CN105154056B - A kind of anhydrous pressure break liquid and preparation method thereofs of LPG suitable for unconventional reservoir and application - Google Patents
A kind of anhydrous pressure break liquid and preparation method thereofs of LPG suitable for unconventional reservoir and application Download PDFInfo
- Publication number
- CN105154056B CN105154056B CN201510557698.1A CN201510557698A CN105154056B CN 105154056 B CN105154056 B CN 105154056B CN 201510557698 A CN201510557698 A CN 201510557698A CN 105154056 B CN105154056 B CN 105154056B
- Authority
- CN
- China
- Prior art keywords
- lpg
- crosslinking agent
- anhydrous fracturing
- parts
- anhydrous
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- 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
- C09K8/64—Oil-based compositions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G79/00—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule
- C08G79/02—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule a linkage containing phosphorus
- C08G79/04—Phosphorus linked to oxygen or to oxygen and carbon
Abstract
The invention discloses a kind of brand-new anhydrous fracturing fluids of the LPG suitable for unconventional reservoir and preparation method and application.In terms of mass parts, the raw material composition of the anhydrous fracturing fluids of the LPG includes：12 parts of phosphate gelling agent, 0.5 1.5 parts of crosslinking agent, 100 parts of propane.The preparation method includes：(1) the anhydrous fracturing fluid single methanol gelling agents of brand-new LPG are prepared；(2) preparing can be with the novel crosslinker of PLG Quick cross-linkings；(3) 50 DEG C of gelling agents and crosslinking agent that LPG liquefies and added according to a certain ratio in step (1) and step (2) carry out crosslinking and can be prepared by the anhydrous fracturing fluids of LPG in a kettle.By the anhydrous fracturing fluid fanout free regions of LPG made from the crosslinking agent of the present invention, surface tension is low, density is low, viscosity is low, and the row of returning leads height after pressure break；Outstanding sand, solid-carrying performance are excellent and miscible with reservoir fluid, and caused effective crack length is longer after pressure, and then the purpose increased production.
Description
Technical field
The invention belongs to petrochemical industry, and in particular to it is a kind of can with the crosslinking agents of LPG Quick cross-linkings and its prepare and
Using.
Background technology
In recent years, as the fast development of China's economy, oil gas imbalance between supply and demand grow in intensity, crude oil import amount increases year by year
Add.And conventional gas and oil resource is faced with the problem of production capacity seriously reduces or even be exhausted, this allows for shale gas, coal bed gas, fine and close
The unconventional petroleum resourceses such as oil gas are increasingly paid attention to by whole world various countries.China's unconventional petroleum resources very abundant, always
Reserves are about twice of conventional gas and oil resource, have very big exploitation exploration prospect.The core skill of unconventionaloil pool reservoir exploitation
Art is fracturing reform, and fracturing fluid system is the key of fracturing reform successful implementation.Due to Unconventional reservoir poor properties, infiltration
Rate and porosity are relatively low, and conventional fracturing fluid easily causes Water trapping injury, is unfavorable for fracturing yield increasing, but also are accompanied with serious
Problem of environmental pollution.To solve the above problems, occur the new anhydrous fracturing technique using LPG as representative, LPG both at home and abroad
Anhydrous fracturing technique can not only solve water shortage problem, moreover it is possible to reduce hydrocarbon reservoir development pollution on the environment.
Liquefied petroleum gas (LPG) is used as fracturing fluid, and its main component is exactly propane (C3H8) there are a small amount of ethane, propylene, fourth
Alkane and chemical addition agent, to stratum without any injury.Performance and hydraulic fracturing of the LPG pressure breaks in underground are different, in pressure break
During take sand characteristic there is the feature of liquid medium.Gasify in LPG between returning waiting because of pressure, temperature variation, embody again
Gas characteristic, then returned again together with natural gas and drain into ground, repeat and utilize after separation, when return period only needs several days
Between, it is directly entered production flow line even without separation and gel breaker need not be added, is by changing bottom pressure after fracturing work
The propane gasification row of returning can be made.This pressure break means, also need not input compared to water is not needed substantially for conventional hydraulic fracturing technique
Fund allocation waste water, greatly alleviates environment and Water Resources Pressure, has prevented payzone infringement, is the new side of fracturing technique development
To.It is effective fracture that conventional hydraulic pressure break, which only has 20%-50% fracture length, and fracture length caused by LPG pressure breaks is whole
Ultimate recovery can be improved 20%-30% for effective fracture.LPG viscosity is higher, proppant can be made to suspend completely, avoided
The proppant depositional phenomenon that conventional hydraulic fracturing fluid occurs because viscosity is relatively low, can open payzone completely, obtain more preferable
Fracturing effect.
There is a kind of method that fracturing fluid is prepared using butane as base fluid in the prior art, and made using sodium aluminate, sodium metaaluminate
For crosslinking agent.But the fracturing fluid its viscosity at 65 DEG C only has 50mPas, can not meet the increasing of high temperature oil field and ultradeep well
Production operation and the fracturing fluid will also add gel breaker, and preparation technology is complicated, plastic speed is slow, temperature and shearing sustainability is poor.
Hydraulic fracturing at present is still the main method of oilfield stimulation stable yields, but it is taken that husky effect is poor, water consumption is big, uncomfortable
For being promoted the use of in water-deficient area, especially in NORTHWEST CHINA area.And the fracturing fluid recovery (backflow) cycle grow up the several months or on
Year, hydraulic fracturing about 40%-60% fracturing fluid, which can not return to discharge, will residue in stratum so as to be damaged to reservoir.
In addition also polluted the environment after fracturing fluid recovery (backflow), return discharge opeing and be difficult to handle, do not meet the theory of environmental protection and sustainable development.And
Which part aqueous-based polymers can also block fracturing fracture, reduce fracturing effect.
The content of the invention
The present invention makes improvements for above-mentioned problem, i.e., suitable the technical problem to be solved in the present invention is to provide one kind
Anhydrous fracturing fluids of LPG for unconventional reservoir and preparation method and application.
The present invention adopts the following technical scheme that：
It is described in terms of mass parts the invention provides a kind of brand-new anhydrous fracturing fluids of the LPG suitable for unconventional reservoir
The raw material composition of the anhydrous fracturing fluids of LPG includes：Phosphate gelling agent 1-2 parts, crosslinking agent 0.5-1.5 parts, 100 parts of propane.
Present invention also offers one kind to prepare the anhydrous fracturing fluid methods of LPG, comprises the following steps：
(1) the anhydrous fracturing fluid single methanol gelling agents of brand-new LPG are prepared；
(2) preparing can be with the novel crosslinker of PLG Quick cross-linkings；
(3) -50 DEG C of gellings that LPG liquefies and added according to a certain ratio in step (1) and step (2) in a kettle
Agent and crosslinking agent carry out crosslinking and can be prepared by the anhydrous fracturing fluids of LPG.
The novel crosslinker is made up of following material according to parts by weight：
The compound host is ferric sulfate, ironic citrate by 2:1-10:1 ratio mixes, wherein optimal is 4:1.
The assistant crosslinking agent is N, and N- lutidines, a kind of or their mixture of BTA are described
N, N- lutidines structure is：
Wherein R1, R2, R3 are the straight chain or branched hydrocarbyl of 1-12 carbon atom, or oxygen alkyl, pyridine；It is described
BTA structure is：
Wherein R1, R2 are the straight chain or branched hydrocarbyl of 1-7 carbon atom, or oxygen alkyl, quinoline.
The active additive is PEG400, PEG2000, isopropanolamine, tetrabutylammonium iodide, octadecyl trimethyl
A kind of or their mixture of ammonium chloride.
The novel crosslinker is prepared to comprise the following steps：
(1) deionized water necessarily matched is added in reaction vessel and is warming up to 60 DEG C or so；
(2) active additive is added, compound host stirs reaction；
(3) it is cooled at 30 DEG C and is eventually adding assistant crosslinking agent stirring reaction 20 minutes.
The preparation method of described phosphate gelling agent is as follows：
(1) triethyl phosphate and phosphoric acid under the conditions of 80 DEG C -95 DEG C with normal heptane, dimethylbenzene, toluene or theirs is mixed
Compound is as 2-4 hour generation polyphosphate intermediate of solvent reaction；
(2) the polyphosphate intermediate in step (1) and C2-C18 monohydric alcohol, dihydric alcohol, polyalcohol or they
Mixture reacts 4-6 hour generation phosphate gelling agent under the conditions of 120 DEG C -135 DEG C.
Beneficial effects of the present invention：The present invention by the way that propane is liquefied under the conditions of -50 DEG C, add phosphate gelling agent and
The anhydrous fracturing fluids of LPG are made in novel crosslinker crosslinking.And in the type HTHP rotational rheometers of Mars III, carry out that heatproof is resistance to cuts
Cutting property is tested, and is 170s in rotating speed-1, its viscosity of continuous shear stress 120min remains to reach 125mPa under conditions of 120 DEG C of temperature
S, the purpose of most oil field compression fracture volume increase can be met completely；Secondly, propane of the invention can multiple recycling,
Pressure break cost will be substantially reduced, also fully demonstrates the theory of economical environment-protective；And the anhydrous fracturing fluids of LPG produced by the present invention without
Injury, surface tension is low, density is low, viscosity is low, and the row of returning leads height after pressure break；Outstanding sand, solid-carrying performance is excellent and is mixed with reservoir fluid
Molten, caused effective crack length is longer after pressure, and then the purpose increased production.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is the 170s at 80 DEG C-1Under conditions of in embodiment one fracturing fluid gel rubber system carry out heatproof endurance of cutting
Can test chart；
Fig. 2 is the 170s at 100 DEG C-1Under conditions of in embodiment two fracturing fluid gel rubber system carry out heatproof resistant to shearing
Performance test figure；
Fig. 3 is the 170s at 120 DEG C-1Under conditions of in embodiment three fracturing fluid gel rubber system carry out heatproof resistant to shearing
Performance test figure；
Fig. 4 is the 170s at 150 DEG C-1Under conditions of in example IV fracturing fluid gel rubber system carry out heatproof resistant to shearing
Performance test figure；
η is viscosity in accompanying drawing；T is temperature；T is the time.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of creative work is not made
Embodiment, belong to the scope of protection of the invention.
Embodiment 1：
The anhydrous fracturing fluids of LPG of the present embodiment are made up of the raw material of following mass percent：4.0% gelling agent, 2.0%
Crosslinking agent and alkyl hydro carbons.Wherein alkyl hydro carbons is 80%-95% propane and a small amount of butane.The gelling agent is alkyl
Phosphate gelling agent, mixed alcohol therein include n-amyl alcohol, n-hexyl alcohol and Decanol.N-amyl alcohol mass percent is in mixed alcohol
21%, the mass percent of n-hexyl alcohol is 54%, and the mass percent of Decanol is 25%.Compound host in the crosslinking agent
For ferric sulfate and ironic citrate, mass percent 3:1.Active additive is PEG400, assistant crosslinking agent N, N- dimethyl pyrazole
Pyridine, wherein R1For normal-butyl, R2For ethyl, R3For oxygen alkyl.The preparation method of the alkyl phosphate gelling agent is as follows：
(1) triethyl phosphate and phosphoric acid are poly- using normal heptane as 3 hour generations of solvent reaction under the conditions of 80 DEG C -95 DEG C
Phosphate intermediate.Wherein the mol ratio of triethyl phosphate and phosphoric acid is 1.2:1.
(2) the polyphosphate intermediate in step (1) and the mixed alcohol described in the present embodiment are under the conditions of 120 DEG C -135 DEG C
6 hour generation alkyl phosphate gelling agents of reaction.Wherein the mol ratio of mixed alcohol and phosphoric acid is 2.8:1.
The anhydrous pressure break liquid and preparation method thereofs of LPG of the present embodiment are：Alkyl phosphate gelling agent and friendship are measured according to a certain ratio
Join agent, under the conditions of -50 DEG C by propane liquefy and add crosslinking agent and gelling agent stirring 5 minutes or so.
Embodiment 2：
The anhydrous fracturing fluids of LPG of the present embodiment are made up of the raw material of following mass percent：3.0% gelling agent, 1.5%
Crosslinking agent and alkyl hydro carbons.Wherein alkyl hydro carbons is 80%-95% propane and a small amount of butane.The gelling agent is alkyl
Phosphate gelling agent, mixed alcohol therein include normal propyl alcohol, n-hexyl alcohol and hexadecanol.Normal propyl alcohol mass percent is in mixed alcohol
14%, the mass percent of n-hexyl alcohol is 74%, and the mass percent of hexadecanol is 12%.Compound host in the crosslinking agent
For ferric sulfate and ironic citrate, mass percent 5:1.Active additive is tetrabutylammonium iodide, and assistant crosslinking agent is benzo
Triazole, wherein R1For normal-butyl, R2For propyl group, R3For pyridine.The preparation method of the alkyl phosphate gelling agent is as follows：
(1) triethyl phosphate and phosphoric acid are poly- using normal heptane as 4 hour generations of solvent reaction under the conditions of 80 DEG C -95 DEG C
Phosphate intermediate.Wherein the mol ratio of triethyl phosphate and phosphoric acid is 1.3:1.
(2) the polyphosphate intermediate in step (1) and the mixed alcohol described in the present embodiment are under the conditions of 120 DEG C -135 DEG C
5 hour generation alkyl phosphate gelling agents of reaction.Wherein the mol ratio of mixed alcohol and phosphoric acid is 3.0:1.
The anhydrous pressure break liquid and preparation method thereofs of LPG of the present embodiment are：Alkyl phosphate gelling agent and friendship are measured according to a certain ratio
Join agent, under the conditions of -50 DEG C by propane liquefy and add crosslinking agent and gelling agent stirring 5 minutes or so.
Embodiment 3：
The anhydrous fracturing fluids of LPG of the present embodiment are made up of the raw material of following mass percent：1.0% gelling agent, 1.5%
Crosslinking agent and alkyl hydro carbons.Wherein alkyl hydro carbons is 80%-95% propane and a small amount of butane.The gelling agent is alkyl
Phosphate gelling agent, mixed alcohol therein include n-heptanol, n-hexyl alcohol and n-nonyl alcohol.N-heptanol mass percent is in mixed alcohol
3%, the mass percent of n-hexyl alcohol is 91%, and the mass percent of n-nonyl alcohol is 6%.Compound host in the crosslinking agent is
Ferric sulfate and ironic citrate, mass percent 9:1.Active additive is OTAC, and assistant crosslinking agent is
N, N- lutidines, wherein R1For methyl, R2For normal-butyl, R3For quinoline.The preparation method of the alkyl phosphate gelling agent
It is as follows：
(1) triethyl phosphate and phosphoric acid are poly- using normal heptane as 4 hour generations of solvent reaction under the conditions of 80 DEG C -95 DEG C
Phosphate intermediate.Wherein the mol ratio of triethyl phosphate and phosphoric acid is 1.25:1.
(2) the polyphosphate intermediate in step (1) and the mixed alcohol described in the present embodiment are under the conditions of 120 DEG C -135 DEG C
4 hour generation alkyl phosphate gelling agents of reaction.Wherein the mol ratio of mixed alcohol and phosphoric acid is 2.6:1.
The anhydrous pressure break liquid and preparation method thereofs of LPG of the present embodiment are：Alkyl phosphate gelling agent and friendship are measured according to a certain ratio
Join agent, under the conditions of -50 DEG C by propane liquefy and add crosslinking agent and gelling agent stirring 5 minutes or so.
Embodiment 4：
The anhydrous fracturing fluids of LPG of the present embodiment are made up of the raw material of following mass percent：1.5% gelling agent, 1.0%
Crosslinking agent and alkyl hydro carbons.Wherein alkyl hydro carbons is 80%-95% propane and a small amount of butane.The gelling agent is alkyl
Phosphate gelling agent, mixed alcohol therein include normal propyl alcohol, n-heptanol and n-nonyl alcohol.Normal propyl alcohol mass percent is in mixed alcohol
24%, the mass percent of n-heptanol is 46%, and the mass percent of n-nonyl alcohol is 30%.Compound host in the crosslinking agent
For ferric sulfate and ironic citrate, mass percent 8:1.Active additive is isopropanolamine, and assistant crosslinking agent is BTA,
Wherein R1For isopropyl, R2For normal-butyl, R3For methyl.The preparation method of the alkyl phosphate gelling agent is as follows：
(1) triethyl phosphate and phosphoric acid are poly- using normal heptane as 2 hour generations of solvent reaction under the conditions of 80 DEG C -95 DEG C
Phosphate intermediate.Wherein the mol ratio of triethyl phosphate and phosphoric acid is 1.25:1.
(2) the polyphosphate intermediate in step (1) and the mixed alcohol described in the present embodiment are under the conditions of 120 DEG C -135 DEG C
2 hour generation alkyl phosphate gelling agents of reaction.Wherein the mol ratio of mixed alcohol and phosphoric acid is 2.6:1.
The anhydrous pressure break liquid and preparation method thereofs of LPG of the present embodiment are：Alkyl phosphate gelling agent and friendship are measured according to a certain ratio
Join agent, under the conditions of -50 DEG C by propane liquefy and add crosslinking agent and gelling agent stirring 5 minutes or so.
Rock core flowing experiment is done to the fracturing fluid in embodiment 1,2,3,4, rock core is derived from Sichuan Jiao's masonry dam shale gas reservoir,
Core permeability is 3.78 × 10-4μm2~5.34 × 10-4μm2.As a result show that the fracturing fluid is to the average injury rate of reservoir
5.69%, hence it is evident that less than injury of the aqueous fracturing fluid to reservoir.
In the type HTHP rotational rheometers of Mars III, at 80 DEG C, 170s-1Under conditions of to the pressure break in embodiment one
Lyogel system carries out temperature and shearing sustainability test.(experimental result is referring to accompanying drawing 1)
As can be seen that being sheared since 79 DEG C from accompanying drawing 1, with the increase of shear time, the viscosity of fracturing fluid is rapid
Increase to 300mPas or so and settle out.As temperature stabilization is at 80 DEG C, the viscosity of fracturing fluid also arrives in 280mPas
Settled out between 300mPas.Shear time was continuously increased until 60 minutes, and the viscosity of fracturing fluid stills remain in
Between 280mPas to 300mPas.
According to test result, this kind of fracturing fluid is at 80 DEG C, 170s-1Under conditions of shear a hour, fracturing fluid viscosity energy
It is maintained at 300mPas.This viscosity is considerably beyond professional standard SY/T 6376-2008《Fracturing fluid general technical specifications》's
Regulation, considerably beyond the viscosity required for site operation.
In the type HTHP rotational rheometers of Mars III, at 100 DEG C, 170s-1Under conditions of to the pressure in embodiment two
Split lyogel system and carry out temperature and shearing sustainability test.(experimental result is referring to accompanying drawing 2)
From accompanying drawing 2 it can be seen that under the conditions of 100 DEG C, with the increase of shear time, the fracturing fluid viscosity is held first
It is continuous to drop to 240mPas, then in 240mPas stable a period of times.Then fracturing fluid viscosity bust is to 170map.s,
After a period of stabilisation, fracturing fluid viscosity is again lowered to 160mPas to 170mPas.After undergoing 2 this processes repeatedly,
Fracturing fluid viscosity finally slowly rises and stably in 200mPas.
According to test result, this kind of fracturing fluid is at 100 DEG C, 170s-1Under conditions of shear a hour, fracturing fluid viscosity energy
It is maintained at 300mPas.This viscosity is considerably beyond professional standard SY/T 6376-2008《Fracturing fluid general technical specifications》's
Regulation, considerably beyond the viscosity required for site operation.
In the type HTHP rotational rheometers of Mars III, at 120 DEG C, 170s-1Under conditions of to the pressure in embodiment three
Split lyogel system and carry out temperature and shearing sustainability test.(experimental result is referring to accompanying drawing 3)
When since accompanying drawing 3 it will be seen that shearing just, with the increase of shear time, fracturing fluid viscosity rapidly from
175mPas is down to 125mPas, then fracturing fluid the viscosity stabilization for a period of time after.Viscosity experienced from 125mPas
Rise to 175mPas and then drop back to 125mPas process rapidly again, thus it is speculated that be fracturing fluid and unstabilized reason.Herein it
Fracturing fluid whole process is stably held in 120mPas or so afterwards, and this viscosity fully meets site operation demand and meets industry mark
It is accurate.
In the type HTHP rotational rheometers of Mars III, at 150 DEG C, 170s-1Under conditions of to the pressure in example IV
Split lyogel system and carry out temperature and shearing sustainability test.(experimental result is referring to accompanying drawing 4)
From accompanying drawing 4 as can be seen that as the rise of temperature, the viscosity of pressure break lyogel are gradually reduced；When temperature raises
During to 140 DEG C, the viscosity of pressure break lyogel can also reach 500mPas；When after the 20min that heats up and when temperature is increased to 150 DEG C,
The viscosity of pressure break lyogel can still maintain more than 100mPas.This viscosity fully meets site operation demand and met
Professional standard.Show that the fracturing fluid gel has simultaneously and take husky effect well,
According to 4 heatproof cutting performance experiments as can be seen that the LPG obtained by using novel crosslinker and gelling agent is anhydrous
Fracturing fluid shows extremely outstanding at high temperature, fully meets site operation and industry requirement, and heatproof cutting performance is fabulous, can be with
Fully meet the requirement of live pressing crack construction operation.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (4)
- A kind of 1. brand-new anhydrous fracturing fluids of the LPG suitable for unconventional reservoir, it is characterised in that：In terms of mass parts, the LPG The raw material composition of anhydrous fracturing fluid includes：Phosphate gelling agent 1-2 parts, crosslinking agent 0.5-1.5 parts, 100 parts of propane；The crosslinking agent is made up of following material according to parts by weight：The compound host is ferric sulfate, ironic citrate by 2:1-10:1 ratio mixes；The assistant crosslinking agent is N, N- lutidines, a kind of or their mixture of BTA, described N, N- Lutidines structure is：Wherein R1,R2,R3For the straight chain or branched hydrocarbyl of 1-12 carbon atom, or it is oxygen alkyl, pyridine；The nitrogen of benzo three Azoles structure is：Wherein R1,R2For the straight chain or branched hydrocarbyl of 1-7 carbon atom, or it is oxygen alkyl, quinoline；The active additive is PEG400, PEG2000, isopropanolamine, tetrabutylammonium iodide, octadecyl trimethyl chlorination A kind of or their mixture of ammonium.
- 2. the anhydrous fracturing fluids of LPG according to claim 1, it is characterised in that：The preparation side of described phosphate gelling agent Method is as follows：(1) triethyl phosphate and phosphoric acid under the conditions of 80 DEG C -95 DEG C with normal heptane, dimethylbenzene, toluene or their mixture As 2-4 hour generation polyphosphate intermediate of solvent reaction；(2) monohydric alcohol, dihydric alcohol, polyalcohol or their mixing of the polyphosphate intermediate and C2-C18 in step (1) Thing reacts 4-6 hour generation phosphate gelling agent under the conditions of 120 DEG C -135 DEG C.
- A kind of 3. method of the anhydrous fracturing fluids of LPG prepared described in claim 1 or claim 2, it is characterised in that：Including with Lower step：(1) the anhydrous fracturing fluid phosphate gelling agents of brand-new LPG are prepared；(2) preparing can be with the crosslinking agent of PLG Quick cross-linkings；(3) in a kettle -50 DEG C by LPG liquefy and according to a certain ratio addition step (1) and step (2) in phosphoric acid ester gum Solidifying agent and crosslinking agent carry out crosslinking and can be prepared by the anhydrous fracturing fluids of LPG.
- 4. the anhydrous fracturing fluid methods of preparation LPG according to claim 3, it is characterised in that：Preparing the crosslinking agent includes Following steps：(1) deionized water necessarily matched is added in reaction vessel and is warming up to 60 DEG C；(2) active additive is added, compound host stirs reaction；(3) it is cooled at 30 DEG C and is eventually adding assistant crosslinking agent stirring reaction 20 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510557698.1A CN105154056B (en) | 2015-09-02 | 2015-09-02 | A kind of anhydrous pressure break liquid and preparation method thereofs of LPG suitable for unconventional reservoir and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510557698.1A CN105154056B (en) | 2015-09-02 | 2015-09-02 | A kind of anhydrous pressure break liquid and preparation method thereofs of LPG suitable for unconventional reservoir and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105154056A CN105154056A (en) | 2015-12-16 |
| CN105154056B true CN105154056B (en) | 2018-01-12 |
Family
ID=54795116
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510557698.1A Expired - Fee Related CN105154056B (en) | 2015-09-02 | 2015-09-02 | A kind of anhydrous pressure break liquid and preparation method thereofs of LPG suitable for unconventional reservoir and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105154056B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107760292A (en) * | 2016-08-15 | 2018-03-06 | 中国石油化工股份有限公司 | A kind of lower carbon number hydrocarbons gelling agent of polyalcohol synergy and preparation method thereof |
| CN106497535A (en) * | 2016-10-18 | 2017-03-15 | 佛山慧创正元新材料科技有限公司 | Anhydrous fracturing fluid of a kind of high temperature resistant resistant to shearing and preparation method thereof |
| CN108285782A (en) * | 2017-01-10 | 2018-07-17 | 中国石油化工股份有限公司 | A kind of lower carbon number hydrocarbons gelling agent of polyalcohol synergy and preparation method thereof |
| CN106905360A (en) * | 2017-04-07 | 2017-06-30 | 西南石油大学 | One-step synthesis phosphate gelling agent and the method for preparing the anhydrous fracturing fluid of lower carbon number hydrocarbons |
| CN108300449A (en) * | 2018-03-16 | 2018-07-20 | 中国石油大学(华东) | A kind of ethers fracturing fluid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103468236A (en) * | 2013-08-16 | 2013-12-25 | 中国石油天然气股份有限公司 | Butane-containing fracturing fluid and preparation method thereof |
| CN104004506A (en) * | 2014-06-18 | 2014-08-27 | 西安石油大学 | Anhydrous fracturing fluid suitable for unconventional reservoir fracturing and preparing method of anhydrous fracturing fluid |
| CN104293335A (en) * | 2014-10-14 | 2015-01-21 | 西南石油大学 | Anhydrous fracturing fluid suitable for shale gas and preparation method of anhydrous fracturing fluid |
| CN104498017A (en) * | 2014-12-22 | 2015-04-08 | 中国石油天然气股份有限公司 | Fracturing fluid cross-linking agent and preparation method and application thereof |
-
2015
- 2015-09-02 CN CN201510557698.1A patent/CN105154056B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103468236A (en) * | 2013-08-16 | 2013-12-25 | 中国石油天然气股份有限公司 | Butane-containing fracturing fluid and preparation method thereof |
| CN104004506A (en) * | 2014-06-18 | 2014-08-27 | 西安石油大学 | Anhydrous fracturing fluid suitable for unconventional reservoir fracturing and preparing method of anhydrous fracturing fluid |
| CN104293335A (en) * | 2014-10-14 | 2015-01-21 | 西南石油大学 | Anhydrous fracturing fluid suitable for shale gas and preparation method of anhydrous fracturing fluid |
| CN104498017A (en) * | 2014-12-22 | 2015-04-08 | 中国石油天然气股份有限公司 | Fracturing fluid cross-linking agent and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105154056A (en) | 2015-12-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105154056B (en) | A kind of anhydrous pressure break liquid and preparation method thereofs of LPG suitable for unconventional reservoir and application | |
| US10301919B2 (en) | Phase-change hydraulic fracturing process | |
| US10138405B2 (en) | Fiber suspending agent for lost-circulation materials | |
| CN104109528B (en) | Acidifying liquid capable of sand stabilization and plug removal, and preparation method thereof | |
| CN109751029B (en) | Deep shale gas fracturing method | |
| CN103937475B (en) | Carbon dioxide acidification blocking remover and process of not reversely discharging raffinate after acidification | |
| CN102587858B (en) | Method for blocking water for fracture and hole type reservoir | |
| CN104119853B (en) | A kind of preparation method of air foam fracturing fluid | |
| CN106905947A (en) | A kind of displacement of reservoir oil fracturing fluid and preparation method and application | |
| CN104727799A (en) | Pulse sand fracturing method realizing high fracture conductivity of cracks | |
| CN103502386A (en) | Thickened viscoelastic fluids and uses thereof | |
| CN110388199A (en) | A kind of compound acid fracturing remodeling method of carbonate reservoir huge discharge | |
| CN109337663A (en) | Low permeability reservoir continuous mixed displacement of reservoir oil type fracturing fluid and its preparation method and application | |
| CN103834379B (en) | A kind of vermiculate glues foam system and the method improving recovery ratio with it | |
| CN106566521B (en) | Preparation and application of anion clean fracturing fluid and gel breaker thereof | |
| CN106318358A (en) | Green and environmentally friendly foam oil displacement system based on alkyl glycoside and preparation method and application thereof | |
| CN108285784B (en) | Gelled emulsified acid and preparation method thereof | |
| CN107216866A (en) | A kind of method that Carbonate Reservoir seam dictyosome accumulates acidfracturing treatment | |
| CN107686724A (en) | A kind of ultralow aqueous carbon dioxide pressure break liquid and preparation method thereof | |
| CN104479656A (en) | Variable-viscosity acid liquid used for acidifying processing | |
| Wang et al. | High-temperature-resistant, clean, and environmental-friendly fracturing fluid system and performance evaluation of tight sandstone | |
| CN104334677A (en) | Rheology modifiers | |
| CN105176510A (en) | Preparation method of fracturing fluid for anhydrous organic temporary plugging turnaround fracturing | |
| CN106167699B (en) | A kind of anhydrous fracturing fluid aluminum crosslinker of novel low carbon hydrocarbon and its preparation method and application | |
| CN103215022A (en) | Low-friction liquid for volume fracture |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180112 Termination date: 20180902 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |