CN114479781B - Low-condensation-point emulsifier and preparation method thereof - Google Patents
Low-condensation-point emulsifier and preparation method thereof Download PDFInfo
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- CN114479781B CN114479781B CN202011148426.3A CN202011148426A CN114479781B CN 114479781 B CN114479781 B CN 114479781B CN 202011148426 A CN202011148426 A CN 202011148426A CN 114479781 B CN114479781 B CN 114479781B
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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
- 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
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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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Abstract
The invention relates to a low-condensation-point emulsifier which comprises oleic alcohol amine, alkyl sulfonate or a derivative thereof, dipropylene glycol ether and alkali. The invention also provides a preparation method of the low-freezing-point emulsifier, which comprises the following steps: mixing and heating the oleyl alcohol amine and the alkyl sulfonate or the derivative thereof according to a proportion, stirring and dissolving; adding alkali to react for 1-4 hours at 100-150 ℃; adding dipropylene glycol ether, reacting for 1-2 hours, and cooling to obtain the low-condensation-point emulsifier. The preparation method is simple, the process is reasonable and mild, and the obtained low-condensation-point emulsifier has good emulsifying effect and can resist the temperature of 150 ℃.
Description
Technical Field
The invention relates to the technical field of oilfield chemistry, in particular to a low-condensation-point emulsifier, a preparation method and application thereof.
Background
An oil-based drilling fluid refers to a drilling fluid that has oil as the continuous phase. Compared with water-based drilling fluid, the oil-based drilling fluid has the advantages of high temperature resistance, salt and calcium invasion resistance, good lubricity, contribution to well wall stability, less damage to oil and gas layers and the like. With the increase of complex stratum drilling and the rapid development of shale oil and gas resources, the oil-based drilling fluid in China has a wide technical demand market.
The emulsifier is an important treating agent in the oil-based drilling fluid, and the advantages and disadvantages of the emulsifier directly determine the stability of the oil-based drilling fluid system and have important influence on the rheological property of the oil-based drilling fluid. The emulsifier commonly used at present mainly comprises nonionic surfactants such as span, tween, naphthenic acid amide and the like, anionic surfactants such as calcium stearate, calcium oleate, iron naphthenate and the like, and high molecular polyamide and polyether surfactants. Along with the low-temperature construction in winter or alpine regions, the surfactant has the advantages of increased viscosity under low-temperature conditions (for example, the temperature below 0 ℃), difficult storage and influence on site use, and limits the popularization and application range of the oil-based drilling fluid.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a low-condensation-point emulsifier which comprises an oleic alcohol amine, alkyl sulfonate or a derivative thereof and dipropylene glycol ether which are used as main raw materials, and a preparation method with a reasonable route and mild reaction conditions, so that the problem that the conventional emulsifier is difficult to flow at low temperature can be solved, and the application scale of oil-based drilling fluid in a low-temperature environment can be enlarged.
Accordingly, a first aspect of the present invention provides a low-set point emulsifier comprising an oleyl amine, an alkyl sulfonate or derivative thereof, a dipropylene glycol ether and a base.
In an embodiment of the present invention, the oleyl amine comprises one or two of oleyl monoethanolamine and oleyl diethanolamine.
In an embodiment of the present invention, the alkyl sulfonate or the derivative thereof includes one or more of alkyl aryl sulfonate, alkyl sulfonate, aryl sulfonate, alkyl sulfamate, cycloalkyl sulfamate, alkyl cycloalkyl sulfamate, aryl sulfamate, alkyl aryl sulfamate, fatty acid-2-sulfonate, cycloalkyl sulfonate, alkyl disulfonate, cycloalkyl disulfonate, aryl disulfonate, alkylaryl disulfonate, aryl trisulfonate and alkylaryl trisulfonate having 6 to 40 carbon atoms, and petroleum sulfonate; preferably, in an embodiment of the present invention, the alkyl sulfonate or the derivative thereof includes one or more of alkyl sulfonate, alkylaryl sulfonate, petroleum sulfonate having 6 to 40 carbon atoms; more preferably, in an embodiment of the present invention, the alkyl sulfonate or its derivative is one or more of sodium dodecyl sulfonate, calcium petroleum sulfonate or alkyl sulfonate. Preferably, in an embodiment of the present invention, the sulfonate is one or several of calcium sulfonate, sodium sulfonate and potassium sulfonate.
In an embodiment of the present invention, the dipropylene glycol ethers include one or more of dipropylene glycol methyl ether and dipropylene glycol ethyl ether.
In an embodiment of the invention, the base comprises an alkaline earth metal carbonate, bicarbonate, hydroxide or oxide; more preferably, the alkali comprises one or more of calcium oxide, calcium hydroxide, sodium hydroxide, and potassium hydroxide.
In the embodiment of the invention, the low-freezing point emulsifier comprises the following components in parts by weight:
another aspect of the present invention is to provide a method for preparing the above low-freezing point emulsifier, comprising the steps of:
(1) Mixing and heating the oleyl alcohol amine and the alkyl sulfonate or the derivative thereof according to a proportion, stirring and dissolving;
(2) Adding alkali to react for 1-4 hours at 100-150 ℃;
(3) Adding dipropylene glycol ether, reacting for 1-2 hours, and cooling to obtain the low-condensation-point emulsifier.
Preferably, in an embodiment of the present invention, the preparation method of the low-freezing point emulsifier includes the following steps: 100 parts by weight of the oleyl alcohol amine and 200-350 parts by weight of the alkyl sulfonate are mixed and heated to 120-150 ℃, stirred and fully dissolved, 4-17 parts by weight of alkali is added to react for 1-4 hours at 100-150 ℃, 20-40 parts by weight of dipropylene glycol ether is added to react for 1-2 hours, and the low-condensation-point emulsifier is prepared after cooling.
It is a further aspect of the present invention to provide an oil-based drilling fluid system comprising a low set point emulsifier as described above and a base oil, wherein the low set point emulsifier is present in an amount of 2 to 6% by weight.
A further aspect of the invention is to provide the use of a low congealing point emulsifier as described above in a drilling fluid; more preferably, in an embodiment of the present invention, the use of the low-freezing point emulsifier in a drilling fluid is the use of an emulsifier in an oil-based drilling fluid.
Compared with the prior art, the invention has at least the following advantages:
1. the reaction process used in the preparation method of the low-condensation-point emulsifier is simple, reasonable and mild;
2. the emulsifier can be applied to oil-based drilling fluid systems with diesel oil, white oil, alpha-long-chain olefin, long-chain ester, gas-produced oil and mixtures thereof as base oil, and has good emulsifying effect and temperature resistance reaching 150 ℃.
3. The solidifying point of the emulsifier is-20 ℃ to-25 ℃, so that the viscosity of the emulsifier at low temperature is greatly reduced, and the construction of the oil-based drilling fluid under high and cold conditions is facilitated.
In addition, the raw materials of the oleyl alcohol amine, the alkyl sulfonate and the dipropylene glycol ether are easy to obtain, the product quality is stable, and the large-scale production is easy, so that the invention has better application prospect.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
The invention will be further illustrated with reference to the following examples, which are not intended to limit the invention.
Unless otherwise indicated, in the examples of the present invention, "parts" refer to parts by weight.
Example 1: preparation example of the emulsifier of the invention
(1) The raw materials of the emulsifier are the composition of alcohol amine oleate, alkyl sulfonate, dipropylene glycol ether and alkali.
(2) The main materials used in this example are as follows: the oleyl amine is produced by Zhengzhou good Hongjia chemical products, the sodium dodecyl sulfonate (chemical purity) is produced by Beijing chemical agents, the calcium alkyl benzene sulfonate is produced by the Chen-lan auxiliary agent factory, the calcium petroleum sulfonate is produced by the Chen-lan auxiliary agent factory, the dipropylene glycol ether is produced by the American Dow chemical agents, the calcium oxide, the calcium hydroxide, the sodium hydroxide and the potassium hydroxide (chemical purity) are all produced by Beijing chemical agents, the organic soil is produced by Zhejiang Feng Hong new materials, and the filtrate loss reducer is American energy Co.
(3) The composition of the emulsifier of this example is as follows (total weight 150 g):
emulsifier 1 is sodium hydroxide, oleic acid monoethanolamine, dipropylene glycol methyl ether and sodium dodecyl sulfonate in the ratio of 1:25:5:50; emulsifier 2 is potassium hydroxide, oleic acid monoethanolamine, dipropylene glycol ethyl ether and sodium dodecyl sulfonate in the ratio of 1:25:10:85;
the emulsifier 3 is calcium hydroxide, oleic acid monoethanolamine, dipropylene glycol methyl ether and petroleum calcium sulfonate in the ratio of 1:6:2:15;
emulsifier 4 is potassium hydroxide, diethanolamine oleate, dipropylene glycol methyl ether and calcium petroleum sulfonate in the ratio of 1:12:2:26;
emulsifier 5 is calcium hydroxide, oleic acid diethanolamine, dipropylene glycol ethyl ether and calcium alkyl benzene sulfonate in the ratio of 1:20:6:50;
emulsifier 6: the ratio of sodium hydroxide to oleic acid diethanolamine to dipropylene glycol ethyl ether to calcium alkyl benzene sulfonate is 1:10:20:30.
(4) The emulsifier of this example was prepared as follows in the proportions shown in (3):
emulsifier 1: and (3) placing the oleic acid monoethanolamine and the sodium dodecyl sulfonate into a glass inclined-diameter four-neck flask, mixing and heating to 100 ℃, stirring for full dissolution, adding sodium hydroxide to react for 4 hours at 100 ℃, adding dipropylene glycol methyl ether to react for 1 hour, and cooling to obtain the low-condensation-point emulsifier 1.
Emulsifier 2: and (3) placing the oleic acid monoethanolamine and sodium dodecyl sulfonate into a glass inclined-diameter four-neck flask, mixing and heating to 120 ℃, stirring for full dissolution, adding potassium hydroxide, reacting for 4 hours at 120 ℃, adding dipropylene glycol ethyl ether, reacting for 2 hours, and cooling to obtain the low-condensation-point emulsifier 2.
Emulsifier 3: and (3) placing the oleic acid monoethanolamine and the petroleum calcium sulfonate into a glass inclined-diameter four-neck flask, mixing and heating to 150 ℃, stirring for full dissolution, adding calcium hydroxide for reaction for 2 hours at 150 ℃, adding dipropylene glycol methyl ether for reaction for 2 hours, and cooling to obtain the low-condensation-point emulsifier 3.
Emulsifier 4: and (3) putting the oleic acid diethanolamine and the petroleum calcium sulfonate into a glass inclined-diameter four-neck flask, mixing and heating to 150 ℃, stirring for full dissolution, adding potassium hydroxide for reaction for 1 hour at 150 ℃, adding dipropylene glycol methyl ether for reaction for 1 hour, and cooling to obtain the low-condensation-point emulsifier 4.
Emulsifier 5: and (3) putting the oleic acid diethanolamine and the calcium alkylbenzenesulfonate into a glass inclined-diameter four-neck flask, mixing and heating to 120 ℃, stirring for full dissolution, adding calcium hydroxide, reacting for 4 hours at 120 ℃, adding dipropylene glycol ethyl ether, reacting for 4 hours, and cooling to obtain the low-condensation-point emulsifier 5.
Emulsifier 6: and (3) putting the oleic acid diethanolamine and the calcium alkylbenzenesulfonate into a glass inclined-diameter four-neck flask, mixing and heating to 100 ℃, stirring for full dissolution, adding sodium hydroxide for reaction for 4 hours at 100 ℃, adding dipropylene glycol ethyl ether for reaction for 3 hours, and cooling to obtain the low-condensation-point emulsifier 6.
Example 2: oil-based drilling fluid preparation examples containing the emulsifier of the invention
In order to effectively evaluate the effect of the emulsifier, an oil-based drilling fluid system is prepared by adopting the following formula, wherein the formula comprises the following components: 100 parts by weight of base oil (diesel oil, white oil, alpha-long-chain olefin, refined mineral oil or gas oil), 33 parts by weight of CaCl with mass concentration of 25% 2 The water solution, 7 parts by weight of the emulsifier 1 to 6 parts by weight of the emulsifier 1 in the embodiment of the invention, 3 parts by weight of CaO, 4 parts by weight of organic soil and 4 parts by weight of filtrate reducer.
The formula is configured according to the following steps:
in the stirring cupAdding base oil for oil-based drilling fluid, adding an emulsifying agent under 12000 r/min stirring, and stirring at high speed for 20min; then CaCl is added 2 Brine is stirred at a high speed for 20min; and sequentially adding organic soil, calcium oxide and a filtrate reducer into the mixed system, stirring for 20min at 12000 r/min after each material is added, and stirring for 30min after all materials are added, so that the oil-based drilling fluid system can be obtained.
Example 3: oil-based drilling fluid performance determination
The emulsion breaking voltage ES, the plastic viscosity PV and the dynamic shear force YP of the oil-based drilling fluid systems with different emulsifier configurations are measured by referring to GB/T16782-1997, and the test results are shown in Table 1.
Referring to GB/T510 "petroleum product congeal Point determination method", the congeal points of different emulsifiers were determined by using a full-automatic Handa HD510-2Z pour point congeal point determination device from Johnda instruments and meters, inc., and the test results are shown in Table 1.
TABLE 1 oil-based drilling fluid system Performance of different emulsifiers
Table 1 shows that the emulsifier prepared by the invention has a condensation point of-20 ℃ to-25 ℃ and has good emulsifying effect after aging at 150 ℃ in oil-based drilling fluids consisting of different base oils. Compared with the common commercially produced span 80 emulsifier, the emulsifier prepared by the invention has lower condensation point and better emulsion stability; compared with the common polyether triol emulsifier, the emulsion breaking voltage before and after aging is higher, which indicates that the emulsion stability is stronger, and the plastic viscosity and the dynamic shear force of the prepared oil-based drilling fluid are higher, which indicates that the rheological property is better.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (6)
1. The low-freezing point emulsifier suitable for the oil-based drilling fluid comprises the following components in parts by weight:
100 parts of oleyl alcohol amine;
200-350 parts of alkyl sulfonate or a derivative thereof;
4-17 parts of alkali;
20-40 parts of dipropylene glycol ether;
the preparation method of the low-freezing-point emulsifier comprises the following steps:
(1) Mixing and heating the oleyl alcohol amine and the alkyl sulfonate or the derivative thereof according to a proportion, stirring and dissolving;
(2) Adding alkali to react for 1-4 hours at 100-150 ℃;
(3) Adding dipropylene glycol ether, reacting for 1-2 hours, and cooling to obtain the low-condensation-point emulsifier;
the oleyl amine comprises one or two of oleyl monoethanolamine and oleyl diethanolamine;
the alkyl sulfonate or the derivative thereof comprises one or more of alkyl aryl sulfonate, alkyl sulfonate, aryl sulfonate, cycloalkyl sulfonate, alkyl disulfonate, cycloalkyl disulfonate, aryl disulfonate, alkyl aryl disulfonate, aryl trisulfonate, alkyl aryl trisulfonate and petroleum sulfonate with the carbon number of 6-40; wherein the sulfonate is one or more of calcium sulfonate, sodium sulfonate and potassium sulfonate;
the dipropylene glycol ether comprises one or more of dipropylene glycol methyl ether and dipropylene glycol ethyl ether;
the alkali includes carbonate of alkaline earth metal, bicarbonate of alkaline earth metal, hydroxide of alkaline earth metal, oxide of alkaline earth metal, sodium hydroxide, potassium hydroxide.
2. The low-freezing point emulsifier of claim 1, wherein the base comprises one or more of calcium oxide, calcium hydroxide, sodium hydroxide, potassium hydroxide.
3. A process for preparing the low-freezing point emulsifier according to claim 1 or 2, comprising the steps of:
(1) Mixing and heating the oleyl alcohol amine and the alkyl sulfonate or the derivative thereof according to a proportion, stirring and dissolving;
(2) Adding alkali to react for 1-4 hours at 100-150 ℃;
(3) And adding dipropylene glycol ether, reacting for 1-2 hours, and cooling to obtain the low-condensation-point emulsifier.
4. A method according to claim 3, comprising the steps of:
mixing 100 parts by weight of oleyl alcohol amine and 200-350 parts by weight of alkyl sulfonate, heating to 120-150 ℃, stirring and dissolving, adding 4-17 parts by weight of alkali, reacting for 1-4 hours at 100-150 ℃, adding 20-40 parts of dipropylene glycol ether, reacting for 1-2 hours, and cooling to obtain the low-condensation-point emulsifier.
5. An oil-based drilling fluid system comprising the low set point emulsifier of claim 1 or 2 in combination with a base oil, wherein the low set point emulsifier is 2 to 6% by weight.
6. Use of a low set point emulsifier according to claim 1 or 2 in a drilling fluid.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB446314A (en) * | 1935-06-04 | 1936-04-28 | Standard Oil Dev Co | Improvements relating to the emulsification of oils |
| US6793025B2 (en) * | 1998-01-08 | 2004-09-21 | M-I L. L. C. | Double emulsion based drilling fluids |
| US6855673B2 (en) * | 2002-11-08 | 2005-02-15 | Kelsan Technologies Corporation | Freeze tolerant friction control compositions |
| CN102719296B (en) * | 2012-06-12 | 2013-07-31 | 河南师范大学 | General type oil compound emulsifying agent and preparation method thereof |
| CN103897671B (en) * | 2012-12-27 | 2017-02-01 | 中国石油化工股份有限公司 | High-performance composite oil-based emulsifier and its preparation method |
| EP3022272A4 (en) * | 2013-09-11 | 2017-02-22 | Halliburton Energy Services, Inc. | Asphaltene-dissolving oil-external emulsion for acidization and methods of using the same |
| CN104689754A (en) * | 2013-12-10 | 2015-06-10 | 王东奎 | Rubber emulsifying agent |
| US10544354B2 (en) * | 2014-02-12 | 2020-01-28 | Halliburton Energy Services, Inc. | Viscosifier for enhanced oil recovery |
| CN105131927B (en) * | 2015-09-01 | 2020-04-17 | 石家庄长宏能源科技有限公司 | Surfactant for binary combination flooding and preparation method thereof |
| US11214726B2 (en) * | 2016-11-01 | 2022-01-04 | Timothy B Jeter | Compositions for drilling applications |
| CN107828391A (en) * | 2017-12-07 | 2018-03-23 | 联技精细材料(珠海)有限公司 | A kind of high temperature emulsifying agent applied to oil base drilling fluid and preparation method thereof |
| CN109021954A (en) * | 2018-08-13 | 2018-12-18 | 常州艾乐森动力技术有限公司 | Less toxic oil emulsifier |
| CN109055060A (en) * | 2018-09-28 | 2018-12-21 | 何治伟 | A kind of preparation method of oil smoke high-efficient purification additive |
| 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 |
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