CN109536155A - Salt-resistant type Shuangzi cationic viscoelastic surfactants and preparation method thereof and salt tolerance clean fracturing fluid - Google Patents
Salt-resistant type Shuangzi cationic viscoelastic surfactants and preparation method thereof and salt tolerance clean fracturing fluid Download PDFInfo
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Abstract
The invention discloses a kind of salt-resistant type Shuangzi cationic viscoelastic surfactants and preparation method thereof and salt tolerance clean fracturing fluids, salt-resistant type Shuangzi cationic viscoelastic surfactants of the invention are obtained using fatty acid amide propyl dimethylamine and dibromoneopentyl glycol as Material synthesis, it can form micella in the seawater or water flooding of high salinity, solution is set to embody good viscoplasticity, the resistance to salinity of the viscoelastic surfactant is up to 150000mg/L or more, it can be used for configuring seawater base clean fracturing fluid, it avoids that broken glue occurs after encountering highly mineralized formation brines simultaneously；And it can also be used to configuration seawater base clean fracturing fluid, the maximum salinity that can be born reaches 200000mg/L.Preparation method of the invention is simple, and the yield of product is substantially improved, and generally reaches 96% or more, and the by-product furthermore reacted is few, influences on the performance of product small.When preparing clean fracturing fluid, dosage is reduced, and is reduced costs.
Description
Technical field
The present invention relates to petroleum reservoir technical field of surfactant, and in particular to a kind of salt-resistant type Shuangzi cation is viscous
Elastic surface activating agent and preparation method thereof and salt tolerance clean fracturing fluid.
Background technique
With the fast development of oil-gas exploration cause, a large amount of hyposmosis or the unconventional oily oil-gas reservoir of Oil in Super-low Permeability increasingly by
The concern of petroleum worker, the exploitation of this kind of oil-gas reservoir need to undergo reservoir stimulation transformation that can realize cost-effective exploitation.
In stimulation technology, hydraulic fracturing technology is one of the main measure for improving oil gas field production efficiency.It mentions within nearly 20 years
Out viscoelastic surfactant configuration clean fracturing fluid in hydraulic fracturing, play it is good take sand, seam, reduce storage
The effect of layer injury.
Viscoelastic surfactant (Viscoelastic Surfactant, abbreviation VES) fracturing fluid, is commonly referred to as in the industry
Clean fracturing fluid.Compared with the water-based fracturing liquid system with traditional polymer or guar gum for main thickening agent, VES fracturing fluid has
Plurality of advantages, such as: 1. extemporaneous preparation work is simple, and when preparation is not necessarily to crosslinking agent；2. low frictional resistance, viscoplasticity is good, has good
Solid-carrying performance；3. surfactant molecule amount is small, easily the row of returning, energy self-breaking glue is contacted with hydrocarbon fluid in stratum, without broken glue
Agent；4. do not form filter cake, it is small to formation damage, therefore oil gas field volume increase in many fields and link applied, have
There is superfine effect of increasing production.
However, the configuration of fracturing fluid needs to consume a large amount of freshwater resources, therefore, at sea job platform or hinterland
Implement hydraulic fracturing and just bring sizable freshwater resources problem, how directly to be configured using seawater or highly mineralized formation brines
High-performance fracturing fluid is by concern both domestic and external out.Existing viscoelastic surfactant includes single-stranded viscoelastic surfactant
With Gemini surface active agent surface-active.Wherein, single-stranded viscoelastic surfactant is usually present that temperature tolerance is poor, dosage is biggish
Problem；Gemini surface active agent temperature tolerance is strong, but since surface-active is stronger, is easy to reunite under the action of counter ion, from
And lead to easily occur phenomenon of phase separation compared with the Gemini surface active agent under high salinity, so that solution system is lost viscosity to nothing
The functions such as sand, seam are taken in method realization.
Therefore, in conjunction with marine and hinterland freshwater resources problem in short supply, a kind of salt-resistant type viscoelastic surface is developed
Activating agent directly configures VES clean fracturing fluid and has a very important significance to realization seawater or highly mineralized formation brines.
Summary of the invention
The object of the present invention is to provide a kind of salt-resistant type Shuangzi cationic viscoelastic surfactants and preparation method thereof with
And salt tolerance clean fracturing fluid, with solve existing viscoelastic surfactant clean fracturing fluid application present in intolerant to mineralising
The problem of spending.
The technical scheme to solve the above technical problems is that
A kind of salt-resistant type Shuangzi cationic viscoelastic surfactants, have the following structure formula:
Wherein, R is the saturated hydrocarbon chain or aliphatic unsaturated hydrocarbon of carbon atom number 17-21.
Further, in preferred embodiments of the present invention, R is the hydrophobic carbochain of erucic acid, the hydrophobic carbochain of oleic acid or hard
The hydrophobic carbochain of resin acid.
Wherein, the hydrophobic carbon-chain structure formula of erucic acid are as follows:
Wherein, the hydrophobic carbon-chain structure formula of oleic acid are as follows:
Wherein, stearic hydrophobic carbon-chain structure formula are as follows:
The molecular formula of above-mentioned salt-resistant type Shuangzi cationic viscoelastic surfactants is R2C17H36N4O4.The carbon atom number of R
It can be 17 or 21.
Salt-resistant type Shuangzi cationic viscoelastic surfactants of the invention, brown paste have special odor, close
Degree is in 0.86-0.92g/cm3Within the scope of.Since salt-resistant type Shuangzi cationic viscoelastic surfactants of the invention have
Stronger surface-active, and salt tolerance is preferable, can be used as self-diverting acid diversion agent, salt-resistant type emulsifier, foaming agent or is used for glue
Shu Zengqiang ultrafiltration waste water treatment process.
The preparation method of above-mentioned salt-resistant type Shuangzi cationic viscoelastic surfactants, by fatty acid amide propyl dimethylamine
It is dissolved in organic solvent with dibromoneopentyl glycol, salt-resistant type Shuangzi cationic viscoelastic surfactants are made in heating reaction.
Compared with other non-salt-resistant type Gemini surface active agents, dibromoneopentyl glycol provides for the type Shuangzi surfactant
A pair of adjacent hydroxyl, so that structure water-soluble enhancing on the original basis.Meanwhile adjacent double hydroxyl structures can be with calcium and magnesium
Equal polyvalent cations chelating, avoids metal cation from hindering the reunion of surfactant.
The reaction process of the above method is as follows:
Further, in preferred embodiments of the present invention, above-mentioned fatty acid amide propyl dimethylamine and dibromo new penta 2
The molar ratio of alcohol is (2-2.5): 1, heating temperature is 135-150 DEG C, reaction time 22-26h.Preferably, fatty acid amide
The molar ratio of diemethylamine and dibromoneopentyl glycol is (2.1-2.5): 1, heating temperature is 140-145 DEG C, and the reaction time is
22-24h。
Further, in preferred embodiments of the present invention, above-mentioned fatty acid amide propyl dimethylamine is erucyl amide third
One of base dimethylamine, oleamide diemethylamine and stearic amide diemethylamine or multiple combinations.
Further, in preferred embodiments of the present invention, above-mentioned organic solvent is that boiling point is organic molten higher than 130 DEG C
Agent.For example, n,N-Dimethylformamide or dimethyl sulfoxide.
Further, in preferred embodiments of the present invention, above-mentioned preparation method further include: before heating, catalysis is added
The molar ratio of agent, catalyst and fatty acid amide propyl dimethylamine is 1:(10-13), the catalyst is potassium iodide, potassium carbonate
With one of sodium carbonate or multiple combinations.Preferably, the molar ratio of catalyst and fatty acid amide propyl dimethylamine is 1:
(11-12)。
Further, in preferred embodiments of the present invention, above-mentioned preparation method further includes purification step:
Reaction product is evaporated under reduced pressure under conditions of 4-6 negative pressure, 70-85 DEG C, to remove reaction dissolvent, is obtained
Sticky paste crude product；Crude product is dissolved at 30-50 DEG C with ethyl acetate, removes unreacted dibromo new penta 2 by filtering
Pure and mild catalyst, obtains ethyl acetate solution；The ethyl acetate solution is recrystallized in 0-5 DEG C again, it is unreacted to remove
Fatty acid amide propyl dimethylamine, obtains crystallized product；The crystallized product is handled by rotary evaporation, to remove acetic acid second
Ester obtains pure salt-resistant type Shuangzi cationic viscoelastic surfactants.
A kind of salt tolerance clean fracturing fluid comprising above-mentioned salt-resistant type Shuangzi cationic viscoelastic surfactants 2-
5wt%, counter ion salt 2-15wt%, surplus is water.
Preferably, the weight ratio of salt-resistant type Shuangzi cationic viscoelastic surfactants is 2wt%, 3wt% or 5wt%.
Preferably, the weight ratio of counter ion salt is 8-15wt%.It is highly preferred that the weight ratio of counter ion salt be 2wt%,
3wt%, 8wt%, 10wt% or 15wt%.
Further, in preferred embodiments of the present invention, above-mentioned counter ion salt be potassium chloride, magnesium chloride, calcium chloride or
Sodium chloride.
The invention has the following advantages:
Salt-resistant type Shuangzi cationic viscoelastic surfactants of the invention can be in the seawater or water flooding of high salinity
Micella is formed, so that solution is embodied good viscoplasticity, the resistance to salinity of the viscoelastic surfactant is up to 150000mg/L
More than, it can be used for configuring seawater base clean fracturing fluid, while avoiding that broken glue occurs after encountering highly mineralized formation brines.Of the invention
Salt-resistant type Shuangzi cationic viscoelastic surfactants can be in the calcium and magnesium ion aqueous solution more than salinity 100000mg/L
It normally forms vermiculate glues and associates and form network-like structure, there is good viscoplasticity, still can be used for taking sand and make
Seam can be used to configure seawater base clean fracturing fluid, and the maximum salinity that can be born reaches 200000mg/L.And conventional viscoplasticity table
Phenomenon of phase separation will occur under the salinity of 15000mg/L for the clean fracturing fluid of face activating agent configuration, and system is caused to lose
Viscosity, so that proppant can not be carried.Therefore, the resistance to salinity ability of Shuangzi cationic viscoelastic surfactants of the invention
It is 10 times or more of conventional viscoelastic surfactant.
The high salinity clean fracturing fluid that Shuangzi cationic viscoelastic surfactants of the invention are prepared, it is resistance to
Temperature, resistant to shearing ability are strong, can be in 140 DEG C, 170s-1Under the conditions of shear 120min after, viscosity remains at 40mPas or more,
Rheological property is excellent, and does not need using addition auxiliary agent.Shuangzi cationic viscoelastic surfactants of the invention are with obtained
To high salinity clean fracturing fluid broken glue occurs after encountering hydro carbons, viscosity is 3.5mPa.s after breaking gel, is less than 5mPa.s.It is poly-
After vinyl alcohol capsule breaker addition system, it can make fracturing fluid under no hydrocarbon ring border, at 140 DEG C, 1 hour broken glue, after breaking gel
Viscosity 4.8mPa.s is less than 5mPa.s.
The preparation method of Shuangzi cationic viscoelastic surfactants of the invention is simple, and the yield of product is substantially improved,
Generally reach 96% or more, the by-product furthermore reacted is few, influences on the performance of product small.Shuangzi cation viscoelastic of the invention
Property surfactant when preparing clean fracturing fluid, dosage reduce, reduce costs, surfactant of the invention it is critical
Micellar concentration is 7~9 × 10-5Mol/L, far below viscoelastic surfactant more single-stranded than tradition.
Detailed description of the invention
Fig. 1 is the viscoelastic surfactant solution apparent viscosity of 3wt% embodiment 1 with the variation of calcium chloride concentration；
Fig. 2 is the viscoelastic surfactant solution apparent viscosity of 3wt% embodiment 1 with the variation of density of magnesium chloride；
Fig. 3 is the viscoelastic surfactant+150000mg/L calcium chloride solution rheological curve of 3wt% embodiment 1；
Fig. 4 is the viscoelastic surfactant+150000mg/L magnesium chloride solution rheological curve of 3wt% embodiment 1；
Fig. 5 is the seawater base of the viscoelastic surfactant of the embodiment containing 3wt% 1 of simulated seawater configuration in test example 2
The rheological curve of clean fracturing fluid；
Fig. 6 is the seawater base of the viscoelastic surfactant of the embodiment containing 3wt% 4 of simulated seawater configuration in test example 3
The rheological curve of clean fracturing fluid；
Fig. 7 is the nmr spectrum chart of the Shuangzi cation viscoelastic surfactant of oleic acid type of the invention.
Specific embodiment
The principle and features of the present invention will be described below with reference to the accompanying drawings, and the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the invention.The person that is not specified actual conditions in embodiment, according to normal conditions or the item suggested of manufacturer
Part carries out.Reagents or instruments used without specified manufacturer is the conventional products that can be obtained by commercially available purchase.
Embodiment 1
The salt-resistant type Shuangzi cationic viscoelastic surfactants of the present embodiment the preparation method is as follows:
Oleamide diemethylamine and dibromoneopentyl glycol are dissolved in N,N-dimethylformamide with the molar ratio of 2.1:1
(DMF) in, potassium iodide is added and does catalyst (molar ratio of potassium iodide and oleamide diemethylamine is 1:10), at 145 DEG C,
Magneton stirs 300r/min, and condenser pipe is added to be heated at reflux 24 hours；It is vacuumized with oil pump, under 5 negative pressure, 80 DEG C of vacuum distillations,
DMF solvent is removed, sticky paste crude product is obtained；It is new to filter the unreacted dibromo of removing for 40 DEG C of dissolution crude products of ethyl acetate
Pentanediol and potassium iodide catalyst；Ethyl acetate solution is recrystallized as 3 DEG C, removes unreacted oleic acid amido propyl dimethylamine,
After recrystallizing three times, rotary evaporation removes ethyl acetate and obtains more pure product.
Embodiment 2
The salt-resistant type Shuangzi cationic viscoelastic surfactants of the present embodiment the preparation method is as follows:
Erucyl amide diemethylamine and dibromoneopentyl glycol are dissolved in N,N-dimethylformamide with the molar ratio of 2.1:1
(DMF) in, potassium carbonate is added and does catalyst (molar ratio of potassium carbonate and erucyl amide diemethylamine is 1:13), at 135 DEG C,
Magneton stirs 300r/min, and condenser pipe is added to be heated at reflux 22 hours；It is vacuumized with oil pump, under 4 negative pressure, 70 DEG C of vacuum distillations,
DMF solvent is removed, sticky paste crude product is obtained；It is new to filter the unreacted dibromo of removing for 30 DEG C of dissolution crude products of ethyl acetate
Pentanediol and potassium iodide catalyst；Ethyl acetate solution is recrystallized as 0 DEG C, removes unreacted erucyl amide diemethylamine,
After recrystallizing three times, rotary evaporation removes ethyl acetate and obtains more pure product.
Embodiment 3
The salt-resistant type Shuangzi cationic viscoelastic surfactants of the present embodiment the preparation method is as follows:
Stearic amide diemethylamine and dibromoneopentyl glycol are dissolved in N, N- dimethyl formyl with the molar ratio of 2.5:1
In amine (DMF), sodium carbonate is added as catalyst (molar ratio of potassium carbonate and stearic amide diemethylamine is 1:11),
At 150 DEG C, magneton stirs 300r/min, and condenser pipe is added to be heated at reflux 26 hours；It is vacuumized with oil pump, under 6 negative pressure, 85 DEG C subtract
Pressure distillation, removes DMF solvent, obtains sticky paste crude product；It is unreacted to filter removing for 50 DEG C of dissolution crude products of ethyl acetate
Dibromoneopentyl glycol and potassium iodide catalyst；Ethyl acetate solution is recrystallized as 0~5 DEG C, removes unreacted stearic amide
Diemethylamine, after recrystallizing three times, rotary evaporation removes ethyl acetate and obtains more pure product.
Embodiment 4
The salt-resistant type Shuangzi cationic viscoelastic surfactants of the present embodiment the preparation method is as follows:
Erucyl amide diemethylamine and dibromoneopentyl glycol are dissolved in N,N-dimethylformamide with the molar ratio of 2:1
(DMF) in, potassium iodide is added as catalyst (molar ratio of potassium iodide and erucyl amide diemethylamine is 1:13), 145 DEG C
Under, magneton stirs 300r/min, and condenser pipe is added to be heated at reflux 24 hours；It is vacuumized with oil pump, under 5 negative pressure, 80 DEG C of decompressions are steamed
It evaporates, removes DMF solvent, obtain sticky paste crude product；40 DEG C of dissolution crude products of ethyl acetate filter and remove unreacted dibromo
Neopentyl glycol and potassium iodide catalyst；Ethyl acetate solution is recrystallized as 3 DEG C, removes unreacted erucyl amide dimethylamine
Amine, after recrystallizing three times, rotary evaporation removes ethyl acetate and obtains more pure product.
Test example 1
The clean fracturing fluid for the viscoelastic surfactant configuration that Example 1 synthesizes, surfactant concentration are
3wt%, apparent viscosity is as shown in Figure 1, Figure 2 with the trend that calcium chloride concentration and density of magnesium chloride change and change, test-strips
Part is 25 DEG C, 170s-1。
It can be seen that viscoelastic surfactant that the present embodiment synthesizes to the resistance to of calcium chloride and magnesium chloride from Fig. 1 and Fig. 2
All reached 200000mg/L or more by ability.3wt% surfactant+150000mg/L calcium chloride and 3wt% surface-active
The high salinity clean fracturing fluid of agent+150000mg/L magnesium chloride configuration is at 140 DEG C, 170s-1Under conditions of rheological curve such as
Fig. 3, Fig. 4.
Containing 3wt% surfactant+150000mg/L calcium chloride at 140 DEG C, 170s-1Under conditions of, apparent viscosity can
To maintain 30mPa.s or more, the requirement of professional standard SY/T6376-2008 is complied fully with.Equally, living containing the surface 3wt%
Property agent+150000mg/L magnesium chloride is at 140 DEG C, 170s-1Under conditions of, apparent viscosity still can maintain 30mPa.s or more,
Meet the requirement of professional standard SY/T6376-2008.
Test example 2
For taking the salt-resistant type Shuangzi cationic viscoelastic surfactants of the present embodiment 1:
Simulated seawater is formulated 24000mg/L sodium chloride+28000mg/L magnesium chloride+12000mg/L calcium chloride+700mg/L chlorine
Change potassium+900mg/L sodium sulphate, it is clear to make the seawater base that concentration containing viscoelastic surfactant is 3wt% using simulated seawater
Clean fracturing fluid, 140 DEG C, 170s-1Under conditions of rheological curve such as Fig. 5.
Pass through the seawater base clean fracturing fluid for the surfactant containing 3wt% that simulated seawater configures, at 140 DEG C, 170s-1
Shear at high temperature under the conditions of, after 140 minutes, apparent viscosity still is able to maintain 60mPa.s or more, meets professional standard SY/
The requirement of T6376-2008.
Test example 3
The seawater base for taking the surfactant of 3wt% in the present embodiment 4 to make using the simulated seawater in test example 2 is clear
Clean fracturing fluid, 140 DEG C, 170s-1Under conditions of rheological curve such as Fig. 6.
Same simulated seawater condition utilizes the surfactant of the longer hydrophobic chain of erucyl amide dimethyl tertiary amine synthesis
With better temperature tolerance and endurance of cutting, Fig. 6 illustrates the seawater-based fracturing fluid of the surfactant configuration of 3wt% 140
℃,170s-1Shear at high temperature under the conditions of, after 140 minutes, apparent viscosity still is able to maintain 100mPa.s or more.
In conclusion Shuangzi cationic viscoelastic surfactants of the invention have very strong resistance to salinity ability, it can
To be directly configured to clean fracturing fluid with highly mineralized formation brines, seawater, seawater base clean fracturing fluid has excellent heatproof resistance to
Cutting performance, hanging grittiness can be strong, and extemporaneous preparation is simple, breaks glue automatically, and formation damage is small, and at low cost, preparation process is simple, and
Temperature tolerance is strong, in 140 DEG C, 170s-1Viscosity is able to satisfy professional standard after lower 120 minutes, is higher than site operation to clean fracturing fluid
Viscosity requirement (25mPas).
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of salt-resistant type Shuangzi cationic viscoelastic surfactants, which is characterized in that have the following structure formula:
Wherein, R is the saturated hydrocarbon chain or aliphatic unsaturated hydrocarbon of carbon atom number 17-21.
2. salt-resistant type Shuangzi cationic viscoelastic surfactants according to claim 1, which is characterized in that R is erucic acid
Hydrophobic carbochain, the hydrophobic carbochain of oleic acid or stearic hydrophobic carbochain.
3. the preparation method of salt-resistant type Shuangzi cationic viscoelastic surfactants of any of claims 1 or 2, feature exist
In, fatty acid amide propyl dimethylamine and dibromoneopentyl glycol are dissolved in organic solvent, heats and reacts, obtained salt-resistant type pair
Sub- cationic viscoelastic surfactants.
4. salt-resistant type Shuangzi cationic viscoelastic surfactants according to claim 3, which is characterized in that the fat
The molar ratio (2-2.5) of sour amido propyl dimethylamine and dibromoneopentyl glycol: 1, heating temperature is 135-150 DEG C, the reaction time
For 22-26h.
5. salt-resistant type Shuangzi cationic viscoelastic surfactants according to claim 3, which is characterized in that the fat
Sour amido propyl dimethylamine is erucyl amide diemethylamine, oleamide diemethylamine and stearic amide diemethylamine
One of or multiple combinations.
6. salt-resistant type Shuangzi cationic viscoelastic surfactants according to claim 3, which is characterized in that described organic
Solvent is the organic solvent that boiling point is higher than 130 DEG C.
7. according to the described in any item salt-resistant type Shuangzi cationic viscoelastic surfactants of claim 3-6, which is characterized in that
The preparation method further include: before heating, catalyst, mole of the catalyst and fatty acid amide propyl dimethylamine is added
Than for 1:(10-13), the catalyst is one of potassium iodide, potassium carbonate and sodium carbonate or multiple combinations.
8. salt-resistant type Shuangzi cationic viscoelastic surfactants according to claim 7, which is characterized in that the preparation
Method further includes purification step:
Reaction product is evaporated under reduced pressure under conditions of 4-6 negative pressure, 70-85 DEG C, to remove reaction dissolvent, is obtained sticky
Paste crude product；Dissolve crude product at 30-50 DEG C with ethyl acetate, by filter remove unreacted dibromoneopentyl glycol and
Catalyst obtains ethyl acetate solution；The ethyl acetate solution is recrystallized in 0-5 DEG C again, to remove unreacted fat
Sour amido propyl dimethylamine, obtains crystallized product；The crystallized product is handled by rotary evaporation, to remove ethyl acetate, is obtained
To pure salt-resistant type Shuangzi cationic viscoelastic surfactants.
9. a kind of salt tolerance clean fracturing fluid, which is characterized in that it include salt-resistant type Shuangzi sun of any of claims 1 or 2 from
Sub- viscoelastic surfactant 2-5wt%, counter ion salt 2-15wt%, surplus is water.
10. salt tolerance clean fracturing fluid according to claim 9, which is characterized in that the counter ion salt is potassium chloride, chlorine
Change magnesium, calcium chloride or sodium chloride.
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| CN110483340A (en) * | 2019-09-12 | 2019-11-22 | 西南石油大学 | The preparation and the application in oilfield stimulation working solution of heat-resistant salt-resistant type viscoelastic surfactant |
| CN112552894A (en) * | 2019-12-31 | 2021-03-26 | 西南石油大学 | Ultra-high temperature resistant low-viscosity low-corrosion emulsifier and emulsified acid system containing same |
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| 于开华等: "新型酯基咪唑类表面活性剂的合成与性能 ", 《精细化工》 * |
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| CN110483340A (en) * | 2019-09-12 | 2019-11-22 | 西南石油大学 | The preparation and the application in oilfield stimulation working solution of heat-resistant salt-resistant type viscoelastic surfactant |
| CN112552894A (en) * | 2019-12-31 | 2021-03-26 | 西南石油大学 | Ultra-high temperature resistant low-viscosity low-corrosion emulsifier and emulsified acid system containing same |
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