CN105647500A - Molecular deposition film oil displacement agent as well as preparation method and application thereof - Google Patents
Molecular deposition film oil displacement agent as well as preparation method and application thereof Download PDFInfo
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- CN105647500A CN105647500A CN201610101214.7A CN201610101214A CN105647500A CN 105647500 A CN105647500 A CN 105647500A CN 201610101214 A CN201610101214 A CN 201610101214A CN 105647500 A CN105647500 A CN 105647500A
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- 230000008021 deposition Effects 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000006073 displacement reaction Methods 0.000 title claims abstract description 16
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N dimethyl sulfate Chemical compound COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- -1 hexamethyl hexanediamine dimethyl sulfate Chemical group 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims description 59
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 52
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexamethylene diamine Natural products NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 43
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 42
- 239000003795 chemical substances by application Substances 0.000 claims description 42
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 40
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 230000006837 decompression Effects 0.000 claims description 22
- 238000004821 distillation Methods 0.000 claims description 22
- 238000001914 filtration Methods 0.000 claims description 22
- 229920006395 saturated elastomer Polymers 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 22
- 238000010792 warming Methods 0.000 claims description 22
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical group COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 20
- 235000019253 formic acid Nutrition 0.000 claims description 20
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000002904 solvent Substances 0.000 claims description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 13
- 238000009835 boiling Methods 0.000 claims description 11
- 238000013461 design Methods 0.000 claims description 11
- GGHDAUPFEBTORZ-UHFFFAOYSA-N propane-1,1-diamine Chemical compound CCC(N)N GGHDAUPFEBTORZ-UHFFFAOYSA-N 0.000 claims description 11
- 230000004044 response Effects 0.000 claims description 11
- 235000002639 sodium chloride Nutrition 0.000 claims description 11
- 239000011780 sodium chloride Substances 0.000 claims description 11
- 238000013517 stratification Methods 0.000 claims description 11
- 238000001291 vacuum drying Methods 0.000 claims description 11
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- GUMULFRCHLJNDY-UHFFFAOYSA-N 2,2,4,4-tetramethylpentane Chemical compound CC(C)(C)CC(C)(C)C GUMULFRCHLJNDY-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000010276 construction Methods 0.000 abstract description 3
- UMIZXRWZTDPABF-UHFFFAOYSA-N 2,3,4,4-tetramethylpent-2-ene Chemical group CC(C)=C(C)C(C)(C)C UMIZXRWZTDPABF-UHFFFAOYSA-N 0.000 abstract 1
- RPLBHWPNMFJLJM-UHFFFAOYSA-N S(=O)(=O)(OC)OC.CN(C(C(C)(C)C)(N)C)C Chemical compound S(=O)(=O)(OC)OC.CN(C(C(C)(C)C)(N)C)C RPLBHWPNMFJLJM-UHFFFAOYSA-N 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 47
- 239000000243 solution Substances 0.000 description 43
- 239000010410 layer Substances 0.000 description 12
- 238000001035 drying Methods 0.000 description 9
- 239000011435 rock Substances 0.000 description 9
- 239000000376 reactant Substances 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000010779 crude oil Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 235000019504 cigarettes Nutrition 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 3
- 244000005700 microbiome Species 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 2
- 125000003916 ethylene diamine group Chemical group 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000005213 imbibition Methods 0.000 description 2
- 239000003129 oil well Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001768 cations Chemical group 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004454 trace mineral analysis Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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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
- C07C209/68—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
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
- E21B43/16—Enhanced recovery methods for obtaining hydrocarbons
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- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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Abstract
The invention belongs to the technical field of oil-field chemicals and particularly relates to a molecular deposition film oil displacement agent as well as a preparation method and an application thereof. The molecular deposition film oil displacement agent is hexamethyl hexanediamine dimethyl sulfate, hexamethyl propylene diamine dimethyl sulfate or hexamethyl ethanediamine dimethyl sulfate. The molecular deposition film oil displacement agent has the advantages that few displacing agents are used, the oil displacement efficiency is high, a construction process is simple, the stratum is not damaged, the application range is wide and the like. The preparation method of the molecular deposition film oil displacement agent is simple in technological process.
Description
Technical field
The invention belongs to Oilfield Chemicals technical field, be specifically related to a kind of molecule deposition film oil-displacing agent and its preparation method and application.
Background technology
Tertiary oil recovery is to be most widely used, and is also the one that recovery ratio is the highest. Especially in China, it has become old filed and has reduced moisture, to improve oil recovery factor major measure. At present, tertiary oil recovery technology is of a great variety, common are polymer flooding, surfactant flooding, and microorganism is driven exists bigger drawback in varying degrees, the unstability of such as polymer flooding, and the breakdown of emulsion intricate operation of follow-up extraction oil. The large usage quantity of surfactant, mechanism of oil displacement is more complicated, also has substantial amounts of work to do. Microorganism is driven microorganism operation and is obscured with oil field relation, does not have general where applicable.
Summary of the invention
Present invention aims to defect and deficiency that prior art exists, a kind of molecule deposition film oil-displacing agent and its preparation method and application is provided, the oil displacement agent displacing agent consumption prepared by the method is few, oil displacement efficiency is high, use is simple, does not damage stratum and applied widely.
For achieving the above object, the present invention is by the following technical solutions:
Molecule deposition film oil-displacing agent provided by the invention, its molecular structural formula is: hexamethyl hexamethylene diamine dimethyl sulfide hydrochlorate, or hexamethyl propane diamine dimethyl sulfide hydrochlorate, or hexamethyl ethylenediamine dimethyl sulfide hydrochlorate.
The preparation method of a kind of molecule deposition film oil-displacing agent provided by the invention, comprises the following steps:
1) 0.2:2.1:1.2=A:B:C takes raw material for standby in molar ratio, wherein A is hexamethylene diamine or the one of propane diamine or ethylenediamine, B is formic acid, C is that 37wt% formalin is standby, A is placed in reaction bulb, psychrolusia is slowly added dropwise B and C in reaction bulb, when question response is complete, is warming up to 90-140 DEG C of backflow 2.5-5h; Being subsequently cooled to room temperature, adjustment solution PH is 3-5, and rotation is evaporated off solvent, obtains the thick shape solid of brown color; In psychrolusia, in the thick shape solid of gained brown color, it is slowly added dropwise 10mol/l sodium hydroxide solution, stirs to solution saturated simultaneously; It is cooled to room temperature, stratification in separatory funnel; Release water layer, by oil reservoir with saturated common salt water washing; By oil reservoir decompression distillation, collect the fraction of boiling point 133-134 DEG C, obtain colourless liquid;
2) by step 1) gained colourless liquid mixes in the ratio of 1:5 with dimethylformamide; Colourless liquid in molar ratio: dimethyl sulfate=1:2 takes dimethyl sulfate, is slowly added to dimethyl sulfate when psychrolusia and reacts, and stirs to mix homogeneously;It is warming up to 50-90 DEG C, reacts 1-3h, cool down sucking filtration; Solid after sucking filtration is washed, dried white solid.
Further, step 1) described in after hexamethylene diamine is placed in reaction bulb, add 10ml water-wet hexamethylene diamine solid.
Further, step 1) described adjustment solution PH adopt concentration be the hydrochloric acid solution of 6mol/l.
Further, step 1) described decompression distillation design parameter be: pressure is 8-11kPa.
Further, step 1) described washing adopt 50ml saturated aqueous common salt wash.
Further, step 2) described washing adopt concentration be 7% ethyl acetate wash 3 times.
Further, step 2) described dry it is specially at 50-80 DEG C, vacuum drying 2.5-4h.
Compared with prior art, the present invention has following useful technique effect: molecule deposition film oil-displacing agent provided by the invention in use, has displacing agent consumption few, and oil displacement efficiency is high, and construction technology is simple, does not damage stratum and the advantage such as applied widely. The preparation method technological process of oil displacement agent provided by the invention is simple.
Further, by adding water-wet on hexamethylene diamine solid, make reactant contact area increase, react completely.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
Molecule deposition film oil-displacing agent provided by the invention, its molecular structural formula is:
Hexamethyl hexamethylene diamine dimethyl sulfide hydrochlorate, chemical formula is:
Or hexamethyl propane diamine dimethyl sulfide hydrochlorate, chemical formula is:
Or hexamethyl ethylenediamine dimethyl sulfide hydrochlorate, chemical formula is:
The preparation method of molecule deposition film oil-displacing agent provided by the invention, comprises the following steps:
1) A:B:C=0.2:2.1:1.2 takes raw material for standby in molar ratio, and wherein A is hexamethylene diamine or the one of propane diamine or ethylenediamine, and B is formic acid, and C is 37wt% formalin. A is placed in reaction bulb, adds 10ml water-wet solid. Psychrolusia is slowly added dropwise formic acid and formaldehyde in reaction bulb, when question response is complete, is warming up to 90-140 DEG C of backflow 2.5-5h; Being subsequently cooled to room temperature, it is 3-5 that the hydrochloric acid solution adopting concentration to be 6mol/l regulates solution PH, and rotation is evaporated off solvent, obtains the thick shape solid of brown color;
In psychrolusia, in the thick shape solid of gained brown color, it is slowly added dropwise 10mol/l sodium hydroxide solution, stirs to solution saturated simultaneously; It is cooled to room temperature, stratification in separatory funnel; Release water layer, oil reservoir is washed with 50ml saturated aqueous common salt; By oil reservoir decompression distillation, the design parameter of decompression distillation is: pressure is 8-11kPa. Collect the fraction of boiling point 133-134 DEG C, obtain colourless liquid;
2) by step 1) gained colourless liquid mixes in the ratio of 1:5 with dimethylformamide; Colourless liquid in molar ratio: dimethyl sulfate=1:2 takes dimethyl sulfate, is slowly added to dimethyl sulfate when psychrolusia and reacts, and stirs to mix homogeneously; It is warming up to 50-90 DEG C, reacts 1-3h, cool down sucking filtration; Solid after sucking filtration is washed, dried white crystalline solid, obtain end product. The ethyl acetate that described washing adopts concentration to be 7% is washed 3 times. Described drying is specially at 50-80 DEG C, vacuum drying 2.5-4h.
When reactant is hexamethylene diamine, the molecule deposition film oil-displacing agent of preparation is hexamethyl hexamethylene diamine sulfate; When reactant is propane diamine, product is hexamethyl propane diamine sulfate; When reactant is ethylenediamine, product is hexamethyl ethylenediammonium sulfate.
Embodiment 1
Reactant is hexamethylene diamine, and product is the preparation method of the oil displacement agent of hexamethyl hexamethylene diamine sulfate, comprises the following steps:
1) 0.2mol takes hexamethylene diamine in molar ratio, and 2.1mol formic acid and 100ml formaldehyde 37wt% aqueous solution standby, hexamethylene diamine is placed in reaction bulb, adds 10ml water-wet solid.Being slowly added dropwise formic acid and formaldehyde in psychrolusia in reaction bulb, produce a large amount of bubble, when question response is complete, bubble produces acutely, be not warming up to 110 DEG C of backflow 4h; Being subsequently cooled to room temperature, adding the hydrochloric acid solution adjustment solution PH that 85ml concentration is 6mol/l is 3-5, and rotation is evaporated off solvent, obtains the thick shape solid of brown color;
In psychrolusia, being slowly added dropwise the sodium hydroxide solution that 80ml concentration is 10mol/l in the thick shape solid of gained brown color, produce a large amount of white cigarette, very exothermic, finishes simultaneously, then adds the oxidation of a small amount of solid hydrogen, stirs to solution saturated simultaneously; It is cooled to room temperature, stratification in separatory funnel; Release water layer, oil reservoir is washed with 50ml saturated aqueous common salt; By oil reservoir decompression distillation, the design parameter of decompression distillation is: pressure is 10kPa. Collect the fraction of boiling point 133-134 DEG C, obtain colourless liquid 25.9g;
2) by step 1) gained colourless liquid 19.25g (0.1mol), it is placed in flask, add 40ml dimethylformamide to mix as solvent, be slowly added to 0.2mol dimethyl sulfate when psychrolusia and react, stir to mix homogeneously; It is warming up to 80 DEG C, reacts 1h, cool down sucking filtration; Solid after sucking filtration is washed, dried white crystalline solid. The ethyl acetate that described washing adopts concentration to be 7% is washed 3 times, ethyl acetate 20ml/ time during washing. Described drying is specially at 60 DEG C, vacuum drying 3h.
Embodiment 2
Reactant is propane diamine, and product is the preparation method of the molecule deposition film oil-displacing agent of hexamethyl propane diamine sulfate, comprises the following steps:
1) 0.2mol takes propane diamine in molar ratio, and 2.1mol formic acid and 100ml formaldehyde 37wt% aqueous solution standby, hexamethylene diamine is placed in reaction bulb, adds 10ml water-wet solid. Being slowly added dropwise formic acid and formaldehyde in psychrolusia in reaction bulb, produce a large amount of bubble, when question response is complete, bubble produces acutely, be not warming up to 110 DEG C of backflow 4h; Being subsequently cooled to room temperature, adding the hydrochloric acid solution adjustment solution PH that 85ml concentration is 6mol/l is 3-5, and rotation is evaporated off solvent, obtains the thick shape solid of brown color;
In psychrolusia, being slowly added dropwise the sodium hydroxide solution that 80ml concentration is 10mol/l in the thick shape solid of gained brown color, produce a large amount of white cigarette, very exothermic, finishes simultaneously, then adds the oxidation of a small amount of solid hydrogen, stirs to solution saturated simultaneously; It is cooled to room temperature, stratification in separatory funnel; Release water layer, oil reservoir is washed with 50ml saturated aqueous common salt; By oil reservoir decompression distillation, the design parameter of decompression distillation is: pressure is 10kPa. Collect the fraction of boiling point 133-134 DEG C, obtain colourless liquid 25.9g;
2) by step 1) gained colourless liquid 19.25g (0.1mol), it is placed in flask, add 40ml dimethylformamide to mix as solvent, be slowly added to 0.2mol dimethyl sulfate when psychrolusia and react, stir to mix homogeneously; It is warming up to 80 DEG C, reacts 1h, cool down sucking filtration; Solid after sucking filtration is washed, dried white crystalline solid. The ethyl acetate that described washing adopts concentration to be 7% is washed 3 times, ethyl acetate 20ml/ time during washing. Described drying is specially at 60 DEG C, vacuum drying 3h.
Embodiment 3
Reactant is ethylenediamine, and product is the preparation method of the molecule deposition film oil-displacing agent of hexamethyl ethylenediammonium sulfate, comprises the following steps:
1) 0.2mol takes ethylenediamine in molar ratio, and 2.1mol formic acid and 100ml formaldehyde 37wt% aqueous solution standby, hexamethylene diamine is placed in reaction bulb, adds 10ml water-wet solid.Being slowly added dropwise formic acid and formaldehyde in psychrolusia in reaction bulb, produce a large amount of bubble, when question response is complete, bubble produces acutely, be not warming up to 110 DEG C of backflow 4h; Being subsequently cooled to room temperature, adding the hydrochloric acid solution adjustment solution PH that 85ml concentration is 6mol/l is 3-5, and rotation is evaporated off solvent, obtains the thick shape solid of brown color;
In psychrolusia, being slowly added dropwise the sodium hydroxide solution that 80ml concentration is 10mol/l in the thick shape solid of gained brown color, produce a large amount of white cigarette, very exothermic, finishes simultaneously, then adds the oxidation of a small amount of solid hydrogen, stirs to solution saturated simultaneously; It is cooled to room temperature, stratification in separatory funnel; Release water layer, oil reservoir is washed with 50ml saturated aqueous common salt; By oil reservoir decompression distillation, the design parameter of decompression distillation is: pressure is 10kPa. Collect the fraction of boiling point 133-134 DEG C, obtain colourless liquid 25.9g;
2) by step 1) gained colourless liquid 19.25g (0.1mol), it is placed in flask, add 40ml dimethylformamide to mix as solvent, be slowly added to 0.2mol dimethyl sulfate when psychrolusia and react, stir to mix homogeneously; It is warming up to 80 DEG C, reacts 1h, cool down sucking filtration; Solid after sucking filtration is washed, dried white crystalline solid. The ethyl acetate that described washing adopts concentration to be 7% is washed 3 times, ethyl acetate 20ml/ time during washing. Described drying is specially at 60 DEG C, vacuum drying 3h.
Embodiment 4
The preparation method of molecule deposition film oil-displacing agent provided by the invention, comprises the following steps:
1) A:B:C=0.2:2.1:1.2 takes raw material for standby in molar ratio, and wherein A is hexamethylene diamine or the one of propane diamine or ethylenediamine, and B is formic acid, and C is 37wt% formalin. A is placed in reaction bulb, adds 10ml water-wet solid. Psychrolusia is slowly added dropwise formic acid and formaldehyde in reaction bulb, when question response is complete, is warming up to 90 DEG C of backflow 5h; Being subsequently cooled to room temperature, it is 3-5 that the hydrochloric acid solution adopting concentration to be 6mol/l regulates solution PH, and rotation is evaporated off solvent, obtains the thick shape solid of brown color;
In psychrolusia, in the thick shape solid of gained brown color, it is slowly added dropwise 10mol/l sodium hydroxide solution, stirs to solution saturated simultaneously; It is cooled to room temperature, stratification in separatory funnel; Release water layer, oil reservoir is washed with 50ml saturated aqueous common salt; By oil reservoir decompression distillation, the design parameter of decompression distillation is: pressure is 8-11kPa. Collect the fraction of boiling point 133-134 DEG C, obtain colourless liquid;
2) by step 1) gained colourless liquid mixes in the ratio of 1:5 with dimethylformamide, is slowly added to dimethyl sulfate when psychrolusia and reacts, stirs to mix homogeneously; It is warming up to 590 DEG C, reacts 1h, cool down sucking filtration; Solid after sucking filtration is washed, dried white crystalline solid. The ethyl acetate that described washing adopts concentration to be 7% is washed 3 times. Described drying is specially at 50 DEG C, vacuum drying 4h.
Embodiment 5
The preparation method of molecule deposition film oil-displacing agent provided by the invention, comprises the following steps:
1) A:B:C=0.2:2.1:1.2 takes raw material for standby in molar ratio, and wherein A is hexamethylene diamine or the one of propane diamine or ethylenediamine, and B is formic acid, and C is 37wt% formalin. A is placed in reaction bulb, adds 10ml water-wet solid. Psychrolusia is slowly added dropwise formic acid and formaldehyde in reaction bulb, when question response is complete, is warming up to 140 DEG C of backflow 2.5h; Being subsequently cooled to room temperature, it is 3-5 that the hydrochloric acid solution adopting concentration to be 6mol/l regulates solution PH, and rotation is evaporated off solvent, obtains the thick shape solid of brown color;
In psychrolusia, in the thick shape solid of gained brown color, it is slowly added dropwise 10mol/l sodium hydroxide solution, stirs to solution saturated simultaneously; It is cooled to room temperature, stratification in separatory funnel; Release water layer, oil reservoir is washed with 50ml saturated aqueous common salt; By oil reservoir decompression distillation, the design parameter of decompression distillation is: pressure is 8-11kPa. Collect the fraction of boiling point 133-134 DEG C, obtain colourless liquid;
2) by step 1) gained colourless liquid mixes in the ratio of 1:5 with dimethylformamide, is slowly added to dimethyl sulfate when psychrolusia and reacts, stirs to mix homogeneously; It is warming up to 50 DEG C, reacts 3h, cool down sucking filtration; Solid after sucking filtration is washed, dried white crystalline solid. The ethyl acetate that described washing adopts concentration to be 7% is washed 3 times. Described drying is specially at 50 DEG C, vacuum drying 4h.
Embodiment 6
The preparation method of molecule deposition film oil-displacing agent provided by the invention, comprises the following steps:
1) A:B:C=0.2:2.1:1.2 takes raw material for standby in molar ratio, and wherein A is hexamethylene diamine or the one of propane diamine or ethylenediamine, and B is formic acid, and C is 37wt% formalin. A is placed in reaction bulb, adds 10ml water-wet solid. Psychrolusia is slowly added dropwise formic acid and formaldehyde in reaction bulb, when question response is complete, is warming up to 100 DEG C of backflow 4h; Being subsequently cooled to room temperature, it is 3-5 that the hydrochloric acid solution adopting concentration to be 6mol/l regulates solution PH, and rotation is evaporated off solvent, obtains the thick shape solid of brown color;
In psychrolusia, in the thick shape solid of gained brown color, it is slowly added dropwise 10mol/l sodium hydroxide solution, stirs to solution saturated simultaneously; It is cooled to room temperature, stratification in separatory funnel; Release water layer, oil reservoir is washed with 50ml saturated aqueous common salt; By oil reservoir decompression distillation, the design parameter of decompression distillation is: pressure is 8-11kPa. Collect the fraction of boiling point 133-134 DEG C, obtain colourless liquid;
2) by step 1) gained colourless liquid mixes in the ratio of 1:5 with dimethylformamide, is slowly added to dimethyl sulfate when psychrolusia and reacts, stirs to mix homogeneously; It is warming up to 70 DEG C, reacts 2h, cool down sucking filtration; Solid after sucking filtration is washed, dried white crystalline solid. The ethyl acetate that described washing adopts concentration to be 7% is washed 3 times. Described drying is specially at 60 DEG C, vacuum drying 3.5h.
Embodiment 7
The preparation method of molecule deposition film oil-displacing agent provided by the invention, comprises the following steps:
1) A:B:C=0.2:2.1:1.2 takes raw material for standby in molar ratio, and wherein A is hexamethylene diamine or the one of propane diamine or ethylenediamine, and B is formic acid, and C is 37wt% formalin. A is placed in reaction bulb, adds 10ml water-wet solid. Psychrolusia is slowly added dropwise formic acid and formaldehyde in reaction bulb, when question response is complete, is warming up to 90-140 DEG C of backflow 2.5-5h; Being subsequently cooled to room temperature, it is 3-5 that the hydrochloric acid solution adopting concentration to be 6mol/l regulates solution PH, and rotation is evaporated off solvent, obtains the thick shape solid of brown color;
In psychrolusia, in the thick shape solid of gained brown color, it is slowly added dropwise 10mol/l sodium hydroxide solution, stirs to solution saturated simultaneously; It is cooled to room temperature, stratification in separatory funnel; Release water layer, oil reservoir is washed with 50ml saturated aqueous common salt; By oil reservoir decompression distillation, the design parameter of decompression distillation is: pressure is 8-11kPa. Collect the fraction of boiling point 133-134 DEG C, obtain colourless liquid;
2) by step 1) gained colourless liquid mixes in the ratio of 1:5 with dimethylformamide, is slowly added to dimethyl sulfate when psychrolusia and reacts, stirs to mix homogeneously; It is warming up to 90 DEG C, reacts 1h, cool down sucking filtration; Solid after sucking filtration is washed, dried white crystalline solid. The ethyl acetate that described washing adopts concentration to be 7% is washed 3 times. Described drying is specially at 80 DEG C, vacuum drying 2.5h.
Embodiment 8
The preparation method of molecule deposition film oil-displacing agent provided by the invention, comprises the following steps:
1) A:B:C=0.2:2.1:1.2 takes raw material for standby in molar ratio, and wherein A is hexamethylene diamine or the one of propane diamine or ethylenediamine, and B is formic acid, and C is 37wt% formalin. A is placed in reaction bulb, adds 10ml water-wet solid. Psychrolusia is slowly added dropwise formic acid and formaldehyde in reaction bulb, when question response is complete, is warming up to 120 DEG C of backflow 3.5h; Being subsequently cooled to room temperature, it is 3-5 that the hydrochloric acid solution adopting concentration to be 6mol/l regulates solution PH, and rotation is evaporated off solvent, obtains the thick shape solid of brown color;
In psychrolusia, in the thick shape solid of gained brown color, it is slowly added dropwise 10mol/l sodium hydroxide solution, stirs to solution saturated simultaneously; It is cooled to room temperature, stratification in separatory funnel; Release water layer, oil reservoir is washed with 50ml saturated aqueous common salt; By oil reservoir decompression distillation, the design parameter of decompression distillation is: pressure is 8-11kPa. Collect the fraction of boiling point 133-134 DEG C, obtain colourless liquid;
2) by step 1) gained colourless liquid mixes in the ratio of 1:5 with dimethylformamide, is slowly added to dimethyl sulfate when psychrolusia and reacts, stirs to mix homogeneously; It is warming up to 70 DEG C, reacts 2.5h, cool down sucking filtration; Solid after sucking filtration is washed, dried white crystalline solid. The ethyl acetate that described washing adopts concentration to be 7% is washed 3 times. Described drying is specially at 60 DEG C, vacuum drying 3.5h.
The molecule deposition film oil-displacing agent of the present invention is the filming flooding agent that structure is special, with aqueous solution for Transfer Medium, rely on strong interionic electrostatic interaction, be deposited on reservoir surface and form firmly nanoscale monolayer ultrathin membrane, thus improving displacement efficiency and oil recovery factor. Various oil reservoirs (comprising hyposmosis and extra-low permeability oil reservoirs) are all had adaptability by nanometer filming flooding agent, it is not only suitable for each stage of oilfield exploitation, it is adapted to again well and oil well, and field conduct by the restriction of formation temperature, permeability and salinity, does not have the universality of popularization and application.
Containing cation group in the effective ingredient of film oil-displacing agent, when film oil-displacing agent solution reaches a certain concentration value, elecrtonegativity surface conversion is electropositive surface, namely there is the concentration of a zero zeta current potential. Under this concentration, the phenomenon that is electrically attracting or that repel each other between interface disappears, and the displacement of reservoir oil can obtain higher recovery ratio with this understanding.
Membrane achieves the unimolecular layer membrane of a layer on reservoir rocks surface, and crude oil adhesion and adhesion energy substantially reduce so that the interaction between rock and crude oil weakens, and crude oil is more easily peelable rock surface.
After waterflooding extraction is implemented in oil field, through water drive effect, the imperfection of oil film is strengthened further, there is substantial amounts of oil film obscission zone in rock surface, when molecule deposition film oil-displacing agent is with after injecting water entrance oil reservoir, filming flooding agent is in rock surface absorption and spreads further, and the polar substances in crude oil releases absorption gradually, and reservoir rock surface produces wettability reversal effect. Molecule membrane can increase angle of wetting so that any wettability rock surface all can be changed into strongly hydrophilic, and wettability reversal will not occur.
When molecule deposition film oil-displacing agent is with after injecting water entrance oil reservoir, the absorption of filming flooding agent extends gradually with diffusion in rock capillary tube, the generation capillary tube imbibition when filming flooding agent occupies hole wall and smaller hole road due to absorption and diffusion.Capillary tube spontaneous imbibition effect is conducive to the crude oil in pores with dead end and non-hydrodynamics interconnected pore to flush out, and produces " degrading " effect. Thus improving the utilization rate in space.
It is embodied as: new 5th district, Jian Shan oil field (length celebrates six factories of recovering the oil) recklessly
Form of construction work: inject in slug mode stage by stage.
Product: the concentration with about 10% is injected, every mouthful of well injects molecule deposition film oil-displacing agent (Bond's 007MD membrane) 20 tons, injection rate 220m3��
By the molecular film displacement of reservoir oil is implemented in new 5 and new 22-17 well, after trace analysis test, oil well production is dynamic, can be seen that Hu Jianshanxin 5 district ensemble average takes effect 16 months cycles, take effect period comprehensive water cut by 94.2 �� 87.1%, block day, oil-producing was by 6.19 �� 10.5t, and increase day by day oil 4.31 tons, ended oily 2316 tons of accumulative increasing on July 31st, 2014, more than input-output ratio 1:11, achieves reasonable economic benefit.
In actual implementation process, rock core simulation experiment need to be carried out according to the geological conditions in different oil fields and oil recovery situation, obtain the membrane implantation concentration of the best.
Claims (9)
1. a molecule deposition film oil-displacing agent, it is characterised in that its molecular structural formula is: hexamethyl hexamethylene diamine dimethyl sulfide hydrochlorate, or hexamethyl propane diamine dimethyl sulfide hydrochlorate, or hexamethyl ethylenediamine dimethyl sulfide hydrochlorate.
2. the preparation method of a molecule deposition film oil-displacing agent, it is characterised in that comprise the following steps:
1) 0.2:2.1:1.2=A:B:C takes raw material for standby in molar ratio, wherein A is hexamethylene diamine or the one of propane diamine or ethylenediamine, B is formic acid, C is that 37wt% formalin is standby, A is placed in reaction bulb, psychrolusia is slowly added dropwise B and C in reaction bulb, when question response is complete, is warming up to 90-140 DEG C of backflow 2.5-5h; Being subsequently cooled to room temperature, adjustment solution PH is 3-5, and rotation is evaporated off solvent, obtains the thick shape solid of brown color;
In psychrolusia, in the thick shape solid of gained brown color, it is slowly added dropwise 10mol/l sodium hydroxide solution, stirs to solution saturated simultaneously; It is cooled to room temperature, stratification in separatory funnel; Release water layer, by oil reservoir with saturated common salt water washing; By oil reservoir decompression distillation, collect the fraction of boiling point 133-134 DEG C, obtain colourless liquid;
2) by step 1) gained colourless liquid mixes with the ratio of dimethylformamide 1:5 in molar ratio; Colourless liquid in molar ratio: dimethyl sulfate=1:2 takes dimethyl sulfate, is slowly added to dimethyl sulfate when psychrolusia and reacts, and stirs to mix homogeneously; It is warming up to 50-90 DEG C, reacts 1-3h, cool down sucking filtration; Solid after sucking filtration is washed, dried white solid.
3. the preparation method of a kind of molecule deposition film oil-displacing agent according to claim 2, it is characterised in that step 1) described in after hexamethylene diamine is placed in reaction bulb, add 10ml water-wet hexamethylene diamine solid.
4. the preparation method of a kind of molecule deposition film oil-displacing agent according to claim 2, it is characterised in that step 1) described adjustment solution PH adopt concentration be the hydrochloric acid solution of 6mol/l.
5. the preparation method of a kind of molecule deposition film oil-displacing agent according to claim 2, it is characterised in that step 1) described decompression distillation design parameter be: pressure is 8-11kPa.
6. the preparation method of a kind of molecule deposition film oil-displacing agent according to claim 2, it is characterised in that step 1) described washing adopt 50ml saturated aqueous common salt wash.
7. the preparation method of a kind of molecule deposition film oil-displacing agent according to claim 2, it is characterised in that step 2) described washing adopt concentration be 7% ethyl acetate wash 3 times.
8. the preparation method of a kind of molecule deposition film oil-displacing agent according to claim 2 or 7, it is characterised in that step 2) described dry it is specially at 50-80 DEG C, vacuum drying 2.5-4h.
9. Molecular Deposition Film Oil-displacing Agent described in any one of claim 1-8 is as the application of oil displacement agent.
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