CN102051243A - Diesel emulsion and preparation method thereof - Google Patents
Diesel emulsion and preparation method thereof Download PDFInfo
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- CN102051243A CN102051243A CN201110000286XA CN201110000286A CN102051243A CN 102051243 A CN102051243 A CN 102051243A CN 201110000286X A CN201110000286X A CN 201110000286XA CN 201110000286 A CN201110000286 A CN 201110000286A CN 102051243 A CN102051243 A CN 102051243A
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- diesel oil
- milk sap
- lauramide
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Abstract
The invention relates to a diesel emulsion and a preparation method thereof. The diesel emulsion is prepared by mixing N, N'-ethylene bis [N(sodium ethane sulfonate)-dodecanoic acid amide as a main agent of the emulsion with 0-model diesel oil, and adding an NaCl aqueous solution, alcohol and ethanolamine. The diesel emulsion has the advantages of good stability, low viscosity and good atomization effect, the combustion ratio of the diesel emulsion can be effectively improved, and the environmental pollution is reduced.
Description
Technical field
The invention belongs to petrochemical industry, be specifically related to the preparation of diesel oil milk sap.
Background technology
Because petroleum resources shortage and price increase thereof and environmental pollution day by day are serious day by day, the development low emission has caused the attention of countries in the world for oil fuel, particularly combustion diesel fuel-emulsifying water the fuel that comes into the picture now, compare with ordinary diesel oil, diesel oil emulsification has characteristics such as have good burning performance, energy consumption is low, pollution is few, is a kind of novel fuel.
The emulsifying agent that present diesel oil emulsification is used mainly is with carboxylate salt, Span series and Tween more composite cats products of series and polymer.Though these diesel oil emulsion systems can reach emulsifying effectiveness and bigger water capacity preferably, also there is more problem in the emulsion system for preparing with this emulsifying agent, and (1) milk sap shelf time is short, and steady time is generally all at 6-30 days; (2) viscosity ratio of milk sap is bigger, and mobile bad, the particle of atomizing is bigger, is not easy abundant burning, has increased environmental pollution; (3) the compound system cost is than higher; (4) existing diesel oil emulsification corrodibility height has reduced the work-ing life of engine etc., has therefore limited applying of diesel oil emulsification.
In order to overcome existing milk sap weak point steady time, highly corrosive, full-bodied shortcoming, and then reach the purpose of energy-conserving and environment-protective, just need look for a kind of emulsify well, cheap emulsifying agent.Because the special construction of Gemini surface active agent can and then greatly reduce oil water interfacial tension so that surfactant molecule is arranged closely on the interface, reduced the energy of emulsion system effectively, the formation that helps milk sap more is with stable.
In January, 2007, Yang Yang has introduced it and has utilized heavy alkyl benzene to prepare the method for diesel oil milk sap as diesel oil emulsifier for a kind of sulphonate type gemini surfactant of main raw material synthetic at its Master's thesis " the synthetic research that reaches diesel oil microemulsion of Gemini tensio-active agent " 38-48 page or leaf, utilize the diesel oil emulsion's stability of this Gemini surface active agent preparation to have more superior stability than the diesel oil milk sap that conventional surfactant prepares, but its viscosity very high (viscosity 15mPaS) is not suitable for as oil fuel.
CN101906333A (CN201010253683.3) provides a kind of engine diesel oil emulsifier and engine emulsified diesel oil.The engine diesel oil emulsifier includes 2: 5 by volume: the sodium oleate of (8～12) is full, and to close solution, OP-ethanol, Nonyl pheno (4) ether NP-4 mixed.Engine diesel oil emulsifier and moisture diesel oil are pressed 1: 500 volume ratio, and wherein the water content of diesel oil accounts for the 9-10% of diesel oil volume, and emulsification makes engine emulsified diesel oil in 40-55 ℃ of temperature.The engine diesel oil emulsifier of the technical program and engine emulsified diesel oil has the viscosity close with pure diesel oil and density, transparency height, it is not stratified to stablize, and the emulsification consumption is low, the emulsification cost is low.But the milk sap of its preparation can only be stablized 60d, and need prepare being higher than under the condition of room temperature, has improved the preparation cost of milk sap.
Summary of the invention
At the deficiencies in the prior art, the invention provides with a kind of diesel oil milk sap and preparation method thereof.
The present invention adopts a kind of Gemini surface active agent of sulfonate type as diesel oil emulsifier, and prepared diesel oil milk sap has advantages such as stability is better, milk sap viscosity is low.
Technical solution of the present invention is as follows:
Diesel oil milk sap of the present invention is that the raw material by following mass percent makes:
N, two [N (the ethyl sulfonic acid sodium)-lauramide] 15-25% of N '-ethylene
Sapn or tween surfactants 0-5%
0
#Diesel oil 50-65%
NaCl aqueous solution 5-10%
Alcohol 10-20%
Thanomin 2-7%.
More than each component sum be 100%.
Described alcohol is one of Virahol, propyl carbinol, Pentyl alcohol or n-Octanol or its combination, and preferred Virahol and propyl carbinol are pressed 1: 1 combination of mass ratio.
Described sapn or tween surfactants are selected from span80, span60, span20, tween80, tween60 or tween20.
The described NaCl aqueous solution, mass concentration are 0.5%-2%; Preferred NaCl aqueous solution mass concentration is 1%-1.5%.
According to the present invention, preferred, diesel oil milk sap is that the raw material by following mass percent makes:
N, two [N (the ethyl sulfonic acid sodium)-lauramide] 15-20% of N '-ethylene
Sapn or tween surfactants 0-3%
0
#Diesel oil 50-65%
The NaCl aqueous solution 5-8% of 1wt%
Pentyl alcohol, n-Octanol or 1: 1 Virahol of mass ratio and propyl carbinol 10-20%
Thanomin 3-6%.
More than each component sum be 100%.
According to the present invention, further preferred scheme is as follows:
Diesel oil milk sap raw material is formed mass percent:
0
#Diesel oil 54.12%
N, two [N (ethyl sulfonic acid sodium)-lauramide] 17.21% of N '-ethylene
The NaCl solution 7.28% of 1wt%
span80 2.06％
Thanomin 5.25%
Virahol and propyl carbinol (mass ratio 1: 1) 14.08%.
Diesel oil milk sap raw material is formed mass percent:
0
#Diesel oil 60.42%
N, two [N (ethyl sulfonic acid sodium)-lauramide] 16.20% of N '-ethylene
The NaCl solution 5.22% of 1wt%
Thanomin 5.14%
tween80 2.00％
1: 1 Virahol and propyl carbinol 11.02%.
Diesel oil milk sap raw material is formed mass percent:
0
#Diesel oil 55.40%
N, two [N (ethyl sulfonic acid sodium)-lauramide] 15.88% of N '-ethylene
The NaCl solution 5.47% of 1wt%
Thanomin 3.26%
span60 2.25％
N-Octanol 17.74%.
N of the present invention, the preparation method of N '-ethylene two [N (ethyl sulfonic acid sodium)-lauramide] is as follows:
(1) quadrol and 2-bromotrifluoromethane sodium sulfonate in molar ratio 1: (2-2.5), prepared in reaction intermediate compound I under temperature 50-70 ℃, the condition of pH value 9-10, the molecular formula of intermediate compound I is: NaSO
3(CH
2)
2NH (CH
2)
2NH (CH
2)
2SO
3Na.
Chemical equation is as follows:
(2) lauroyl chloride and intermediate compound I (2-2.5) in molar ratio: 1, reaction obtains sulphonate type gemini surfactant N under the ice-water bath condition, N '-ethylene two [N (ethyl sulfonic acid sodium)-lauramide], molecular formula is:
Chemical equation is as follows:
More specifically, N, the preparation method of N '-ethylene two [N (ethyl sulfonic acid sodium)-lauramide], step is as follows:
1) in the there-necked flask that stirring, actuator temperature meter, reflux condensing tube are housed, adds 4mL quadrol and less water, stir and be heated to 60 ℃.42.2g 2-bromotrifluoromethane sodium sulfonate is soluble in water, after the dissolving fully, drip 2-bromotrifluoromethane sodium sulfonate solution, after dropwising, be 9-10 with the pH value of NaOH solution regulation system, reacted 12 hours.After reaction finished, cooling added people's dehydrated alcohol reaction product is separated out in solution, and suction filtration is dried products therefrom at vacuum drying oven, and faint yellow solid is intermediate compound I.
2) the 17.14g intermediate compound I is dissolved in the mixing solutions of distilled water/acetone, pour in the there-necked flask that agitator is housed, under violent stirring, slowly drip the 25.5mL lauroyl chloride, drip triethylamine/acetone soln simultaneously, keeping the pH value is 7.5-8.5, and ice-water bath reacted 6 hours down.After reaction finishes, pour reaction solution into beaker, but spending the night in refrigerator and cooled has precipitation to separate out, suction filtration is used 95% washing with alcohol 4 times, recrystallization again, 45 ℃ of oven dry down obtain the white solid powder and are N, and N '-ethylene two [N (ethyl sulfonic acid sodium)-lauramide] (DTM-12).
The preparation method of diesel oil milk sap of the present invention, step is as follows:
Get 0
#Diesel oil, add in the container, add sapn or tween surfactivity, pure and mild thanomin, under the room temperature, after stirring, add N again, N '-ethylene two [N (ethyl sulfonic acid sodium)-lauramide] slowly drips the NaCl aqueous solution, constantly stir simultaneously, after dropwising, fully stir 10-15min, get transparent diesel oil milk sap.
Diesel oil milk sap of the present invention also claims diesel oil emulsification, can be used for the fuel and the industrial combustion fuel of diesel motor.
Compared with prior art, advantage of the present invention and useful effect:
1, diesel oil milk sap of the present invention is with Gemini surface active agent N, N '-ethylene two [N (ethyl sulfonic acid sodium)-lauramide] is an emulsifying agent host (DTM-12), adds auxiliary agent and prepares stable diesel oil milk sap, through centrefuge experiment, it is above not stratified that milk sap can be stablized half a year, and stability better;
2, diesel oil milk sap of the present invention is transparent, and color and ordinary diesel oil are suitable;
3, diesel oil milk sap viscosity of the present invention is low than other diesel oil milk sap, under 20 ℃, 6rpm condition, and the minimum 8mPas that reaches of the viscosity of diesel oil milk sap, atomizing effect is better, can improve the rate of combustion of diesel oil milk sap effectively, reduces environmental pollution;
4, diesel oil milk sap of the present invention is compared basic non-corrosiveness with the carboxylic acid type tensio-active agent, can effectively prolong engine life;
5, the preparation method of diesel oil milk sap of the present invention is simple, can reduce cost effectively.
Embodiment
The present invention will be further described below in conjunction with embodiment.Per-cent is mass percent described in the embodiment.
[embodiment 1]
(1) N, the preparation of N '-ethylene two [N (ethyl sulfonic acid sodium)-lauramide]
In the there-necked flask that stirring, actuator temperature meter, reflux condensing tube are housed, add 4mL quadrol and less water, stir and be heated to 60 ℃.42.2g 2-bromotrifluoromethane sodium sulfonate is soluble in water, after the dissolving fully, slowly drip 2-bromotrifluoromethane sodium sulfonate solution, after dropwising, be about 10 with the pH value of NaOH solution regulation system, reacted 12 hours.After reaction finished, cooling added people's dehydrated alcohol reaction product is separated out in solution, and suction filtration is dried products therefrom at vacuum drying oven, and faint yellow solid is intermediate.
The 17.14g intermediate is dissolved in the mixing solutions of distilled water/acetone, pour in the there-necked flask that agitator is housed, under violent stirring, slowly drip the 25.5mL lauroyl chloride, drip triethylamine/acetone soln simultaneously, keeping the pH value is about 8, and ice-water bath reacted 6 hours down.After reaction finishes, pour reaction solution into beaker, but spending the night in refrigerator and cooled has precipitation to separate out, suction filtration is used 95% washing with alcohol 4 times, recrystallization again, 45 ℃ of oven dry down obtain the white solid powder and are N, and N '-ethylene two [N (ethyl sulfonic acid sodium)-lauramide] (DTM-12).
(2) preparation of diesel oil milk sap:
Diesel oil milk sap raw material is formed:
0
#Diesel oil 54.12%
N, two [N (ethyl sulfonic acid sodium)-lauramide] 17.21% of N '-ethylene
The NaCl solution 7.28% of 1wt%
span80 2.06％
Thanomin 5.25%
Virahol and propyl carbinol (mass ratio 1: 1) 14.08%
With 0
#Diesel oil, add in the container, add span80, thanomin, Virahol and 1: 1 composition of propyl carbinol, after stirring under the room temperature, add N again, N '-ethylene two [N (ethyl sulfonic acid sodium)-lauramide], slowly drip the NaCl aqueous solution, constantly stir simultaneously, after dropwising, fully stir 15min, get transparent diesel oil milk sap.
Gained diesel emulsion diesel oil system is a homogeneous transparent, and 20 ℃, viscosity is 9.5mPas under the 6rpm, with under the same terms 0
#Diesel oil viscosity (5mPas) is compared slightly high.Through centrefuge experiment, it is not stratified to stablize 2h under the 3000rpm.
According to formula: T
2=T
1* 4 π
2Rn
2/ g
T
1, T
2-represent the settling time of liquid pearl under gravity field and centrifugal field effect, h respectively;
Distance between R-sample and the rotation axis, m; The n-rotating speed, r/s; G-universal gravity constant, m/s
2
Can be converted into to be equivalent to leave standstill under the normal temperature and be at least 120 days steady time.
Conversion method steady time in following examples is all identical with this example.
[embodiment 2]
As described in embodiment 1, different is that diesel oil milk sap raw material is composed as follows:
0
#Diesel oil 50.10%
N, two [N (ethyl sulfonic acid sodium)-lauramide] 19.28% of N '-ethylene
The NaCl solution 7.46% of 1wt%
Thanomin 5.28%
Pentyl alcohol 18.10%
Gained diesel oil emulsion system homogeneous transparent, 20 ℃, viscosity is 8.5mPas under the 6rpm.Through centrefuge experiment, it is not stratified to stablize 1.5h under the 3000rpm, is equivalent to leave standstill under the normal temperature be at least 90 days steady time.
[embodiment 3]
As described in embodiment 1, different is that diesel oil milk sap raw material is composed as follows:
0
#Diesel oil 60.42%
N, two [N (ethyl sulfonic acid sodium)-lauramide] 16.20% of N '-ethylene
The NaCl solution 5.22% of 1wt%
Thanomin 5.14%
tween80 2.00％
1: 1 Virahol and propyl carbinol 11.02%
Gained diesel oil emulsion system homogeneous transparent, 20 ℃, viscosity is 8.0mPas under the 6rpm.Through centrefuge experiment, it is not stratified to stablize 3h under the 3000rpm, is equivalent to leave standstill under the normal temperature be at least 180 days steady time.
[embodiment 4]
As described in embodiment 1, different is that diesel oil milk sap raw material is composed as follows:
0
#Diesel oil 55.40%
N, two [N (ethyl sulfonic acid sodium)-lauramide] 15.88% of N '-ethylene
The NaCl solution 5.47% of 1wt%
Thanomin 3.26%
span60 2.25％
N-Octanol 17.74%
Gained diesel oil emulsion system homogeneous transparent, 20 ℃, viscosity is 9.0mPas under the 6rpm.Through centrefuge experiment, it is not stratified to stablize 1h under the 3000rpm.
[embodiment 5]
As described in embodiment 1, different is that diesel oil milk sap raw material is composed as follows:
0
#Diesel oil 60.00%
N, two [N (ethyl sulfonic acid sodium)-lauramide] 16.42% of N '-ethylene
1% NaCl solution 6.37%
Thanomin 3.82%
span20 3.25％
1: 1 Virahol and propyl carbinol 10.14%
Gained diesel oil emulsion system homogeneous transparent, 20 ℃, viscosity is 11.5mPas under the 6rpm.Through centrefuge experiment, it is not stratified to stablize 0.5h under the 3000rpm.
[embodiment 6]
As described in embodiment 1, different is that diesel oil milk sap raw material is composed as follows:
0
#Diesel oil 55.82%, N, the NaCl solution 6.37% of two [N (ethyl sulfonic acid sodium)-lauramide] 19.49%, 1% of N '-ethylene, thanomin 3.83%, tween202.15%, 1: 1 Virahol and propyl carbinol 12.34%.
Gained diesel oil emulsion system homogeneous transparent, 20 ℃, viscosity is 10.5mPas under the 6rpm.Through centrefuge experiment, it is not stratified to stablize 40min under the 3000rpm.
[embodiment 7]
As described in embodiment 1, different is that diesel oil milk sap raw material is composed as follows:
0
#Diesel oil 52.67%
N, two [N (ethyl sulfonic acid sodium)-lauramide] 17.25% of N '-ethylene
1% NaCl solution 8.54%
Thanomin 6.73%
tween60 3.26％
1: 1 Virahol and propyl carbinol 11.55%
Gained diesel oil emulsion system homogeneous transparent, 20 ℃, viscosity is 12.5mPas under the 6rpm.Through centrefuge experiment, it is not stratified to stablize 1.5h under the 3000rpm.
The diesel oil emulsification of Comparative Examples: CN101906333A (CN201010253683.3) embodiment 1-3 preparation
The diesel oil emulsification contrast of table 1, embodiment 1-3 diesel oil milk sap and Comparative Examples
As can be seen from the above table, the milk sap of the present invention's preparation can prepare at normal temperatures, and needs the time of stirring short, can reduce cost effectively; The diesel oil milk sap of the present invention's preparation is compared with the milk sap of the diesel oil emulsification of CN101906333A (CN201010253683.3) preparation has better stability.
Claims (10)
1. diesel oil milk sap is characterized in that it being that raw material by following mass percent makes:
N, two [N (the ethyl sulfonic acid sodium)-lauramide] 15-25% of N '-ethylene
Sapn or tween surfactants 0-5%
0
#Diesel oil 50-65%
NaCl aqueous solution 5-10%
Alcohol 10-20%
Thanomin 2-7%
More than each component sum be 100%;
Described alcohol is one of Virahol, propyl carbinol, Pentyl alcohol or n-Octanol or its combination.
2. diesel oil milk sap as claimed in claim 1 is characterized in that described alcohol is that Virahol and propyl carbinol are by 1: 1 combination of mass ratio.
3. diesel oil milk sap as claimed in claim 1 is characterized in that described sapn or tween surfactants are selected from span80, span60, span20, tween80, tween60 or tween20.
4. diesel oil milk sap as claimed in claim 1 is characterized in that the described NaCl aqueous solution, and mass concentration is 0.5%-2%; Preferred NaCl aqueous solution mass concentration is 1%-1.5%.
5. as claim 1 or 3 or 4 described diesel oil milk sap, it is characterized in that diesel oil milk sap, is that the raw material by following mass percent makes:
N, two [N (the ethyl sulfonic acid sodium)-lauramide] 15-20% of N '-ethylene
Sapn or tween surfactants 0-3%
0
#Diesel oil 50-65%
The NaCl aqueous solution 5-8% of 1wt%
Pentyl alcohol, n-Octanol or 1: 1 Virahol of mass ratio and propyl carbinol 10-20%
Thanomin 3-6%;
More than each component sum be 100%.
6. diesel oil milk sap as claimed in claim 1 is characterized in that raw material composition mass percent is:
0
#Diesel oil 54.12%
N, two [N (ethyl sulfonic acid sodium)-lauramide] 17.21% of N '-ethylene
The NaCl solution 7.28% of 1wt%
span80 2.06％
Thanomin 5.25%
Virahol and propyl carbinol (mass ratio 1: 1) 14.08%.
7. diesel oil milk sap as claimed in claim 1 is characterized in that raw material composition mass percent:
0
#Diesel oil 60.42%
N, two [N (ethyl sulfonic acid sodium)-lauramide] 16.20% of N '-ethylene
The NaCl solution 5.22% of 1wt%
Thanomin 5.14%
tween80 2.00％
1: 1 Virahol and propyl carbinol 11.02%.
8. diesel oil milk sap as claimed in claim 1 is characterized in that raw material composition mass percent:
0
#Diesel oil 55.40%
N, two [N (ethyl sulfonic acid sodium)-lauramide] 15.88% of N '-ethylene
The NaCl solution 5.47% of 1wt%
Thanomin 3.26%
span60 2.25％
N-Octanol 17.74%.
9. as each described diesel oil milk sap of claim 1-8, it is characterized in that described N, N '-ethylene two [N (ethyl sulfonic acid sodium)-lauramide] prepares by the following method:
(1) quadrol and 2-bromotrifluoromethane sodium sulfonate in molar ratio 1: (2-2.5), prepared in reaction intermediate compound I under temperature 50-70 ℃, the condition of pH value 9-10, the molecular formula of intermediate compound I is: NaSO
3(CH
2)
2NH (CH
2)
2NH (CH
2)
2SO
3Na;
(2) lauroyl chloride and intermediate compound I (2-2.5) in molar ratio: 1, reaction obtains sulphonate type gemini surfactant N under the ice-water bath condition, N '-ethylene two [N (ethyl sulfonic acid sodium)-lauramide]; Molecular formula is:
Perhaps, adopt following concrete steps preparation:
1) in the there-necked flask that stirring, actuator temperature meter, reflux condensing tube are housed, adds 4mL quadrol and less water, stir and be heated to 60 ℃.42.2g 2-bromotrifluoromethane sodium sulfonate is soluble in water, after the dissolving fully, drip 2-bromotrifluoromethane sodium sulfonate solution, after dropwising, be 9-10 with the pH value of NaOH solution regulation system, reacted 12 hours; After reaction finished, cooling added people's dehydrated alcohol reaction product is separated out in solution, and suction filtration is dried products therefrom at vacuum drying oven, and faint yellow solid is intermediate compound I;
2) the 17.14g intermediate is dissolved in the mixing solutions of distilled water/acetone, pour in the there-necked flask that agitator is housed, under violent stirring, slowly drip the 25.5mL lauroyl chloride, drip triethylamine/acetone soln simultaneously, keeping the pH value is 7.5-8.5, and ice-water bath reacted 6 hours down; After reaction finishes, pour reaction solution into beaker, but spending the night in refrigerator and cooled has precipitation to separate out, and suction filtration is used 95% washing with alcohol 4 times again, recrystallization, and 45 ℃ of oven dry down obtain the white solid powder and are N, N '-ethylene two [N (ethyl sulfonic acid sodium)-lauramide].
10. the preparation method of each described diesel oil milk sap of claim 1-9, step is as follows:
Get 0
#Diesel oil, add in the container, add sapn or tween surfactivity, pure and mild thanomin, under the room temperature, after stirring, add N again, N '-ethylene two [N (ethyl sulfonic acid sodium)-lauramide] drips the NaCl aqueous solution, constantly stir simultaneously, after dropwising, fully stir 10-15min, get transparent diesel oil milk sap.
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|---|---|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109971441A (en) * | 2019-04-15 | 2019-07-05 | 西南石油大学 | A kind of interpenetrating composite, preparation method and drilling fluid containing the microemulsion and preparation method thereof |
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| CN1935346A (en) * | 2006-09-22 | 2007-03-28 | 西南石油大学 | Bisamide bissulfosalt double surface active agent, and its synthesizing method |
| CN101824343A (en) * | 2010-05-27 | 2010-09-08 | 熊道陵 | Clean and energy-saving micro-emulsified diesel oil with high flash point and preparation method thereof |
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2011
- 2011-01-04 CN CN 201110000286 patent/CN102051243B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1935346A (en) * | 2006-09-22 | 2007-03-28 | 西南石油大学 | Bisamide bissulfosalt double surface active agent, and its synthesizing method |
| CN101824343A (en) * | 2010-05-27 | 2010-09-08 | 熊道陵 | Clean and energy-saving micro-emulsified diesel oil with high flash point and preparation method thereof |
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| 曹建喜等: "微乳化柴油的研制及性能", 《中国石油大学学报》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109971441A (en) * | 2019-04-15 | 2019-07-05 | 西南石油大学 | A kind of interpenetrating composite, preparation method and drilling fluid containing the microemulsion and preparation method thereof |
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