CN104263328B - High-temperature-resistant oil-base drilling fluid emulsifier and preparation method thereof - Google Patents
High-temperature-resistant oil-base drilling fluid emulsifier and preparation method thereof Download PDFInfo
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- CN104263328B CN104263328B CN201410454965.8A CN201410454965A CN104263328B CN 104263328 B CN104263328 B CN 104263328B CN 201410454965 A CN201410454965 A CN 201410454965A CN 104263328 B CN104263328 B CN 104263328B
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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
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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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
- C09K8/02—Well-drilling compositions
- C09K8/32—Non-aqueous well-drilling compositions, e.g. oil-based
- C09K8/36—Water-in-oil emulsions
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Abstract
The invention discloses a high-temperature-resistant oil-base drilling fluid emulsifier which is prepared by reacting the following components in parts by weight: 9-12 parts of polyolefin, 1-3 parts of maleic anhydride, 18-22 parts of xylene, 3-5 parts of polyethylene polyamine, 2-4 parts of polyethyleneglycol and 1-3 parts of octyl phenol polyethenoxy ether. The invention also discloses a preparation method of the emulsifier. The emulsifier has better emulsifying effect on the water-in-oil drilling fluid system which uses diesel and white oil as continuous phases, has superhigh high-temperature resistance, can keep high emulsion-breaking voltage of the oil-base drilling fluid at the high temperature of 200 DEG C or so, and can enduringly ensure the emulsifying stability, rheological property and pollution resistance of the oil-base drilling fluid.
Description
Technical field：
The present invention relates to field of oil drilling, more particularly to a kind of high temperature resistance oil base drilling fluid emulsifying agent and its preparation side
Method.
Background technology：
Oil base drilling fluid have high inhibition, high temperature resistance, antipollution, can the admirably good characteristic such as formation protection, in the whole world
Drilling fluid market share critical role.Oil base drilling fluid is applied to brill bad ground, and as strong stratum in water sensitivity, Temperature Deep are high
Pressure stratum, huge thickness saline bed and rock salt stratum etc., its advantage is that water-base drilling fluid can not be compared.At present, oil base drilling fluid
Become the important means boring highly difficult, high temperature deep well, high-inclination directional well, horizontal well and various Holes of Complicated Wells.
The selection of emulsifying agent is the key whether determining oil base drilling fluid function admirable.Practice have shown that, the type of emulsifying agent,
Dosage and with the compatibility of base oil the performances such as the emulsion stability of oil base drilling fluid, rheological characteristic and filter loss are had aobvious
The impact writing.Domestic oil base drilling fluid emulsifying agent is mostly dehydrating sorbitol monooleate (Span-80) or it is derivative at present
Thing, its maximum shortcoming is that high temperature emulsifying effectiveness is not good and dosage is larger, and gap is larger compared with foreign same type product, sternly
Constrain the application in high temperature deep well for the domestic oil base drilling fluid technology again.Therefore, it is necessary to develop a kind of new high temperature resistance oil base
Well-drilling liquid emulgent, can ensure emulsion stability, rheological characteristic and the antipollution energy of oil base drilling fluid at high temperature high-efficient and lasting
Power.
Content of the invention：
It is an object of the present invention to provide a kind of high temperature resistance oil base drilling fluid emulsifying agent, being capable of high-efficient and lasting at high temperature
Ground ensures emulsion stability, rheological characteristic and the contamination resistance of oil base drilling fluid.
It is a further object of the present invention to provide a kind of preparation method of high temperature resistance oil base drilling fluid emulsifying agent.
For this reason, technical scheme is as follows：
Described high temperature resistance oil base drilling fluid emulsifying agent is prepared from by the component reaction of following weight portion：
Realize especially by following preparation processes：
(1) additive reaction：Polyolefin and maleic anhydride are dissolved in solvent, are heated to 150～160 DEG C, are forced into 0.5
～0.7MPa, reacts 8～10h, obtains polyolefin succinic anhydride；
(2) condensation reaction：Cool the temperature to pressure release after room temperature, add polyethylene polyamine, continue under 110～130 DEG C, normal pressure
Continuous reaction 4～6h, makes polyethylene polyamine, with polyolefin succinic anhydride, condensation reaction occur；
(3) impurity removal and purification：Temperature is risen to 150～155 DEG C, air-distillation recycling design, distills temperature liter after finishing
To 200～205 DEG C, Distillation recovery unreacted completely reactant, products therefrom is that emulsifying agent early-products polyolefin succinyl is sub-
Amine；
(4) compound strengthening：By uniform with Polyethylene Glycol and OPEO for emulsifying agent early-products mix obtain
High temperature resistance oil base drilling fluid emulsifier production.
In said components, the polyisobutylene that described polyolefin is 1000～1200 for molecular weight, with described maleic two
Anhydride, polyethylene polyamine, Polyethylene Glycol, are the reactant of synthetic emulsifier；Described solvent is dimethylbenzene；Described octylphenol polyethylene
Oxygen vinyl Ether, reaches so that emulsifier production can reach oil-base mud emulsifying agent optimum HLB value as HLB value regulator
Good emulsifiability.
The high temperature resistance oil base drilling fluid emulsifying agent being obtained by technical solution of the present invention is bronzing thick liquid, with existing breast
Agent is compared, and its advantage is embodied in：More preferable breast is respectively provided with to the Water-In-Oil drilling fluid system with diesel oil and white oil as continuous phase
Change acts on, and has extremely strong high-temperature resistance simultaneously, and oil base drilling fluid still can be made after 200 DEG C of high-temperature process to keep higher
Emulsion-breaking voltage, enduringly ensures emulsion stability, rheological characteristic and the contamination resistance of oil base drilling fluid.
Specific embodiment
Below in conjunction with specific embodiment, technical solution of the present invention and technique effect are described further.
Embodiment 1
(1) 9 parts of polyisobutylene (molecular weight is 1000～1200) and 2 parts of maleic anhydrides are dissolved in 22 parts of solvent diformazans
In benzene, add in reactor, be heated to 150 DEG C, logical nitrogen is forced into 0.6MPa, react 8h, obtain polyisobutylene butanedioic anhydride；
(2) temperature in reactor is down to pressure release after room temperature, adds 4 parts of polyethylene polyamines, be warming up to 110 DEG C, under normal pressure
Reaction 6h, makes polyethylene polyamine, with polyisobutylene butanedioic anhydride, condensation reaction occur；
(3) be warming up to 150 DEG C of air-distillation recycling design, to be distilled finish, then temperature is risen to 200 DEG C of Distillation recoveries not
Reaction completely reactant, the product obtaining is emulsifying agent early-products polyolefin succimide；
(4) obtain anti-height after emulsifying agent early-products uniformly being mixed with 4 parts of Polyethylene Glycol and 2 parts of OPEOs
Warm oil base drilling fluid emulsifier production.
Embodiment 2
(1) 12 parts of polyisobutylene (molecular weight is 1000～1200) and 1 part of maleic anhydride are dissolved in 20 parts of solvents two
In toluene, add in reactor, be heated to 160 DEG C, logical nitrogen is forced into 0.7MPa, react 10h, obtain polyisobutylene succinic acid
Acid anhydride；
(2) temperature in reactor is down to pressure release after room temperature, adds 3 parts of polyethylene polyamines, be warming up to 120 DEG C, under normal pressure
Reaction 5h, makes polyethylene polyamine, with polyisobutylene butanedioic anhydride, condensation reaction occur；
(3) be warming up to 155 DEG C of air-distillation recycling design, to be distilled finish, then temperature is risen to 205 DEG C of Distillation recoveries not
Reaction completely reactant, the product obtaining is emulsifying agent early-products polyolefin succimide；
(4) obtain anti-height after emulsifying agent early-products uniformly being mixed with 3 parts of Polyethylene Glycol and 3 parts of OPEOs
Warm oil base drilling fluid emulsifier production.
Embodiment 3
(1) 10 parts of polyisobutylene (molecular weight is 1000～1200) and 3 parts of maleic anhydrides are dissolved in 18 parts of solvents two
In toluene, add in reactor, be heated to 160 DEG C, logical nitrogen is forced into 0.5MPa, react 9h, obtain polyisobutylene succinic acid
Acid anhydride；
(2) temperature in reactor is down to pressure release after room temperature, adds 5 parts of polyethylene polyamines, be warming up to 130 DEG C, under normal pressure
Reaction 4h, makes polyethylene polyamine, with polyisobutylene butanedioic anhydride, condensation reaction occur；
(3) be warming up to 155 DEG C of air-distillation recycling design, to be distilled finish, then temperature is risen to 205 DEG C of Distillation recoveries not
Reaction completely reactant, the product obtaining is emulsifying agent early-products polyolefin succimide；
(4) obtain after emulsifying agent early-products uniformly being mixed with 2 parts of Polyethylene Glycol and 1 part of OPEO OP-7
High temperature resistance oil base drilling fluid emulsifier production.
Performance test
(1) comprehensive performance evaluation of high temperature resistance oil base drilling fluid emulsifying agent
Including：Emulsion-breaking voltage test before high temperature, the high-temperature resistance evaluation after high-temperature process, water resistant pollution capacity are evaluated
And anti-landwaste pollution capacity evaluates.Method is specific as follows：
Prepare drilling fluid according to the following formulation：
(1) (profit volume ratio is 90 to bavin Water-In-Oil:10)：360mL diesel oil+12mL efficient emulsifying agent+12g oxidized asphalt+
12g organoclay+6g calcium oxide+40mL water+360g barite；
(2) (profit volume ratio is 80 to bavin Water-In-Oil:20)：320mL diesel oil+16mL efficient emulsifying agent+12g oxidized asphalt+
8g organoclay+6g calcium oxide+80mL water+360g barite；
(3) (profit volume ratio is 90 to white Water-In-Oil:10)：360mL white oil+12mL efficient emulsifying agent+20g oxidized asphalt+
16g organoclay+6g calcium oxide+40mL water+360g barite；
(4) (profit volume ratio is 80 to white Water-In-Oil:20)：320mL white oil+16mL efficient emulsifying agent+20g oxidized asphalt+
12g organoclay+6g calcium oxide+80mL water+360g barite.
High-temperature resistance is evaluated：Stand 16 hours by putting in 200 DEG C of baking ovens by the drilling fluid that above four kinds of formula are prepared,
Emulsion-breaking voltage before test high temperature and after high temperature and rheological property.
Water resistant pollution capacity is evaluated：It is separately added into 40mL water in above four kinds of drilling fluids, 200 DEG C of test stands 16 hours
Emulsion-breaking voltage afterwards and rheological property.
Anti- landwaste pollution capacity is evaluated：It is separately added into 40g landwaste, 200 DEG C of standings 16 of test in above four kinds of drilling fluids
Emulsion-breaking voltage after hour and rheological property.
Assay method reference《GB/T 16782-1997 oil base drilling fluid On-Site Test Procedure》, test result is shown in Table 1.
The efficient emulsifying agent comprehensive performance evaluation of table 1
Note：In table, 1～4 corresponds to the drilling fluid that formula is (1)～(4) respectively；AV apparent viscosity, unit is mPa s；
PV plastic viscosity, unit is mPa s；YP yield value, unit is Pa；ES emulsion-breaking voltage, unit is V.
From data in table 1, the white oil base prepared by high temperature resistance oil base drilling fluid emulsifying agent and diesel oil base drilling fluid, often
In the case of temperature, emulsion-breaking voltage is above 800V.Through 200 DEG C of quiescence in high temperatures process, add after 40mL water (10% water pollution) again through height
Process through quiescence in high temperature again after warm stewing process and addition 40g landwaste (10% cuttings contamination), the emulsion-breaking voltages of 3 kinds of process are equal
More than 400V, show that emulsifiability meets field demand, and viscosity index has no significant change, rheological property is hardly subject to shadow
Ring.The above results illustrate that this emulsifying agent all has very strong emulsification in white oil base and diesel oil base drilling fluid, can be high at 200 DEG C
Ensure that oil base drilling fluid has good emulsion stability, rheological characteristic and contamination resistance under temperature.
(2) performance comparison with span 80 (Span-80)
By high temperature resistance oil base drilling fluid emulsifying agent, test and comparison breakdown of emulsion in diesel oil bag aqueous drilling fluid system is electric with Span-80
Pressure, diesel oil bag aqueous drilling fluid basic components are as follows：
(1) (profit volume ratio is 90 to bavin Water-In-Oil:10)：360mL diesel oil+12mL emulsifying agent+12g oxidized asphalt+12g has
Machine soil+6g calcium oxide+40mL water+360g barite；
(2) (profit volume ratio is 80 to bavin Water-In-Oil:20)：320mL diesel oil+16mL efficient emulsifying agent+12g oxidized asphalt+
8g organoclay+6g calcium oxide+80mL water+360g barite.
Test result is shown in Table 2：
Table 2 emulsifier performance comparison is tested
From data in table 2, under equal conditions, add the drilling fluid breakdown of emulsion electricity of high temperature resistance oil base drilling fluid emulsifying agent
Pressure all far above the drilling fluid adding Span-80, illustrates high temperature resistance oil base drilling fluid emulsifying agent in oil base drilling fluid system
Emulsifying capacity is higher.
Claims (3)
1. a kind of high temperature resistance oil base drilling fluid emulsifying agent it is characterised in that：Component by following weight portion：
Prepare in accordance with the following steps：
(1) described polyolefin and maleic anhydride are dissolved in solvent, are heated to 150～160 DEG C, it is forced into 0.5～
0.7MPa, reacts 8～10h, obtains polyolefin succinic anhydride；
(2) cool the temperature to pressure release after room temperature, add described polyethylene polyamine, be warming up to 110～130 DEG C, continue under normal pressure
Reaction 4～6h, makes described polyethylene polyamine, with described polyolefin succinic anhydride, condensation reaction occur；
(3) temperature is risen to 150～155 DEG C, air-distillation recycling design, temperature is risen to 200～205 DEG C after finishing by distillation,
Distillation recovery unreacted completely reactant, obtains reacted resultant polyolefin succimide；
(4) described polyolefin succimide is uniformly mixed to get product with described Polyethylene Glycol and OPEO
Product.
2. high temperature resistance oil base drilling fluid emulsifying agent according to claim 1 it is characterised in that：Described polyolefin is molecular weight
Polyisobutylene for 1000～1200.
3. high temperature resistance oil base drilling fluid emulsifying agent according to claim 1 it is characterised in that：Described solvent is dimethylbenzene.
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| CN201410454965.8A CN104263328B (en) | 2014-09-09 | 2014-09-09 | High-temperature-resistant oil-base drilling fluid emulsifier and preparation method thereof |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105368416A (en) * | 2015-12-10 | 2016-03-02 | 中国石油集团川庆钻探工程有限公司 | Modified polymer acids shear-enhancing agent for oil-based drilling fluids and preparation method thereof |
| CN105315973B (en) * | 2015-12-10 | 2018-06-29 | 中国石油集团川庆钻探工程有限公司 | High temperature resistance oil base drilling fluid modified fat acids primary emulsion and preparation method |
| CN110776883A (en) * | 2019-10-29 | 2020-02-11 | 中国海洋石油集团有限公司 | Emulsifier for oil-based drilling fluid |
| CN114181677B (en) * | 2021-11-24 | 2023-06-16 | 中国石油天然气集团有限公司 | Emulsifier, preparation method and application thereof and water-in-oil emulsified drilling fluid |
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Effective date of registration: 20210809 Address after: 100007 No. 9 North Main Street, Dongcheng District, Beijing, Dongzhimen Patentee after: CHINA NATIONAL PETROLEUM Corp. Patentee after: CNPC Bohai Drilling Engineering Co.,Ltd. Address before: 300457 Tianjin Binhai New Area Development Zone Huanghai Road 106 Bohai Drilling Engineering Co., Ltd. science and Technology Development Office Patentee before: CNPC Bohai Drilling Engineering Co.,Ltd. |