CN106634934A - Environment-friendly alcohol group fracturing fluid and preparation method thereof - Google Patents
Environment-friendly alcohol group fracturing fluid and preparation method thereof Download PDFInfo
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- CN106634934A CN106634934A CN201611049436.5A CN201611049436A CN106634934A CN 106634934 A CN106634934 A CN 106634934A CN 201611049436 A CN201611049436 A CN 201611049436A CN 106634934 A CN106634934 A CN 106634934A
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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
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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
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
Abstract
The invention relates to the technical field of oilfield chemistry, and particularly relates to an environment-friendly alcohol group fracturing fluid and a preparation method thereof. Water-soluble organic acid is adopted to generate a condensation reaction with organic amine containing alkenyl to prepare the environment-friendly alcohol group fracturing fluid, so that the fracturing fluid is relatively excellent in water solubility, high in viscosity and easy to degrade, does not generate exhaust gas and reduces the disposal difficulty in water returning and draining, and the material cost is low; by carrying out performance detection on products, the kinematic viscosity of the fracturing fluid is 42-45mm<2>/s at 50 DEG C, and the content by mass percent of water is 13.8-19.8%; and the concentration by mass percent is 1%, and the surface tension of an aqueous solution of the fracturing fluid is less than or equal to 20-28mN/m.
Description
Technical field
The present invention relates to technical field of oilfield chemistry, especially a kind of environment-friendly type alcohol-base fracturing fluid and preparation method thereof.
Background technology
Recently, National Energy Board issues《Shale gas development plan 2016～2020》, it is desirable to produce to the year two thousand twenty shale gas
Amount reaches 300 billion cubic meters.In order that some unconventional petroleum resourceses are escaped from organic mud shale or oil-gas reservoir stratum
Effusion comes, and needs to these local performances well, and the fracturing fluid little to environmental injury.
Prior art, fracturing fluid is mainly natural polymer and the big class of chemical synthesis compound two；Natural polymer
Sub- compound mainly with guar gum and with guar gum through chemical graft macromolecular compound, such as Patent No.
201110282631.3 200 DEG C of fracturing fluids of heatproof employ homemade modifyed guar gum as thickening agent, and the thickening agent has good
Good temperature tolerance.For another example number of patent application is 201410731391.4 shale gas novel environment friendly fracturing fluid, and it adopts guar gum, hands over
Connection agent, gel breaker, friction reducer etc. so that fracturing fluid has the good feature of environmental protection, heat resisting and pressure resisting, endurance of cutting, break glue control
It is good, injury of the fracturing fluid to unconventionaloil pool layer and crack is effectively reduced, improve the effect of fracturing reform.But, its preparation
It is relatively costly, especially expensive raw material price.Chemical synthesis compound mainly uses acrylamide (AM) monomer, and Jing causes
The molecular weight that polymerization is obtained, from millions of to several ten million polyacrylamides (PAM), synthetic price is relatively above-mentioned using natural
Macromolecular compound is cheap, such as aqueous fracturing fluid of Patent No. 201210566415.6 and preparation method thereof, its thickening agent by
Cellulose derivative and partially hydrolyzed polyacrylamide (PHPA) composition etc., but, PAM be difficult to it is degradable within a period, even if
Monomer AM is degraded into, is also noxious material, cause the unfriendly of environment；Cause to return blowdown Water warfare difficulty larger.
The content of the invention
In order to solve above-mentioned technical problem present in prior art, the present invention provide a kind of environment-friendly type alcohol-base fracturing fluid and
Its preparation method.
For alcohol radical, mainly C1～C18 alcohol and their esterification, hydroformylation and acetalation etc. are reacted into the various of generation
Product is defined with alcohol radical.Alcohol radical in the invention is defined also as this.
It is achieved particular by technical scheme below：
There is condensation reaction using water-soluble organic acid and the organic amine containing thiazolinyl and prepare fracturing fluid, the fracturing fluid can be molten
Yu Shui, and its viscosity is higher, after mixing with the powder such as clay, manganese ore, titanium ore, can form stable emulsion, Neng Gouying
For in shale gas field, coal bed gas field, oil gas field.
By there is condensation reaction with the organic amine containing thiazolinyl using water-soluble organic acid, it can occur at normal temperatures instead
Should prepare, and noxious material will not be generated, improve the environmental-protecting performance of fracturing fluid.
It is preferred that, the water-soluble organic acid of employing, based on acetic acid, especially with by methyl alcohol as raw material obtained in acetic acid or
Pyroligneous acid obtained in biomass carbonization, is aided with butanedioic acid, malic acid, formic acid, wherein based on the acid added for food especially.
It is preferred that, the organic amine containing thiazolinyl for adopting for diethylenetriamine and/or polyethylene polyamine, in diethylenetriamine and many
Mixing ratio when ethylene polyamine mixes is by quality ratio 4.5-7.5:4, preferably 6:4.
By the selection to water-soluble organic acid, the organic amine containing thiazolinyl so that product prepared by condensation reaction occurs, drop
Xie Hou, can be miscible with water, and does not have toxicity, reduces and returns blowdown Water warfare difficulty.
The fracturing fluid of the invention, it is preferable that material composition in parts by weight for acetic acid 700-810 parts, formic acid 0-20 parts,
Butanedioic acid 0-50 parts, malic acid 0-20 parts, the organic amine 100-200 parts containing thiazolinyl.By acetic acid and the organic amine phase containing thiazolinyl
Interaction so that the viscosity of the fracturing fluid of acquisition is higher, and water soluble characteristic is more excellent, effectively can form with the water in formation rock
Discharge opeing is returned, and this returns discharge opeing and easily purifies, and reduces to shale gas exploitation cost, it is to avoid environment is caused to shale gas exploitation
Pollution.
Above-mentioned fracturing fluid, its material composition, it is preferable that be in parts by weight 780 parts of acetic acid, 15 parts of formic acid, 25 parts of butanedioic acid,
15 parts of malic acid, 160 parts of the organic amine containing thiazolinyl.
It is preferred that, described acetic acid, its purity is calculated as 95-99.5% with weight/mass percentage composition；Butanedioic acid, its purity is with quality
Percentage composition is calculated as more than 99%；Formic acid, its purity is calculated as more than 95% with weight/mass percentage composition.
It is preferred that, described diethylenetriamine, its purity is calculated as ＞ 96% with weight/mass percentage composition；Polyethylene polyamine, its is pure
Degree is calculated as 95% with weight/mass percentage composition.
Preparation method is to take raw material according to proportioning, and water-soluble organic acid is pumped into into warding off with reflux condenser and mixer
In glass reactor, the organic amine containing thiazolinyl is fitted in the measuring tank at the top of glass lined reaction vessel, opens mixer, instillation contains
The organic amine of thiazolinyl, and drip off in 1-2h, after dripping off, it is stirred for 0.3-0.7h；And contain thiazolinyl in above-mentioned whole dropwise addition
During organic amine, temperature≤90 DEG C in reactor, temperature≤40 DEG C in reflux condenser, and question response product are controlled
After naturally cooling to 40 DEG C, put into finished pot through filter, obtain environment-friendly type alcohol-base fracturing fluid.
The pressure break liquid preparing process flow process of the invention is simple, produces without waste gas, and after for reservoir treating,
What it was formed returns discharge opeing nontoxicity, and the organic matter for remaining easily is degraded, and is dissolved in water, and its COD easily reaches dirt
Water discharge standard.The abundant raw material source of selection, low raw-material cost.
In the invention it is water miscible acid choose when, its individually using formic acid come with contain thiazolinyl organic amine
Effect, obtains fracturing fluid and also has higher water solubility, and still relatively low to returning the intractability of discharge opeing, and cost also compared with
It is low, it is seen then that for the selection of water-soluble organic acid, can using any water soluble acid, but using based on acetic acid, other
Supplemented by water-soluble organic acid, and act on diethylenetriamine and the mixed mixed organic acid of polyethylene polyamine, can be effective
Improve viscosity, it is to avoid in preparation process, using crosslinking agent, effectively reduce the preparation cost of fracturing fluid, improve pressure break
The quality of liquid.
Specific embodiment
Technical scheme is further limited with reference to specific embodiment, but claimed
Scope is not only limited to description.
Specifically there is condensation reaction using water-soluble organic acid and the organic amine containing thiazolinyl and prepare in the invention so that
The water solubility of fracturing fluid is more excellent, and viscosity is high, and is easy to degraded, produces without waste gas, reduces and returns drainage sunk well difficulty, raw material into
This is low, and by carrying out performance detection to product, its 50 DEG C of kinematic viscosity are 42-45 ㎜2╱ s, the weight/mass percentage composition of moisture content is
13.8-19.8%；It is≤20-28mN ╱ m that mass percentage concentration is the surface tension of the 1% fracturing fluid aqueous solution.
In certain embodiments, described water-soluble organic acid is acetic acid or acetic acid and formic acid and/or butanedioic acid and/or apple
Tartaric acid.
In certain embodiments, the described organic amine containing thiazolinyl is diethylenetriamine and/or polyethylene polyamine.
In certain embodiments, described diethylenetriamine and polyethylene polyamine, its mixing quality ratio is 4.5～7.5:4.
It is preferred that adopting 6：4.
In certain embodiments, described fracturing fluid, its material composition is in parts by weight acetic acid 700-810 parts, formic acid
0-20 parts, butanedioic acid 0-50 parts, malic acid 0-20 parts, the organic amine 100-200 parts containing thiazolinyl.
In certain embodiments, it is preferable that described fracturing fluid, its material composition is in parts by weight 780 parts of acetic acid, formic acid
15 parts, 25 parts of butanedioic acid, 15 parts of malic acid, 160 parts of the organic amine containing thiazolinyl.
In certain embodiments, described acetic acid, its purity is calculated as 95-99.5% with weight/mass percentage composition；Butanedioic acid, its
Purity is calculated as more than 99% with weight/mass percentage composition；Formic acid, its purity is calculated as more than 95% with weight/mass percentage composition.
In certain embodiments, described diethylenetriamine, its purity is calculated as ＞ 96% with weight/mass percentage composition；Many ethene
Polyamines, its purity is calculated as 95% with weight/mass percentage composition.
In certain embodiments, described acetic acid is pyroligneous acid obtained in biomass carbonization or is prepared as raw material with methyl alcohol
Acetic acid.
In certain embodiments, its preparation method is：Raw material is taken according to proportioning, water-soluble organic acid is pumped into backflow
In the glass lined reaction vessel of condenser and mixer, the organic amine containing thiazolinyl is loaded into the measuring tank at the top of glass lined reaction vessel
In, mixer is opened, the organic amine containing thiazolinyl is instilled, and drip off in 1-2h, after dripping off, it is stirred for 0.3-0.7h；And
During above-mentioned whole organic amine of the dropwise addition containing thiazolinyl, temperature≤90 DEG C in reactor, the temperature in reflux condenser are controlled
≤ 40 DEG C of degree, and after question response product naturally cools to 40 DEG C, put into finished pot through filter, obtain environment-friendly type alcohol radical pressure
Split liquid.
Embodiment 1
A kind of environment-friendly type alcohol-base fracturing fluid, the material composition of the fracturing fluid is by weight, acetic acid 780kg, formic acid
20kg, butanedioic acid 50kg, diethylenetriamine and polyethylene polyamine mixture 150kg.
Described quality of acetic acid percentage composition 98%；
Described formic acid weight/mass percentage composition 95%；
Described butanedioic acid weight/mass percentage composition 99%；
Described diethylenetriamine weight/mass percentage composition 96%；
Described polyethylene polyamine weight/mass percentage composition 95%.
Preparation method is：Raw acetic acid, formic acid and butanedioic acid are taken by proportioning add the reaction of the enamel with reflux condenser
In kettle, 10min is stirred, after dissolving, be passed through cold water to reflux condenser and open reactor top measuring tank, in terms of adding at a slow speed
Measured diethylenetriamine and polyethylene polyamine mixed liquor are added in 2h.In amine exothermal reaction process is added, with observation temperature
The change of degree, reflux condenser temperature is not higher than 40 DEG C, and the temperature of reactor is not higher than 90 DEG C, question response temperature in the kettle drop after 2h
Environment-friendly type alcohol-base fracturing fluid is to after 40 DEG C into finished pot Jing after filter filtration.
The performance of product is detected, assay is：50 DEG C of kinematic viscosity of the fracturing fluid are 42 ㎜2╱ s, moisture content
Weight/mass percentage composition 15%, it is≤20mn ╱ m that mass percentage concentration is the surface tension of the 1% fracturing fluid aqueous solution.
Embodiment 2
A kind of environment-friendly type alcohol-base fracturing fluid：The material composition of the fracturing fluid is by weight acetic acid 810kg, formic acid 15kg,
Malic acid 15kg, diethylenetriamine and polyethylene polyamine mixture 160kg.
Described quality of acetic acid percentage composition 96%；
Described formic acid weight/mass percentage composition 95%；
Described malic acid weight/mass percentage composition 96%.
Preparation method is：Raw material is taken by proportioning.Acetic acid, formic acid and malic acid add band reflux cooler and reacting kettle jacketing
It is passed through cooling water and opens reactor top point measuring tank, the diethylenetriamine and polyethylene polyamine mixing for measuring is added at a slow speed
Thing, adds in 2h.In amine exothermal reaction process is added, the temperature in observing reflux cooler and reactor at any time, returned cold
But the temperature in device is not higher than 40 DEG C, and the temperature in reactor is not higher than 90 DEG C, and the temperature after 2h in question response kettle is down to 40 DEG C
Afterwards, it is environment-friendly type alcohol-base fracturing fluid into finished pot through filter filter.
Performance detection is carried out to product, assay is：The ㎜ of kinematic viscosity 45 of 50 DEG C of the fracturing fluid2The matter of ╱ s moisture
Amount percentage composition 13.8%, mass percentage concentration is the surface tension≤26mN ╱ m of the 1% fracturing fluid aqueous solution.
Embodiment 3
A kind of preparation method of environment-friendly type alcohol-base fracturing fluid, the material composition of the fracturing fluid is by weight wooden vinegar acetic acid
730kg, butanedioic acid 50kg, malic acid 20kg, diethylenetriamine and polyethylene polyamine mixture 200kg.
Described wooden vinegar quality of acetic acid percentage composition 91%；
Described butanedioic acid weight/mass percentage composition 99%；
Described malic acid weight/mass percentage composition 94%；
Described Diethylenetriamine weight/mass percentage composition 96%；
Described polyethylene polyamine weight/mass percentage composition 95%.
Preparation method is：The enamel that raw material wood vinegar acetic acid, butanedioic acid and malic acid add reflux condenser is taken by proportioning
In reactor, after stirring 30min dissolvings, it is passed through cold water to reflux condenser and reacting kettle jacketing and opens the metering of reactor top
Tank, to add the diethylenetriamine and polyethylene polyamine mixed liquor that measure at a slow speed, adds in 2h, plus amine during with
The change of observation temperature, reflux condenser is not higher than 40 DEG C, and the temperature in reactor is not higher than 90 DEG C, question response kettle interior temperature after 2h
After degree is down to 40 DEG C, environment-friendly type alcohol-base fracturing fluid is into finished pot after filter filter.
Properties of product are detected, assay is：Kinematic viscosity at 50 DEG C of the fracturing fluid is 44 ㎜2╱ s, the matter of moisture
Amount percentage composition 19.8%, mass percentage concentration is the surface tension≤28mN ╱ m of the aqueous solution of 1% fracturing fluid.
Here is necessary explanation, and above-described embodiment is only limitted to make further the technical scheme of the invention
Explain and illustrate, in order to the technical scheme of those skilled in the art's correct understanding the invention, those skilled in the art exist
On the basis of this, the essential characteristics of the non-protruding made and the improvement of non-significant progress belong to the protection category of the present invention.
Claims (10)
1. a kind of environment-friendly type alcohol-base fracturing fluid, it is characterised in that the fracturing fluid using water-soluble organic acid with contain the organic of thiazolinyl
There is condensation reaction and prepare in amine.
2. environment-friendly type alcohol-base fracturing fluid as claimed in claim 1, it is characterised in that described water-soluble organic acid is acetic acid or second
Acid and formic acid and/or butanedioic acid and/or malic acid.
3. environment-friendly type alcohol-base fracturing fluid as claimed in claim 1, it is characterised in that the described organic amine containing thiazolinyl is divinyl
Triamine and/or polyethylene polyamine.
4. environment-friendly type alcohol-base fracturing fluid as claimed in claim 3, it is characterised in that described diethylenetriamine and many ethene is more
Amine, its mixing quality ratio is 4.5～7.5:4.
5. environment-friendly type alcohol-base fracturing fluid as claimed in claim 1, it is characterised in that described fracturing fluid, its material composition is with weight
Amount part is calculated as acetic acid 700-810 parts, formic acid 0-20 parts, butanedioic acid 0-50 parts, malic acid 0-20 parts, the organic amine 100- containing thiazolinyl
200 parts.
6. the environment-friendly type alcohol-base fracturing fluid as described in claim 1 or 5, it is characterised in that described fracturing fluid, its material composition with
Weight portion is calculated as 780 parts of acetic acid, 15 parts of formic acid, 25 parts of butanedioic acid, 15 parts of malic acid, 160 parts of the organic amine containing thiazolinyl.
7. the environment-friendly type alcohol-base fracturing fluid as described in claim 2 or 5, it is characterised in that described acetic acid, its purity is with quality hundred
Point content is calculated as 95-99.5%；Butanedioic acid, its purity is calculated as more than 99% with weight/mass percentage composition；Formic acid, its purity is with quality
Percentage composition is calculated as more than 95%.
8. the environment-friendly type alcohol-base fracturing fluid as described in claim 3 or 4, it is characterised in that described diethylenetriamine, its purity with
Weight/mass percentage composition is calculated as ＞ 96%；Polyethylene polyamine, its purity is calculated as 95% with weight/mass percentage composition.
9. the environment-friendly type alcohol-base fracturing fluid as described in claim 2 or 5, it is characterised in that described acetic acid is biomass carbonization system
The pyroligneous acid for obtaining or the acetic acid prepared as raw material with methyl alcohol.
10. the environment-friendly type alcohol-base fracturing fluid preparation method as described in any one of claim 1～9, it is characterised in that take according to proportioning
Raw material, water-soluble organic acid is pumped in the glass lined reaction vessel with reflux condenser and mixer, will be organic containing thiazolinyl
Amine is fitted in the measuring tank at the top of glass lined reaction vessel, opens mixer, instills the organic amine containing thiazolinyl, and drips off in 1-2h,
After dripping off, 0.3-0.7h is stirred for；And during above-mentioned whole organic amine of the dropwise addition containing thiazolinyl, in control reactor
Temperature≤90 DEG C, temperature≤40 DEG C in reflux condenser, and after question response product naturally cools to 40 DEG C, through filter
Put into finished pot, obtain environment-friendly type alcohol-base fracturing fluid.
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| CN201611049436.5A CN106634934A (en) | 2016-11-24 | 2016-11-24 | Environment-friendly alcohol group fracturing fluid and preparation method thereof |
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| CN201611049436.5A CN106634934A (en) | 2016-11-24 | 2016-11-24 | Environment-friendly alcohol group fracturing fluid and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112391154A (en) * | 2020-11-24 | 2021-02-23 | 中国石油大学(华东) | Alcohol-containing fracturing fluid and preparation method and application thereof |
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| CN1120836A (en) * | 1993-04-13 | 1996-04-17 | 汉克尔股份两合公司 | Fatty-acid amides with improved cold-water dispersibility |
| US5536370A (en) * | 1992-11-28 | 1996-07-16 | Basf Aktiengesellschaft | Condensates of polyalkylenepolyamines, their preparation and their use in papermaking |
| CN101955441A (en) * | 2010-04-06 | 2011-01-26 | 孙安顺 | Preparation method and application of fatty amide polyethylene polyamine amino acid for tertiary oil recovery |
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2016
- 2016-11-24 CN CN201611049436.5A patent/CN106634934A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5536370A (en) * | 1992-11-28 | 1996-07-16 | Basf Aktiengesellschaft | Condensates of polyalkylenepolyamines, their preparation and their use in papermaking |
| CN1120836A (en) * | 1993-04-13 | 1996-04-17 | 汉克尔股份两合公司 | Fatty-acid amides with improved cold-water dispersibility |
| CN101955441A (en) * | 2010-04-06 | 2011-01-26 | 孙安顺 | Preparation method and application of fatty amide polyethylene polyamine amino acid for tertiary oil recovery |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112391154A (en) * | 2020-11-24 | 2021-02-23 | 中国石油大学(华东) | Alcohol-containing fracturing fluid and preparation method and application thereof |
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Application publication date: 20170510 |