WO2018090944A1 - Émulsion stable d'abaisseur de point d'écoulement réduisant la viscosité de l'ordre du nanomètre, son procédé de préparation et son utilisation - Google Patents

Émulsion stable d'abaisseur de point d'écoulement réduisant la viscosité de l'ordre du nanomètre, son procédé de préparation et son utilisation Download PDF

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Publication number
WO2018090944A1
WO2018090944A1 PCT/CN2017/111267 CN2017111267W WO2018090944A1 WO 2018090944 A1 WO2018090944 A1 WO 2018090944A1 CN 2017111267 W CN2017111267 W CN 2017111267W WO 2018090944 A1 WO2018090944 A1 WO 2018090944A1
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pour point
point depressant
component
weight
nano
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Chinese (zh)
Inventor
阳明书
丁艳芬
王峰
陈娟
高冲
张世民
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Institute of Chemistry CAS
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Institute of Chemistry CAS
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
    • C09K8/588—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/52—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
    • C09K8/524—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning organic depositions, e.g. paraffins or asphaltenes
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17D—PIPE-LINE SYSTEMS; PIPE-LINES
    • F17D1/00—Pipe-line systems
    • F17D1/08—Pipe-line systems for liquids or viscous products
    • F17D1/16—Facilitating the conveyance of liquids or effecting the conveyance of viscous products by modification of their viscosity

Definitions

  • the invention relates to the technical field of pipeline transportation of organic chemistry, petroleum industry, oil recovery and crude oil, and particularly relates to a nanometer viscosity reducing pour point stabilizer emulsion for crude oil, a preparation method thereof and use thereof.
  • Crude oil is a complex mixture of paraffin, colloid, asphaltene, aromatic hydrocarbons and light hydrocarbons.
  • the paraffin component is the main factor affecting the fluidity of waxy crude oil.
  • paraffin is dissolved in liquid crude oil and has good fluidity.
  • the wax gradually crystallizes out, and the wax crystals form a three-dimensional network structure by cross-linking.
  • the crude oil gels and loses fluidity.
  • the exploitation and transportation of oil brings great difficulties. Traditionally, such crude oil has been transported station by station, but this method has large equipment investment, high fuel and power consumption, large environmental pollution, and the danger of “condensation pipe” in the pipeline, which is difficult to achieve efficient and safe transportation. purpose.
  • Adding a chemical pour point depressant to crude oil is the easiest and most effective way to achieve low temperature or normal temperature transport of crude oil.
  • a good chemical pour point depressant not only reduces the freezing point of the crude oil, but also reduces the viscosity of the crude oil.
  • the basic mechanism of pour point depressing is to change the wax crystal morphology precipitated by paraffin wax during the cooling process of crude oil, inhibit the formation of three-dimensional network structure of wax crystal in crude oil, produce the effect of depressing and viscosity reduction, and improve the low temperature fluidity of crude oil to achieve waxy
  • the purpose of crude oil transport at low temperature or normal temperature The pour point depressant achieves the purpose of pour point reduction through nucleation, eutectic and adsorption.
  • CN201110004024.0 discloses a crude oil viscosity reducing pour point depressant composition and a preparation method and application thereof, and the nano pour point depressant particles are mainly prepared by using an ethylene-vinyl acetate copolymer and an organic modified clay.
  • CN200910243238.6 discloses a crude oil viscosity reducing pour point depressant composition which is composed of clay, organic pour point depressant and dispersion medium, and the weight ratio of clay to organic pour point depressant is 1:0 to 1:5, and the dispersion medium accounts for 1% to 99% of the total weight ratio.
  • pour point depressant composition there are the following problems: (1) Some pour point depressant compositions are mixtures of different copolymers, which have different solubility in an organic solvent or a mixed solvent, and may not completely dissolve. Phenomenon After the pour point depressant composition solution is stored for a period of time, the phase separation occurs, and the stability is poor. Therefore, it is difficult to obtain a commercially stable solution; (2) the concentration of the polymer pour point depressant used at normal temperature is lower than 5 wt% due to the solubility problem. If the concentration is increased, the viscosity of the pour point depressant solution will increase, which will bring difficulties to the on-site application of the pour point depressant. (3) The pour point depressant solution has a high freezing point and should not be used in areas with low temperature.
  • pour point depressant In the engineering to solve the above-mentioned pour point depressant defects, generally can add a stirring device in the pour point depressant solution storage tank to solve the phase separation problem of the pour point depressant solution, or to heat the storage tank to avoid coagulation solution coagulation;
  • the component pour point depressant uses a plurality of injection lines to inject the pour point depressant; in these solutions, equipment and energy consumption must be increased, which causes difficulties in production management and leads to increased costs. But for crude oil offshore platforms, adding equipment is very difficult.
  • the object of the present invention is to provide a nano-viscosity-lowering pour point depressant emulsion with better depressing and viscosity-reducing effect, which can stably store for a long time, has a low freezing point and a high concentration of a pour point depressant, in particular It is suitable for the use of crude oil in low temperature environment, and it does not need additional equipment when it is used. It is economical and practical and easy to promote.
  • the present invention provides a nano viscosity reducing pour point depressant emulsion comprising the following components:
  • nano viscosity reducing pour point depressant composition comprises the following components: (i) an organic polymer a pour point depressant, and (ii) an inorganic nano pour point depressant;
  • the nano-viscosity reducing pour point depressant masterbatch for the crude oil is from the above-described nano-viscosity depressant composition, optionally a coupling agent, and optionally high a solid particle prepared by melt blending a molecular processing aid;
  • the emulsion further comprises (d) at least one surfactant comprising a cationic surfactant and/or an anionic surfactant and/or a nonionic surfactant and/or a parent Ionic surfactant.
  • At least one emulsion stabilizer is also included in the emulsion.
  • the emulsion further comprises (f) water and/or at least one water-miscible organic solvent which is the same as or different from component (c).
  • the nano-visbreaking pour point depressant composition further comprises a component (iii) graft polymer.
  • the emulsion comprises at least:
  • component (f) 0-100 parts by weight of water and/or at least one water-miscible organic solvent which is the same as or different from component (c).
  • the emulsion is present in a stable form. Specifically, the emulsion is stored at 0-60 ° C for at least 7 days without phase separation.
  • the (i) organic polymeric pour point depressant is selected from the group consisting of ethylene-vinyl acetate copolymer, ethylene-acrylate copolymer, ethylene-vinyl acetate-acrylate terpolymer, ethylene-vinyl acetate-polyether.
  • One or any combination of acrylate terpolymers One or any combination of acrylate terpolymers.
  • the (ii) inorganic nano-pour point depressant is selected from one or any combination of unmodified or surface-modified materials: silica, titania, calcium carbonate, talc, smectite Stone clay and so on.
  • the (iii) graft polymer is selected from the group consisting of maleic anhydride grafted ethylene-vinyl acetate copolymer, maleic anhydride grafted polystyrene, maleic anhydride grafted ethylene-octene copolymer, and Yikang.
  • the graft polymer accounts for from 0 to 60% by weight, preferably from 1 to 55% by weight, and more preferably 5, based on the weight of the organic polymer pour point depressant and the graft polymer. ⁇ 50% by weight, more preferably 10% to 35% by weight.
  • the mass ratio of the inorganic nano-pour point depressant to the organic polymer pour point depressant is 1:0.05 to 0.05:1, preferably 1: 0.1 to 0.1:1.
  • the coupling agent accounts for 0 to 3% by weight based on the total weight of the mother particles
  • the polymer processing aid accounts for 0 to 10% by weight based on the total weight of the mother particles.
  • the coupling agent is a silane coupling agent, a titanate coupling agent or a combination thereof.
  • the invention further provides a method for preparing the above-mentioned nano viscosity reducing pour point depressant emulsion, the method comprising the following steps:
  • Step 1 Prepare one of solution A or solution B to prepare dispersion A;
  • the preparation solution A comprises: mixing with component (b) and (i) an organic polymeric pour point depressant to prepare solution A; said component (b) is an organic solvent immiscible with water or a mixture thereof;
  • Formulating the dispersion A comprises: mixing with the component (c) and (ii) an inorganic nano pour point depressant to prepare a dispersion A;
  • Component (c) is a water-soluble organic solvent or a mixture thereof;
  • the preparation solution B comprises: mixing the component (b) with the above-mentioned crude oil with a nano viscosity reducing pour point depressant master batch to prepare a solution B;
  • the component (b) is an organic solvent which is immiscible with water or a mixture thereof;
  • Step 2 mixing solution A and dispersion A, or mixing solution B and dispersion A, or mixing solution B and component (c), said component (c) being a water-soluble organic solvent or a mixture thereof;
  • the nano-viscosity depressant emulsion of the present invention is obtained.
  • the method further comprises:
  • Step 3 Dispersing component (d) in component (f) to obtain a surfactant solution;
  • component (d) is at least one surfactant, and the surfactant includes a cationic surfactant and Or an anionic surfactant and / or a nonionic surfactant and / or an amphiphilic surfactant;
  • said component (f) is water and / or at least one of the same or different from component (c) Water-miscible organic solvent;
  • Step 4 mixing the solution A of the step 1, the dispersion A of the step 1 with the surfactant solution of the step 3, or mixing the solution B of the step 1 and the component (c) with the surfactant solution of the step 3, or The solution B of the step 1 and the dispersion A of the step 1 are mixed with the surfactant solution of the step 3 to obtain the nano-viscosity-lowering pour point depressant emulsion of the present invention.
  • the step 4 is further preferably: mixing the solution A of the step 1, the dispersion A of the step 1 with the surfactant solution of the step 3, or the solution B, the component (c) of the step 1 and the step Mixing the surfactant solution of 3, or mixing solution B of step 1, the dispersion A of step 1 with the surfactant solution of step 3; then adding component (e), optionally further adding component (f) Obtaining the nano pour point depressant emulsion of the invention; wherein component (e) is an emulsion stabilizer, component (f) is water and/or at least one water-miscible with the same or different component (c) Organic solvents.
  • the formulation solution A is further preferably prepared by mixing the component (b) and (i) an organic polymeric pour point depressant and (iii) a graft polymer to prepare a solution A.
  • the preparation solution A 10 to 70 parts by weight of the (i) organic polymeric pour point depressant is dissolved in 10 to 60 parts by weight of the component (b) to obtain a solution A.
  • the preparation solution A 10 to 70 parts by weight of (i) an organic polymeric pour point depressant and (iii) a graft polymer are dissolved in 10 to 60 parts by weight of the component (b) to obtain a solution.
  • the graft polymer accounts for from 0 to 60% by weight, preferably from 1 to 55% by weight, and more preferably from 5 to 5% by weight based on the weight of the organic polymeric pour point depressant and the graft polymer. 50% by weight, more preferably 10 to 35% by weight.
  • dispersion A 5 to 70 parts by weight of (ii) an inorganic nano pour point depressant is dispersed in 5 to 60 parts of the component (c) to obtain a dispersion A.
  • the preparation solution B 5 to 70 parts by weight of the crude oil is dissolved in 5 to 60 parts by weight of the component (b) with the nano viscosity reducing pour point depressant master batch to obtain a solution B.
  • 0.1 to 10 parts by weight of the component (d) is dispersed in the component (f) to obtain a surfactant solution.
  • step 4 the solution A of the step 1, the dispersion A of the step 1 is mixed with the surfactant solution of the step 3, or the surface active of the solution B, the component (c) of the step 1 and the step 3 Mixing the solution, or mixing the solution B of the step 1 and the dispersion A of the step 1 with the surfactant solution of the step 3; adding 0-3 parts by weight of the component (e), further adding 0-30 parts by weight of the group Sub-(f), the nano-pour point depressant emulsion of the present invention is obtained.
  • the present invention further provides a second preparation method of the above nano-viscosity-lowering pour point depressant emulsion, which comprises a one-pot method comprising the steps of: adding components (a)-(c) in the above emulsion to the reaction kettle.
  • the nano-viscosity-lowering pour point depressant emulsion of the present invention is obtained by heating and stirring.
  • the method preferably comprises the steps of: adding the components (a) to (f) in the above emulsion to the reaction vessel, and heating and stirring to obtain the nano-viscosity-setting pour point depressant emulsion of the present invention.
  • nano-viscosity depressant masterbatch for crude oil; 1-80% by weight of component (b); 1-80% by weight of component (c); 0.1-10 Component (d) of % by weight; component (e) of 0.1-3% by weight and component (f) of the balance are added to the reaction vessel and stirred under heating to obtain a nano-pour point depressant emulsion.
  • the invention also provides an additive crude oil comprising crude oil and the above-mentioned nano viscosity reducing pour point depressant emulsion, wherein the nano viscosity reducing pour point depressant emulsion is added in an amount of 10-50,000 ppm.
  • the present invention also provides the use of the above-described nano-viscosity depressant emulsion for use in crude oil, particularly as a viscosity reducing pour point depressant and/or a wax crystal inhibitor for waxy crude oil.
  • the invention provides a nano viscosity reducing pour point depressant emulsion containing a nano viscosity reducing pour point depressant composition or a nano viscosity reducing pour point depressant masterbatch for crude oil, which has better depressing and viscosity reducing effect on crude oil and can Long-term stable storage, low freezing point and high concentration of pour point depressant are especially suitable for the use of crude oil in low temperature environment, and it does not need additional equipment when used, which is economical and practical and easy to promote.
  • the composition or the master batch may further be added with a graft polymer to obtain a nano hybrid blend, based on
  • the stabilized emulsion of the blend has a low freezing point and a high concentration, and is used as a pour point depressant for waxy crude oil, which significantly reduces the viscosity, freezing point and yield stress of the crude oil.
  • the present invention discloses a nano viscosity reducing pour point depressant emulsion.
  • the nano viscosity reducing pour point depressant masterbatch for crude oil used in the emulsion may be CN201110004024.0
  • the masterbatch disclosed in the above, the crude nanometer viscosity reducing pour point depressant masterbatch is a solid particle prepared by melt blending of the above nano pour point depressant composition, a coupling agent and a polymer processing aid.
  • the coupling agent is selected from a silane coupling agent, a titanate coupling agent, or a combination thereof, and the polymer processing aid includes an antioxidant and/or a lubricant and the like.
  • the composition or masterbatch contains a graft polymer in addition to the organic polymer pour point depressant and the inorganic nano pour point depressant to obtain a nano hybrid blend.
  • the graft polymer is selected from the group consisting of maleic anhydride grafted ethylene-vinyl acetate copolymer, maleic anhydride grafted polystyrene, maleic anhydride grafted ethylene-octene copolymer, One of or a combination of an anhydride-grafted ethylene-vinyl acetate copolymer, an isaconic anhydride grafted ethylene-octene copolymer, and the like.
  • the graft polymer acts as a bridge between the organic polymer pour point depressant and the inorganic nano pour point depressant, increasing the interaction between the organic polymer pour point depressant and the nanoparticles in the inorganic nano pour point depressant, so that the inorganic nano drop
  • the coagulant has better depressing and viscosity reducing effect on crude oil
  • the graft polymer has good compatibility with saturated alkanes in crude oil, and has good compatibility with crude oil colloid and asphaltene. Viscosity reduction and pour point.
  • the inventors have found through a series of experiments that the synergistic effect of the graft polymer, the inorganic nano-pour point depressant and the organic polymer pour point depressant greatly enhances the viscosity-lowering and pour point-reducing ability, and has significant viscosity-lowering and pour point reduction on the crude oil.
  • the effect is also surprisingly found that the inorganic nano-pour point depressant can be more closely adsorbed in the crude oil because of the good compatibility of the grafted polymer with the components of the crude oil and the inorganic nano-pour point depressant.
  • the surface of the wax crystals makes the internal structure of the low-temperature crude oil more stable, and can better play its important role in the low-temperature storage of crude oil.
  • the test results show that after the low-temperature storage of the additive crude oil for 3-6 months, the freezing point, The viscosity rises low, the thixotropic time is long, and the modulus is low when gelation occurs.
  • the graft polymer accounts for from 0 to 60% by weight or less. Preferably, from 1 to 55% by weight, further preferably from 5 to 50% by weight, more preferably from 10 to 35% by weight, the above synergistic effect can be maximized to achieve the above effects.
  • the inorganic nano-pour point depressant is selected from one or any combination of unmodified or surface-modified materials: silica, titania, calcium carbonate, talc Powder, smectite clay, etc.
  • the smectite clay is at least one selected from the group consisting of montmorillonite, hectorite, nontronite and saponite; the smectite clay can be further modified by an organic cationic compound Sex and/or coupling agent treatment.
  • the organic cationic compound is selected from the group consisting of organic ammonium salts and/or organic phosphonium salts with long carbon chains; the organic ammonium salts are selected from the group consisting of dodecyltrimethylammonium and tetradecyltrimethylammonium.
  • the emulsion comprises the following components:
  • component (f) 0-100 parts by weight of water and/or at least one water-miscible organic solvent which is the same as or different from component (c).
  • the organic solvent in the organic solvent which is immiscible with water or a mixture thereof is selected from the group consisting of toluene, xylene, mineral spirits, diesel oil and the like.
  • the organic solvent in the water-soluble organic solvent or the mixture of organic solvents is selected from the group consisting of ketones, alcohols, glycols, polyglycol ethers, and triols; specifically, methyl ethyl ketone, methanol, pentanol, and ethyl Glycol, propylene glycol, glycerol, isopropanol, and the like.
  • the surfactant is selected from the group consisting of a quaternary ammonium salt surfactant, a sulfate salt surfactant, a sulfonate surfactant, a sorbitan fatty acid ester (Span) surfactant, a polyoxygen Ethylene sorbitan fatty acid ester (Tween) surfactant, carboxylic acid based salt surfactant, and the like.
  • the emulsion stabilizer is selected from the group consisting of methyl cellulose, lecithin, cholesteryl and the like.
  • the reason why the emulsion stabilizer is added in the present invention is to keep the emulsion stable and prevent phase separation.
  • the water-miscible organic solvent different from the component (C) is selected from the group consisting of tetrahydrofuran, amides, diamines and the like.
  • nonionic surfactant (Span 60) was dissolved in 12 g of water, and mechanically stirred at 60 ° C for 30 min to obtain a surfactant solution;
  • step 4 The mixed solution of step 4 was cooled to room temperature to obtain a nano-viscosity depressant emulsion having a pour point depressant concentration of 30% by weight.
  • ethylene vinyl acetate copolymer (EVA), 30g maleic anhydride grafted-ethylene vinyl acetate copolymer (MAH-g-EVA), 40g of behenyltrimethylammonium bromide modified montmorillonite
  • EVA ethylene vinyl acetate copolymer
  • MAH-g-EVA maleic anhydride grafted-ethylene vinyl acetate copolymer
  • behenyltrimethylammonium bromide modified montmorillonite Into the reaction kettle, then add 136g of xylene, 80g of glycerol, 80g of methyl ethyl ketone and 40g of water, and then add 12g of surfactant sodium lauryl sulfate and 12g of nonionic surfactant (Span 60), and heat up to 75 °C, mechanical stirring for 6 hours, a nano-viscosity depressant emulsion with a pour point depressant concentration of 25 wt% was obtained.
  • nano-viscosity depressant particles 25 g of the above-mentioned nano-viscosity depressant particles, 45 g of a toluene/xylene mixed solvent, 20 g of pentanol/ethylene glycol, 5 g of water, and 5 g of a nonionic surfactant (Span 85) were placed in the reactor at 75 °C, mechanical stirring treatment for 4-6 hours, a nano-pour point depressant emulsion with a pour point depressant concentration of 25 wt% was obtained.
  • a nonionic surfactant Span 85
  • the nano-viscosity-lowering pour point depressant emulsion of the present invention has a significantly higher concentration of the pour point depressant than the existing pour point depressant solution, and the freezing point is lowered, and can be stably existed for a long period of time.
  • nano-viscosity depressant emulsions or solutions obtained in Examples 1-4 and Comparative Examples 1-2 were separately added to the South China Sea crude oil at a ratio of 100 ppm nano-pour point depressant, and the results of the measurement were shown in Table 2.
  • the nano-viscosity-reducing pour point depressant emulsion of the present invention has superior post-condensation point, viscosity drop and yield properties compared to the prior art after it is added to the crude oil.

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Abstract

La présente invention concerne une émulsion stable d'un abaisseur de point d'écoulement réduisant la viscosité de l'ordre du nanomètre, son procédé de préparation et son utilisation. L'émulsion comprend les constituants suivants : (a) une composition d'abaisseur de point d'écoulement réduisant la viscosité de l'ordre du nanomètre ou un lot maître d'abaisseur de point d'écoulement réduisant la viscosité de l'ordre du nanomètre pour pétrole brut, la composition d'abaisseur de point d'écoulement réduisant la viscosité de l'ordre du nanomètre comprenant les constituants suivants : (i) un abaisseur de point d'écoulement macromoléculaire organique et (ii) un abaisseur de point d'écoulement inorganique de l'ordre du nanomètre, et le lot maître d'abaisseur de point d'écoulement réduisant la viscosité de l'ordre du nanomètre pour pétrole brut étant des particules solides préparées par mélange à l'état fondu de la composition d'abaisseur de point d'écoulement réduisant la viscosité de l'ordre du nanomètre ci-dessus mentionné, éventuellement un agent de couplage et des auxiliaires de transformation macromoléculaires ; (b) un solvant organique non miscible dans l'eau ou un mélange de ce dernier ; et (c) un solvant organique soluble dans l'eau ou un mélange de ce dernier. L'émulsion stable présente un faible point de condensation et une concentration élevée, est utilisée comme abaisseur de point d'écoulement pour pétrole brut contenant de la cire, et réduit significativement la viscosité, le point de condensation et la limite apparente d'élasticité du pétrole brut.
PCT/CN2017/111267 2016-11-21 2017-11-16 Émulsion stable d'abaisseur de point d'écoulement réduisant la viscosité de l'ordre du nanomètre, son procédé de préparation et son utilisation Ceased WO2018090944A1 (fr)

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CN201611039541.0A CN108084982B (zh) 2016-11-21 2016-11-21 纳米降粘降凝剂稳定乳液及其制备方法和用途

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