CN105524606A - Preparing method of nano membrane oil dispersant - Google Patents
Preparing method of nano membrane oil dispersant Download PDFInfo
- Publication number
- CN105524606A CN105524606A CN201610034013.XA CN201610034013A CN105524606A CN 105524606 A CN105524606 A CN 105524606A CN 201610034013 A CN201610034013 A CN 201610034013A CN 105524606 A CN105524606 A CN 105524606A
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- Prior art keywords
- diethylenetriamine
- oil
- solid
- cooling
- slowly
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- 239000012528 membrane Substances 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 title abstract 5
- 239000003924 oil dispersant Substances 0.000 title abstract 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000001816 cooling Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007787 solid Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 8
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 8
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 7
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 235000019253 formic acid Nutrition 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 6
- UKODFQOELJFMII-UHFFFAOYSA-N pentamethyldiethylenetriamine Chemical compound CN(C)CCN(C)CCN(C)C UKODFQOELJFMII-UHFFFAOYSA-N 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- JZMJDSHXVKJFKW-UHFFFAOYSA-M methyl sulfate(1-) Chemical compound COS([O-])(=O)=O JZMJDSHXVKJFKW-UHFFFAOYSA-M 0.000 claims description 3
- 150000005451 methyl sulfates Chemical class 0.000 claims description 3
- 229950000081 metilsulfate Drugs 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 238000001953 recrystallisation Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 7
- 239000010779 crude oil Substances 0.000 abstract description 4
- 239000003921 oil Substances 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 abstract 1
- 235000011167 hydrochloric acid Nutrition 0.000 abstract 1
- 238000010992 reflux Methods 0.000 abstract 1
- 230000000630 rising effect Effects 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 238000003912 environmental pollution Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000000638 stimulation Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
Classifications
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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
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/24—Preparation of compounds containing amino groups bound to a carbon skeleton by reductive alkylation of ammonia, amines or compounds having groups reducible to amino groups, with carbonyl compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/68—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/24—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of esters of sulfuric acids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Cosmetics (AREA)
Abstract
The invention relates to the technical field of a preparing method of an oil dispersant, in particular to a preparing method of a nano membrane oil dispersant. By the method, a water cut of crude oil is effectively reduced, and an oil field is increased in yield; defects of insufficient stability, limited applicable scope, short effect taking period and environment pollution of a traditional oil dispersant are overcome; the method comprises following steps: (1) placing 0.3mol of diethylenetriamine into a reaction bottle, adding deionized water, slowly adding dropwise 2.7mol of formic acid and 1.8mol formalin with a content of 37% in cold water bath, and generating massive bubbles; (2) after adding dropwise, after the bubbles are not acutely generated, rising temperature to 80-120 DEG C, refluxing for 8-12h, cooling for 10min, adding 120ml, 6mol/L of muriatic acid, and spin-evaporating to remove a solvent and obtain red thick liquid, and obtaining solid after cooling; (3) slowly adding dropwise 130ml, 10mol/L of sodium hydroxide solution into the solid in cold water bath.
Description
Technical field
The present invention relates to the technical field of the preparation method of oil-displacing agent, particularly relate to a kind of preparation method of nm-membrane oil-displacing agent.
Background technology
As everyone knows, the new oil-gas field number found along with exploration and the minimizing year by year of the overall reserves of petroleum-bearing formation, the recovery ratio and exploitation heterogeneous reservoirs, low permeability and the high sticky heavy oil reservoirs that improve high water-cut stage maturing field have become the eternal theme of oil-field development, the water ratio of existing oil-displacing agent is higher, and stability is not enough, the scope of application is limited, the shortcoming such as the cycle that takes effect short, environmental pollution.
Summary of the invention
For solving the problems of the technologies described above, the invention provides one and effectively reducing crude oil water content, is oilfield stimulation; Also solve that traditional oil-displacing agent stability is not enough, the scope of application is limited, the preparation method of the nm-membrane oil-displacing agent of the shortcomings such as the cycle that takes effect short, environmental pollution simultaneously.
The preparation method of nm-membrane oil-displacing agent of the present invention, comprises the following steps:
1), by 0.3mol diethylenetriamine be placed in reaction flask, add deionized water, stir lower slowly dropping 2.7mol formic acid and 1.8mol in cooling bath, content is the formalin of 37%, produces a large amount of bubble;
2), drip and finish, treat that bubble produces not acutely, be warming up to 80-120 DEG C of backflow 8-12h, cool 10min, add 120ml, 6mol/L hydrochloric acid, revolve and steam except desolventizing, obtain red-brown thick liquid, after cooling, become solid;
3), in cooling bath, in this solid, slowly 130ml is dripped under stirring, the sodium hydroxide solution of 10mol/L;
4), finishing, adding a small amount of solid sodium hydroxide to precipitating generation in a large number, cooling, suction filtration, filtrate leaves standstill more than 1-3h and carries out layering in separating funnel;
5), release water layer, oil reservoir underpressure distillation 8-11kPa, collect the cut of boiling point 135-136 DEG C, obtain colourless liquid pentamethyl-diethylenetriamine;
6), by 0.2mol pentamethyl-diethylenetriamine be dissolved in 40ml dimethyl formamide, in cooling bath, stir lower dropping 0.3mol methyl-sulfate;
7), drip and finish, react 1-2h under room temperature, produce a large amount of orange-yellow oily liquids;
8), warming-in-water to 60-90 DEG C, in reaction solution, slowly add dehydrated alcohol clarify to solution, hold over night recrystallization, colourless acicular crystal separate out;
9), suction filtration, solid with ethyl acetate washing (20ml, three times), vacuum-drying 1-3h at 50-70 DEG C, obtains colourless bulk crystals prestox diethylenetriamine three metilsulfate.
Compared with prior art beneficial effect of the present invention is: by above-mentioned steps, can reach and effectively reduce crude oil water content, is oilfield stimulation; Also solve that traditional oil-displacing agent stability is not enough, the scope of application is limited, the effect of the shortcomings such as the cycle that takes effect short, environmental pollution simultaneously.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is described in further detail.Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
The preparation method of nm-membrane oil-displacing agent of the present invention, comprises the following steps:
1), by 0.3mol diethylenetriamine be placed in reaction flask, add deionized water, stir lower slowly dropping 2.7mol formic acid and 1.8mol in cooling bath, content is the formalin of 37%, produces a large amount of bubble;
2), drip and finish, treat that bubble produces not acutely, be warming up to 80-120 DEG C of backflow 8-12h, cool 10min, add 120ml, 6mol/L hydrochloric acid, revolve and steam except desolventizing, obtain red-brown thick liquid, after cooling, become solid;
3), in cooling bath, in this solid, slowly 130ml is dripped under stirring, the sodium hydroxide solution of 10mol/L;
4), finishing, adding a small amount of solid sodium hydroxide to precipitating generation in a large number, cooling, suction filtration, filtrate leaves standstill more than 1-3h and carries out layering in separating funnel;
5), release water layer, oil reservoir underpressure distillation 8-11kPa, collect the cut of boiling point 135-136 DEG C, obtain colourless liquid pentamethyl-diethylenetriamine;
6), by 0.2mol pentamethyl-diethylenetriamine be dissolved in 40ml dimethyl formamide, in cooling bath, stir lower dropping 0.3mol methyl-sulfate;
7), drip and finish, react 1-2h under room temperature, produce a large amount of orange-yellow oily liquids;
8), warming-in-water to 60-90 DEG C, in reaction solution, slowly add dehydrated alcohol clarify to solution, hold over night recrystallization, colourless acicular crystal separate out;
9), suction filtration, solid with ethyl acetate washing (20ml, three times), vacuum-drying 1-3h at 50-70 DEG C, obtains colourless bulk crystals prestox diethylenetriamine three metilsulfate.
The preparation method of nm-membrane oil-displacing agent of the present invention, by above-mentioned steps, can reach and effectively reduce crude oil water content, is oilfield stimulation; Also solve that traditional oil-displacing agent stability is not enough, the scope of application is limited, the effect of the shortcomings such as the cycle that takes effect short, environmental pollution simultaneously.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Claims (1)
1. a preparation method for nm-membrane oil-displacing agent, is characterized in that, comprises the following steps:
1), by 0.3mol diethylenetriamine be placed in reaction flask, add deionized water, stir lower slowly dropping 2.7mol formic acid and 1.8mol in cooling bath, content is the formalin of 37%, produces a large amount of bubble;
2), drip and finish, treat that bubble produces not acutely, be warming up to 80-120 DEG C of backflow 8-12h, cool 10min, add 120ml, 6mol/L hydrochloric acid, revolve and steam except desolventizing, obtain red-brown thick liquid, after cooling, become solid;
3), in cooling bath, in this solid, slowly 130ml is dripped under stirring, the sodium hydroxide solution of 10mol/L;
4), finishing, adding a small amount of solid sodium hydroxide to precipitating generation in a large number, cooling, suction filtration, filtrate leaves standstill more than 1-3h and carries out layering in separating funnel;
5), release water layer, oil reservoir underpressure distillation 8-11kPa, collect the cut of boiling point 135-136 DEG C, obtain colourless liquid pentamethyl-diethylenetriamine;
6), by 0.2mol pentamethyl-diethylenetriamine be dissolved in 40ml dimethyl formamide, in cooling bath, stir lower dropping 0.3mol methyl-sulfate;
7), drip and finish, react 1-2h under room temperature, produce a large amount of orange-yellow oily liquids;
8), warming-in-water to 60-90 DEG C, in reaction solution, slowly add dehydrated alcohol clarify to solution, hold over night recrystallization, colourless acicular crystal separate out;
9), suction filtration, solid with ethyl acetate washing (20ml, three times), vacuum-drying 1-3h at 50-70 DEG C, obtains colourless bulk crystals prestox diethylenetriamine three metilsulfate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610034013.XA CN105524606A (en) | 2016-01-19 | 2016-01-19 | Preparing method of nano membrane oil dispersant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610034013.XA CN105524606A (en) | 2016-01-19 | 2016-01-19 | Preparing method of nano membrane oil dispersant |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105524606A true CN105524606A (en) | 2016-04-27 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610034013.XA Pending CN105524606A (en) | 2016-01-19 | 2016-01-19 | Preparing method of nano membrane oil dispersant |
Country Status (1)
| Country | Link |
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| CN (1) | CN105524606A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362941A (en) * | 2008-09-05 | 2009-02-11 | 关俊华 | Nano molecule deposition film oil-displacing agent and preparation method thereof |
| US20150191645A1 (en) * | 2013-11-20 | 2015-07-09 | Weatherford/Lamb, Inc. | Anti-agglomerants for the prevention of hydrates |
-
2016
- 2016-01-19 CN CN201610034013.XA patent/CN105524606A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101362941A (en) * | 2008-09-05 | 2009-02-11 | 关俊华 | Nano molecule deposition film oil-displacing agent and preparation method thereof |
| US20150191645A1 (en) * | 2013-11-20 | 2015-07-09 | Weatherford/Lamb, Inc. | Anti-agglomerants for the prevention of hydrates |
Non-Patent Citations (1)
| Title |
|---|
| Z. HU等: ""Wettability of compound organobentonites with ultra-low swellingmodified by a series of bis-quaternary ammonium salts"", 《COLLOIDS AND SURFACES A: PHYSICOCHEM. ENG.》 * |
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| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
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Application publication date: 20160427 |