CN104650287A - Novel powder cationic polymer for preventing clay from hydration swelling - Google Patents
Novel powder cationic polymer for preventing clay from hydration swelling Download PDFInfo
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Abstract
The invention relates to a novel powder cationic polymer for preventing clay from hydration swelling, and belongs to the technical field of clay hydration swelling prevention in oil-gas field development. The novel powder cationic polymer is prepared from acrylamide, dimethyl diallyl ammonium chloride and methyl acrylyl ethyl trimethyl ammonium chloride as raw materials, and an ammonium persulfate and sodium hydrogen sulfite redox initiation system is adopted to prepare a novel powder cationic polymer solution for preventing clay from hydration swelling through polymerization of solution free radicals, and the cationic polymer solution is further transferred into micro drying equipment to be dried, and is successively further prepared into crude powder and fine powder, thereby obtaining the powder cationic polymer. By adopting the novel powder cationic polymer, a great amount of expensive, combustible or even toxic solvents are not used, separation equipment is not needed, and the problems that to maintain the flowability of a polymer solution, a conventional solution cationic polymer is relatively low in effective concentration, the package and transportation cost can be increased, a raw material holding space is large and the cationic polymer is inadaptive to the space of an ocean marine petroleum exploitation working platform can be solved.
Description
Technical field
The present invention relates to a kind of novel powdery cationic polymers preventing hydration and expansion of clay, belong in oilfield exploitation procedure and prevent hydration and expansion of clay technical field.
Background technology
The hydration swelling of clay mineral can be divided into following two stages: one is the surface hydration expansion stages: because the siloxane bond on clay crystal face top layer and hydrogen-oxygen key all have polarity, they can the water molecules of adsorb polar, and what now play a major role is the aquation energy of surface of clay.Two is infiltration aquation expansion stagess: clay particle surface forms hydration shell, and the distance between clay lattice aspect increases, and produce and expand so that dispersion, surface hydration can weaken greatly to the effect of aquation, and surface hydration also comes to an end.When clay is in the low mineralization aqueous solution, cation concn between clay mineral surface and crystal layer is higher than cation concn in bulk solution, now clay mineral interlayer and just produce an osmotic pressure between surface water solution and bulk aqueous solution, thus cause concentration diffusion, namely water molecules is between clay mineral crystal layer and crystal face spreads, originally the positively charged ion being adsorbed on surface of clay just spreads in bulk aqueous solution, and forms diffusion double layer.The effect of diffusion double layer repulsion, makes the bonding force of clay crystal layer weaken further, and clay is brilliant in greatly increasing, and defines hydration swelling.When clay mineral hydration swelling to a certain extent, just can disperse, form thinner particle (i.e. particulate), these particulates can be migrated in hole with fluid, blocking is produced at duct place, cause permeability reduction, produce to oil-gas field and cause high risks, cause Recoverable oil and gas reserves to reduce.Clay stabilizer can effectively solve the problems such as clay mineral hydration swelling as oilfield chemistry admixture.
The application of clay stabilizer can be divided into three phases: the later stage fifties to the sixties mainly uses inorganic salt as clay stabilizer; The seventies mainly with inorganic multinuclear polymkeric substance and cats product as clay stabilizer; After the eighties, mainly carry out the investigation and application stablizing clay with cationic organic polymer.
Inorganic salt clay stabilizer can only temporary stabilization clay particle, when oil reservoir environmental change, such stablizer generation cationic exchange, clay is made to return to original water-sensitive state, this kind of clay stabilizer can not produce multipoint adsorption as polymkeric substance, therefore to preventing clay movement DeGrain.
At present, oil field mainly contains two kinds for the polynuclear hydroxy bridge complex ion of clay stabilizer: oxyaluminum and zirconyl hydroxy, polynuclear hydroxy bridge complex ion class clay stabilizer can be used as long-acting clay stabilizer and uses, the harm of fine migration and hydration and expansion of clay can be eliminated, large-area reservoir can be processed, but acid resistance is poor, the source of goods is insufficient, on the high side.Cats product owing to can dissociate surface-active positively charged ion in water, and the surface that can be adsorbed on clay particle neutralizes the negative charge on clay particle, therefore cats product also can cook clay stabilizer.After cats product is adsorbed on the surface of clay particle, cationic have drive end unit to stretch to space, form the adsorption layer of one deck oleophyllie hydrophobic, water and clay are separated, neutralized the negative charge of surface of clay by the positively charged ion adsorbed simultaneously, reduce the repulsion between crystal layer, thus avoid the aquation of clay particle, expansion, dispersion, migration.When the organic group chain of cats product is longer, just stop other positively charged ion to enter the center of absorption, the cats product be adsorbed in clay particle surface can not be replaced by other positively charged ion.The effect that cats product stablizes clay is better than inorganic salt, and lasting for a long time, but its maximum shortcoming makes the wettability of reservoir become oil-wet, causes the relative permeability of water to decline.
Organic cationic polymer positive charge density is high, and after it is added to the water, the organic cation ionized out can be adsorbed on the surface of clay particle by electrostatic interaction.Due to organic cationic polymer with positive charge more; can simultaneously with multiple clay particle; form multipoint adsorption; form the absorption protective membrane of one deck organic cationic polymer on the surface of clay particle after absorption; clay particle is protected, prevents the aquation of clay particle, expansion, dispersion, migration.The ability that organic cationic polymer stablizes clay exceedes inorganic salts and inorganic multinuclear polymkeric substance and cats product class clay stabilizer, and have that consumption is few, usefulness is high, high adsorption capacity, affect the advantages such as little, formation strong adaptability by pH value, be the object of primary study and application both at home and abroad in recent years.
The synthetic method of current water-soluble cationic polymer mainly contains aqueous solution polymerization and inverse emulsion polymerization two kinds.
Inverse emulsion polymerization is for external phase polymerization single polymerization monomer is water-soluble with non-polar liquid (as varsol hexanaphthene, normal hexane etc.), then be scattered in oil phase by emulsifying agent, form " water-in-oil " (W/O) type emulsion and the polymerization carried out.Be since medium carries out the inverse emulsion polymerization of water-soluble monomer first from Vanderhoff in 1962 etc. with organic solvent, be developed so far the history of existing more than 40 years as one of the important method of producing superpolymer inverse emulsion polymerization.Inverse emulsion polymerization has that reaction is easy to heat radiation, rate of polymerization is high, can obtain the advantages such as high-molecular weight polymer, of many uses.But use and reclaim a large amount of costliness, flammable, even poisonous solvent, not only greatly increase production cost and facility investment, reduction equipment capacity, also can cause environmental pollution.As purity high solid polymkeric substance will be obtained, also to configure separating device, increase washing, solvent recuperation and the operation such as refining.
Aqueous solution polymerization is monomer, initiator (catalyzer) is dissolved in the process of carrying out in aqueous solvent being polymerized.The viscosity ratio mass polymerization of aqueous solution polymerization system is low, and mixing and heat radiation are than being easier to, and production operation and temperature are all easy to control, and the evaporation of solvent also can be utilized to get rid of heat of polymerization.If radical polymerization, can avoid when monomer concentration is low occurring auto-acceleration effect, thus avoid implode and polymerization reactor design is simplified.Shortcoming is that the polymerization degree is also little than additive method for aqueous free radical polymerization often because monomer concentration is lower, as the effective concentration of the mobility of polymers soln then polymkeric substance will be kept lower, increases packaging and transportation cost.Organic cationic polymer is comparatively large in aqueous solution polymerization reaction later stage gained aqueous copolymers solution viscosity, and form gel, and cationic polymers has extremely strong surfactivity, drying process forms spherical particle, brings great difficulty to drying process.Traditional drying mode is by granulator granulation, then puts into revolving drum dryer, through a few hours high-temperature hot-air dry up, then grind, sieve, pack.This drying mode dehydration intensity is low, residence time of material long, granulation time particle uneven and in revolving drum delivery speed very inconsistent, cause product to be dried uneven, cause poorly water-soluble and molecular weight and molecular weight obvious, thus quality product to be had an impact.And this drying plant heat exchange coefficient is lower, energy consumption is huge, is unfavorable for energy-conservation.
Summary of the invention
The object of the invention is to, for above-mentioned the deficiencies in the prior art, there is provided one with acrylamide, dimethyl diallyl ammonium chloride and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride for raw material, use ammonium persulphate and sodium bisulfite redox initiation system, prevent the cationic polymer solution of hydration and expansion of clay through aqueous free radical polymerization preparation; Proceeded to by the cationic polymers aqueous solution after microwave dryer dries again, material is again through the novel powdery cationic polymers preventing hydration and expansion of clay that meal, fine powder obtain.
The present invention realizes above-mentioned purpose by the following technical solutions:
The novel powdery cationic polymers preventing hydration and expansion of clay, is characterized in that: described cationic polymers is polymerized through aqueous free radical by acrylamide, dimethyl diallyl ammonium chloride and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride;
In described cationic polymers, the massfraction of polymerization single polymerization monomer is as follows:
Acrylamide 45% ~ 70%,
Dimethyl diallyl ammonium chloride 10% ~ 25%,
MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride 45% ~ 5%;
This novel preparation method of the powdery cationic polymers of hydration and expansion of clay that prevents is:
In the 2000L reactor with mechanical stirring, thermometer, condenser, logical nitrogen device, first drop into deionized water, add acrylamide, be stirred to and dissolve completely; Add dimethyl diallyl ammonium chloride and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride successively again, be stirred to and be uniformly dissolved; The sodium carbonate solution of slow dropping 15%, adjust reacting liquid pH value to 7.0 ~ 9.5, the massfraction of aqueous free radical polymerization reaction system monomer is 10 ~ 30%; Vacuumize 10 ~ 40 minutes, nitrogen concora crush, continue logical nitrogen 10 ~ 30 minutes, slowly heat up, aqueous free radical polymeric reaction temperature is 40 ~ 60 DEG C, adds 15% ammonium persulfate aqueous solution, stirs after 10 minutes, then adds 15% aqueous solution of sodium bisulfite simultaneously; React 1 ~ 3 hour, obtain the cationic polymers aqueous solution; Again the cationic polymers aqueous solution is proceeded to microwave dryer, microwave power is adjusted to 20 kilowatts ~ 40 kilowatts, the dry materials time is 10 ~ 40 minutes, and namely material drying obtains powdered cationic polymkeric substance through meal, fine powder.
In described cationic polymers, dimethyl diallyl ammonium chloride is massfraction is 60% aqueous solution, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride is massfraction 75% aqueous solution.
The present invention's beneficial effect is compared with prior art:
This is novel prevents the powdery cationic polymers of hydration and expansion of clay with acrylamide, dimethyl diallyl ammonium chloride and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride for raw material, use ammonium persulphate and sodium bisulfite redox initiation system, prevent the cationic polymer solution of hydration and expansion of clay through aqueous free radical polymerization preparation.Again the cationic polymers aqueous solution is proceeded to microwave dryer, microwave power is adjusted to 20 kilowatts ~ 40 kilowatts, the dry materials time is 10 ~ 40 minutes, and namely material drying obtains powdered cationic polymkeric substance through meal, fine powder.Compared with conventional inverter letex polymerization, avoid and use a large amount of expensive, flammable, even poisonous solvent, without the need to configuring separating device, the operation such as decrease washing, solvent recuperation and refine.Solving traditional aqueous cationic polymers is the mobility keeping polymers soln, makes the effective concentration of polymkeric substance lower, increases packaging and transportation cost, and raw material placement space is large, is not suitable with the problem that marine petroleum development job platform space is restricted.
Embodiment
This prevents the powdery cationic polymers of hydration and expansion of clay from adopting shale rolling rate of recovery method to evaluate cationic polymers to the rejection ability of clay particle hydration swelling.Getting distilled water 350 grams stirs in cup in height, to add after 0.7 gram of sodium carbonate, 17.5 grams of Repone K and 0.5% treatment agent to be evaluated high-speed stirring 15 ~ 20 minutes, treatment agent is fully disperseed, then be poured in roller furnace digestion tank, stir evenly after adding 6 ~ 10 order drilling cuttings 30 grams again, after rolling 6 hours at 60 DEG C, the drilling cuttings going out not disperse with 40 mesh screen, drying is weighed as W, calculates the shale rolling rate of recovery (W/30 × 100%).The rate of recovery is larger, and the rejection ability of cationic polymers to clay particle hydration swelling is stronger, otherwise rejection ability is poorer.
Below by several specific embodiment, that the invention will be further described is as follows:
Embodiment 1:
In the 2000L reactor with mechanical stirring, thermometer, condenser, logical nitrogen device, drop into deionized water 1340 kilograms, add acrylamide 225 kilograms, be stirred to and dissolve completely; Add dimethyl diallyl ammonium chloride (massfraction is 60% aqueous solution) 62 kilograms again, be stirred to and be uniformly dissolved; Add MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (75% aqueous solution) 60 kilograms again, be stirred to and be uniformly dissolved.The sodium carbonate solution of slow dropping 15%, adjust reacting liquid pH value to 7.1, vacuumize 20 minutes, nitrogen concora crush, continue logical nitrogen 30 minutes, slowly heat up and keep temperature 47 DEG C simultaneously, adding 15% ammonium persulfate aqueous solution 8 kilograms, stir after 10 minutes, then add 15% aqueous solution of sodium bisulfite 4.5 kilograms.React 2 hours, obtain this cationic polymers aqueous solution, above-mentioned material proceeds to microwave dryer, regulate microwave power 40 kilowatts, the dry materials time is 22 minutes, obtains cationic polymers crude product, namely obtains powdered cationic polymkeric substance through meal, fine powder.
Shale rolling rate of recovery method is adopted to evaluate cationic polymers to the rejection ability of clay particle hydration swelling.Blank sample system: distilled water+0.2% sodium carbonate+5% Repone K; Control sample system: the above-mentioned powdered cationic polymkeric substance of distilled water+0.2% sodium carbonate+5% Repone K+0.5%.Test result: the blank sample system shale rolling rate of recovery 22.76%, the control sample system shale rolling rate of recovery 78.46%.
Embodiment 2:
In the 2000L reactor with mechanical stirring, thermometer, condenser, logical nitrogen device, drop into deionized water 1180 kilograms, add acrylamide 205 kilograms, be stirred to and dissolve completely; Add dimethyl diallyl ammonium chloride (massfraction is 60% aqueous solution) 68 kilograms again, be stirred to and be uniformly dissolved; Add MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (75% aqueous solution) 40 kilograms again, be stirred to and be uniformly dissolved.The sodium carbonate solution of slow dropping 15%, adjust reacting liquid pH value to 7.8, vacuumize 20 minutes, nitrogen concora crush, continue logical nitrogen 30 minutes, slowly heat up and keep temperature 55 DEG C simultaneously, adding 15% ammonium persulfate aqueous solution 10 kilograms, stir after 10 minutes, then add 15% aqueous solution of sodium bisulfite 5.5 kilograms.React 3 hours, obtain this cationic polymers aqueous solution, above-mentioned material proceeds to microwave dryer, regulate microwave power 30 kilowatts, the dry materials time is 38 minutes, obtains cationic polymers crude product, namely obtains powdered cationic polymkeric substance through meal, fine powder.
Shale rolling rate of recovery method is adopted to evaluate cationic polymers to the rejection ability of clay particle hydration swelling.Blank sample system: distilled water+0.2% sodium carbonate+5% Repone K; Control sample system: the above-mentioned powdered cationic polymkeric substance of distilled water+0.2% sodium carbonate+5% Repone K+0.5%.Test result: the blank sample system shale rolling rate of recovery 22.76%, the control sample system shale rolling rate of recovery 84.53%.
Embodiment 3:
In the 2000L reactor with mechanical stirring, thermometer, condenser, logical nitrogen device, drop into deionized water 1500 kilograms, add acrylamide 185 kilograms, be stirred to and dissolve completely; Add dimethyl diallyl ammonium chloride (massfraction is 60% aqueous solution) 55 kilograms again, be stirred to and be uniformly dissolved; Add MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (75% aqueous solution) 35 kilograms again, be stirred to and be uniformly dissolved.Slow dropping is the sodium carbonate solution of 15%, adjusts reacting liquid pH value to 8.8, vacuumizes 20 minutes, nitrogen concora crush, continues logical nitrogen 30 minutes, slowly heats up and keep temperature 52 DEG C simultaneously, adding 15% ammonium persulfate aqueous solution 10 kilograms; Stir after 10 minutes, then add 15% aqueous solution of sodium bisulfite 5.5 kilograms.React 2 hours, obtain this cationic polymers aqueous solution, above-mentioned material proceeds to microwave dryer, regulate microwave power 20 kilowatts, the dry materials time is 33 minutes, obtains cationic polymers crude product, namely obtains powdered cationic polymkeric substance through meal, fine powder.
Shale rolling rate of recovery method is adopted to evaluate cationic polymers to the rejection ability of clay particle hydration swelling.Blank sample system: distilled water+0.2% sodium carbonate+5% Repone K; Control sample system: the above-mentioned powdered cationic polymkeric substance of distilled water+0.2% sodium carbonate+5% Repone K+0.5%.Test result: the blank sample system shale rolling rate of recovery 22.76%, the control sample system shale rolling rate of recovery 87.32%.
The above is preferred embodiment of the present invention, above-mentioned illustrating does not do any pro forma restriction to flesh and blood of the present invention, any simple modification that person of an ordinary skill in the technical field has done above embodiment according to technical spirit of the present invention after having read this specification sheets or distortion, and the technology contents of above-mentioned announcement may be utilized to be changed or be modified to the Equivalent embodiments of equivalent variations, all still belong in the scope of technical solution of the present invention, and do not deviate from the spirit and scope of the invention.
Claims (2)
1. the novel powdery cationic polymers preventing hydration and expansion of clay, is characterized in that: described cationic polymers is polymerized through aqueous free radical by acrylamide, dimethyl diallyl ammonium chloride and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride;
In described cationic polymers, the massfraction of polymerization single polymerization monomer is as follows:
Acrylamide 45% ~ 70%,
Dimethyl diallyl ammonium chloride 10% ~ 25%,
MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride 45% ~ 5%;
This novel preparation method of the powdery cationic polymers of hydration and expansion of clay that prevents is:
In the 2000L reactor with mechanical stirring, thermometer, condenser, logical nitrogen device, first drop into deionized water, add acrylamide, be stirred to and dissolve completely; Add dimethyl diallyl ammonium chloride and MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride successively again, be stirred to and be uniformly dissolved; The sodium carbonate solution of slow dropping 15%, adjust reacting liquid pH value to 7.0 ~ 9.5, the massfraction of aqueous free radical polymerization reaction system monomer is 10 ~ 30%; Vacuumize 10 ~ 40 minutes, nitrogen concora crush, continue logical nitrogen 10 ~ 30 minutes, slowly heat up, aqueous free radical polymeric reaction temperature is 40 ~ 60 DEG C, adds 15% ammonium persulfate aqueous solution, stirs after 10 minutes, then adds 15% aqueous solution of sodium bisulfite simultaneously; React 1 ~ 3 hour, obtain the cationic polymers aqueous solution; Again the cationic polymers aqueous solution is proceeded to microwave dryer, microwave power is adjusted to 20 kilowatts ~ 40 kilowatts, the dry materials time is 10 ~ 40 minutes, and namely material drying obtains powdered cationic polymkeric substance through meal, fine powder.
2. a kind of novel powdery cationic polymers preventing hydration and expansion of clay according to claim 1, it is characterized in that: in described cationic polymers, dimethyl diallyl ammonium chloride is massfraction 60% aqueous solution, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride is massfraction 75% aqueous solution.
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| CN112851372A (en) * | 2021-01-22 | 2021-05-28 | 佛山市山有海科技有限公司 | Solid dispergation reinforcing agent and preparation method thereof |
| CN113150765A (en) * | 2021-04-25 | 2021-07-23 | 陕西科技大学 | Expansion shrinkage agent for acidizing and fracturing and preparation method thereof |
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| CN113150765A (en) * | 2021-04-25 | 2021-07-23 | 陕西科技大学 | Expansion shrinkage agent for acidizing and fracturing and preparation method thereof |
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Application publication date: 20150527 |