CN104312572A - Coal bed gas clean-fracturing fluid - Google Patents

Coal bed gas clean-fracturing fluid Download PDF

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Publication number
CN104312572A
CN104312572A CN201410497570.6A CN201410497570A CN104312572A CN 104312572 A CN104312572 A CN 104312572A CN 201410497570 A CN201410497570 A CN 201410497570A CN 104312572 A CN104312572 A CN 104312572A
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fracturing fluid
coal
gas clean
general formula
clean fracturing
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杨志远
王晓华
杨伏生
任晓媛
曹水静
管保山
刘萍
龙江
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Xian University of Science and Technology
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Xian University of Science and Technology
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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
    • C09K8/60—Compositions for stimulating production by acting on the underground formation
    • C09K8/62—Compositions for forming crevices or fractures
    • C09K8/66—Compositions based on water or polar solvents
    • C09K8/68—Compositions based on water or polar solvents containing organic compounds
    • 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
    • C09K8/60—Compositions for stimulating production by acting on the underground formation
    • C09K8/602—Compositions for stimulating production by acting on the underground formation containing surfactants
    • 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
    • C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/26—Gel breakers other than bacteria or enzymes

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  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)

Abstract

The invention discloses a coal bed gas clean-fracturing fluid. The coal bed gas clean-fracturing fluid is prepared from 0.3-3% by mass of a gemini surfactant shown in the general formula III, 1-6% by mass of an counter ion auxiliary agent and the balance water by mixing. The counter ion auxiliary agent is sodium salicylate, potassium chloride, potassium bromide or sodium bromide. The coal bed gas clean fracturing fluid has the characteristics of high efficiency, low damage and low cost, realizes residue-free coal bed gas yield increasing, has temperature resistance and shearing resistance better than those of the traditional clean fracturing fluid, has excellent breaking property, can realize complete breaking after use of a breaking agent for two hours and does not produce residue in the broken liquid. The coal bed gas clean fracturing fluid can be prepared by simple processes, has a low cost, has tiny influence on coal surface interface properties, stratum and coal seam, has excellent fracturing performances and can be widely used.

Description

A kind of coal-seam gas clean fracturing fluid
Technical field
The invention belongs to CBM Fracturing technical field, be specifically related to a kind of coal-seam gas clean fracturing fluid.
Background technology
Coal-seam gas is a kind of very important Unconventional forage, and its methane content is generally greater than 95%, is one of high-quality clean Gas Energy Source, but the Young's modulus in coal seam and gas reservoir pressure less, and compression factor is higher, and air water is also deposited, its natural fracture is grown, and gas-bearing formation is also easily impaired.Fracturing technique makes coal-bed-gas production-increase very important means, and wherein fracturing liquid plays transmission of pressure and carries propping agent effect, is integral part important in pressing crack construction.Fracturing liquid obtains the successful important factor of pressure break as coal bed gas well, and finite concentration proppant transport can enter in crack, coal seam by requirement on the one hand, guarantees that coal petrography reservoir there will not be physics or chemistry injury on the other hand.Coal bed gas well fracturing liquid comprises active water type, linear glue-type, foam type and clean four kinds.
Clean fracturing fluid is most widely used a kind of fracturing liquid in current fracturing technique, and its host is generally quaternary ammonium salt surface active agent.It is little that clean fracturing fluid has residue, injures the advantages such as low, have application prospect well in CBM Fracturing liquid to bottom.The use of current coal seam construction clean fracturing fluid, still in experimental stage, causes restriction because its cost is higher to its widespread use.Therefore, current primary task develops high-effect, Low Damage, low cost clean fracturing fluid, provide a kind of can the novel coal-seam gas clean fracturing fluid of widespread use.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of coal-seam gas clean fracturing fluid.This coal-seam gas clean fracturing fluid has high-effect, the feature such as Low Damage and low cost, can realize without residue volume increase coal-seam gas, the impact of coal-seam gas clean fracturing fluid on the surface and interface character of coal, stratum and coal seam is small, and fracturing fluid property is excellent, can extensively come into operation.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of coal-seam gas clean fracturing fluid, is characterized in that, is become: the double type tensio-active agent 0.3% ~ 3% with general formula III by the mixed raw material of following mass percentage, gegenion auxiliary agent 1% ~ 6%, surplus is water; Described gegenion auxiliary agent is sodium salicylate, Repone K, Potassium Bromide or Sodium Bromide;
The described double type tensio-active agent with general formula III is made up with the p-Xylol substituent reaction with general formula II of the tertiary amine with formula I, and reaction equation is:
In formula, R is C 12h 25, C 14h 29or C 16h 33; X is Cl or Br.
Above-mentioned a kind of coal-seam gas clean fracturing fluid, is characterized in that, become by the mixed raw material of following mass percentage: the double type tensio-active agent 0.5% ~ 2% with general formula III, gegenion auxiliary agent 2% ~ 5%, surplus is water.
Above-mentioned a kind of coal-seam gas clean fracturing fluid, is characterized in that, become by the mixed raw material of following mass percentage: the double type tensio-active agent 0.5% with general formula III, gegenion auxiliary agent 3%, surplus is water.
Above-mentioned a kind of coal-seam gas clean fracturing fluid, is characterized in that, described in there is the double type tensio-active agent of general formula III preparation method comprise the following steps:
Step one, back flow reaction: the tertiary amine with formula I is added in ethanol with the p-Xylol substituent with general formula II, is back flow reaction 24h ~ 72h under the condition of 75 DEG C ~ 95 DEG C in temperature, then distills, obtain crude product;
Step 2, recrystallization: crude product described in step one is dissolved in ethanol, then in the solution after dissolving, drip ethyl acetate, until solution is muddy, have crystal to separate out after left at room temperature 10h ~ 14h, suction filtration obtains crystallographic;
Step 3, according to the method for step 2,1 ~ 2 recrystallization is carried out to crystallographic described in step 2, obtain solia particle, vacuum-drying is carried out to described solia particle, obtain the double type tensio-active agent with general formula III.
Above-mentioned a kind of coal-seam gas clean fracturing fluid, is characterized in that, the tertiary amine described in step one with formula I is (2 ~ 2.5) with the mol ratio of the p-Xylol substituent with general formula II: 1.
Above-mentioned a kind of coal-seam gas clean fracturing fluid, is characterized in that, the volume of ethanol described in step one is (100 ~ 300) mL:1mol with the ratio of molar weight of the tertiary amine with formula I.
Above-mentioned a kind of coal-seam gas clean fracturing fluid, is characterized in that, the temperature of back flow reaction described in step one is 85 DEG C, and the time of back flow reaction is 48h.
Above-mentioned a kind of coal-seam gas clean fracturing fluid, is characterized in that, vacuum drying temperature described in step 3 is 50 DEG C ~ 70 DEG C, and the vacuum drying time is 12h ~ 24h.
The preparation method of coal-seam gas clean fracturing fluid of the present invention is: by having the mixing of the double type tensio-active agent of general formula III, gegenion auxiliary agent and water, stir.
The present invention compared with prior art has the following advantages:
1, coal-seam gas clean fracturing fluid of the present invention has the features such as high-effect, Low Damage and low cost, can realize without residue volume increase coal-seam gas.
2, the present invention adopts the double type tensio-active agent of tertiary amine and p-Xylol substituent reaction preparation, this tensio-active agent is the tensio-active agent of a kind of hydrophobic group together with positively charged hydrophilic group covalent bonds, surfactivity is higher and Kraft point is very low, water-soluble also fine, its thickening property is not a halfpenny the worse compared with polymeric surface active agent; The chemical bond connected achieves the compact siro spinning technology of the monomer ion of two or more tensio-active agent, and strengthen hydrophobic binding power between hydrocarbon chain, the repulsive force between ion head base also declines to some extent, improves the effect of tensio-active agent.
3, the heatproof endurance of cutting of coal-seam gas clean fracturing fluid of the present invention is better than traditional clean fracturing fluid, and broken colloidality is good, adds gel breaker and substantially just can break glue completely, without residue in breaking glue solution afterwards in two hours.
4, coal-seam gas clean fracturing liquid and preparation method thereof of the present invention is simple, cost is low, and the impact of coal-seam gas clean fracturing fluid on the surface and interface character of coal, stratum and coal seam is small, and fracturing fluid property is excellent, can extensively come into operation.
Below in conjunction with drawings and Examples, technical scheme of the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the heat stability testing curve of the coal-seam gas clean fracturing fluid of the embodiment of the present invention 1.
Fig. 2 is the flow curve of coal-seam gas clean fracturing fluid at 40 DEG C of the embodiment of the present invention 1.
Fig. 3 is the heat stability testing curve of traditional clean fracturing fluid of comparative example 1.
Fig. 4 is the flow curve of traditional gas clean fracturing fluid at 40 DEG C of comparative example 1.
Fig. 5 is the infrared spectrogram of double type tensio-active agent prepared by the embodiment of the present invention 1.
Embodiment
Embodiment 1
The coal-seam gas clean fracturing fluid of the present embodiment, become by the mixed raw material of following mass percentage: the double type tensio-active agent 0.5% with general formula III, gegenion auxiliary agent 3%, surplus is water; Described gegenion auxiliary agent is sodium salicylate;
The described double type tensio-active agent with general formula III is made up with the p-Xylol substituent reaction with general formula II of the tertiary amine with formula I, and reaction equation is:
In formula, R is C 12h 25; X is Cl;
The described preparation method with the double type tensio-active agent of general formula III comprises the following steps:
Step one, back flow reaction: 0.2mol is had the p-Xylol substituent that the tertiary amine of formula I and 0.1mol have a general formula II and add in 20mL ethanol (chemical pure or analytical pure), be back flow reaction 48h under the condition of 85 DEG C in temperature, then distill, obtain crude product;
Step 2, recrystallization: crude product described in step one is dissolved in ethanol (chemical pure or analytical pure), then in the solution after dissolving, ethyl acetate is dripped, until solution is muddy, have crystal to separate out after left at room temperature 12h, suction filtration obtains crystallographic;
Step 3, according to the method for step 2,2 recrystallizations are carried out to crystallographic described in step 2, obtain solia particle, vacuum-drying is carried out to described solia particle, obtain the double type tensio-active agent with general formula III; Described vacuum drying temperature is 60 DEG C, and the vacuum drying time is 18h.
The preparation method of the coal-seam gas clean fracturing fluid of the present embodiment is: by having the mixing of the double type tensio-active agent of general formula III, gegenion auxiliary agent and water, stir.
Carry out magnetic resonance detection to double type tensio-active agent prepared by the present embodiment, total number of hydrogen atom is 70, and fit like a glove with the number of hydrogen atom in target product, magnetic resonance detection the results are shown in Table 1.The infrared spectra map analysis of composition graphs 5 draws the product target product just of synthesis.Employing tetrabromophenol sulfonphthalein detects, and result shows, and double type tensio-active agent prepared by the present embodiment is double-type cationic surfactant.
Table 1 nuclear magnetic resonance spectroscopy table
Comparative example 1
Tradition clean fracturing fluid, become by the mixed raw material of following mass percentage: Cetyltrimethylammonium bromide 0.5%, sodium salicylate 4%, surplus is water.
Fig. 1 is the heat stability testing curve of the coal-seam gas clean fracturing fluid of embodiment 1, Fig. 2 is the flow curve of coal-seam gas clean fracturing fluid at 40 DEG C of embodiment 1, Fig. 3 is the heat stability testing curve of traditional clean fracturing fluid of comparative example 1, and Fig. 4 is the flow curve of traditional clean fracturing fluid at 40 DEG C of comparative example 1.Comparison diagram 1 and Fig. 3, when temperature rises to 40 DEG C, the viscosity of the coal-seam gas clean fracturing fluid of embodiment 1 is about 20mPas, apparently higher than traditional clean fracturing fluid of comparative example 1, illustrates that the temperature and shearing sustainability of the coal-seam gas clean fracturing fluid of embodiment 1 at 40 DEG C is better than traditional clean fracturing fluid.Comparison diagram 2 and Fig. 4 can find out, the coal-seam gas clean fracturing fluid of embodiment 1 belongs to pseudoplastic fluid, traditional clean fracturing fluid of comparative example 1 belongs to dilatant fluid, tradition clean fracturing fluid viscosity at 40 DEG C is less, become shear-stress change when shearing not obvious, show that viscosity versus shear rate change is insensitive, calculate rheological property inaccurate, and the coal-seam gas clean fracturing fluid of embodiment 1 viscosity at 40 DEG C is high, rheological property is good.
Adopt polyoxyethylene nonylphenol ether TX-10 and diesel oil to carry out brokenly glue test as gel breaker to the coal-seam gas clean fracturing fluid of embodiment 1 and traditional clean fracturing fluid of comparative example 1 respectively, the quality of gel breaker is 0.1% of fracturing liquid quality, the results are shown in Table 2.
Table 2 fracturing liquid rubber-breaking test-results
As can be seen from Table 2, after adding gel breaker, the coal-seam gas clean fracturing fluid viscosity of embodiment 1 there will be reduction sharply, along with the increase viscosity of time remains unchanged substantially after 2h, illustrates that fracturing liquid rubber-breakingization is comparatively thorough.And use bavin oil viscosity under using the fracturing liquid viscosity of TX-10 to be significantly less than identical conditions, TX-10 gel breaker as coal-seam gas clean fracturing fluid more preferably than diesel oil is described.
Embodiment 2
The coal-seam gas clean fracturing fluid of the present embodiment, become by the mixed raw material of following mass percentage: the double type tensio-active agent 0.5% with general formula III, gegenion auxiliary agent 2%, surplus is water; Described gegenion auxiliary agent is Sodium Bromide;
The described double type tensio-active agent with general formula III is made up with the p-Xylol substituent reaction with general formula II of the tertiary amine with formula I, and reaction equation is:
In formula, R is C 12h 25; X is Br;
The described preparation method with the double type tensio-active agent of general formula III comprises the following steps:
Step one, back flow reaction: 0.22mol is had the p-Xylol substituent that the tertiary amine of formula I and 0.1mol have a general formula II and add in 35mL ethanol (chemical pure or analytical pure), be back flow reaction 48h under the condition of 85 DEG C in temperature, then distill, obtain crude product;
Step 2, recrystallization: crude product described in step one is dissolved in ethanol (chemical pure or analytical pure), then in the solution after dissolving, ethyl acetate is dripped, until solution is muddy, have crystal to separate out after left at room temperature 12h, suction filtration obtains crystallographic;
Step 3, according to the method for step 2,2 recrystallizations are carried out to crystallographic described in step 2, obtain solia particle, vacuum-drying is carried out to described solia particle, obtain the double type tensio-active agent with general formula III; Described vacuum drying temperature is 60 DEG C, and the vacuum drying time is 12h.
The preparation method of the coal-seam gas clean fracturing fluid of the present embodiment is identical with embodiment 1.
Carry out magnetic resonance detection to double type tensio-active agent prepared by the present embodiment, total number of hydrogen atom is 70, fits like a glove with the number of hydrogen atom in target product, draws the product target product just of synthesis in conjunction with Infrared spectroscopy.Employing tetrabromophenol sulfonphthalein detects, and result shows, and double type tensio-active agent prepared by the present embodiment is double-type cationic surfactant.
Embodiment 3
The coal-seam gas clean fracturing fluid of the present embodiment, become by the mixed raw material of following mass percentage: the double type tensio-active agent 3% with general formula III, gegenion auxiliary agent 6%, surplus is water; Described gegenion auxiliary agent is Potassium Bromide;
The described double type tensio-active agent with general formula III is made up with the p-Xylol substituent reaction with general formula II of the tertiary amine with formula I, and reaction equation is:
In formula, R is C 14h 29; X is Cl;
The described preparation method with the double type tensio-active agent of general formula III comprises the following steps:
Step one, back flow reaction: 0.24mol is had the p-Xylol substituent that the tertiary amine of formula I and 0.1mol have a general formula II and add in 50mL ethanol (chemical pure or analytical pure), be back flow reaction 24h under the condition of 95 DEG C in temperature, then distill, obtain crude product;
Step 2, recrystallization: crude product described in step one is dissolved in ethanol (chemical pure or analytical pure), then in the solution after dissolving, ethyl acetate is dripped, until solution is muddy, have crystal to separate out after left at room temperature 14h, suction filtration obtains crystallographic;
Step 3, according to the method for step 2,1 recrystallization is carried out to crystallographic described in step 2, obtain solia particle, vacuum-drying is carried out to described solia particle, obtain the double type tensio-active agent with general formula III; Described vacuum drying temperature is 70 DEG C, and the vacuum drying time is 12h.
The preparation method of the coal-seam gas clean fracturing fluid of the present embodiment is identical with embodiment 1.
Carry out magnetic resonance detection to double type tensio-active agent prepared by the present embodiment, total number of hydrogen atom is 78, fits like a glove with the number of hydrogen atom in target product, draws the product target product just of synthesis in conjunction with Infrared spectroscopy.Employing tetrabromophenol sulfonphthalein detects, and result shows, and double type tensio-active agent prepared by the present embodiment is double-type cationic surfactant.
Embodiment 4
The coal-seam gas clean fracturing fluid of the present embodiment, become by the mixed raw material of following mass percentage: the double type tensio-active agent 0.3% with general formula III, gegenion auxiliary agent 1%, surplus is water; Described gegenion auxiliary agent is sodium salicylate;
The described double type tensio-active agent with general formula III is made up with the p-Xylol substituent reaction with general formula II of the tertiary amine with formula I, and reaction equation is:
In formula, R is C 16h 33; X is Cl;
The described preparation method with the double type tensio-active agent of general formula III comprises the following steps:
Step one, back flow reaction: 0.25mol is had the p-Xylol substituent that the tertiary amine of formula I and 0.1mol have a general formula II and add in 75mL ethanol (chemical pure or analytical pure), be back flow reaction 72h under the condition of 75 DEG C in temperature, then distill, obtain crude product;
Step 2, recrystallization: crude product described in step one is dissolved in ethanol (chemical pure or analytical pure), then in the solution after dissolving, ethyl acetate is dripped, until solution is muddy, have crystal to separate out after left at room temperature 10h, suction filtration obtains crystallographic;
Step 3, according to the method for step 2,2 recrystallizations are carried out to crystallographic described in step 2, obtain solia particle, vacuum-drying is carried out to described solia particle, obtain the double type tensio-active agent with general formula III; Described vacuum drying temperature is 50 DEG C, and the vacuum drying time is 24h.
The preparation method of the coal-seam gas clean fracturing fluid of the present embodiment is identical with embodiment 1.
Carry out magnetic resonance detection to double type tensio-active agent prepared by the present embodiment, total number of hydrogen atom is 86, fits like a glove with the number of hydrogen atom in target product, draws the product target product just of synthesis in conjunction with Infrared spectroscopy.Employing tetrabromophenol sulfonphthalein detects, and result shows, and double type tensio-active agent prepared by the present embodiment is double-type cationic surfactant.
Embodiment 5
The coal-seam gas clean fracturing fluid of the present embodiment, become by the mixed raw material of following mass percentage: the double type tensio-active agent 2% with general formula III, gegenion auxiliary agent 5%, surplus is water; Described gegenion auxiliary agent is Repone K;
The described double type tensio-active agent with general formula III is made up with the p-Xylol substituent reaction with general formula II of the tertiary amine with formula I, and reaction equation is:
In formula, R is C 14h 29; X is Cl;
The described preparation method with the double type tensio-active agent of general formula III comprises the following steps:
Step one, back flow reaction: 0.2mol is had the p-Xylol substituent that the tertiary amine of formula I and 0.1mol have a general formula II and add in 25mL ethanol (chemical pure or analytical pure), be back flow reaction 36h under the condition of 90 DEG C in temperature, then distill, obtain crude product;
Step 2, recrystallization: crude product described in step one is dissolved in ethanol (chemical pure or analytical pure), then in the solution after dissolving, ethyl acetate is dripped, until solution is muddy, have crystal to separate out after left at room temperature 12h, suction filtration obtains crystallographic;
Step 3, according to the method for step 2,2 recrystallizations are carried out to crystallographic described in step 2, obtain solia particle, vacuum-drying is carried out to described solia particle, obtain the double type tensio-active agent with general formula III; Described vacuum drying temperature is 65 DEG C, and the vacuum drying time is 20h.
The preparation method of the coal-seam gas clean fracturing fluid of the present embodiment is identical with embodiment 1.
Carry out magnetic resonance detection to double type tensio-active agent prepared by the present embodiment, total number of hydrogen atom is 78, fits like a glove with the number of hydrogen atom in target product, draws the product target product just of synthesis in conjunction with Infrared spectroscopy.Employing tetrabromophenol sulfonphthalein detects, and result shows, and double type tensio-active agent prepared by the present embodiment is double-type cationic surfactant.
In the coal-seam gas clean fracturing fluid and distilled water of the embodiment of the present invention 1 to embodiment 5, all add the polyoxyethylene nonylphenol ether TX-10 of 0.1% and fully mix, obtain mixing solutions, adopt mixing solutions to measure the contact angle of Jincheng Coal, Hancheng coal coal dust different from Baode coal, structure is in table 3.
The contact angle of table 3 coal dust
As can be seen from Table 3, coal-seam gas clean fracturing fluid of the present invention significantly can reduce the contact angle of coal dust, strengthens the wettability of coal dust.
The coal-seam gas clean fracturing fluid of the embodiment of the present invention 1 to embodiment 5 is adopted to soak Coal rank respectively, soak the polyoxyethylene nonylphenol ether TX-10 fully mixing that add 0.1% of fracturing liquid quality in forward direction fracturing liquid, measure the pore structure of coal after soaking, the results are shown in Table 4.
Table 4 soaks the pore structure of rear coal
As can be seen from Table 4, after adopting coal-seam gas clean fracturing fluid of the present invention to soak, the specific surface area of three kinds of coals reduces all to some extent, but total pore volume, micropore hold and the change of mean pore size is all little.Visible, coal seam of the present invention clean fracturing fluid add the void distribution not do not destroyed in coal, thus for the injury that texture of coal seam is too not large.
Adopt the coal-seam gas clean fracturing fluid of the embodiment of the present invention 1 and embodiment 2, carried out the test in place of 6 mouthfuls of wells at the coal-seam gas such as Hancheng, Ningwu Basin block, be constructed into power 100%.
Table 5 clean fracturing fluid effect is added up
Test-results shows, coal-seam gas clean fracturing fluid of the present invention has following characteristics: (1) leak-off is low, makes seam efficiency high: pressure drop section matching leakoff coefficent 4.2m/min 1/2~ 8.0 × 10 -4m/min 1/2, be 20% of clear water; (2) frictional resistance is low: construction friction 4.32MPa, is 30% of clear water; (3) prop-carrying capacity is high: most high sand ratio 43%, average sand is than 29.5%, and every meter adds sand amount is 10m 3~ 12m 3; (4) breaking glue solution viscosity 3mPas ~ 5mPas, the row's of returning efficiency is high, stablizes aerogenesis apparently higher than block mean level (ML).
The above; it is only preferred embodiment of the present invention; not any restriction is done to the present invention, every above embodiment is done according to invention technical spirit any simple modification, change and equivalent structure change, all still belong in the protection domain of technical solution of the present invention.

Claims (8)

1. a coal-seam gas clean fracturing fluid, is characterized in that, become by the mixed raw material of following mass percentage: the double type tensio-active agent 0.3% ~ 3% with general formula III, gegenion auxiliary agent 1% ~ 6%, surplus is water; Described gegenion auxiliary agent is sodium salicylate, Repone K, Potassium Bromide or Sodium Bromide;
The described double type tensio-active agent with general formula III is made up with the p-Xylol substituent reaction with general formula II of the tertiary amine with formula I, and reaction equation is:
In formula, R is C 12h 25, C 14h 29or C 16h 33; X is Cl or Br.
2. a kind of coal-seam gas clean fracturing fluid according to claim 1, is characterized in that, become by the mixed raw material of following mass percentage: the double type tensio-active agent 0.5% ~ 2% with general formula III, gegenion auxiliary agent 2% ~ 5%, surplus is water.
3. a kind of coal-seam gas clean fracturing fluid according to claim 2, is characterized in that, become by the mixed raw material of following mass percentage: the double type tensio-active agent 0.5% with general formula III, gegenion auxiliary agent 3%, surplus is water.
4. a kind of coal-seam gas clean fracturing fluid according to claim 1,2 or 3, is characterized in that, described in there is the double type tensio-active agent of general formula III preparation method comprise the following steps:
Step one, back flow reaction: the tertiary amine with formula I is added in ethanol with the p-Xylol substituent with general formula II, is back flow reaction 24h ~ 72h under the condition of 75 DEG C ~ 95 DEG C in temperature, then distills, obtain crude product;
Step 2, recrystallization: crude product described in step one is dissolved in ethanol, then in the solution after dissolving, drip ethyl acetate, until solution is muddy, have crystal to separate out after left at room temperature 10h ~ 14h, suction filtration obtains crystallographic;
Step 3, according to the method for step 2,1 ~ 2 recrystallization is carried out to crystallographic described in step 2, obtain solia particle, vacuum-drying is carried out to described solia particle, obtain the double type tensio-active agent with general formula III.
5. a kind of coal-seam gas clean fracturing fluid according to claim 4, is characterized in that, the tertiary amine described in step one with formula I is (2 ~ 2.5) with the mol ratio of the p-Xylol substituent with general formula II: 1.
6. a kind of coal-seam gas clean fracturing fluid according to claim 4, is characterized in that, the volume of ethanol described in step one is (100 ~ 300) mL:1mol with the ratio of molar weight of the tertiary amine with formula I.
7. a kind of coal-seam gas clean fracturing fluid according to claim 4, is characterized in that, the temperature of back flow reaction described in step one is 85 DEG C, and the time of back flow reaction is 48h.
8. a kind of coal-seam gas clean fracturing fluid according to claim 4, is characterized in that, vacuum drying temperature described in step 3 is 50 DEG C ~ 70 DEG C, and the vacuum drying time is 12h ~ 24h.
CN201410497570.6A 2014-09-25 2014-09-25 Coal bed gas clean-fracturing fluid Pending CN104312572A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106000217A (en) * 2016-05-24 2016-10-12 江南大学 Viscoelastic system formed by functional Gemini surface active agent

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