CN104140792B - A kind of oil base drilling fluid emulsifying agent and its preparation method and application - Google Patents
A kind of oil base drilling fluid emulsifying agent and its preparation method and application Download PDFInfo
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- CN104140792B CN104140792B CN201410166050.7A CN201410166050A CN104140792B CN 104140792 B CN104140792 B CN 104140792B CN 201410166050 A CN201410166050 A CN 201410166050A CN 104140792 B CN104140792 B CN 104140792B
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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
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
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- Oil, Petroleum & Natural Gas (AREA)
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- General Chemical & Material Sciences (AREA)
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- General Life Sciences & Earth Sciences (AREA)
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Abstract
It is an object of the invention to provide a kind of oil base drilling fluid emulsifying agent, the emulsifying agent selected from waste grease, waste grease saponified and waste grease amidate in any two or three.The saponified of the waste grease is reacted to obtain by waste grease with alkali, and the amidate of the waste grease is reacted by waste grease with organic amine under the catalytic condition of alkali to be obtained.The present invention also provides the preparation method of the emulsifying agent and its application in oil base drilling fluid.The emulsifying agent has good emulsifying effectiveness.Bio-toxicity is low, and the cost of oil base drilling fluid emulsifying agent can not only be greatly lowered, and realizes turning waste into wealth for waste grease, pollution of the waste grease to environment is reduced, beneficial to environmental protection.
Description
Technical field
The invention provides the preparation method and application of a kind of oil base drilling fluid emulsifying agent and the drilling fluid, belong to
Oil drilling oil base drilling fluid field.
Background technology
Oil base drilling fluid have strong inhibition capability, lubricity it is excellent, beneficial to many merits such as wellbore stability and reservoir protections,
It is the effective means of drilling applications reply bad ground, is used widely.Usual oil base drilling fluid system is also known as Water-In-Oil
Drilling fluid or inverse emulsion drilling fluid.Oil base drilling fluid system is that dispersed phase (aqueous phase) is dispersed in into continuous phase by emulsifying agent
In (oil phase), therefore also known as inverse emulsification system.The quality of usual emulsifying agent performance directly determines the stabilization of inverse emulsification system
Performance.Being presently used for the emulsifying agent of oil base drilling fluid mainly includes the work of the nonionic class surfaces such as sapn, tween, cycloalkanoimide
The property anionic based surfactants such as agent and calcium stearate, calcium oleate, iron naphthenate and high-molecular polyamide, polyethers surface
Activating agent, the reasonable compounding of mentioned emulsifier has preferable emulsifying effectiveness, but deficiency with high costs be present.Above-mentioned material exists
The cost of oil base drilling fluid has significantly been drawn high in extensive application in oil base drilling fluid, is limited the popularization of oil base drilling fluid and is made
With.
The content of the invention
The present invention is raw material using waste greases such as various oil foots or gutter oils, passes through rational route and gentle reaction
Condition, cost-efficiently oil base drilling fluid emulsifying agent is prepared, the cost of oil base drilling fluid emulsifying agent is not only greatly lowered,
And turning waste into wealth for waste grease is realized, reduce pollution of the waste grease to environment.For waste grease recycling and
The sustainable development of oil resource provides an effective road, great economic implications and social effect.
Therefore, an object of the present invention is to provide a kind of oil base drilling fluid emulsifying agent.
It is yet another object of the invention to provide the preparation method of the emulsifying agent.
Another object of the present invention is to provide application of the emulsifying agent in oil base drilling fluid.
Oil base drilling fluid of the present invention is selected from the saponified and waste grease of waste grease, waste grease with emulsifying agent
Amidate in any two or three.
In one embodiment of the invention, saponified and waste grease the acid amides of the waste grease, waste grease
The weight ratio of compound is 100:0~300:0~100, preferably 100:100~150:10~30.
Specifically, the waste grease is selected from the oil foot of refining vegetable oil, refines oil foot, gutter oil, the swill of animal oil
At least one of oil and hogwash fat.
The saponified of the waste grease reacts to obtain by waste grease with alkali.In the specific embodiment of the present invention
In, 100 parts of waste greases and 10~100 parts of alkali are heated to 60~200 DEG C, stirred by saponification to count in parts by weight
Under the conditions of react 1~8 hour, cooling can be prepared by the saponified of waste grease.
The amidate of the waste grease is reacted by waste grease with organic amine under the catalytic condition of alkali to be obtained.
In the specific embodiment of the present invention, amidation process is counts in parts by weight, by 100 parts of waste greases and 10~100 parts
Organic amine and 5~50 parts of alkali are heated to 80~180 DEG C, react 2~8 hours under agitation, and cooling can be prepared by abandoned oil
The amidate of fat.
Any one of in above-mentioned amidation process, the organic amine is selected from 1) -3) compound that represents：
1)HO-C2H4-NH2、NH(-C2H4-OH)2With N (- C2H4-OH)3At least one of；
2)R1-HN-R2, wherein R1Selected from C1-C30Straight or branched saturated hydrocarbyl, C2-C30Straight or branched it is unsaturated
Alkyl, C3-C20Cycloalkyl, C6-C20Alkaryl, carbon number be 6-20 substituted or unsubstituted aralkyl；R2It is selected from
Hydrogen, C1-C30Straight or branched saturated hydrocarbyl, C2-C30Straight or branched unsaturated alkyl, C3-C20Cycloalkyl, C6-C20
Alkaryl, C6-C20Substituted or unsubstituted aralkyl；It is preferred that R1For C1-C6Straight or branched saturated hydrocarbyl, R2For hydrogen
Or C1-C6Straight or branched saturated hydrocarbyl.
3)H2N-R3-(NH-CnH2n)m-NH2, wherein R3Selected from C1-C20Straight or branched saturated hydrocarbyl, C2-C30Straight chain
Or side chain unsaturated alkyl, C3-C20Cycloalkyl, C6-C20Alkaryl, C6-C20Substituted or unsubstituted aralkyl, n is
1-6 integer, m be 0-20 integer, preferably R3For C1-C6Straight or branched saturated hydrocarbyl, n be 1-3 integer, m 0-5
Integer.
The alkali used in the saponification and amidation process is selected from calcium hydroxide, lithium hydroxide, sodium hydroxide, hydrogen-oxygen
Change at least one of potassium, calcium oxide, sodium oxide molybdena and potassium oxide.
The present invention also provides the preparation method of the emulsifying agent, including by the waste grease, waste grease it is saponified
With any two or three of mixing in the amidate of waste grease, 2-4h is stirred under 10000-15000rpm rotating speed,
It is well mixed to obtain the emulsifying agent.
Invention further provides application of the emulsifying agent in oil base drilling fluid.Specifically, in oil base drilling fluid
The middle emulsifying agent of the invention using 2~8 weight %.Base oil in the oil base drilling fluid is selected from diesel oil, white oil, α-long-chain
At least one of gentle liquefaction of alkene, long-chain ester.Further preferably contain salt solution in drilling fluid, as a rule, using sodium, calcium
And/or magnesium salts water.Also organic clay, emulsifying agent, pH value regulator, heavy weight additive and drop filter humectant etc. can be contained in drilling fluid
Component, these components are well-known to those skilled in the art.
The emulsifying agent of the present invention is high activity, it is believed that known is used for oil base drilling fluid system all or almost all
In it is all effective.The emulsifying agent of the present invention can also assign drilling fluid higher viscosity, thus preferably before any heavy weight additive is added
It is added in base drilling fluid.
The effect of invention
The present invention is realized using the inexpensive oil base drilling fluid emulsifying agent that waste grease is that primary raw material is prepared
Waste grease is turned waste into wealth, and reduces environmental pollution caused by the unordered discharge of waste grease；Moreover, the waste grease comes
The animals and plants of nature are come from, bio-toxicity is low, therefore emulsifying agent prepared therefrom has preferable biodegradation character, can be with
Drilling liquid technology for environmentally sensitive area is constructed, beneficial to environmental protection.
Using the emulsifying agent be applied to diesel oil, white oil, α-long-chain olefin, at least one of gentle liquefaction of long-chain ester as
The oil base drilling fluid system of base oil has good emulsifying effectiveness.And raw material sources are extensive, cost is low, therefore can be significantly
Reduce the cost of oil base drilling fluid emulsifying agent.
Embodiment
With reference to specific embodiment, the present invention will be further described, but the present invention is not limited in following embodiments.
Note：Unless otherwise specified, " part " in embodiment is parts by weight.
(1) preparation of emulsifying agent
(1) waste grease used in embodiment be the vegetable seed dregs of fat (Zhangbei County like fragrant vegetable oil purchase and sell Co., Ltd's production),
Animal oil foot (production of grease Co., Ltd of Hebei PCI-SLR Technology) and dining room swill oil (voluntarily being collected in unit dining room).
(2) the saponified of the waste grease used in embodiment is prepared by following operation：
1. by 100 parts of vegetable seed dregs of fat and the mixture of 100 parts of calcium oxide and calcium hydroxide, (the two weight ratio is 3:1) heat
To 65 DEG C, react 8 hours under agitation, cooling can be prepared by the saponified of vegetable seed grease.
2. by 100 parts of animal oil foots and the mixture of 10 parts of sodium hydroxides and potassium hydroxide, (the two weight ratio is 1:1) add
Heat is reacted 1 hour under agitation to 190 DEG C, and cooling can be prepared by the saponified of animal oil foot.
3. 100 parts of dining room swill oils and 50 parts of calcium oxide are heated into 100 DEG C, react 4 hours under agitation, cooling
It can be prepared by the saponified of swill oil.
(3) amidate of the waste grease used in embodiment is prepared by following operation：
1. by 100 parts of vegetable seed dregs of fat and 10 parts of HO-C2H4-NH2, 5 parts of sodium hydroxides and potassium hydroxide mixture (the two
Weight ratio is 1:1) 80 DEG C are heated to, is reacted 8 hours under agitation, cooling can be prepared by the amidate of vegetable seed grease.
2. by 100 parts of animal oil foots and 100 parts of N- methyl n-propylamines, the mixture (two of 50 parts of calcium oxide and lithium hydroxide
Person's weight ratio is 1:4) 180 DEG C are heated to, is reacted 2 hours under agitation, cooling can be prepared by the amidatioon of animal oil foot
Thing.
3. it is H by 100 parts of dining room swill oils and 40 parts of chemical formulas2N-C2H4-NH-C2H4-NH2Organic amine, 25 parts oxidation
Calcium is heated to 100 DEG C, reacts 6 hours under agitation, and cooling can be prepared by the amidate of swill grease.
(4) saponified, waste grease the amidate of the waste grease, waste grease is added by following parts by weight
Into mixing reactor, uniform stirring 3h is well mixed, and obtains emulsifying agent, as embodiment 1-6.By one-component and commonly use
Oil base drilling fluid emulsifying agent SP-80 1-4 as a comparison case.Wherein：
Comparative example 1：SP-80；
Comparative example 2：The vegetable seed dregs of fat；
Comparative example 3：Animal oil foot it is saponified；
Comparative example 4：The amidate of swill grease；
Embodiment 1：The vegetable seed dregs of fat：Vegetable seed grease it is saponified：The weight ratio of the amidate of vegetable seed grease is 100:
200:50；
Embodiment 2：Animal oil foot：Animal oil foot it is saponified：The weight ratio of the amidate of animal oil foot is 100:25:
25；
Embodiment 3：Dining room swill oil：Swill grease it is saponified：The weight ratio of the amidate of swill grease is 100:
125:20；
Embodiment 4：The vegetable seed dregs of fat：The weight ratio of the amidate of animal oil foot is 100:50；
Embodiment 5：Animal oil foot it is saponified：The weight ratio of the amidate of swill grease is 100:20；
Embodiment 6：Dining room swill oil：The saponified weight ratio of vegetable seed grease is 100:100.
(2) preparation of oil base drilling fluid
For the effect of effective evaluation emulsifying agent of the present invention, using following recipe configuration oil base drilling fluid, consisting of：
100 parts of base oils (in diesel oil, white oil, α-long-chain olefin, long-chain ester, gas liquefaction any one), 33 parts of mass concentrations are
25% CaCl2Emulsifying agent that the aqueous solution, 5 parts of embodiment/comparative examples are prepared, 3 parts of CaO, 4 parts of organoclays, 4 parts of oxidation drips
It is blue or green.
The preparation process of the oil base drilling fluid is：Base oil is put into jar first, in 12000rpm rotating speed
Lower addition emulsifier for mixing 10min, secondly add CaCl2The aqueous solution stirs 40min；Then organoclay, calcium oxide are sequentially added
And oxidized asphalt, every kind of material stir 20min after adding, all material is stirred for 30min after adding, you can obtains oil base drilling well
Liquid.
(3) oil base drilling fluid performance measurement
The oil base drilling fluid that different emulsifiers preparation is added with reference to GB/T16782-1997 measure is old in 80~200 DEG C of high temperature
Change emulsion-breaking voltage (ES), plastic viscosity (PV), yield value (YP) and the HTHP FL before and after 16hHTHPEtc. performance indications, as a result
It is shown in Table 1.
The oil base drilling fluid system performance of the different emulsifiers of table 1
For oil base drilling fluid, ES is higher, and explanation oil base drilling fluid emulsion stability is better, FLHTHPLower explanation oil
Base drilling fluid filtrate reducing effect is better.Usual ES values reach more than 400V, FLHTHPLess than 8mL, oil base drilling fluid just meets scene
The technical requirements of construction.
The experimental data of table 1 shows that waste grease, saponified, waste grease the amidate of waste grease individually make
Used time (comparative example 2-4), it is that emulsion stability drastically deteriorates under 150 DEG C of aging condition, ES is rapidly decreased to below 400V,
FLHTHPUnprecedented soaring, performance can not meet the requirement of wellbore construction at all；Conventional oil base drilling fluid emulsifying agent SP-80 (contrasts
Example 1) it can not also realize the stable emulsifying of oil base drilling fluid under the temperature conditionss.And use emulsifying agent (embodiment 1-6) of the present invention
From different base oils prepare oil base drilling fluid after high temperature ageing 16h within the temperature range of 80~200 DEG C, oil base drilling fluid
ES values reach more than 600V, FLHTHP6mL is below, emulsifying agent shows good emulsifying effectiveness；Wherein use embodiment 3
(dining room swill oil：Swill grease it is saponified：The amidate of swill grease is 100:125:20) the white oil base drilling well prepared
Liquid its ES after 150 DEG C of high temperature ageing 16h is up to 1386V, FLHTHPOnly 2.2mL.
(4) emulsifying agent bio-toxicity determines
In order to evaluate the bio-toxicity of emulsifying agent, the present invention is using the toxicity detection side described in GB/T18420.2-2009
Method, the toxicity of the oil base drilling fluid to configuring according to the following formulation are tested, and test result is shown in Table 2.
Oil base drilling fluid formula forms：The CaCl that 100 parts of No. 3 white oils, 33 parts of mass concentrations are 25%2The aqueous solution, 5 parts
Emulsifying agent, 3 parts of CaO, 4 parts of organoclays and 4 parts of oxidized asphalts prepared by embodiment 1-6.
The oil base drilling fluid toxotest of the different emulsifiers of table 2
According to GB/T18420.2-2009, the LC for the oil base drilling fluid of drilling at the sea50(LC50) is higher than
During 15000mg/L, reach environmental requirement of China one-level sea area to oil base drilling fluid, it is relatively low to show that the oil base drilling fluid has
Bio-toxicity；LC50When reaching 10000mg/L, reach China's two level sea area environmental requirement, it is certain to show that the oil base drilling fluid has
Bio-toxicity, but can be used for the wellbore construction in two level sea area.Table 2 detects as shown by data, emulsifying agent tool prepared by the present invention
There is extremely low bio-toxicity, China's one-level, the environmental protection standard in two level marine site can be met, available for all kinds of environmentally sensitive areas
Wellbore construction.
It should be noted that embodiment described above is only used for explaining the present invention, do not form to any of the present invention
Limitation.By referring to exemplary embodiments, invention has been described, it should be appreciated that word wherein used is descriptive
With explanatory vocabulary, rather than limited vocabulary.The present invention can be made within the scope of the claims by regulation
Modification, and the present invention is revised in without departing substantially from scope and spirit of the present invention.Although the present invention described in it relates to
And specific method, material and embodiment, it is not intended that the present invention is limited to wherein disclosed particular case, on the contrary, this hair
It is bright to can be extended to other all methods and applications with identical function.
Claims (9)
1. a kind of oil base drilling fluid emulsifying agent, the emulsifying agent is selected from waste grease, the saponified and abandoned oil of waste grease
The amidate of fat；The waste grease, waste grease saponified and waste grease amidate weight ratio be 100:0
~300:0~100, at least one of amidate of saponified and waste grease of waste grease dosage is not 0；Or
The emulsifying agent is the amidate of the saponified and waste grease of waste grease, and the waste grease is saponified and discarded
The weight ratio of the amidate of grease is 100:20；
Wherein, the amidate of the waste grease is reacted under the catalytic condition of alkali with organic amine by waste grease and obtained,
Amidation process to count in parts by weight, by 100 parts of waste greases and 10 ~ 100 parts of organic amines and 5 ~ 50 parts of alkali is heated to 80 ~
180 DEG C, react 2 ~ 8 hours under agitation, cooling can be prepared by the amidate of waste grease；
Any one of the organic amine is selected from 1) -3) compound that represents：
1) HO-C2H4-NH2、NH(-C2H4-OH)2With N (- C2H4-OH)3At least one of；
2) R1-HN-R2, wherein R1Selected from C1-C30Straight or branched saturated hydrocarbyl, C2-C30Straight or branched unsaturated hydrocarbons
Base, C3-C20Cycloalkyl, C6-C20Alkaryl, carbon number be 6-20 substituted or unsubstituted aralkyl；R2Selected from hydrogen,
C1-C30Straight or branched saturated hydrocarbyl, C2-C30Straight or branched unsaturated alkyl, C3-C20Cycloalkyl, C6-C20Alkane
Aryl, C6-C20Substituted or unsubstituted aralkyl；
3) H2N-R3-(NH-CnH2n)m-NH2, wherein R3Selected from C1-C20Straight or branched saturated hydrocarbyl, C2-C30Straight chain or
Side chain unsaturated alkyl, C3-C20Cycloalkyl, C6-C20Alkaryl, C6-C20Substituted or unsubstituted aralkyl, n 1-6
Integer, m be 0-20 integer.
2. emulsifying agent according to claim 1, it is characterised in that oil foot of the waste grease selected from refining vegetable oil,
Refine at least one of oil foot, gutter oil, swill oil and hogwash fat of animal oil.
3. emulsifying agent according to claim 1, it is characterised in that the waste grease it is saponified by waste grease with
Alkali reacts to obtain, and saponification is to count in parts by weight, and 100 parts of waste greases and 10 ~ 100 parts of alkali are heated into 60 ~ 200 DEG C,
React 1 ~ 8 hour under agitation, cooling can be prepared by the saponified of waste grease；The alkali choosing used in the saponification
From at least one of calcium hydroxide, sodium hydroxide, potassium hydroxide, calcium oxide, sodium oxide molybdena and potassium oxide.
4. emulsifying agent according to claim 1, it is characterised in that the alkali used in the amidation process is selected from hydroxide
At least one of calcium, lithium hydroxide, sodium hydroxide, potassium hydroxide, calcium oxide, sodium oxide molybdena and potassium oxide.
5. emulsifying agent according to claim 1, it is characterised in that 2) R1-HN-R2, wherein R1For C1-C6Straight chain or branch
Chain saturated hydrocarbyl, R2For hydrogen or C1-C6Straight or branched saturated hydrocarbyl；3) H2N-R3-(NH-CnH2n)m-NH2, wherein R3For
C1-C6Straight or branched saturated hydrocarbyl, n be 1-3 integer, m be 0-5 integer.
6. according to the emulsifying agent described in any one of claim 1 to 5, it is characterised in that the waste grease, the soap of waste grease
The weight ratio of the amidate of compound and waste grease is 100:100~150:10~30.
7. the preparation method of the emulsifying agent according to any one of claim 1 to 6, including by the waste grease, abandoned oil
The amidate mixing of the saponified and waste grease of fat, 2-4 h are stirred under 10000-15000rpm rotating speed, are well mixed
Obtain.
8. application of the emulsifying agent according to any one of claim 1 to 6 in oil base drilling fluid, the emulsifying agent is in oil base
Dosage in drilling fluid is 2~8 weight %.
9. application according to claim 8, it is characterised in that the base oil that the oil base drilling fluid uses is diesel oil, in vain
At least one of oil, α-long-chain olefin, the gentle liquefaction of long-chain ester.
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| CN106318349A (en) * | 2015-07-08 | 2017-01-11 | 中石化石油工程技术服务有限公司 | High-density whole-oil-base drilling fluid |
| CN111378419A (en) * | 2018-12-28 | 2020-07-07 | 天津市海罗兰科技发展股份有限公司 | High-temperature-resistant emulsifier for oil-based drilling fluid and preparation method thereof |
| CN110152645B (en) * | 2019-05-31 | 2020-10-09 | 江南大学 | Calcium-based catalyst and method for catalytically synthesizing alkanolamide surfactant by using same |
| CN110591802B (en) * | 2019-08-05 | 2022-11-25 | 浙江工业大学 | Method for preparing release agent by using waste emulsion |
| CN112322260A (en) * | 2020-10-22 | 2021-02-05 | 库尔勒郑豫石油物资有限公司 | Temperature-resistant and salt-resistant environment-friendly lubricant for drilling fluid and production and detection methods thereof |
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