CN106565007A - Ternary compound flooding produced water deoiling agent and preparation method thereof - Google Patents
Ternary compound flooding produced water deoiling agent and preparation method thereof Download PDFInfo
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- CN106565007A CN106565007A CN201610983357.5A CN201610983357A CN106565007A CN 106565007 A CN106565007 A CN 106565007A CN 201610983357 A CN201610983357 A CN 201610983357A CN 106565007 A CN106565007 A CN 106565007A
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- degreaser
- formic acid
- formaldehyde
- preparation
- ternary composite
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 title abstract description 8
- 150000001875 compounds Chemical class 0.000 title abstract description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 66
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 45
- 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 33
- 235000019253 formic acid Nutrition 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000013527 degreasing agent Substances 0.000 claims description 90
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 24
- 239000011206 ternary composite Substances 0.000 claims description 23
- 238000010792 warming Methods 0.000 claims description 22
- AJCKOXJKWPVQGU-UHFFFAOYSA-L C(CCCCCCCCCCC)(=O)[O-].[Na+].[Cl+].C(CCCCCCCCCCC)(=O)[O-] Chemical compound C(CCCCCCCCCCC)(=O)[O-].[Na+].[Cl+].C(CCCCCCCCCCC)(=O)[O-] AJCKOXJKWPVQGU-UHFFFAOYSA-L 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 18
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 18
- 238000003809 water extraction Methods 0.000 claims description 18
- 235000019256 formaldehyde Nutrition 0.000 claims description 17
- 229960004279 formaldehyde Drugs 0.000 claims description 17
- 238000004448 titration Methods 0.000 claims description 16
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 13
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 12
- 238000009835 boiling Methods 0.000 claims description 12
- 239000012043 crude product Substances 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 9
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 150000002500 ions Chemical class 0.000 claims description 7
- 239000012467 final product Substances 0.000 claims description 6
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 6
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 5
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical group OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 2
- -1 pyridine diamidogen Chemical class 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 claims 1
- 239000010865 sewage Substances 0.000 abstract description 31
- 238000000034 method Methods 0.000 abstract description 18
- 230000000694 effects Effects 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 3
- WYUBFIMNMLLGEW-UHFFFAOYSA-M [Cl-].[Na+].C(CCCCCCCCCCC)(=O)O Chemical compound [Cl-].[Na+].C(CCCCCCCCCCC)(=O)O WYUBFIMNMLLGEW-UHFFFAOYSA-M 0.000 abstract 2
- 230000015784 hyperosmotic salinity response Effects 0.000 abstract 2
- 239000003921 oil Substances 0.000 abstract 2
- MIROPXUFDXCYLG-UHFFFAOYSA-N pyridine-2,5-diamine Chemical compound NC1=CC=C(N)N=C1 MIROPXUFDXCYLG-UHFFFAOYSA-N 0.000 abstract 2
- 239000010779 crude oil Substances 0.000 abstract 1
- 230000018044 dehydration Effects 0.000 abstract 1
- 238000006297 dehydration reaction Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 5
- 229920002401 polyacrylamide Polymers 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 229960004756 ethanol Drugs 0.000 description 4
- 238000005189 flocculation Methods 0.000 description 4
- 230000016615 flocculation Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 150000001450 anions Chemical class 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 241001044369 Amphion Species 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- 239000004368 Modified starch Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000001348 alkyl chlorides Chemical class 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960003237 betaine Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000000481 breast Anatomy 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/68—Treatment of water, waste water, or sewage by addition of specified substances, e.g. trace elements, for ameliorating potable water
- C02F1/682—Treatment of water, waste water, or sewage by addition of specified substances, e.g. trace elements, for ameliorating potable water by addition of chemical compounds for dispersing an oily layer on water
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/547—Tensides
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/72—Nitrogen atoms
- C07D213/74—Amino or imino radicals substituted by hydrocarbon or substituted hydrocarbon radicals
-
- 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
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Pyridine Compounds (AREA)
Abstract
The invention belongs to the technical field of oil field sewage treatment, and in particular, relates to a ternary compound flooding produced water deoiling agent; the deoiling agent is a zwitterionic deoiling agent prepared by the steps of carrying out a reaction of 2,5-pyridine diamine with formaldehyde and formic acid to generate an intermediate and then carrying out a reaction of the intermediate with sodium laurate chloride, wherein the molar ratio of 2,5-pyridine diamine to formaldehyde to formic acid to sodium laurate chloride is 1 to (2.5-6) to (2.5-5.5) to (0.8-2.5), preferably (1-3) to 3 to 3 to 1.5. The deoiling agent has the advantages of simple preparation, strong adaptability, low cost, strong salt tolerance and good deoiling effect, the salt tolerance reaches 2.3*10<4> mg/L, and the deoiling rate of ternary compound flooding produced water reaches more than or equal to 97%. Recovered oil produced by separation does not affect subsequent dehydration of crude oil, so the deoiling agent can be widely applied in the deoiling process of the ternary compound flooding produced water.
Description
Technical field
The present invention relates to a kind of degreaser for disposing polluted water in oil, and in particular to a kind of ternary composite flooding water extraction
Degreaser and preparation method thereof.
Background technology
In recent years China accelerates to have promoted tertiary oil recovery production technique, to maintain and improve crude output.Alkali-surface activity
Agent-polymer ternary combination flooding is grown up on the basis of surfactant flooding, caustic flooding and polymer displacement of reservoir oil method
A chemical displacement of reservoir oil technology.Relevant research shows that ternary composite driving can significantly improve recovery ratio, front with wide application
Scape.
But due to ternary combination flooding extraction sewage water quality it is complicated, the alkali containing a large amount of residuals, surfactant and poly-
Compound (such as polyacrylamide PAM), the viscosity for causing sewage becomes big, and sewage oil bead diameter diminishes, and causes sewage emulsifying serious, increases
The difficulty of Produced Liquid breakdown of emulsion and purification is added.Meanwhile, the process side of " two grades of sedimentation+cascade filtrations " that oil field generally adopts now
Formula can not meet environmental requirement, occur in that equipment disposal ability is reduced, the sedimentation time is long, effluent quality is unqualified etc. and ask
Topic.
At present frequently with measure mainly have：1. physical means polymer-contained sewage.At present electrochemical method is main
Physical means processing method, wherein electric flocculation technique are more ripe because of its study mechanism, and electrode material is easily obtained, small investment,
The features such as being easy to automatization two is gradually widely used in sewage disposal；2. chemical method polymer-contained sewage.Such technology is first
Breakdown of emulsion process is first carried out, then the medicament such as further preferably suitable degreaser carries out purification technique.At present conventional medicament mainly has
Quaternary, polymer modified clays type, polyacrylamide organic polymer type and modified starch etc., and achieve preferably
Flocculation, oil removing action effect.
Patent ZL201410455664.7 " a kind of degreaser for oil field binary combination flooding output sewage " employs third
Alkene acyloxyethyl dimethyl amine, alkyl chloride, acrylamide, N, N '-methylene-bisacrylamide, Ammonium persulfate. and sodium sulfite are anti-
Should form, the degreaser has consumption few, low cost, the characteristics of oil removal rate is high, oil removal efficiency is high, prepare simple, cost is low
Feature, but the degreaser belongs to reverse demulsifier, it is poor for the demulsification of emulsion oil-in-water, meanwhile, the degreaser
It is not suitable for the oil removal treatment of the ternary combination flooding extraction sewage of complicated component.
The content of the invention
The present invention provides a kind of degreaser and its system of ternary composite flooding water extraction for the deficiency of currently available technology
Preparation Method, the degreaser has process is simple, a with low cost, strong adaptability, and strong with anti-salt property and deoiling effect is good
Feature, salt tolerant reaches 2.3 × 104Mg/L, the oil removal rate of ternary composite flooding water extraction is up to more than 97%.
It is an object of the invention to provide a kind of degreaser of ternary composite flooding water extraction, described degreaser is by 2,5-
Pyridine diamidogen generates intermediate with formaldehyde, formic acid reaction, then generates amphoteric ion type degreaser with the reaction of chlorine sodium laurate, its
Molecular formula is as follows：
The mol ratio of described 2,5- pyridine diamidogen, formaldehyde, formic acid and chlorine sodium laurate is 1: 2.5～6: 2.5～5.5:
0.8～2.5, preferably 1: 3: 3: 1.5.
Further object is that providing a kind of preparation method of the degreaser of ternary composite flooding water extraction, this is removed
The preparation method of oil preparation specifically includes following steps：
(1) 2, the 5- pyridines diamidogen and solvent of above-mentioned mol ratio are added in there-necked flask, are loaded onto with water knockout drum
Reflux condensing tube, stir speed (S.S.) is 200～300rpm, is warming up to 30～40 DEG C, pours the formic acid of above-mentioned mol ratio into constant pressure drop
In liquid funnel, rate of titration is controlled, formic acid is dripped off in 20～30min, after formic acid is dripped off, it is 500 to adjust stir speed (S.S.)
～600rpm, is warming up to 50～55 DEG C, and the formaldehyde of aforementioned proportion is poured in constant pressure funnel, controls rate of titration, makes first
Aldehyde is dripped off in 40～60min, after formol titration is finished, is warming up to 80～85 DEG C, and Temperature fall is obtained after 10～24h of reaction
Solution A；
(2) it is 12～13 to pH value with the above-mentioned solution A of potassium hydroxide alkalization that mass concentration is 20%, uses n-hexane extraction
Upper strata liquid, removes solvent, obtains crude product B；
(3) above-mentioned crude product B is poured in four-hole boiling flask, adds dehydrated alcohol, load onto condensing tube, be in stir speed (S.S.)
It is under 100～300rpm, the chlorine sodium laurate of aforementioned proportion is soluble in water, then it is slowly added in four-hole boiling flask with funnel,
70～75 DEG C are then heated to, stir speed (S.S.) is 350～400rpm, is alkalized to pH value with the sodium bicarbonate that mass concentration is 25%
For 8～9, Temperature fall obtains solution C after 10～14h of reaction；
(4) pH to 2～3 of solution C is adjusted with the HCl of 6mol/L, stands 24～36h, then rotation is steamed under vacuum environment
Second alcohol and water is sent, is vacuum dried；Finally washed with ether 3～5 times, obtain the degreaser of the final product present invention.
Described solvent is Hexalin or benzene, and consumption is 10～25 times of 2,5- pyridine diamidogen quality；Described normal hexane
Consumption be 2～3 times of 2,5- pyridine diamidogen quality；The consumption of described dehydrated alcohol for 2,5- pyridine diamidogen quality 5～
10 times；The consumption of described ether is 0.5～1 times of 2,5- pyridine diamidogen quality.
Described reaction equation is as follows：
A kind of degreaser of ternary composite flooding water extraction, it uses technical process as follows：
According to oil-containing situation in ternary compound oil drive output water, the degreaser of the present invention is added in sewage, realized broken
Breast and oil-water separation, after reclaiming petroleum substance, are further processed for subsequent technique.The concrete addition of degreaser is as follows：
(1) during oil-containing α >=500mg/L, it is 50～150mg/L to add degreaser to make the mass concentration of degreaser in sewage；
During (2) 500 ＞ oil-containings α >=300mg/L, add degreaser make degreaser in sewage mass concentration be 30～
50mg/L；
During (3) 300 ＞ oil-containings α >=100mg/L, add degreaser make degreaser in sewage mass concentration be 10～
30mg/L；
(4) during oil-containing α ＜ 100mg/L, it is 0.1～10mg/L to add degreaser to make the mass concentration of degreaser in sewage.
The degreaser of the ternary composite flooding water extraction that the present invention is provided, it belongs to glycine betaine (amphion) type surface activity
Agent, the molecule has cation and anion amphion group, and its cation can attract each other with anion, is easily formed
More firm skin covering of the surface, after greasy surfaces are adsorbed onto, can shell in the surfactant in ternary combination flooding extraction sewage
From going down, with stronger interfacial activity.Heterocyclic group containing N in the molecule and the hydrophobic group being attached thereto have with greasy dirt
There is analog structure, it is easy to greasy dirt absorption, promote the degreaser flocculation dirty with Oil in Sewage Water；Due to both having on molecule
Anion and cation, extraneous ion be difficult to it is close with degreaser, so its anti-salt property is stronger；Additionally, going back on molecule
Can tangle with polyacrylamide amine molecule so that extensibility of the polyacrylamide in sewage is deteriorated, so as to reduce dirt
The viscosity of water, accelerates the speed of oil-water separation.
The present invention has the advantage that compared with prior art and beneficial effect：
(1) extensively, synthesis technique is simple, and strong adaptability can meet environmental conservation for the raw material sources of degreaser of the invention
With the needs of oil field development；
(2) degreaser of the invention can reduce the viscosity of sewage, and anti-salt property is good, and salt tolerant is up to 2.3 × 104Mg/L and
Inorganic flocculation composition is not contained；
(3) the characteristics of degreaser of the invention has oil removal efficiency high, the oil removal rate of ternary composite flooding water extraction is up to 97%
More than, more existing medicament improves more than 50%, meets the requirement of the oil removing pretreatment of ternary composite flooding water extraction.
Specific embodiment
With reference to specific embodiment, and the present invention is described in further detail with reference to data.It should be understood that these embodiments
It is of the invention solely for the purpose of illustration, rather than the scope of the present invention is limited by any way.
Embodiment 1：Degreaser H1And preparation method thereof
(1) degreaser H1Composition, component and molecular formula it is as follows：
Degreaser H1Intermediate is generated by 2,5- pyridines diamidogen and formaldehyde, formic acid reaction, is then reacted with chlorine sodium laurate
Amphoteric ion type degreaser is generated, wherein, the mol ratio of 2,5- pyridine diamidogen, formaldehyde, formic acid and chlorine sodium laurate is 1: 2.5:
2.5∶0.8.Degreaser H1Molecular formula it is as follows：
(2) degreaser H1Preparation method it is as follows：
1. 2, the 5- pyridines diamidogen and 1091.5g Hexalin of 1mol are added in there-necked flask, are loaded onto with water knockout drum
Reflux condensing tube, stir speed (S.S.) is 230rpm, is warming up to 30 DEG C, and the formic acid of 2.5mol is poured in constant pressure funnel, control
Rate of titration processed, makes formic acid drip off in 20min, and after formic acid is dripped off, regulation stir speed (S.S.) is 530rpm, is warming up to 50 DEG C,
The formaldehyde of 2.5mol is poured in constant pressure funnel, rate of titration is controlled, formaldehyde is dripped off in 40min, treat formol titration
After finishing, 82 DEG C are warming up to, Temperature fall obtains solution A after reaction 10h；
2. it is 12 to pH value with the above-mentioned solution A of potassium hydroxide alkalization that mass concentration is 20%, uses n-hexane extraction upper strata
Liquid, normal hexane consumption is 218.3g, removes solvent, obtains crude product B；
3. above-mentioned crude product B is poured in four-hole boiling flask, adds 545.8g dehydrated alcohol, load onto condensing tube, in stirring
Speed be 100rpm under, the chlorine sodium laurate of 0.8mol is soluble in water, be then slowly added in four-hole boiling flask with funnel, so
After be warming up to 72 DEG C, stir speed (S.S.) is 350rpm, with the sodium bicarbonate that mass concentration is 25% alkalize to pH value be 8, react 10h
Afterwards Temperature fall obtains solution C；
4. the pH to 2 of solution C is adjusted with the HCl of 6mol/L, stands 24h, then rotation evaporates ethanol under vacuum environment
And water, vacuum drying；Finally washed with ether 3 times, the consumption of ether is 54.6g, obtains the degreaser of the final product present invention
H1。
Embodiment 2：Degreaser H2And preparation method thereof
(1) degreaser H2Composition, component and molecular formula it is as follows：
Degreaser H2Intermediate is generated by 2,5- pyridines diamidogen and formaldehyde, formic acid reaction, is then reacted with chlorine sodium laurate
Amphoteric ion type degreaser is generated, wherein, the mol ratio of 2,5- pyridine diamidogen, formaldehyde, formic acid and chlorine sodium laurate is 1: 3: 3:
1.5.Degreaser H1Molecular formula it is as follows：
(2) degreaser H2Preparation method it is as follows：
1. 2, the 5- pyridines diamidogen and 1637.3g benzene of 1mol are added in there-necked flask, load onto returning with water knockout drum
Stream condensing tube, stir speed (S.S.) is 200rpm, is warming up to 32 DEG C, and the formic acid of 3mol is poured in constant pressure funnel, control titration
Speed, makes formic acid drip off in 28min, and after formic acid is dripped off, regulation stir speed (S.S.) is 500rpm, 52 DEG C is warming up to, by 3mol
Formaldehyde pour in constant pressure funnel, control rate of titration, formaldehyde is dripped off in 50min, after formol titration is finished, rise
To 80 DEG C, Temperature fall obtains solution A to temperature after reaction 16h；
2. it is 12 to pH value with the above-mentioned solution A of potassium hydroxide alkalization that mass concentration is 20%, uses n-hexane extraction upper strata
Liquid, normal hexane consumption is 265.2g, removes solvent, obtains crude product B；
3. above-mentioned crude product B is poured in four-hole boiling flask, adds 756.3g dehydrated alcohol, load onto condensing tube, in stirring
Speed be 150rpm under, the chlorine sodium laurate of 1.5mol is soluble in water, be then slowly added in four-hole boiling flask with funnel, so
After be warming up to 70 DEG C, stir speed (S.S.) is 360rpm, with the sodium bicarbonate that mass concentration is 25% alkalize to pH value be 9, react 12h
Afterwards Temperature fall obtains solution C；
4. the pH to 2 of solution C is adjusted with the HCl of 6mol/L, stands 28h, then rotation evaporates ethanol under vacuum environment
And water, vacuum drying；Finally washed with ether 3 times, the consumption of ether is 64.3g, obtains the degreaser of the final product present invention
H2。
Embodiment 3：Degreaser H3And preparation method thereof
(1) degreaser H3Composition, component and molecular formula it is as follows：
Degreaser H3Intermediate is generated by 2,5- pyridines diamidogen and formaldehyde, formic acid reaction, is then reacted with chlorine sodium laurate
Amphoteric ion type degreaser is generated, wherein, the mol ratio of 2,5- pyridine diamidogen, formaldehyde, formic acid and chlorine sodium laurate is 1: 5: 4:
2.Degreaser H3Molecular formula it is as follows：
(2) degreaser H3Preparation method it is as follows：
1. 2, the 5- pyridines diamidogen and 2183g Hexalin of 1mol are added in there-necked flask, are loaded onto with water knockout drum
Reflux condensing tube, stir speed (S.S.) is 270rpm, is warming up to 35 DEG C, and the formic acid of 4mol is poured in constant pressure funnel, control drop
Constant speed degree, makes formic acid drip off in 24min, and after formic acid is dripped off, regulation stir speed (S.S.) is 580rpm, is warming up to 53 DEG C DEG C, will
The formaldehyde of 5mol is poured in constant pressure funnel, controls rate of titration, formaldehyde is dripped off in 45min, treats that formol titration is finished
Afterwards, 84 DEG C are warming up to, Temperature fall obtains solution A after reaction 20h；
2. it is 13 to pH value with the above-mentioned solution A of potassium hydroxide alkalization that mass concentration is 20%, uses n-hexane extraction upper strata
Liquid, normal hexane consumption is 301.5g, removes solvent, obtains crude product B；
3. above-mentioned crude product B is poured in four-hole boiling flask, adds 865.2g dehydrated alcohol, load onto condensing tube, in stirring
Speed be 250rpm under, the chlorine sodium laurate of 2.0mol is soluble in water, be then slowly added in four-hole boiling flask with funnel, so
After be warming up to 73 DEG C, stir speed (S.S.) is 380rpm, with the sodium bicarbonate that mass concentration is 25% alkalize to pH value be 8, react 13h
Afterwards Temperature fall obtains solution C；
4. the pH to 3 of solution C is adjusted with the HCl of 6mol/L, stands 32h, then rotation evaporates ethanol under vacuum environment
And water, vacuum drying；Finally washed with ether 4 times, the consumption of ether is 85.3g, obtains the degreaser of the final product present invention
H3。
Embodiment 4：Degreaser H4And preparation method thereof
(1) degreaser H4Composition, component and molecular formula it is as follows：
Degreaser H4Intermediate is generated by 2,5- pyridines diamidogen and formaldehyde, formic acid reaction, is then reacted with chlorine sodium laurate
Amphoteric ion type degreaser is generated, wherein, the mol ratio of 2,5- pyridine diamidogen, formaldehyde, formic acid and chlorine sodium laurate is 1: 6: 5.5
∶2.5.Degreaser H1Molecular formula it is as follows：
(2) degreaser H4Preparation method it is as follows：
1. 2, the 5- pyridines diamidogen and 2728.7g benzene of 1mol are added in there-necked flask, load onto returning with water knockout drum
Stream condensing tube, stir speed (S.S.) is 300rpm, is warming up to 40 DEG C, and the formic acid of 5.5mol is poured in constant pressure funnel, control drop
Constant speed degree, makes formic acid drip off in 30min, and after formic acid is dripped off, regulation stir speed (S.S.) is 600rpm, is warming up to 55 DEG C, will
The formaldehyde of 6mol is poured in constant pressure funnel, controls rate of titration, formaldehyde is dripped off in 60min, treats that formol titration is finished
Afterwards, 85 DEG C are warming up to, Temperature fall obtains solution A after reaction 24h；
2. it is 13 to pH value with the above-mentioned solution A of potassium hydroxide alkalization that mass concentration is 20%, uses n-hexane extraction upper strata
Liquid, normal hexane consumption is 327.4g, removes solvent, obtains crude product B；
3. above-mentioned crude product B is poured in four-hole boiling flask, adds 1091.5g dehydrated alcohol, load onto condensing tube, in stirring
Speed be 300rpm under, the chlorine sodium laurate of 2.5mol is soluble in water, be then slowly added in four-hole boiling flask with funnel, so
After be warming up to 75 DEG C, stir speed (S.S.) is 400rpm, with the sodium bicarbonate that mass concentration is 25% alkalize to pH value be 9, react 14h
Afterwards Temperature fall obtains solution C；
4. the pH to 3 of solution C is adjusted with the HCl of 6mol/L, stands 36h, then rotation evaporates ethanol under vacuum environment
And water, vacuum drying；Finally washed with ether 5 times, the consumption of ether is 109.15g, obtains the oil removing of the final product present invention
Agent H4。
The degreaser H of embodiment 51Scene application
Multi-purpose station M2Water be ternary composite driving output water, test process scale be 90m3/ d, water oil content 765mg/
L, sewage salinity 22560mg/L, using the degreaser H of the present invention1To multi-purpose station M2Sewage carry out oil removal treatment, degreaser
H1Dosage be 6.3kg/d, add degreaser in sewage after degreaser concentration be 70mg/L, oil content is reduced to after process
19.1mg/L, oil content reduces by 97.5%, reaches technological requirement.
The degreaser H of embodiment 62Scene application
Multi-purpose station L2Water be ternary composite driving output water, test process scale be 60m3/ d, water oil content 586mg/
L, sewage salinity 20253mg/L, using the degreaser H of the present invention2To multi-purpose station L2Sewage carry out oil removal treatment, degreaser
H2Dosage be 3.3kg/d, add degreaser in sewage after degreaser concentration be 55mg/L, oil content is reduced to after process
8.2mg/L, oil content reduces by 98.6%, reaches technological requirement.
The degreaser H of embodiment 73Scene application
Multi-purpose station L5Water be ternary composite driving output water, test process scale be 50m3/ d, water oil content 823mg/
L, sewage salinity 18256mg/L, using the degreaser H of the present invention3To multi-purpose station L5Sewage carry out oil removal treatment, degreaser
H3Dosage be 4.0kg/d, add degreaser in sewage after degreaser concentration be 80mg/L, oil content is reduced to after process
16.5mg/L, oil content reduces by 98.0%, reaches technological requirement.
The degreaser H of embodiment 84Scene application
Multi-purpose station L6Water be ternary composite driving output water, test process scale be 100m3/ d, water oil content
752mg/L, sewage salinity 17650mg/L, using the degreaser H of the present invention4To multi-purpose station L6Sewage carry out oil removal treatment,
Degreaser H4Dosage be 7.0kg/d, add degreaser in sewage after degreaser concentration be 70mg/L, oil content after process
20.3mg/L is reduced to, oil content reduces by 97.3%, reaches technological requirement.
Claims (8)
1. a kind of degreaser of ternary composite flooding water extraction, it is characterised in that described degreaser be by 2,5- pyridines diamidogen with
Formaldehyde, formic acid reaction generate intermediate, then generate amphoteric ion type degreaser with the reaction of chlorine sodium laurate, and its molecular formula is such as
Under：
2. the degreaser of ternary composite flooding water extraction according to claim 1, it is characterised in that described 2,5- pyridines two
The mol ratio of amine, formaldehyde, formic acid and chlorine sodium laurate is 1: 2.5～6: 2.5～5.5: 0.8～2.5.
3. the degreaser of ternary composite flooding water extraction according to claim 1 and 2, it is characterised in that described 2,5- pyrroles
The mol ratio of pyridine diamidogen, formaldehyde, formic acid and chlorine sodium laurate is 1: 3: 3: 1.5.
4. a kind of preparation method of the degreaser of ternary composite flooding water extraction, it is characterised in that the preparation method is specifically included
Following steps：
(1) 2, the 5- pyridines diamidogen and solvent of above-mentioned mol ratio are added in there-necked flask, load onto the backflow with water knockout drum
Condensing tube, stir speed (S.S.) is 200～300rpm, is warming up to 30～40 DEG C, pours the formic acid of above-mentioned mol ratio into constant pressure addition leakage
In bucket, control rate of titration, formic acid is dripped off in 20～30min, after formic acid is dripped off, adjust stir speed (S.S.) be 500～
600rpm, is warming up to 50～55 DEG C, and the formaldehyde of aforementioned proportion is poured in constant pressure funnel, controls rate of titration, makes formaldehyde
Drip off in 40～60min, after formol titration is finished, be warming up to 80～85 DEG C, Temperature fall obtains molten after 10～24h of reaction
Liquid A；
(2) it is 12～13 to pH value with the above-mentioned solution A of potassium hydroxide alkalization that mass concentration is 20%, uses n-hexane extraction upper strata
Liquid, removes solvent, obtains crude product B；
(3) above-mentioned crude product B is poured in four-hole boiling flask, adds dehydrated alcohol, load onto condensing tube, be 100 in stir speed (S.S.)
It is under～300rpm, the chlorine sodium laurate of aforementioned proportion is soluble in water, then it is slowly added in four-hole boiling flask with funnel, then
70～75 DEG C are warming up to, stir speed (S.S.) is 350～400rpm, it is 8 to be alkalized to pH value with the sodium bicarbonate that mass concentration is 25%
～9, Temperature fall obtains solution C after 10～14h of reaction；
(4) pH to 2～3 of solution C is adjusted with the HCl of 6mol/L, stands 24～36h, then rotation is evaporated under vacuum environment
Second alcohol and water, vacuum drying；Finally washed with ether 3～5 times, obtain the degreaser of the final product present invention.
5. the preparation method of the degreaser of ternary composite flooding water extraction according to claim 4, it is characterised in that described
Solvent is Hexalin or benzene, and consumption is 10～25 times of 2,5- pyridine diamidogen quality.
6. the preparation method of the degreaser of the ternary composite flooding water extraction according to claim 4 or 5, it is characterised in that institute
The consumption of the normal hexane stated is 2～3 times of 2,5- pyridine diamidogen quality.
7. the preparation method of the degreaser of ternary composite flooding water extraction according to claim 6, it is characterised in that described
The consumption of dehydrated alcohol is 5～10 times of 2,5- pyridine diamidogen quality.
8. the preparation method of the degreaser of ternary composite flooding water extraction according to claim 7, it is characterised in that described
The consumption of ether is 0.5～1 times of 2,5- pyridine diamidogen quality.
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| CN110182895A (en) * | 2019-05-23 | 2019-08-30 | 中国石油化工股份有限公司 | A kind of degreaser and preparation method thereof for polymer-containing sewage in oil field processing |
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