CN104140792A - Emulsifier for oil-based drilling fluid as well as preparation method and application thereof - Google Patents
Emulsifier for oil-based drilling fluid as well as preparation method and application thereof Download PDFInfo
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- CN104140792A CN104140792A CN201410166050.7A CN201410166050A CN104140792A CN 104140792 A CN104140792 A CN 104140792A CN 201410166050 A CN201410166050 A CN 201410166050A CN 104140792 A CN104140792 A CN 104140792A
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- oil
- waste grease
- emulsifying agent
- grease
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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
-
- 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)
- Chemical Kinetics & Catalysis (AREA)
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- General Life Sciences & Earth Sciences (AREA)
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Abstract
The invention aims at providing an emulsifier for oil-based drilling fluid. The emulsifier is selected from any two or three types of waste oil and grease, a saponified substance of the waste oil and grease and amidate of the waste oil and grease, wherein the saponified substance of the waste oil and grease is obtained through reacting the waste oil and grease with alkali, and the amidate of the waste oil and grease is obtained through reacting the waste oil and grease with organic amine under the catalysis of alkali. The invention further provides a preparation method of the emulsifier and application of the emulsifier in the oil-based drilling fluid. The emulsifier has a good emulsifying effect; the biological toxicity is low, the cost of the emulsifier for the oil-based drilling fluid can be greatly reduced, the waste oil and grease can be changed into the valuable from the waste, and the environment pollution caused by the waste oil and grease is reduced, so that the environmental protection is facilitated.
Description
Technical field
The invention provides the preparation method and application of emulsifying agent and described drilling fluid for a kind of oil base drilling fluid, belong to petroleum drilling and use oil base drilling fluid field.
Background technology
Oil base drilling fluid has strong inhibition capability, oilness excellence, is beneficial to the many merits such as wellbore stability and reservoir protection, is the effective means of drilling well field reply bad ground, is used widely.Usually oil base drilling fluid system is called again invert mud or invert emulsion mud.Oil base drilling fluid system is to rely on emulsifying agent that disperse phase (water) is dispersed in external phase (oil phase), is therefore called again contrary emulsification system.Conventionally the quality of emulsifying agent performance has directly determined the stability of contrary emulsification system.At present, for the emulsifying agent of oil base drilling fluid, mainly comprise the anionic species tensio-active agents such as the nonionic class tensio-active agents such as sapn, tween, cycloalkanoimide and calcium stearate, calcium oleate, iron naphthenate and polyphosphazene polymer acid amides, polyether surfactant, the reasonable composite of mentioned emulsifier has good emulsifying effectiveness, but has deficiency with high costs.The cost of oil base drilling fluid has significantly been drawn high in the extensive application of above-mentioned materials in oil base drilling fluid, has limited popularization and the use of oil base drilling fluid.
Summary of the invention
It is raw material that the present invention utilizes various oil foots or trench wet goods waste grease, by rational route and gentle reaction conditions, prepare cost-efficiently oil base drilling fluid emulsifying agent, not only significantly reduce the cost of oil base drilling fluid emulsifying agent, and realized turning waste into wealth of waste grease, reduced the pollution of waste grease to environment.For the recycling of waste grease and the Sustainable development of oil resource provide an effective road, have economic implications and social effect.
Therefore, one of object of the present invention is to provide a kind of oil base drilling fluid emulsifying agent.
Another object of the present invention is to provide the preparation method of described emulsifying agent.
A further object of the present invention is to provide the application of described emulsifying agent in oil base drilling fluid.
Oil base drilling fluid of the present invention is selected from any two or three in the amidate of saponified and waste grease of waste grease, waste grease with emulsifying agent.
In one embodiment of the invention, the weight ratio of the amidate of the saponified and waste grease of described waste grease, waste grease is 100:0～300:0～100, is preferably 100:100～150:10～30.
Concrete, described waste grease is selected from the oil foot of refining vegetables oil, at least one in oil foot, sewer oil, swill oil and the hogwash fat of refining animal oil.
The saponified of described waste grease obtains by waste grease and alkali reaction.In a specific embodiment of the present invention, saponification reaction is meter by weight, and 100 parts of waste greases and 10～100 parts of alkali are heated to 60～200 ℃, reacts 1～8 hour under agitation condition, coolingly can make the saponified of waste grease.
The amidate of described waste grease is reacted and obtains with organic amine by waste grease under the catalytic condition of alkali.In a specific embodiment of the present invention, amidate action is for counting by weight, 100 parts of waste greases and 10～100 parts of organic amines and 5～50 parts of alkali are heated to 80～180 ℃, under agitation condition, react the cooling amidate that can make waste grease 2～8 hours.
In above-mentioned amidate action, described organic amine is selected from 1)-3) any in the compound that represents:
1) HO-C
2h
4-NH
2, NH (C
2h
4-OH)
2and N (C
2h
4-OH)
3in at least one;
2) R
1-HN-R
2, R wherein
1be selected from C
1-C
30straight or branched saturated hydrocarbyl, C
2-C
30straight or branched unsaturated alkyl, C
3-C
20cycloalkyl, C
6-C
20alkaryl, replacement or the unsubstituted aralkyl that carbonatoms is 6-20; R
2be selected from hydrogen, C
1-C
30straight or branched saturated hydrocarbyl, C
2-C
30straight or branched unsaturated alkyl, C
3-C
20cycloalkyl, C
6-C
20alkaryl, C
6-C
20replacement or unsubstituted aralkyl; Preferred R
1for C
1-C
6straight or branched saturated hydrocarbyl, R
2for hydrogen or C
1-C
6straight or branched saturated hydrocarbyl.
3) H
2n-R
3-(NH-C
nh
2n)
m-NH
2, R wherein
3be selected from C
1-C
20straight or branched saturated hydrocarbyl, C
2-C
30straight or branched unsaturated alkyl, C
3-C
20cycloalkyl, C
6-C
20alkaryl, C
6-C
20replacement or unsubstituted aralkyl, the integer that n is 1-6, the integer that m is 0-20, preferably R
3for C
1-C
6straight or branched saturated hydrocarbyl, the integer that n is 1-3, the integer that m is 0-5.
The alkali using in described saponification reaction and amidate action is selected from least one in calcium hydroxide, lithium hydroxide, sodium hydroxide, potassium hydroxide, calcium oxide, sodium oxide and potassium oxide.
The present invention also provides the preparation method of described emulsifying agent, comprise any two or three in the amidate of the saponified and waste grease of described waste grease, waste grease mixed, under the rotating speed of 10000-15000rpm, stir 2-4h, mix and obtain described emulsifying agent.
The present invention further provides the application of described emulsifying agent in oil base drilling fluid.Particularly, in oil base drilling fluid, use the emulsifying agent of the present invention of 2～8 % by weight.Base oil in described oil base drilling fluid is selected from least one in diesel oil, white oil, α-long-chain olefin, the gentle liquefaction of long-chain ester.In drilling fluid, also preferably contain salt solution, as a rule, adopt sodium, calcium and/or magnesium salts water.In drilling fluid, also can contain such as organic clay, emulsifying agent, pH value conditioning agent, weighting agent and fall the components such as filter humectant, these components are well-known to those skilled in the art.
Emulsifying agent of the present invention is highly active, it is believed that all or nearly all known all effective for oil base drilling fluid system.Emulsifying agent of the present invention also can be given the viscosity that drilling fluid is higher, thereby preferably before adding any weighting agent, joins in basic drilling fluid.
The effect of invention
The present invention utilizes waste grease for the low-cost oil base drilling fluid emulsifying agent that main raw material prepares, and has realized turning waste into wealth of waste grease, has reduced the environmental pollution that the unordered discharge of waste grease causes; And described waste grease derives from natural animals and plants, bio-toxicity is low, and therefore emulsifying agent prepared therefrom has good biodegradation character, can, for the drilling liquid technology construction of environmentally sensitive area, be beneficial to environment protection.
At least one oil base drilling fluid system as base oil that described emulsifying agent is applied in diesel oil, white oil, α-long-chain olefin, the gentle liquefaction of long-chain ester has good emulsifying effect.And starting material wide material sources, cost are low, therefore can significantly reduce the cost of oil base drilling fluid emulsifying agent.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described, but the present invention is not limited in following embodiment.
Note: except specified otherwise, " part " in embodiment is weight part.
(1) preparation of emulsifying agent
(1) waste grease using in embodiment is the vegetable seed dregs of fat (Zhangbei County likes fragrant vegetables oil purchase and sale company limited and produces), animal oil foot (productions of grease company limited of Hebei PCI-SLR Technology) and dining room swill oil (voluntarily in unit dining room collection).
(2) the saponified of the waste grease using in embodiment is prepared by following operation:
1. the mixture (the two weight ratio is 3:1) of 100 parts of vegetable seed dregs of fat and 100 parts of calcium oxide and calcium hydroxide is heated to 65 ℃, under agitation condition, reacts 8 hours, coolingly can make the saponified of vegetable seed grease.
2. the mixture (the two weight ratio is 1:1) of 100 parts of animal oil foots and 10 parts of sodium hydroxide and potassium hydroxide is heated to 190 ℃, under agitation condition, reacts 1 hour, coolingly can make the saponified of animal oil foot.
3. 100 parts of dining room swill oils and 50 parts of calcium oxide are heated to 100 ℃, under agitation condition, react 4 hours, coolingly can make the saponified of swill oil.
(3) amidate of the waste grease using in embodiment is prepared by following operation:
1. by 100 parts of vegetable seed dregs of fat and 10 parts of HO-C
2h
4-NH
2, 5 parts of sodium hydroxide and potassium hydroxide mixture (the two weight ratio is 1:1) be heated to 80 ℃, under agitation condition, react the cooling amidate that can make vegetable seed grease 8 hours.
2. the mixture (the two weight ratio is 1:4) of 100 parts of animal oil foots and 100 parts of N-methyl Tri N-Propyl Amines, 50 parts of calcium oxide and lithium hydroxide is heated to 180 ℃, under agitation condition, reacts the cooling amidate that can make animal oil foot 2 hours.
3. by 100 parts of dining room swill oils and 40 parts of chemical formulas, be H
2n-C
2h
4-NH-C
2h
4-NH
2organic amine, 25 parts of calcium oxide be heated to 100 ℃, under agitation condition, react the cooling amidate that can make swill grease 6 hours.
(4) by following weight part, the amidate saponified, waste grease of described waste grease, waste grease is joined in mixing reactor, uniform stirring 3h mixes, and obtains emulsifying agent, as embodiment 1-6.By one-component and conventional 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 saponified;
Comparative example 4: the amidate of swill grease;
Embodiment 1: the vegetable seed dregs of fat: vegetable seed grease saponified: the weight ratio of the amidate of vegetable seed grease is 100:200:50;
Embodiment 2: animal oil foot: animal oil foot saponified: the weight ratio of the amidate of animal oil foot is 100:25:25;
Embodiment 3: dining room swill oil: swill grease 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 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
Effect for effective evaluation emulsifying agent of the present invention, adopt following recipe configuration oil base drilling fluid, it consists of: 100 parts of base oils (any one in diesel oil, white oil, α-long-chain olefin, long-chain ester, gas liquefaction), 33 parts of CaCl that mass concentration is 25%
2the aqueous solution, 5 parts of emulsifying agent, 3 parts of CaO, 4 parts of organophilic clays, 4 parts of oxidized bitumens that embodiment/comparative example prepares.
The preparation process of described oil base drilling fluid is: first in jar, put into base oil, add emulsifier for mixing 10min under the rotating speed of 12000rpm, next adds CaCl
2the aqueous solution stirs 40min; Then add successively organophilic clay, calcium oxide and oxidized bitumen, every kind of material adds rear stirring 20min, after all material adds, stirs 30min again, can obtain oil base drilling fluid.
(3) oil base drilling fluid performance measurement
With reference to GB/T16782-1997, measure and add the oil base drilling fluid of different emulsifiers preparation at emulsion-breaking voltage (ES), plastic viscosity (PV), yield value (YP) and the High Temperature High Pressure FL of 80～200 ℃ of high temperature ageing 16h front and back
hTHPetc. performance index, the results are shown in Table 1.
The oil base drilling fluid system performance of table 1 different emulsifiers
For oil base drilling fluid, the higher explanation oil base drilling fluid of ES emulsifying stability is better, FL
hTHPit is better that filtration effect falls in lower explanation oil base drilling fluid.Conventionally more than ES value reaches 400V, FL
hTHPlower than 8mL, oil base drilling fluid just meets the technical requirements of site operation.
The experimental data of table 1 shows, when the amidate saponified, waste grease of waste grease, waste grease is used separately (comparative example 2-4), is that emulsifying stability sharply worsens under the aging condition of 150 ℃, and ES is down to rapidly below 400V, FL
hTHPunprecedented soaring, performance cannot meet the requirement of wellbore construction at all; Conventional oil base drilling fluid emulsifying agent SP-80 (comparative example 1) also cannot realize the stable emulsifying of oil base drilling fluid under this temperature condition.And adopt oil base drilling fluid that emulsifying agent of the present invention (embodiment 1-6) prepares with different base oils in the temperature range of 80～200 ℃ after high temperature ageing 16h, and more than the ES value of oil base drilling fluid all reaches 600V, FL
hTHPall, lower than 6mL, emulsifying agent shows good emulsifying effect; The white oil base drilling fluid that wherein adopts embodiment 3 (dining room swill oil: swill grease saponified: the amidate of swill grease is 100:125:20) preparation after 150 ℃ of high temperature ageing 16h its ES up to 1386V, FL
hTHPbe only 2.2mL.
(4) emulsifying agent bio-toxicity is measured
In order to evaluate the bio-toxicity of emulsifying agent, the present invention adopts the detection method of toxicity described in GB/T18420.2-2009, and the toxicity of the oil base drilling fluid configuring is according to the following formulation tested, and test result is in Table 2.
Oil base drilling fluid formula consists of: 100 parts of No. 3 white oils, 33 parts of CaCl that mass concentration is 25%
2the aqueous solution, 5 parts of emulsifying agent, 3 parts of CaO, 4 parts of organophilic clays and 4 parts of oxidized bitumens prepared by embodiment 1-6.
The oil base drilling fluid toxotest of table 2 different emulsifiers
According to GB/T18420.2-2009, for the LC of the oil base drilling fluid of sea boring
50(median lethal concentration) during higher than 15000mg/L, reaches the environmental requirement of China's one-level sea area to oil base drilling fluid, shows that this oil base drilling fluid has lower bio-toxicity; LC
50while reaching 10000mg/L, reach the sea area environmental requirement of China's secondary, show that this oil base drilling fluid has certain bio-toxicity, but can be for the wellbore construction in secondary sea area.Table 2 detects data and shows, emulsifying agent prepared by the present invention has extremely low bio-toxicity, can meet the environmental protection standard in China's one-level, secondary marine site, can be used for the wellbore construction of all kinds of environmentally sensitive areas.
It should be noted in the discussion above that above-described embodiment, only for explaining the present invention, does not form any limitation of the invention.By with reference to exemplary embodiments, invention has been described, but should be understood to word wherein used, be descriptive and explanatory vocabulary, rather than limited vocabulary.Can in the scope of the claims in the present invention, to the present invention, modify in accordance with regulations, and within not deviating from scope and spirit of the present invention, the present invention be revised.Although the present invention who wherein describes relates to specific method, material and embodiment, and does not mean that the present invention is limited to wherein disclosed particular case, on the contrary, the present invention can extend to other all methods and applications with identical function.
Claims (10)
1. an oil base drilling fluid emulsifying agent, described emulsifying agent is selected from any two or three in the amidate of saponified and waste grease of waste grease, waste grease.
2. emulsifying agent according to claim 1, is characterized in that, described waste grease is selected from the oil foot of refining vegetables oil, at least one in oil foot, sewer oil, swill oil and the hogwash fat of refining animal oil.
3. emulsifying agent according to claim 1, it is characterized in that, the saponified of described waste grease obtains by waste grease and alkali reaction, preferably saponification reaction is for counting by weight, 100 parts of waste greases and 10～100 parts of alkali are heated to 60～200 ℃, under agitation condition, react 1～8 hour, coolingly can make the saponified of waste grease.
4. emulsifying agent according to claim 1, it is characterized in that, the amidate of described waste grease is reacted and obtains with organic amine by waste grease under the catalytic condition of alkali, preferred amideization reaction is for counting by weight, 100 parts of waste greases and 10～100 parts of organic amines and 5～50 parts of alkali are heated to 80～180 ℃, under agitation condition, react the cooling amidate that can make waste grease 2～8 hours.
5. according to the emulsifying agent described in claim 3 or 4, it is characterized in that, the alkali using in described saponification reaction and amidate action is selected from least one in calcium hydroxide, lithium hydroxide, sodium hydroxide, potassium hydroxide, calcium oxide, sodium oxide and potassium oxide.
6. emulsifying agent according to claim 4, is characterized in that, described organic amine is selected from 1)-3) any in the compound that represents:
1) HO-C
2h
4-NH
2, NH (C
2h
4-OH)
2and N (C
2h
4-OH)
3in at least one;
2) R
1-HN-R
2, R wherein
1be selected from C
1-C
30straight or branched saturated hydrocarbyl, C
2-C
30straight or branched unsaturated alkyl, C
3-C
20cycloalkyl, C
6-C
20alkaryl, replacement or the unsubstituted aralkyl that carbonatoms is 6-20; R
2be selected from hydrogen, C
1-C
30straight or branched saturated hydrocarbyl, C
2-C
30straight or branched unsaturated alkyl, C
3-C
20cycloalkyl, C
6-C
20alkaryl, C
6-C
20replacement or unsubstituted aralkyl; Preferred R
1for C
1-C
6straight or branched saturated hydrocarbyl, R
2for hydrogen or C
1-C
6straight or branched saturated hydrocarbyl.
3) H
2n-R
3-(NH-C
nh
2n)
m-NH
2, R wherein
3be selected from C
1-C
20straight or branched saturated hydrocarbyl, C
2-C
30straight or branched unsaturated alkyl, C
3-C
20cycloalkyl, C
6-C
20alkaryl, C
6-C
20replacement or unsubstituted aralkyl, the integer that n is 1-6, the integer that m is 0-20, preferably R
3for C
1-C
6straight or branched saturated hydrocarbyl, the integer that n is 1-3, the integer that m is 0-5.
7. according to the emulsifying agent described in claim 1 to 6 any one, it is characterized in that, the weight ratio of the amidate of the saponified and waste grease of described waste grease, waste grease is 100:0～300:0～100, is preferably 100:100～150:10～30.
8. according to the preparation method of the emulsifying agent described in claim 1 to 7 any one, comprise any two or three in the amidate of the saponified and waste grease of described waste grease, waste grease mixed, under the rotating speed of 10000-15000rpm, stir 2-4h, mix and obtain.
9. the application in oil base drilling fluid according to the emulsifying agent described in claim 1 to 8 any one, the dosage of described emulsifying agent in oil base drilling fluid is 2～8 % by weight.
10. application according to claim 9, is characterized in that, the base oil that described oil base drilling fluid is used is at least one in diesel oil, white oil, α-long-chain olefin, the gentle liquefaction of long-chain ester.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN110591802A (en) * | 2019-08-05 | 2019-12-20 | 浙江工业大学 | Method for preparing release agent by using waste emulsion |
| 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 |
| 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 |
| US20210087136A1 (en) * | 2019-05-31 | 2021-03-25 | Jiangnan University | Calcium-based Catalyst and Method for Catalytically Synthesizing Alkanolamide Surfactant thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| US20210087136A1 (en) * | 2019-05-31 | 2021-03-25 | Jiangnan University | Calcium-based Catalyst and Method for Catalytically Synthesizing Alkanolamide Surfactant thereof |
| CN110591802A (en) * | 2019-08-05 | 2019-12-20 | 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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| CN104140792B (en) | 2018-03-30 |
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