 1.5:1 to about 8:1.

33. The method according to p, characterized in that the said molar ratio is approximately 2.5:1.

34. The method according to item 22, wherein the said solvent is water or a mixture containing water and alcohol.

35. The method according to clause 34, wherein the said alcohol is methanol.

36. The method according to clause 34, wherein the said solvent is water.

37. The method according to clause 34, characterized in that the amount of Tris(hydroxymethyl)phosphine is from 1 to 90%, based on the weight of the composition.

38. The method according to clause 37, wherein the amount of Tris(hydroxymethyl)phosphine is 5% based on the weight of the composition.

39. The method according to 38, characterized in that the amount of Tris(hydroxymethyl)phosphine is 1% per weight of the composition.

40. The method according to item 22, wherein the number mentioned amine or its conjugate acid is from 0.05 to 2.0% based on the weight of the composition.

41. The composition obtained by mixing at least one compound of the formula I

in which X is an anion with a valency of n, with at least one amine selected from the group comprising alkylamine, dialkylamide or their conjugates with acids in the presence of an aqueous solvent.

42. The composition according to paragraph 41, in which X is selected from the group comprising chloride, bromide, iodide, lower alkylcarboxylic, bisulfite, bisulfate, hydrocarboncontent, dihydrogen phosphate, nitrate, hexaflurophosphate, sulfate, sulfite, monohydrogenphosphate and phosphate.

43. The composition according to paragraph 41, in which the said compound of formula I is selected from sulfate, tetrakis(hydroxymethyl)phosphonium chloride tetrakis(hydroxymethyl)phosphonium.

44. The composition according to paragraph 41, in which the mentioned bonds alkylamines selected from the group including methylamine, ethylamine, Propylamine, Isopropylamine, butylamine, tertbutylamine.

45. The composition according to item 44, in which the said alkylamine is methylamine.

46. The composition according to paragraph 41, in which the molar ratio of phosphorus to nitrogen in the above-mentioned Amina or its conjugate acid without taking into account the nitrogen content of the composition X is from about 1:1 to about 15:1.

47. The composition according to item 46, in which the mentioned molar ratio is from about 1.5:1 to about 8:1.

48. The composition according to p, in which the mentioned molar ratio is approximately 2.5:1.

49. The composition according to paragraph 41, in which the said solvent is water or a mixture comprising water and alcohol.

50. The composition according to 49, Kotor is th the said alcohol is methanol.

51. The composition according to 49, in which the solvent is water.

52. The composition according to 49, in which the pH of the solvent is from about 4.5 to about 10.

53. The composition according to 49, in which the pH of the solvent is from about 6 to about 9.

54. The composition according to item 53, in which the pH of the solvent is approximately 8.

55. The composition according to paragraph 41, in which the amount of the aforementioned compounds of formula I is from 1 to 90%, based on the weight of the composition.

56. The composition according to 55, in which the amount of the aforementioned compounds of formula I is 5% based on the weight of the composition.

57. The composition according to p, in which the amount of the aforementioned compounds of formula I is 1% per weight of the composition.

58. The composition according to paragraph 41, in which the number mentioned amine or its conjugate acid is from 0.05 to 2.0%, based on the weight of the compositions.

59. A composition comprising Tris(hydroxymethyl)phosphine, at least one amine selected from the group including alkylamines followed, dialkylamide or their conjugates with acids, and solvent.

60. The composition according to p, in which the mentioned amine or its conjugate acid selected from the group including bonds alkylamines and their conjugates with acids.

61. The composition according to p, in which the mentioned amine or its conjugate acid is ibrani from the group including methylamine, ethylamine, Propylamine, Isopropylamine, butylamine, tertbutylamine and their conjugates with acids.

62. The composition according to p, which mentions alkylamine is a methylamine.

63. The composition according to p, in which the molar ratio of Tris(hydroxymethyl)phosphine to the amine or its conjugate acid is from about 1:1 to about 15:1.

64. The composition according to p, in which the mentioned molar ratio is from about 1.5:1 to about 8:1.

65. The composition according to p, in which the mentioned molar ratio is approximately 2.5:1.

66. The composition according to p, in which the said solvent is water or a mixture containing water and alcohol.

67. The composition according to p, in which the said alcohol is methanol.

68. The composition according to p, in which the said solvent is water.

69. The composition according to p, in which the amount of Tris(hydroxymethyl)phosphine is from 1 to 90%, based on the weight of the composition.

70. The composition according to p, in which the amount of Tris(hydroxymethyl)phosphine is 5% based on the weight of the composition.

71. The composition according to item 70, in which the amount of Tris(hydroxymethyl)phosphine is 1% per weight of the composition.

72. The composition according to p, in which the number mentioned amine or its conjugate acid composition is employed, from 0.05 to 2.0% based on the weight of the composition.



 

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18 cl, 5 ex, 3 tbl

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10 cl, 2 dwg, 2 tbl

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3 cl, 7 dwg, 1 tbl

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46 cl, 1 tbl

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1 tbl, 3 ex

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EFFECT: valuable properties of composition.

1 tbl

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EFFECT: enhanced effectiveness and valuable properties of composition.

1 tbl

Antiscale agent // 2213069
The invention relates to household chemicals, particularly chemicals to remove the inner metal walls of household appliances, including washing machines, dishwashers, steam generators and other scale deposits formed during the heating and boiling of water due to precipitation of the contained salts (caso3, MgCO3, CaSO4)
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