CN1069913C - Oil-displacing agent and its preparing process - Google Patents
Oil-displacing agent and its preparing process Download PDFInfo
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- CN1069913C CN1069913C CN 96109015 CN96109015A CN1069913C CN 1069913 C CN1069913 C CN 1069913C CN 96109015 CN96109015 CN 96109015 CN 96109015 A CN96109015 A CN 96109015A CN 1069913 C CN1069913 C CN 1069913C
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Abstract
The present invention relates to crude oil displacement agents which use natural mixed carboxylate as a main active component, and a preparation method thereof. The natural mixed carboxylate is saponified by lipidic leftover, and comprises the components of animal oil soap, peanut oil soap, soybean oil soap, cottonseed oil soap, tea saponin, etc. Two classes of oil displacement agents which comprise individual well gorge and disgorge oil displacement agents I and ASP composite oil displacement agents II can be proportionally compounded by the natural mixed carboxylate and corresponding various auxiliary agents. The formula is adjusted according to the size of crude oil acid values. The present invention has the advantages of simple preparation progress, low product cost, and good oil displacement effect, and can greatly enhance the recovery ratio of crude oil.
Description
The present invention is the former oil displacement agent that mainly contains effective constituent from natural mixed carboxylic acid's salt, belongs to organic chemistry composition and preparing technical field.
As a kind of non-renewable energy-oil, improve taking rate and be not only the problem that the petroleum industrial circle emphasis is considered, and be the problem that entire society generally is concerned about.Utilize the crude oil of producing energy extraction to be called primary oil recovery, recovery ratio is 10-20%; Thereafter keep reservoir pressure by man-made injection and recover the oil, be called secondary oil recovery, recovery ratio is 15-20%; This twice oil recovery sum, promptly the ordinary method recovery ratio only is 35-40%.That is to say to also have 60-65% crude oil to stay in the stratum not come out by exploitation, this a part of crude oil production belongs to the target of tertiary oil recovery.Tertiary oil recovery need be used various physico-chemical processes.Oil-displacing agent is meant and injects the material that crude oil is driven to behind the stratum producing well.Tertiary oil recovery will be used different oil-displacing agents according to different flooding methods.Some is to improve sweep efficiency in these oil-displacing agents, and some is to improve displacement efficiency, and some is that both have both.
The oil-displacing agent of table 1. tertiary oil recovery
| Displacement of reservoir oil method | Oil-displacing agent |
| Polymer flooding alkali surfactant flooding mixed phase drives steam and drives | Aqueous solutions of polymers alkali aqueous solution active water, micellar solution, microemulsion, foam, liquefied petroleum gas (LPG) such as milk sap, carbonic acid gas, water vapors such as nitrogen |
1997 the U.S. " Society of Petroleum Engineering's magazine " people's such as Reed article " the unmixing microemulsion drives " (" Immiscible Microemulsion Flooding " is disclosed, Reed, R.L., et al, Soc.Petrd.Eng.J., 1977,4,129), the author is by the model oil displacement test, the proof microemulsion flooding is most effective, but because of cost is high can't be in industrial popularization.In order to reduce the tertiary oil recovery cost, the nineties a kind of ternary composite driving that grows up again, promptly with alkali (A), the ASP compound system that tensio-active agent (S) and polymkeric substance (P) etc. are formed.This method fully takes into account the bronsted lowry acids and bases bronsted lowry effect of crude oil PetroChina Company Limited., generates the petroleum soap tensio-active agent, and its oil displacement efficiency is driven near microemulsion.This method add dosage of surfactant only for microemulsion drive 1/3rd, cost for oil production is reduced significantly.The tensio-active agent overwhelming majority who uses in tertiary oil recovery is a sulfonated petro-leum, and alkyl carboxylate's price is cheaper than sulfonated petro-leum, replaces sulfonated petro-leum obviously to be subjected to people's attention with the alkyl carboxylate.United States Patent (USP) U.S.Pat.4,460,484 (1984) disclose FOX people's such as (Force) invention " tertiary oil recovery tensio-active agent " (" Tertiary Oil Recovery Surfactanls "), the contriver vegetables oil not conjugated double bond under catalyst action, reset, and and vinylformic acid, fumaric acid reaction modifying, prepare petroleum carboxylate thus and be used for tertiary oil recovery.This method more complicated, and the data of oil field test in place are not arranged, still remain further perfect.Nineteen ninety " U.S. oiling learn magazine " discloses people's such as road Min human relations article " in the application and carboxylate salt be the oil-water ultra low interfacial tension of tensio-active agent ", [" Uitralow Oil-Water IFT Using Neutralzed Hydrocarbons asSurfactant ", Domellan, W.H., et al, J.Am.Oil Chem, 1990,67 (6) 406] propose petroleum hydrocarbon oxidizing and prepare petroleum carboxylate and be used for tertiary oil recovery, but exist on the high side equally and problem such as field test data is not arranged.
The objective of the invention is to, remedy the deficiency of prior art, a kind of oil-displacing agent based on natural mixed carboxylic acid's salt is provided.This oil-displacing agent, preparation technology is simple, and facility investment is little, and product cost is low, the recovery ratio advantages of higher.
Oil-displacing agent of the present invention comprises by natural mixed carboxylic acid's salt (T) and other composite assistant two parts and forming.According to the difference of flooding method, select composite assistant difference to some extent for use.The main two big classes of dividing: the one, single well stimulation oil-displacing agent, another kind are the ASP compound oil displacement agents.
One, single well stimulation oil-displacing agent I
Natural mixed carboxylic acid's salt T (all being weight percentage, down together) composed as follows:
Animal oil soap 1-20%, peanut oil soap 2-20%, soybean oil soap 2-20%, Oleum Gossypii semen soap 30-90%, tea saponin 0-10%
The degree of neutralization of T is 70-100%, and accounts for the 60-90% of oil-displacing agent total amount.
It is as follows that composite assistant accounts for the percentage composition of oil-displacing agent I total amount:
Na
2CO
30～5%, calcium ions and magnesium ions complexing agent 2-8%, permeate agent 1-5%, synthetic surfactant 2-20%, urea 2-7%.
The height of oil-displacing agent I based on crude acid number is selected the tensio-active agent and the auxiliary agent of suitable proportioning, speaks frankly down specifically:
A. the crude oil with high acid value oil-displacing agent is formed, and this acid value for crude oil is 1～3mg KOH/g crude oil, and oil-displacing agent I A type is advisable below forming:
Natural polymerization carboxylate salt T accounts for the 70-90% of oil-displacing agent gross weight, and degree of neutralization 90～100% is composed as follows:
Animal oil soap 1～10%, peanut oil soap 5～10%, soybean oil soap 5～10%, Oleum Gossypii semen soap 50-90%, tea saponin 1～5%
Auxiliary agent consists of:
Na
2CO
32-5%, calcium ions and magnesium ions complexing agent 3-5%, permeate agent 2-5%, alkylol amide 5-10%, urea 2-6%
B. the former oil displacement agent of low acid number is formed, and this acid value for crude oil is＜1mg KOH/g crude oil that oil-displacing agent I Type B is advisable below forming:
T accounts for and is 65～85% of oil-displacing agent gross weight, and degree of neutralization 70-90% is composed as follows:
Animal oil soap 0-5%, peanut oil soap 3～10%, soybean oil soap 3-15%, Oleum Gossypii semen soap 40-85%, tea saponin 0-3%
Auxiliary agent consists of:
Na
2CO
30-2%, calcium ions and magnesium ions complexing agent 2-4%, permeate agent 1-5%, trimethyl-glycine 3-10%,
Alkyl alcohol Soxylat A 25-7 3-10%, alkyl alcohol polyoxyethylene sodium sulfate 2-10%, urea 2-7%
Above permeate agent is best to draw back powder, the first-selected tripoly phosphate sodium STPP of calcium ions and magnesium ions complexing agent.
Two, ASP composite displacement system oil-displacing agent II
Natural mixed carboxylic acid's salt T form with the oil-displacing agent I in identical, content accounts for the 0.3-3.0% of oil-displacing agent II total amount; Degree of neutralization 65～100%.
It is as follows that composite assistant accounts for the percentage composition of oil-displacing agent II total amount:
Multiple alkali (Na
2CO
3: NaHCO
3=1: 0.7～1.5, weight ratio) 1～5%
Vegetable jelly (containing pectin, polysaccharide and Mierocrystalline cellulose) 3～20%
Polyacrylamide (molecular weight 250-1700 ten thousand) 0.05～1%
Surplus is a water.
Based on crude acid number height, need select optimal proportioning to natural mixed carboxylic acid's salt T and composite assistant:
A. the oil-displacing agent II A of crude oil with high acid value forms
Acid value for crude oil with (one, A), oil-displacing agent II A prescription is as follows:
Natural mixed carboxylic acid's salt T accounts for the 0.3-2.5% of oil-displacing agent gross weight, degree of neutralization 90-100%; Multiple alkali is 1-2% in the auxiliary agent, molecular weight 1, and 000-1,7,000,000 polyacrylamide are 0.07-0.20%, all the other are water.
B. the oil-displacing agent II B of acid number crude oil forms
Acid value for crude oil with (one, B), oil-displacing agent II B prescription is as follows:
Natural mixed carboxylic acid's salt T accounts for the 0.5-3.0% of oil-displacing agent II gross weight, degree of neutralization 65-90%; Vegetable jelly 3-5% in the auxiliary agent, molecular weight 250-600 ten thousand polyacrylamide 0.1-0.2%; All the other are water.
The preparation method of oil-displacing agent of the present invention mainly comprises the production of natural mixed carboxylic acid's salt, carries out each composition composite in proportion then.The production method of natural mixed carboxylic acid's salt is as follows:
1. raw material: the grease tankage comprise animal grease, peanut oil, soybean oil, Oleum Gossypii semen, tea oil.Its main component is: tri-glyceride, diglyceride, monoglyceride, free fatty acids and some lipoids (phosphide, sterol, pigment etc.).Its hydrolysis and saponification resultant, because of fat type different for example slightly different:
Soybean oil C16: 0 (palmitinic acid), C18: 0 (stearic acid), C18: 1 (oleic acid), C18: 2 (linolic acid), C18: 3 (linolenic acid)
％ 2～7 4～7 32～36 52～57 2～7
Peanut oil C16: 0, C18: 0, C18: 1, C18: 2, the high-carbon saturated acid
％ 13.0 3.5 3.7 38 6～8
Oleum Gossypii semen C16: 0 C18: 1 C18: 2
％ 26.17 18.3 52.2
2. above-mentioned different oil foot is carried out twice saponification respectively and saltout obtaining fatty acid soaps, this moment, the product degree of neutralization was 100%.As the product of the different degree of neutralization of need, continue the following step;
3. with above-mentioned fatty acid soaps acid treatment obtain fatty acid;
4. with the above-mentioned all kinds of natural carboxylic acids that make by different material, be neutralized to the degree of neutralization of requirement with alkali, be mixed in proportion then and promptly get natural mixed carboxylic acid's salt;
The concrete working condition of natural mixed carboxylic acid's salt is:
(1) saponification and saltouing: add the oil foot of chopping in 80 ℃ of water, water and oil foot weight ratio 1: 1 stir and are heated to and boil.Hydro-oxidation sodium control PH=13～14, reaction approximately needs 2～5 hours.Add NaCl by 1/10 of oil foot weight after saponification is finished and saltout, the cooling layering discards bottom waste water, promptly obtains once saponified;
(2) secondary saponification and saltouing: saponified repetition said process once, different is to begin promptly to use boiling water, adding NaCl when saltouing is that 1/12 of oil foot weight gets final product; This moment, the product degree of neutralization was 100%.
(3) the above-mentioned secondary of adding is saponified in boiling water, and saponified and weight ratio water is (3～4): 10, and heating while stirring adds 50%H
2SO
4To PH=2, reacted 0.5-2 hour, obtain brownish black lipid acid, discard bottom waste water.Divide washing for several times with heavy 100 ℃ tap water using, be washed till PH=5～6. get the upper strata black liquor, be lipid acid with former boiling water;
(4) above-mentioned lipid acid is added the degree of neutralization that NaOH is neutralized to requirement, in proportion different sorts soap is mixed again, be natural mixed carboxylic acid's salt T.
The salient features of oil-displacing agent of the present invention is as follows:
1. for single well stimulation oil-displacing agent system:
(1) the minimum instantaneous interfacial tension IFTmin=10 of I A system
-2-10
-4MNm
-1
(2) the minimum instantaneous interfacial tension IFTmin=10 of I B system
-1-10
-2MNm
-1
2. for the ASP composite displacement system
(1) the minimum instantaneous interfacial tension of II A system, IFTmin=10
-3～10
-5MNm
-1, indoor oil displacement test recovery ratio 15～25% (OOIP)
(2) the minimum instantaneous interfacial tension of II B system, IFTmin=10
-2～10
-3MNm
-1, indoor oil-recovering rate 10～18% (OOIP)
The invention will be further described below in conjunction with embodiment.
Embodiment 1, single well stimulation oil-displacing agent I A system
(1) oil well situation
Oil density 0.9523g/cm
3, viscosity 278.91mPaS, acid number 1.02mg KOH/g crude oil, core intersection 58.1m/30 layer, productive zone position 2264.8～2610.5m, stratum water quality total mineralization 52.720mgL
-1, Ca Lv 628mg.L wherein
-1, Mg Lv 153mg.L
-1
(2) oil-displacing agent is formed
Animal oil soap 2%, peanut oil soap 10%, soybean oil soap 5%, Oleum Gossypii semen soap 80%, tea saponin 3%.
Natural mixed carboxylic acid's salt accounts for 85% of oil-displacing agent total amount, degree of neutralization 100%.
Auxiliary agent is:
Na
2CO
33%, tripoly phosphate sodium STPP 5%, two (2-ethylhexyl) sulfosuccinate sodium (permeate agent) 2%,
Alkylol amide (synthetic surfactant) 2%, urea 3%.
(3) interfacial tension of the above-mentioned 2% oil-displacing agent aqueous solution and crude oil is 3.36 * 10
-2MNm
-1
(4) oil-displacing agent is used for the working method of oil well:
70 side's solution of 2% oil-displacing agent are gone into the stratum with infusion, and closing well 48 hours drives a well then.
(5) oil-displacing agent cartogram
| Pound sign | Working system | Output situation day production fluid (m before the measure 1), day produce oil (t), moisture | Output situation day production fluid (m after the measure 1), day produce oil (t), moisture | Effective fate (day) | Accumulative total increases oil (t) |
| 2-27 | φ4×5×6.5 | 25.9 0.7 97％ | 31.2 3.4 85％ | 98 | 278 |
Embodiment 2, single well stimulation oil-displacing agent I B
(1) oil well situation
Oil density 0.8927g/cm
3, viscosity 55.1mPaS, acid number 0.32mg KOH/g crude oil, 41.7 meters/17 layers of core intersections, productive zone position 1762.2-2035.9m, stratum water quality total mineralization 136,820mg/L, Ca Lv 3; 794mg/L, Mg Lv 1,5513mg.L.
(2) oil-displacing agent is formed
Animal oil soap 1%, peanut oil soap 8%, soybean oil soap 4%, Oleum Gossypii semen soap 85%, tea saponin 2%.
Natural mixed carboxylic acid's salt accounts for 78% of oil-displacing agent total amount, degree of neutralization 85%.
Auxiliary agent is:
EDTA (divalent ion complexing agent) 0.5% draws back powder 2%, alkyl amido betaine 5%, alkyl polyoxyethylene ether 6%
Alkyl polyvinyl chloride ether sodium sulfate 5%, urea 3.5%.
Interfacial tension IFTmin=8.5 * 10 of (3) 2% oil-displacing agent solution and crude oil
-2MNm
-1
(4) concrete operations
As spearhead, 60 side's solution of 2% oil-displacing agent are gone into the stratum with infusion with 30 side's solution of 1% trisodium phosphate, closing well drove a well after 48 hours.
(5) oil-displacing agent statistical effect table
| Pound sign | Working system | Output situation day production fluid (m before the measure 1), day produce oil (t), moisture | Output situation day production fluid (m after the measure 1), day produce oil (t), moisture | Effective fate (day) | Accumulative total increases oil (t) |
| 7-153 | Φ56×4.8×7 | 20.7 1.4 92％ | 88.6～73.9 9.8～4.4 87％ | 38 | 82 |
Embodiment 3, ASP composite displacement system oil-displacing agent II (1) oil well situation oil density 0.919g/cm
3, viscosity 41.25mPaS, acid number 3.11mg KOH/g crude oil, 68 ℃ of formation temperature, zone permeability 2.563um
2, local water total mineralization 4454mgL
-1, (Ca Lv+Mg Lv) 92mgL
-1
(2) oil-displacing agent II A forms
Natural carboxylic acid's salt T forms:
Animal oil soap 3%, soybean oil soap 7% is changed oil generation soap 10%, Oleum Gossypii semen soap 75%, tea saponin 5%.
Account for 0.5% of oil-displacing agent total amount, degree of neutralization 100% (S)
Auxiliary agent:
Multiple alkali (Na
2CO
3: NaHCO
3=1: 1) (A), 0.7%
Polyacrylamide (PAM), molecular weight 1,500 ten thousand (P), 0.1%, water 98.7%.
(3) the interfacial tension IFTmin=8.83 of flooding system solution and crude oil * 10
-4MNm
-1
(4) indoor oil displacement test:
(a) rock core parameter, pipe range 20cm, caliber 2.5cm, rate of permeation 2.5um
2
(b) injection mode 0.2pv (A+S) → 0.2PV (A+S+P) → 0.2PV (P);
(c) oil-recovering rate 25.0% (OOIP).
Embodiment 4, ASP composite displacement system oil-displacing agent II
(1) oil well situation
Oil density 0.840g/cm
3, acid number 0.1mg KOH/g crude oil, 40 ℃ of formation temperature, zone permeability 1.426um
2, local water total mineralization 3896mgLCa Lv and Mg Lv 80mg.L
(2) oil-displacing agent II B forms
Natural mixed carboxylic acid's salt T forms with embodiment 2, accounts for 0.6% of oil-displacing agent total amount, and degree of neutralization is 80%.
Auxiliary agent: vegetable jelly 0.5%
Multiple alkali (Na
2CO
3: NaHCO
3=1: 0.8) 1.2%
Polyacrylamide (B-P-7) 0.16%
Water: 97.54%
(3) flooding system solution and crude oil interfacial tension, IFTmin=5.0 * LO
-3MNm
-1
(4) indoor oil displacement test
(1) pipe range 45cm, caliber 2.5cm, rate of permeation 1.5um
2
(2) injection mode
(1) S
1(SDC, 0.6%+ vegetable jelly, 0.5%); A. answer alkali 1.2%[Na
2CO
3+ NaH-CO
3(1: 1)], P
0(B-P-T) 0.14%, P
1(B-P-T); 0.07%, P
2(B-P-T) 0.05%.
(2) mode
0.3pv(S+P
0)/0.1pv(A+P
1)/0.1(A+P
2)
(3) oil displacement efficiency 18.8% (OOIP).
Embodiment 5, prepare the method for embodiment 1 oil-displacing agent I A
1. chopping respectively such as various oil foot 100Kg (animal oil foot, peanut oil foot, soybean oil residue, cottonseed oil foot),
2. water filling 100Kg in reactor is heated to 80 ℃, starts to stir the chopping oil foot is added, and continues to be heated to boiling.Reacted 3 hours hydro-oxidation sodium control PH=13～14.Add 10Kg sodium-chlor again and carry out the salt folding, the room temperature that arrives to be cooled is abandoned bottom waste water, obtains once saponified.
3. add boiling water 100Kg above-mentioned in once saponified, heating is controlled PH=13～14 with sodium hydroxide while stirring, reacts 1.5 hours.Add 8Kg sodium-chlor again and carry out the salt folding, the room temperature that arrives to be cooled discards bottom waste water, and it is saponified to obtain secondary.
4. in above-mentioned secondary is saponified, add boiling water 150Kg, add 50%H again
2SO
4Be transferred to PH=2, reacted 1 hour, obtain brownish black lipid acid, discard bottom waste water.
5. neutralize 95% degree of neutralization of hydro-oxidation sodium in above-mentioned lipid acid.
6. mix in proportion preparation 100Kg oil-displacing agent I A, promptly composed as follows:
Animal oil soap 3Kg, peanut oil soap 5Kg, soybean oil soap 10Kg, cotton seed oil soap 6Kg, tea saponin 2Kg, NaCO
33Kg, tripoly phosphate sodium STPP 3Kg draws back powder 3Kg, alkylol amide 8Kg, urea 3Kg.
Claims (2)
1.ASP the composite displacement system oil-displacing agent is characterized in that, natural mixed carboxylic acid's salt accounts for 0.3～3.0% of oil-displacing agent total amount, and composite assistant is: Na
2CO
3: NaHCO
3=1: 0.7～1.5 multiple alkali 1～5%, vegetable jelly 3～20%, molecular weight are 2,500,000 1～1,700 ten thousand polyacrylamide 0.05～1.0%, and surplus is a water; Wherein, natural mixed carboxylic acid's salt degree of neutralization 65～100%, composed as follows:
Animal oil soap 1～20%, peanut oil soap 2～20%, soybean oil soap 2～20%, Oleum Gossypii semen soap 30～90%, tea saponin 0～10%.
2, a kind of preparation method of oil-displacing agent as claimed in claim 1 comprises the following steps:
(1) raw material: the grease tankage comprise animal grease, peanut oil, soybean oil, Oleum Gossypii semen, tea oil;
(2) a kind of saponification and saltouing: the oil foot that in 80 ℃ of water, adds chopping, water and oil foot weight ratio 1: 1, stir and be heated to and boil, hydro-oxidation sodium control PH=13～14, reacted 2～5 hours, saponification is finished latter half of 1/10 adding sodium hydride by oil foot weight and is saltoutd the cooling layering, discard bottom waste water, promptly obtain once saponified;
(3) secondary saponification and saltouing: saponified weight said process once, different is to begin promptly to use boiling water, adding NaCl when saltouing is that 1/12 of oil foot weight get final product: the product degree of neutralization is 100% at this moment;
(4) the above-mentioned secondary of adding is saponified in boiling water, and saponified and weight ratio water is (3～4): 10, and heating while stirring adds 50%H
2SO
4To PH=2, reacted 0.5～2 hour, obtain brownish black lipid acid, discard bottom waste water; Divide washing for several times with heavy 100 ℃ tap water using, be washed till PH=5～6, get the upper strata black liquor, be lipid acid with former boiling water;
(5) above-mentioned lipid acid is added the degree of neutralization that NaOH is neutralized to requirement, be mixed in proportion again, be natural mixed carboxylic acid's salt;
(6) above-mentioned natural mixed carboxylic acid's salt is mixed in proportion into oil-displacing agent with composite assistant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96109015 CN1069913C (en) | 1996-07-23 | 1996-07-23 | Oil-displacing agent and its preparing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96109015 CN1069913C (en) | 1996-07-23 | 1996-07-23 | Oil-displacing agent and its preparing process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1147007A CN1147007A (en) | 1997-04-09 |
| CN1069913C true CN1069913C (en) | 2001-08-22 |
Family
ID=5120150
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|---|---|---|---|
| CN 96109015 Expired - Fee Related CN1069913C (en) | 1996-07-23 | 1996-07-23 | Oil-displacing agent and its preparing process |
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-
1996
- 1996-07-23 CN CN 96109015 patent/CN1069913C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104403653A (en) * | 2014-11-17 | 2015-03-11 | 合肥学院 | Environment-friendly tertiary oil recovery oil-displacing agent based on biosurfactant |
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|---|---|
| CN1147007A (en) | 1997-04-09 |
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