RU2503703C1 - Preparation method of solid inhibitor to prevent asphaltene-resin-paraffin deposits - Google Patents

Abstract

FIELD: oil and gas industry.

SUBSTANCE: invention refers to solid inhibitors to prevent asphaltene-resin-paraffin deposits (ARPD) in wells with a high gas factor and in water-flooded wells that are exposed to ARPD, and in pipelines. In a preparation method of solid inhibitor to prevent ARPD by heating a carrier substance and introducing to it of active base Sevilen - copolymer of ethyleme with vinyl acetate, there used is Sevilen with vinyl acetate content of 21-30 wt %; oil grahamite or construction oil bitumen, or stillage residue of amine C₁₇-C₂₀ production is used as carrier substance; first, Sevilen is cooled to the temperature of - (10°C - 190°C), exposed at that temperature during 10-15 minutes, crushed till powder state, heated to positive temperature, but not higher than 30°C, added in portions of not less than four portions with mixing of each of them during not less than 1 minute to the above carrier substance heated till it is softened at the following component ratio, wt %: the above Sevilen 1-50, and the above carrier substance is the rest. The invention has been developed in dependent claim.

EFFECT: improvement of efficiency at temperature drop, protection of metal, fibreglass, enamelled pipes, and pipes lined with polyethylene; increase of duration of aftereffect and preservation of a property regarding reduction of formation fluid viscosity.

2 cl, 2 ex, 7 tbl

Description

The invention relates to the field of oil production, in particular, to methods for preparing solid inhibitors to prevent asphaltene-tar-paraffin deposits (ARPD), used both in wells with a large gas factor and waterlogged, subject to intense deposition of asphaltene-tar-paraffin substances (ASV), and in pipelines.

One of the conditions for the effective prevention of ARPD is the use of inhibitors with satisfactory technological properties: a solid phase state, optimal solubility when washing with an oil stream, a technologically acceptable method of preparation, and in addition, the components of the inhibitor during preparation and subsequent use should not lose their active properties.

A known method of preparing a solid composition is a granular module that provides the release of the active substance when washing it with well fluid and consisting of a polymeric material and an asphaltene inhibitor (US 2004/0043906, 03/04/2004). The specified method consists in heating the polymer material, mixing it with an inhibitor and in the subsequent production of granules by extrusion or underwater granulation. As a polymeric material, it is recommended to use a number of polymers indicated in the description and in the formula of the indicated US application, for example, selected from the group consisting of polypropylene, polyethylene, high density polyethylene, high density polypropylene, polyethylene terephthalates, polyamides (aliphatic and aromatic), liquid crystal polymers , liquid resins, starch and polyhydroxyalkanoates or mixtures thereof. They all fall under the concept: “A polymer is a high-molecular substance formed by long chains of smaller molecules called monomers. "The molecular weight of polymers can range from several thousand to many millions (atomic units of mass)." (Internet site: Wikipedia). As an inhibitor, it is recommended to use, for example, copolymers.

The main disadvantage of the solid composition obtained by the specified known method is as follows. Given that the predominant area of use of the composition prepared by the known method is the hydraulic fracturing process (hydraulic fracturing), its properties are aimed specifically at retaining sand and use as proppant, therefore, solid polymers that practically do not dissolve are used as a carrier substance in reservoir fluid. Therefore, the use of such a composition, in order to prevent paraffin deposits, will be ineffective, for example, in conditions of low-production wells, as well as wells with low reservoir pressure, because under these conditions, there is a high probability of accumulation of insoluble carrier material in the container (if the prepared composition is delivered to the well in this way) and blocking of its perforations, which can lead to insufficient removal of the asphaltene inhibitor, and therefore to the likelihood of deposits on the downhole equipment and suspensions of tubing (tubing).

Also known are methods of preparing a number of solid formulations (inhibitors) to prevent paraffin, in the first stage of which the carrier substance is melted, in particular, construction oil bitumen (Patents of the Russian Federation No. 2259470, 2132451, 2267006) or, in particular, still residue from the production of primary amines C ₁₇ -C ₂₀ (Patents of the Russian Federation No. 2131969, 2346021, 2244805, Auth. Certificate of the USSR No. 1543052), and at the next stage, the active base is introduced into the molten carrier substance in the form of various additives.

These solid inhibitors, obtained by known methods, work well in wells at various water cuttings, pressure and temperature.

However, the disadvantages of these compositions include the lack of effectiveness in preventing paraffin deposits in both wells and pipelines with temperature differences in different areas. This is especially true for the winter period of time, as well as in violation of the thermal regime of downhole and pipe heaters, for example, due to a malfunction of the control station, an emergency, the presence of sections of main pipelines that are difficult to heat, etc.

In addition, there are a number of limitations in the range of application of these formulations, expressed in the temperature limit of their use since the compositions have a sufficiently low temperature of the onset of softening of the carrier substance and, accordingly, the rapid removal of the active substance.

Compositions for preventing paraffin inhibitors are also known from the state of the art and contain ethylene vinyl acetate copolymer in their formulation as active substance (RF Patent No. 2009141773, 2007103128, 2006137724, Auth. Certificate of the USSR No. 1798356). A method of preparing known formulations consists in the traditional mixing of components.

The disadvantage of these compositions obtained in a known manner is the lack of effectiveness of preventing paraffin.

Closest to the proposed invention is a method of preparing a composition for preventing ASPO (Auth. Certificate of the USSR No. 1369253), by mixing the components: Sevilen - a copolymer of ethylene with vinyl acetate, with a content of vinyl acetate units of 35-38 wt.%, With hydroxyalkylated alkyl phenolamine formaldehyde resin, in the following ratio of components, wt.%: the specified copolymer is 30-70; the specified resin is the rest.

However, the solid composition obtained by the proposed method has several disadvantages, namely:

- insufficient effectiveness to prevent paraffin in case of temperature difference;

- insufficient protective effect against metal pipes, fiberglass, enameled and lined with polyethylene;

- insufficient duration of the aftereffect.

All this reduces the efficiency of using the composition prepared in a known manner, in the field.

The technical result achieved by the invention is to obtain a solid inhibitor that provides high efficiency for the prevention of paraffin in case of temperature difference; high protective effect against metal pipes, fiberglass, enameled and lined with polyethylene; increasing the duration of its aftereffect and at the same time maintaining the property of reducing the viscosity of the reservoir fluid.

The specified technical result is achieved by the proposed method of preparing a solid inhibitor to prevent asphaltene-tar-paraffin deposits by heating the carrier substance and introducing the active Sevilen base - an ethylene-vinyl acetate copolymer into it, while the new one is that Sevilen is used with a vinyl acetate content of 21-30 wt.%, and as carrier material - bitumen brittle, bitumen or building, or the production of amines bottoms C ₁₇ -C _20, pre-cooled to the Sevilen Temperature from minus 10 ° C to minus 190 ° C, kept at the indicated temperature for 10-15 minutes, crushed to a powdery state, heated to a positive temperature, but not higher than 30 ° C, injected in portions of at least four with stirring each at least 1 minute in the specified carrier substance, heated to softening, in the following ratio of components, in wt.%:

specified Savilen 1-50 the specified carrier substance rest

After introducing Sevilen into the carrier material, a blowing agent, azodicarbonamide, is added to the mixture in an amount of up to 8 wt.% To the weight of the mixture.

The achievement of the above technical result is achieved due to the special sequence of methods for introducing the components in the preparation of the solid inhibitor and the processing regimes of these components, as well as due to the joint interaction of the components included in the resulting solid inhibitor.

Due to the fact that Savilen is cooled to a temperature in the range from minus 10 ° C to minus 190 ° C, an intramolecular increase in stresses apparently occurs, as a result of which a partial change in the molecular structure of the copolymer occurs with the emergence of a structural, and possibly partially internal physical chemical modification. Subsequent exposure of Sevilen at the indicated low temperature for 10-15 minutes, apparently, contributes to the consolidation of this process, as a result of which a solid inhibitor prepared using these modes will provide high efficiency for the prevention of ARPD with temperature changes, because . when the supramolecular structure of the copolymer changes at the indicated minus temperature, it is possible that a combination of different molecular structures has formed, each of which will provide high efficiency for preventing ARPD at “its” temperature.

The same changes, in our opinion, explain the effect of increasing the duration of the aftereffect of the prepared solid inhibitor, apparently due to an increase in the adsorption properties in various pipes. Sevilen itself has good adhesive properties, but it was unexpectedly found that upon cooling it provides reinforcement of these properties, and is universal for various types of pipes.

The inner surface of pipelines lined with polyethylene, or enamel, or fiberglass is characterized mainly by hydrophobic properties. AFS deposited on the walls of pipes are of an organic nature, i.e. the probability of their deposition on the surface of the above pipes is quite high. Moreover, their crystallization centers initiate additional deposits. The mechanism of influence of the solid inhibitor prepared by the proposed method is to prevent such deposits. This, in our opinion, is ensured by the formation of complex complex compounds during the dissolution of the inhibitor, which block the access of asphaltene-tar-paraffin substances (ASPV) to the surface of pipelines. Brittle petroleum bitumen, construction bitumen and bottoms from the production of C ₁₇ -C ₂₀ amines, apparently, are not only a carrier substance, which, due to its limited dissolution in the formation fluids, releases the processed active base in a certain way, but also participates with it in the formation of branched structures that impede the formation of crystallization centers ASW.

Due to the fact that Savilen, after cooling and holding at the claimed low temperature, is subjected to grinding to a powder state, a long uniform supply of this active substance from the prepared solid inhibitor to the formation fluid is ensured, because apparently, this is how the prepared active base will have optimal “adhesion” to the carrier substance, as well as to the protected surface of the pipes, which increases the aftereffect.

The heating of the carrier substance to a state of softening is necessary for uniform subsequent mixing with Savilen. In an advantageous embodiment, it is preferable to introduce Sevilen into the carrier substance in small portions (at least four), mixing each portion for at least 1 minute. This, in our opinion, will provide not only mechanical mixing of the components, but also ensure the creation of physicochemical bonds between the molecules, due to which the removal time of the optimal amount of the active base will be increased.

Heating to a positive temperature, but not higher than + 30 ° C, of a powdered active base is necessary, firstly, for the purpose of good mixing with the carrier substance and the elimination of its solidification, and secondly, for the ordering of Savilen molecules and stress relief in them, which will ensure the uniformity of the properties acquired at sub-zero temperatures in the entire mass of the solid inhibitor. Heating above + 30 ° C is impractical, because in this case, particles of powdered Savilen will stick together and the subsequent uniform distribution of its particles in the volume of the carrier substance will be impossible, and in addition, as a result of this, a certain decrease in the protective properties of the inhibitor will occur (table 4 experiment 10).

Experimental data showed that all of the above properties of a solid inhibitor prepared according to the proposed method can be ensured only when Sevilen is used as an active base with a vinyl acetate content of 21-30 wt.%.

It is known from the prior art that previously, for the preparation of solid paraffin inhibitors, two carrier substances were used: bottoms from the production of amines C ₁₇ -C ₂₀ and construction bitumen. These carrier materials provide a limited dosage and unstable dissolution in the produced formation fluids (oil and water), as a result of which the active base is released (self-dosage).

Thus, only due to the special order of input of the components at their stated ratio, as well as due to the applied modes, is it possible to obtain a solid paraffin inhibitor with the required properties.

The specified solid inhibitor to prevent paraffin, prepared by the proposed method, after mixing the components and cooling the mixture, is subsequently formed in the form of cylinders, balls, granules or formations of any other shape. Next, the solid inhibitor is placed in a container, which is a system of perforated pipes of various diameters. Then the obtained tubular container with the inhibitor placed in it is lowered either into the perforation zone of the producing well, or under the pump, or placed in the main pipelines.

Formation fluids passing through holes on the side walls and at the end of the container wash the inhibitor. Due to the gradual dissolution, its constant, necessary, effective and sufficient concentration in the produced fluids is achieved.

The addition of a blowing agent, azodicarbonamide, to the inhibitor provides the porous structure of the inhibitor, which means it can increase the washing area, and at the same consumption of materials it fills the internal space of the container sections as much as possible.

To obtain a solid inhibitor of the present method in laboratory conditions, the following substances were used:

- bottoms production residues of amines C ₁₇ -C ₂₀ according to TU 6-02-750-87, production waste obtained by vacuum distillation of a technical mixture of aliphatic amines C ₁₇ -C ₂₀ , the total mass fraction of primary and secondary amines in the still residue is not less 56%, including primary - not less than 22%, hydrocarbon content not more than 10%; solid brown waxy mass with a pungent unpleasant odor, sparingly soluble in water, soluble in alcohol, chloroform, melting point 63-78 ° C;

- brittle petroleum bitumen according to GOST 21822-87, obtained by oxidation of heavy residues of atmospheric vacuum distillation of highly resinous low-paraffin oils and is used in paint and varnish, tire, electrical and other industries;

- building oil bitumen in accordance with GOST 6617-76 is obtained by oxidizing residual products of direct distillation of oil and their mixtures with asphalts and extracts of oil production or by compounding the oxidized and non-oxidized above products;

- Savilen - TU 6-05-1636-97, a copolymer of ethylene with vinyl acetate - is a high molecular weight compound related to polyolefins, produced in the form of granules 2-5 mm. The properties of Sevilen depend mainly on the content of vinyl acetate (5-30 wt.%). With increasing vinyl acetate content, hardness, heat resistance, crystallinity (tensile stress) decrease, while density, elasticity, transparency and adhesion increase; various brands of Savilen are produced, for example, brands 11808-340 and 12508-150 contain 26-30% of the mass fraction of vinyl acetate; grade 11507-070 contains 21-24% of the mass fraction of vinyl acetate; grade 11908-125 contains 24-26% of the mass fraction of vinyl acetate, etc .;

- blowing agent - azodicarbonamide H ₂ NC (O) N = NC (O) NH ₂ , odorless yellow-orange crystalline substance. Insoluble in most organic solvents, but soluble in N, N-dimethylformamide and dimethyl sulfoxide. The solubility in water at 20 ° C is negligible, less than 50 mg / L. In hot water, the solubility is slightly higher. It has a very low vapor pressure - 2.53 * 10 ^-11 kPa at 20 ° C. Thermally unstable. When heated, decomposes with the release of molecular nitrogen and a small amount of ammonia. Imported, CAS No: 123-77-3, Porofor trademark: gas number more than 220 ml / g; decomposition temperature over 200 ° C; the content of the basic substance is not less than 99%; ash content, less than 0.1%; loss upon heating, not more than 0.15%; fine-grained (through a sieve of 38 microns), not more than 0.1%. Porofor (Azodicarbonamide) is an effective blowing agent and is used as a blowing agent (blowing agent) in the processing of polymers, extrusion and rotational molding,

The possibility of carrying out the claimed invention is confirmed by the following examples.

Example 1. To obtain a solid inhibitor, the proposed method took 40 g of Sevilen grade 11808-340 (vinyl acetate content of 26-30 wt.%), Placed in a cuvette and with the help of liquefied nitrogen was cooled to a temperature of minus 120 ° C. Maintained at this temperature for 10 minutes. Grind the indicated Sevilen to a powder state (for example, to a dispersion of 60-80 microns). He was heated to + 20 ° C (approximately to room temperature) and introduced portionwise in four doses, mixing each portion for 1-2 minutes, in 60 g of bitumen oil brittle grade G, heated to a softening temperature of + 140 ° C, and brought to a uniform viscous mass. Then, after cooling to ambient temperature, a solid inhibitor of the following composition was obtained, wt.%: Sevilen with a vinyl acetate content of 26-30 wt.% - 40; brittle oil bitumen - 60.

Example 2. To obtain a solid inhibitor, the proposed method took 20 g of Sevilen grade 11507-070 (content of vinyl acetate 21-24 wt.%), Placed in a cuvette and using liquefied nitrogen was cooled to a temperature of minus 150 ° C. Maintained at this temperature for 15 minutes. Next, said Savilen was ground to a powder state (for example, to a dispersion of 70-90 μm). He was heated to + 25 ° C and introduced into 80 g of bottoms from the production of amines C ₁₇ -C ₂₀ , previously heated to a softening temperature of + 70 ° C, and brought to a homogeneous viscous mass. Then, after cooling to ambient temperature, a solid inhibitor of the following composition was obtained, wt.%: Sevilen with a vinyl acetate content of 21-24 wt.% - 20; VAT residues of the production of amines C ₁₇ -C ₂₀ - 80.

In a similar manner, other inhibitor compositions were prepared with a different ratio of components.

It is possible to introduce, with stirring, into the resulting mixture of Sevilen and the carrier substance (until it thickens) a blowing agent, azodicarbonamide, in an amount up to 8 wt.% To the weight of the mixture.

Then, the inhibitor obtained by the claimed method is formed in the form of balls or cylinders, which, when used for commercial purposes, are laid in perforated containers installed in a well or in a pipeline.

In the course of laboratory tests, the following properties of a solid inhibitor prepared by the claimed method were determined: the protective effect of the prepared inhibitor to prevent paraffin deposits; protective properties in relation to metal, polyethylene, fiberglass, enamel; aftereffect; protective effect in case of temperature difference.

When testing used the following oil and paraffin (table 1).

The protective effect of a solid inhibitor for the prevention of paraffin, prepared by the proposed method, was established according to the generally accepted "Methodology for assessing the effectiveness of inhibitors of paraffin deposits of complex and multiphase effect on washing a film of oil, dispersing and washing paraffin deposits with formation water". NPO Soyuzneftepromkhim - Kazan, 1987. According to this methodology, the effectiveness of a solid inhibitor prepared by the claimed method for preventing ARPD was evaluated by the following indicators: by washing the oil film with this inhibitor; the dispersion of paraffin particles in the inhibitor medium; according to the characteristics of dispersion properties (sticking, coating, general washing of paraffin deposits from the surface).

Data on the component composition of the investigated solid inhibitor prepared by the proposed and known methods are shown in table 2.

Data on the effectiveness of the prevention of paraffin solid inhibitors prepared by known and proposed methods are shown in table 3.

From the data given in table 3, it follows that the solid inhibitor prepared by the claimed method, in terms of the effectiveness of preventing paraffin, exceeds the prototype (experiment 13), as well as a solid inhibitor prepared without a cooling regime (experiment 11).

Also, in the process of laboratory testing, the effectiveness of the inhibition of paraffin inhibitors by the proposed inhibitor and prototype on the above oils by the "cold rod" method was checked.

The essence of the method is as follows: 400 cm ^{3 of} asphalt-resin-paraffin-containing oil are poured into two glasses and heated to 70 ° C. After melting the paraffins contained in the oil, a test inhibitor of a certain formulation is added to the net box in one of the beakers. The contents of the glasses are thoroughly mixed, kept for 2 hours to dissolve the active base, and after lowering the temperature in them to 65 ° C, the previously weighed cold rod is lowered into the glasses. Then, water with a temperature of + 10 ° C is passed through the indicated rod for 30 minutes. After that, the rods are removed from the glasses and weighed after 10-15 minutes. By the weight gain of the rods, they find the mass of paraffin deposits deposited on them.

The effectiveness of inhibitors is calculated by the formula

where, and ₀ is the mass of deposits on the rod immersed in the original oil, g;

a is the mass of deposits on the rod immersed in the original oil with the tested inhibitor.

The data obtained during these tests are shown in table 4.

The data shown in table 4 show that the solid inhibitor prepared by the proposed method has a higher protective effect (experiments 1, 4, 5). A inhibitor prepared with Sevilen having a vinyl acetate content of 15-20% (experiment 14) (i.e. less than stated), as well as an inhibitor without the required exposure time at a low temperature (experiments 8, 9), and an inhibitor in the preparation of which carried out heating of Sevilen after cooling above + 30 ° C (experiment 10), have a protective effect at the prototype level (experiment 13).

In addition, by the same method, the protective effect of an inhibitor prepared by various methods was established with respect to pipes lined with polyethylene, fiberglass pipes and coated with enamel. The data are shown in table 5.

The data shown in table 5 show that the solid inhibitors prepared by the proposed method (experiments 5, 6) are characterized by high inhibitory properties in relation to all studied types of pipes, while the prototype (experiment 13) has protective properties to prevent AFS by 15 -18% lower.

In addition, in the course of laboratory studies, it was established whether temperature differences affect the protective effect of inhibitors from ASW deposits. For this, the temperature of the cold rod was changed twice, namely: + 20 ° C - + 5 ° C - + 10 ° C, and the protective effect was determined at these temperature differences. The data are shown in table 6.

The data shown in table 6 show that the inhibitor prepared by the proposed method (experiments 3,4,7) practically does not change its high protective properties to prevent paraffin deposits at a temperature difference, therefore, it will provide effective protection of pipelines in all areas: as heated, and unheated, which will increase the inter-treatment period of wells and pipelines.

The aftereffect is an important technological characteristic of inhibitors for oil and gas production, showing how long the protection remains after the supply of the inhibitor to the system is stopped. The aftereffect was determined by the time during which protection is maintained at a fairly acceptable level.

For these tests, the prepared solid inhibitor was introduced into the oil in a mesh container and kept for 2 days at a temperature of + 60 ° C. After that, samples of steel (plates) were placed in this oil and kept in it for 2 days. Then this sample with an inhibitor adsorbed on its surface was taken out of oil and placed in a background oil solution (i.e., without an inhibitor) and the presence of paraffin on its surface was visually monitored at regular intervals. The data are shown in table 7.

The data shown in table 7 show that the effect of the aftereffect of an inhibitor prepared by the proposed method (experiments 2, 5, 6) is approximately 1.5 times greater than that of inhibitors prepared by other methods. This property will allow in commercial conditions to increase the overhaul period and increase the inhibitory effect of the composition over time.

In addition, the presence of this property in the inhibitor prepared by the proposed method was proved by experience in the well of the Kolotovskoye field of OAO Saratovneftegaz. By production necessity, a container filled with a solid inhibitor (composition No. 5 of Table 2) was removed from the indicated well, which stood there for 180 days. And the well was put back into operation. She worked another three weeks already without a container. And in the process of subsequent repair of this well, minor deposits of ASWA were established, which also proves the fact of the aftereffect of the inhibitor (works due to its adsorption on the walls of the tubing), prepared by the present method.

It was established experimentally that a solid inhibitor prepared by the proposed method, along with the above properties, ensures the preservation of the property to reduce the viscosity of oil inherent in Savilen.

Thus, according to the results of laboratory studies, it follows that a solid inhibitor prepared by the proposed method will have the following advantages over known solid inhibitors:

- provides a high protective effect (almost stable) even with a temperature difference;

- provides a high protective effect to prevent deposits ASPA in relation to metal pipes, fiberglass, enameled and lined with polyethylene;

- provides a sufficient duration of its aftereffect and at the same time retains properties to reduce the viscosity of the reservoir fluid.

Thus, a solid inhibitor prepared by the proposed method should ensure uniform removal of the active substance for at least 180 days when operating in a well with a productivity of 10-100 cubic meters / day, with a water cut of 5 to 90%, and the temperature of the produced fluid 20- 100 degrees and pressure up to 25 MPa.

Table 1 Composition of oil and paraffin deposits used during testing No. p / p Field Density Oil content Content in AFS (deposit) oil, kg / cm ³ Asphaltenes,% Resin% Paraffins,% Asphaltenes,% Resin% Paraffins,% one. Gozhansky (Verey) 862 2.45 10.0 6.36 7.72 11.96 28.38 2. Konstantanovskoe (Bashkir) 812 0.32 4.26 5.64 2,37 8.44 20.68

table 2 No. of experience Components of a solid inhibitor, wt.% (prepared by the proposed method) The amount of Savilen / cooling temperature, ° C / exposure time chilled, min COPA Bitumen Foaming agent azodicarbonamide to the mass of a mixture of Sevilen and a carrier substance, wt.% one 5 / -120 ° C / 10 95 - - 2 2 / -100 ° C / 15 - 98 - 3 25 / -30 ° C / 12 75 - 3 four 20 / -170 ° C / 10 - 80 - 5 50 / -190 ° C / 12 fifty - - 6 45 / -75 ° C / 15 - 55 8 7 40 / -10 ° C / 10 60 - - 8 40 / -50 ° C / 5 - 60 - 9 40 / -50 ° C / 20 60 - - 10 45 / -75 ° C / 15 - 55 7 eleven 30 / -170 ° C / 10 - 70 - 12 20 (without cooling) - 80 - 13 50 (without cooling) fifty - 5 14 prototype fifty Octophor N (TU 38.101589) - 50 - fifteen 40 / -40 ° C / 10 60 - - Note: 1. In experiments 3, 5 and 9 used Sevilen brand 11507-070 with a vinyl acetate content of 21-24%; in experiments 1,2, 4, 6-8, 10-14 - Sevilen brand 11808-340 with a vinyl acetate content of 26-30%; in experiment 15 - Savilen brand 12306-020 with a vinyl acetate content of 15-20%. 2. KOPA - bottoms from the production of amines C ₁₇ -C ₂₀ . 3. In experiments 2, 6 and 11 used brittle petroleum bitumen grade G; in experiments 4, 8, 10, 12 - bitumen oil construction grade BN 70/30. 4. In experiments 1-3 were introduced into the carrier substance Sevilen, heated to a temperature of + 30 ° C; in experiments 4-9, 11 - heated to a temperature of + 20 ° C; in experiment 10 - to a temperature of + 40 ° C. 5. Octophor N - alkyl phenolamine resin, is a product of polycondensation of alkyl phenols with urotropine; manufactured by Stroyindustriya Plus LLC (Samara). 6. In experiments 1-5, the dispersion of the powder was 60-80 microns; in experiments 6-10 - 30-60 microns; in other experiments, 70-90 microns.

Table 3 No. of experience from table 2 AFS Prevention Effectiveness Oil film washing, sec /% The dispersion of particles of paraffin, mm /% Sticking,% Putting,% Total flask washing from paraffin,% Oil Gozhansky field, Vereysky deposit. one 100/180 sat. 0.1-5 sat. 5 ex. 5 ex. 90 choir. 2 70/60 choir. > 5 unsuccessful. 0 exc. To 5 exc. 95 choir. 3 60/180 unsuccessful 0.1-5 sat. 0 ex 2 ex. 98 choir. four 70/60 choir. > 5 unsuccessful. 10 choir. 5 ex. 85 choir. 5 70/60 choir. > 5 unsuccessful. 5 ex. 5 ex. 90 choir. 6 70/180 satisfied 0.1-5 sat. 0 ex 5 ex. 95 choir. eleven 60/120 sat. 0.1-5 sat. 5 ex. 3 ex. 98 choir. 13 30/180 > 5 unsuccessful. 20 sat. 20 choir. 60 sat. fifteen 30/180 > 5 fifteen 10 75 Oil Konstantinovskoe, B _w one 70/60 choir. 0.1-5 sat. 4 ex. 5 ex. 91 choir. 2 90/180 sat. 0.1-5 sat. 5 ex. 5 ex. 90 choir. 3 70/60 choir. 0.1-5 sat. 10 choir. 5 ex. 85 choir. four 70/60 choir. > 5 unsuccessful. 5 ex. 2 ex. 93 choir. 5 70/180 sat. > 5 unsuccessful. 2 ex. 10 choir. 88 choir. 7 70/180 sat. 0.1-5 sat. 0 exc. 3 ex. 97 choir. 12 40/180 unsuccessful > 5 unsuccessful. 20 sat. 20 choir. 60 sat. fourteen 50/180 > 5 fifteen 10 75

Table 4 No. of experience from table 2 one four 5 8 9 10 fifteen fourteen Protective effect,% 80 83 90 69 71 70 65 70

Table 5 No. of experience from table 2 The effectiveness of the prevention of paraffin on various surfaces,% Lining with polyethylene Fiberglass Enamel 5 82 85 80 6 81 86 79 fourteen 69 71 70

Table 6 No. of experience from table 2 3 four 7 fourteen Protective effect% at temperature difference + 20 / + 5 / + 10 ° C 83 / 80/82 90/88/89 85/83/87 71/60/69

Table 7 No. of experience from table 2 2 5 6 12 fourteen Subsequent characteristic: Visual inspection time, day / presence or absence of deposits, after this time 1 day / no 1 day / no 1 day / no 1 day / no 1 day / no 2 days / no 2 days / no 2 days / no 2 days / no 2 days / no 7 days / no 7 days / no 7 days / no 7 days / film. 7 days / film. 10 days / no 10 days / no 10 days / no 10 days / deposits 10 days / deposits

Claims (2)

1. A method of preparing a solid inhibitor to prevent asphaltene-tar-paraffin deposits by heating a carrier substance and introducing into it an active Sevilen base - an ethylene-vinyl acetate copolymer, characterized in that Sevilen is used with a vinyl acetate content of 21-30 wt.%, And as a carrier substance - bitumen or bitumen fragile construction or resid producing amine C ₁₇ -C ₂₀ Sevilen pre-cooled to minus 10 ° C to minus 190 ° C, kept at this evap re 10-15 min, crushed to a powder state, heated to a positive temperature, but not higher than 30 ° C, injected in portions of at least four with stirring each for at least 1 min in the specified carrier substance, heated to softening in the following ratio of components, wt .%:
specified Savilen 1-50 the specified carrier substance rest 2. The method of preparation of the solid inhibitor according to claim 1, characterized in that after introducing Sevilen into the carrier material, a blowing agent, azodicarbonamide, is added to the mixture in an amount of up to 8 wt.% To the weight of the mixture.