CN109370553B - Crude oil wax inhibitor for oil field and preparation method thereof - Google Patents
Crude oil wax inhibitor for oil field and preparation method thereof Download PDFInfo
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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
- C09K8/52—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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F218/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
- C08F218/02—Esters of monocarboxylic acids
- C08F218/04—Vinyl esters
- C08F218/08—Vinyl acetate
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/20—Esters of polyhydric alcohols or phenols, e.g. 2-hydroxyethyl (meth)acrylate or glycerol mono-(meth)acrylate
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Abstract
The invention discloses an oil field crude oil wax inhibitor and a preparation method thereof, wherein vinyl acetate and hydroxyl-containing ester are mixed, an organic solvent is added, nitrogen is introduced, the temperature is slowly raised to 50-55 ℃, and the stirring is carried out for 0.5 h; then adding styrene; and (3) beginning to dropwise add an organic solvent solution of the initiator, and controlling the reaction temperature to be not more than 75 ℃ in the dropwise adding process. Reacting for 6-11 hours at 75-80 ℃ to obtain a product A; and mixing the ethylene-vinyl acetate copolymer, pinene and the nonionic surfactant with the A, and uniformly stirring to obtain the crude oil wax inhibitor for the oil field. The crude oil wax inhibitor not only has the wax-proof function, but also does not contain chlorine, is very suitable for the exploitation and the transportation of crude oil of high-wax-content medium-quality crude oil in offshore oil fields, has the characteristics of small dosage, wide application range, remarkable wax-proof effect, high viscosity reduction rate and the like, and simultaneously has the advantages of simpler preparation method, low process requirement and easy batch production.
Description
Technical Field
The invention belongs to the technical field of oil, gas and water gathering and transportation, and particularly relates to a crude oil wax inhibitor and a preparation method thereof.
Background
At present, the characteristics of high wax content oil products, such as high wax precipitation point, high condensation point, high viscosity and the like, seriously restrict the exploitation, collection and transportation of the oil products, and greatly reduce the production efficiency. Therefore, the problems of preventing wax precipitation and blocking and reducing the viscosity of the crude oil are the problems which need to be solved in the process of extracting, gathering and transporting the crude oil with high wax content and the like. Offshore oil field exploitation starts later than land oil fields, but with continuous deepening of oil field exploitation, the exploitation amount of high-wax-content crude oil is obviously increased, and huge pressure is brought to on-site supporting facilities and production.
The wax inhibitor is added, so that the formula can be flexibly adjusted according to the structure, type and content of wax, and the advantages of low equipment management investment and management cost, low potential safety hazard, energy conservation and the like are achieved. Therefore, the addition of the wax inhibitor is a necessary process for the extraction and transportation of the high wax content crude oil.
The wax control technique started in 1931, where Davis synthesized the wax control agent paraflow by Friedel-Crafts condensation using chlorinated paraffin and naphthalene. Thereafter, development and application of wax inhibitors have been greatly developed, and most of them are composite and copolymer wax inhibitors containing ethylene-vinyl acetate copolymer, styrene-maleic anhydride copolymer, acrylate homopolymer or copolymer with other monomers as main components. In recent years, a terpolymer synthesized by introducing a third monomer such as maleic anhydride, methacrylic acid ester, styrene, amine compound and the like has been widely used.
The crude oil has different paraffin and colloid contents, and the molecular structure and size of the crude oil are different, so that the variety of corresponding paraffin inhibitors is various, and the paraffin inhibitors with better foreign effects at present comprise 5 kinds of surfactants, maleic anhydride polymers, acrylates, ethylene-vinyl acetate copolymers, polyampholytes and the like. The wax inhibitor made in China mainly takes high molecular polymer and copolymer as main materials, and makes great progress, but the variety and the quantity are far less than those made in foreign countries.
However, none of the pour point depressants can meet the wax control requirement of the high-wax content medium crude oil in the offshore oil field.
(1) The poly (methyl) acrylate series and maleic anhydride copolymer have the effect on light crude oil; the wax control effect on the offshore high-wax content medium crude oil is poor.
(2) EVA and its modified compound, nitrogen-containing compound have certain wax-proofing effect on marine high-wax-content medium crude oil under the condition of higher dosage, but the self-solidifying point of said type of medicine is very high, and generally is about 10 deg.C, and the land oil field adopts solid granules to make addition, and the crude oil can be heated and dissolved into liquid with a certain content, then the above-mentioned liquid can be added with medicine. The offshore oil field is limited by space, flow, environmental temperature and the like, liquid charging is required, which puts higher requirements on the physical and chemical properties of the medicament, such as the self-solidifying point of the medicament is lower than-20 ℃ in winter, the filling concentration is low and the like.
(3) The natural high molecular compound has large dosage and poor anti-shearing performance, and the crude oil has poor effect on the condition of low water content.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an oil field crude oil wax inhibitor and a preparation method thereof, and solves the problem that the crude oil wax inhibitor in the prior art cannot meet the wax-inhibiting requirement of high-wax content medium crude oil in offshore oil fields.
The technical scheme of the invention is as follows: an oil field crude oil wax inhibitor is prepared by the following preparation method:
(1) mixing vinyl acetate and hydroxyl-containing ester at a mass ratio of 5:1-1:2, adding an organic solvent with the mass being 3-5 times of the total mass of the vinyl acetate and the hydroxyl-containing ester, introducing nitrogen, slowly heating to 50-55 ℃, and stirring for 0.5 h;
(2) then adding styrene with the total mass ratio of the vinyl acetate to the hydroxyl-containing ester being 2-8%;
(3) starting to drip an organic solvent solution of an initiator, wherein the mass of the initiator is 0.1-0.3 percent of the total mass of the vinyl acetate and the hydroxyl-containing ester, and controlling the reaction temperature to be not more than 75 ℃ in the dripping process;
(4) after the organic solvent solution of the initiator is dripped, the mixture reacts for 6 to 11 hours at the temperature of between 75 and 80 ℃ to prepare a product A;
(5) mixing the product A with 3-5% of ethylene-vinyl acetate copolymer, 1-3% of pinene and 1-3% of nonionic surfactant with the product A, and stirring uniformly to obtain the crude oil wax inhibitor for the oil field.
The hydroxyl-containing fatty acid ester is at least one of glycerol acrylate, glycerol methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate and ricinoleic acid vinyl ester.
The initiator is lauroyl peroxide or benzoyl peroxide.
The organic solvent is at least one of benzene, toluene, xylene, trimethylbenzene, mixed benzene and heavy aromatic hydrocarbon.
The pinene is alpha-pinene or beta-pinene.
The non-ionic surfactant is span-40, span-60 or span-80.
A preparation method of an oil field crude oil wax inhibitor comprises the following steps:
(1) mixing vinyl acetate and hydroxyl-containing ester at a mass ratio of 5:1-1:2, adding an organic solvent with the mass being 3-5 times of the total mass of the vinyl acetate and the hydroxyl-containing ester, introducing nitrogen, slowly heating to 50-55 ℃, and stirring for 0.5 h;
(2) then adding styrene with the total mass ratio of the vinyl acetate to the hydroxyl-containing ester being 2-8%;
(3) starting to drip an organic solvent solution of an initiator, wherein the mass of the initiator is 0.1-0.3 percent of the total mass of the vinyl acetate and the hydroxyl-containing ester, and controlling the reaction temperature to be not more than 75 ℃ in the dripping process;
(4) after the organic solvent solution of the initiator is dripped, the mixture reacts for 6 to 11 hours at the temperature of between 75 and 80 ℃ to prepare a product A;
(5) mixing the product A with 3-5% of ethylene-vinyl acetate copolymer, 1-3% of pinene and 1-3% of nonionic surfactant with the product A, and stirring uniformly to obtain the crude oil wax inhibitor for the oil field.
The hydroxyl-containing fatty acid ester is at least one of glycerol acrylate, glycerol methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate and ricinoleic acid vinyl ester.
The initiator is lauroyl peroxide or benzoyl peroxide.
The organic solvent is at least one of benzene, toluene, xylene, trimethylbenzene, mixed benzene and heavy aromatic hydrocarbon.
The pinene is alpha-pinene or beta-pinene.
The non-ionic surfactant is span-40, span-60 or span-80.
The invention has the beneficial effects that: experiments prove that the introduction of hydroxyl can effectively reduce the viscosity of the high-wax-content medium crude oil, and the wax crystal structure in the crude oil is looser and is not easy to form a net structure, so that the wax-proofing effect of the wax-proofing agent is greatly improved. Meanwhile, the ester polymer has obvious synergistic effect with ethylene-vinyl acetate copolymer, pinene and nonionic surfactant, and the cost performance of the product can be effectively improved. The product of the invention is generally applicable to various oil and gas fields, in particular to offshore oil and gas fields. The paraffin inhibitor has a good paraffin inhibition effect on the high-wax content medium crude oil in the offshore oil field, and when the filling concentration is 300mg/L, the paraffin inhibition rate on the high-wax content medium crude oil in the Bohai sea and the south sea oil fields reaches more than 96%, and the viscosity reduction rate reaches more than 92%. The crude oil wax inhibitor not only has the wax-proof function, but also does not contain chlorine, is very suitable for the exploitation and the transportation of crude oil of high-wax-content medium crude oil in offshore oil fields, and has the characteristics of small dosage, wide application range, remarkable wax-proof effect, high viscosity reduction rate and the like.
Detailed Description
The invention is described in further detail below by means of specific examples:
example 1:
(1) firstly, 430g (5mol) of vinyl acetate and 308.5g (1mol) of vinyl ricinoleate are mixed, 477g of dimethylbenzene and 1000g of trimethylbenzene are added, nitrogen is introduced, the temperature is slowly raised to 50-55 ℃, and the mixture is stirred for 0.5 h;
(2) 14.77g of styrene are added;
(3) adding lauroyl peroxide solution in toluene dropwise, wherein the mass of the lauroyl peroxide is 2.2155g, and controlling the reaction temperature to be not more than 75 ℃ in the dropwise adding process.
(4) After the dropwise addition is finished, reacting for 11 hours at the temperature of 75 ℃ to obtain a product A;
(5) 36.925g of ethylene-vinyl acetate copolymer, 7.385g of beta-pinene, 14.77g of span-80 and A are mixed and stirred uniformly to obtain the crude oil paraffin inhibitor 1 #.
Example 2:
(1) firstly, 86g (1mol) of vinyl acetate and 288g (2mol) of hydroxypropyl methacrylate are mixed, 870g of heavy aromatic hydrocarbon and 1000g of dimethylbenzene are added, nitrogen is introduced, the temperature is slowly raised to 50-55 ℃, and the mixture is stirred for 0.5 h;
(2) 29.92g of styrene are added;
(3) adding lauroyl peroxide solution in toluene dropwise, wherein the mass of lauroyl peroxide is 0.374g, and controlling the reaction temperature to be not more than 75 ℃ in the dropwise adding process.
(4) After the addition was completed, the reaction was carried out at 79 ℃ for 8 hours to obtain product A.
(5) Mixing 8.64g of ethylene-vinyl acetate copolymer, 4.32g of alpha-pinene, 3.74g of span-60 and A, and uniformly stirring to obtain the crude oil paraffin inhibitor 2 #.
Example 3:
(1) firstly, 86g (1mol) of vinyl acetate and 130g (1mol) of hydroxypropyl acrylate are mixed, 648g of trimethylbenzene is added, nitrogen is introduced, the temperature is slowly raised to 50-55 ℃, and stirring is carried out for 0.5 h;
(2) 1.296g of styrene were added;
(3) dripping a benzene solution of benzoyl peroxide with the mass of 0.432g, wherein the reaction temperature is controlled not to exceed 75 ℃ in the dripping process.
(4) After the dropwise addition, the reaction was carried out at 80 ℃ for 6 hours to obtain a product A.
(5) Mixing 11.22g of ethylene-vinyl acetate copolymer, 11.22g of alpha-pinene, 6.48g of span-40 and A, and uniformly stirring to obtain the crude oil paraffin inhibitor 3 #.
Example 4:
(1) firstly, 258g (3mol) of vinyl acetate and 142g (1mol) of glycerol acrylate are mixed, 1600g of mixed benzene is added, nitrogen is introduced, the temperature is slowly raised to 50-55 ℃, and the mixture is stirred for 0.5 h;
(2) 16g of styrene were added;
(3) adding dropwise a toluene solution of benzoyl peroxide, wherein the mass of the benzoyl peroxide is 0.8g, and controlling the reaction temperature to be not more than 75 ℃ in the dropwise adding process.
(4) After the addition was completed, the reaction was carried out at 78 ℃ for 7 hours to obtain product A.
(5) Mixing 16g of ethylene-vinyl acetate copolymer, 8g of beta-pinene, 8g of span-80 and A, and uniformly stirring to obtain the crude oil paraffin inhibitor 4# of the oil field.
Example 5:
(1) firstly, 344g (4mol) of vinyl acetate and 142g (1mol) of glycerol methacrylate are mixed, 1000g of toluene and 944g of xylene are added, nitrogen is introduced, the temperature is slowly raised to 50-55 ℃, and the mixture is stirred for 0.5 h;
(2) 14.58g of styrene are added;
(3) adding lauroyl peroxide solution in toluene dropwise, wherein the mass of benzoyl peroxide is 0.972g, and controlling the reaction temperature to be not more than 75 ℃ in the dropwise adding process.
(4) After the addition was completed, the reaction was carried out at 76 ℃ for 9 hours to obtain product A.
(5) Mixing 14.58g of ethylene-vinyl acetate copolymer, 14.58g of alpha-pinene, 14.58g of span-60 and A, and uniformly stirring to obtain the crude oil paraffin inhibitor No. 5 of the oil field.
Example 6:
(1) firstly, 172g (2mol) of vinyl acetate, 72g (0.5mol) of hydroxypropyl methacrylate and 65g (0.5mol) of hydroxypropyl acrylate are mixed, 1236g of dimethylbenzene is added, nitrogen is introduced, the temperature is slowly raised to 50-55 ℃, and stirring is carried out for 0.5 h;
(2) 15.45g of styrene were added;
(3) adding dropwise a toluene solution of benzoyl peroxide, wherein the mass of the benzoyl peroxide is 0.618g, and controlling the reaction temperature to be not more than 75 ℃ in the dropwise adding process.
(4) After the addition was completed, the reaction was carried out at 77 ℃ for 10 hours to obtain product A.
(5) Mixing 15.45g of ethylene-vinyl acetate copolymer, 3.09g of alpha-pinene, 9.27g of span-80 and A, and uniformly stirring to obtain the crude oil paraffin inhibitor 6 #.
Example 7:
experiment raw materials: bohai sea oil field crude oil (high wax content middle quality crude oil)
The evaluation method comprises the following steps: SY/T6300-2009 technical conditions of paraffin removal and prevention agent for oil extraction
Experiment temperature: 60 deg.C
The concentration of the medicament: 300mg/L
Average wax control value/average viscosity value: the number of measurements is 2, the 2 measurements are in accordance with the error specification of the corresponding measurement method, and the arithmetic mean of the 2 measurements is taken
The test results were as follows:
TABLE 1 wax control test
TABLE 2 viscosity reduction Rate test
Example 8:
experiment raw materials: crude oil of certain oil field in south China sea (high wax content middle quality crude oil)
The evaluation method comprises the following steps: SY/T6300-2009 technical conditions of paraffin removal and prevention agent for oil extraction
Experiment temperature: 65 deg.C
The concentration of the medicament: 300mg/L
Average wax control value/average viscosity value: the number of measurements is 2, the 2 measurements are in accordance with the error specification of the corresponding measurement method, and the arithmetic mean of the 2 measurements is taken
The test results were as follows:
TABLE 3 wax control test
TABLE 4 viscosity reduction Rate test
| Reducing the temperature to/° C | Average viscosity number/mPas | Viscosity reduction ratio/%) | |
| Blank space | 30 | 1764 | 0 |
| Example 1 | 30 | 121 | 93.14 |
| Example 2 | 30 | 135 | 92.35 |
| Example 3 | 30 | 104 | 94.10 |
| Examples of the invention4 | 30 | 116 | 93.42 |
| Example 5 | 30 | 107 | 93.93 |
| Example 6 | 30 | 127 | 92.80 |
| Surfactant type product | 30 | 378 | 78.57 |
| Wax crystal modified dosage form product | 30 | 326 | 81.52 |
| Commercial wax control product | 30 | 305 | 82.71 |
| Commercial wax control product | 30 | 413 | 76.59 |
The results of examples 7 and 8 show that the paraffin inhibitor has a good paraffin inhibition effect on high-wax-content medium crude oil in offshore oil fields, and when the filling concentration is 300mg/L, the paraffin inhibition rate on the high-wax-content medium crude oil in Bohai and south China sea oil fields reaches more than 96%, and the viscosity reduction rate reaches more than 92%.
The above description is only a preferred embodiment of the present invention, and all modifications and variations that can be made by the present invention in the specification or directly or indirectly applied to other related technical fields should be considered to be within the scope of the present invention.
Claims (6)
1. The oil field crude oil wax inhibitor is characterized by being prepared by the following preparation method:
(1) mixing vinyl acetate and hydroxyl-containing ester at a mass ratio of 5:1-1:2, adding an organic solvent with the mass being 3-5 times of the total mass of the vinyl acetate and the hydroxyl-containing ester, introducing nitrogen, slowly heating to 50-55 ℃, and stirring for 0.5 h;
(2) then adding styrene with the total mass ratio of the vinyl acetate to the hydroxyl-containing ester being 2-8%;
(3) starting to drip an organic solvent solution of an initiator, wherein the mass of the initiator is 0.1-0.3 percent of the total mass of the vinyl acetate and the hydroxyl-containing ester, and controlling the reaction temperature to be not more than 75 ℃ in the dripping process;
(4) after the organic solvent solution of the initiator is dripped, the mixture reacts for 6 to 11 hours at the temperature of between 75 and 80 ℃ to prepare a product A;
(5) mixing the product A with 3-5% of ethylene-vinyl acetate copolymer, 1-3% of pinene and 1-3% of nonionic surfactant, and stirring to obtain crude oil wax inhibitor;
the hydroxyl-containing fatty acid ester is at least one of glycerol acrylate, glycerol methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate and ricinoleic acid vinyl ester.
2. The oilfield crude oil paraffin inhibitor of claim 1, wherein the initiator is lauroyl peroxide or benzoyl peroxide.
3. The oilfield crude oil paraffin inhibitor of claim 1, wherein the organic solvent is at least one of benzene, toluene, xylene, trimethylbenzene, mixed benzene, and heavy aromatics.
4. The oilfield crude oil paraffin inhibitor of claim 1, wherein the pinene is α -pinene or β -pinene.
5. The oilfield crude oil paraffin inhibitor of claim 1, wherein the nonionic surfactant is span-40, span-60 or span-80.
6. The preparation method of the oil field crude oil paraffin inhibitor is characterized by comprising the following steps:
(1) mixing vinyl acetate and hydroxyl-containing ester at a mass ratio of 5:1-1:2, adding an organic solvent with the mass being 3-5 times of the total mass of the vinyl acetate and the hydroxyl-containing ester, introducing nitrogen, slowly heating to 50-55 ℃, and stirring for 0.5 h;
(2) then adding styrene with the total mass ratio of the vinyl acetate to the hydroxyl-containing ester being 2-8%;
(3) starting to drip an organic solvent solution of an initiator, wherein the mass of the initiator is 0.1-0.3 percent of the total mass of the vinyl acetate and the hydroxyl-containing ester, and controlling the reaction temperature to be not more than 75 ℃ in the dripping process;
(4) after the organic solvent solution of the initiator is dripped, the mixture reacts for 6 to 11 hours at the temperature of between 75 and 80 ℃ to prepare a product A;
(5) mixing the product A with 3-5% of ethylene-vinyl acetate copolymer, 1-3% of pinene and 1-3% of nonionic surfactant, and stirring to obtain crude oil wax inhibitor;
the hydroxyl-containing fatty acid ester is at least one of glycerol acrylate, glycerol methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate and ricinoleic acid vinyl ester;
the initiator is lauroyl peroxide or benzoyl peroxide;
the organic solvent is at least one of benzene, toluene, xylene, trimethylbenzene, mixed benzene and heavy aromatic hydrocarbon;
the pinene is alpha-pinene or beta-pinene;
the non-ionic surfactant is span-40, span-60 or span-80.
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| CN114672295B (en) * | 2022-01-27 | 2023-06-02 | 中海油(天津)油田化工有限公司 | Crude oil wax-proof pour point depressant and preparation method thereof |
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| CN102199421A (en) * | 2010-03-22 | 2011-09-28 | 天津大港油田科远石油工程有限责任公司 | Modifier for high-pour-point crude oil |
| CN104962267A (en) * | 2015-07-21 | 2015-10-07 | 陕西丰登石化有限公司 | Low-temperature oil well chemical wax cleaning agent and preparation method thereof |
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| CN102199421A (en) * | 2010-03-22 | 2011-09-28 | 天津大港油田科远石油工程有限责任公司 | Modifier for high-pour-point crude oil |
| CN104962267A (en) * | 2015-07-21 | 2015-10-07 | 陕西丰登石化有限公司 | Low-temperature oil well chemical wax cleaning agent and preparation method thereof |
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