CN105018057B - A kind of organic zirconium crosslinker and preparation method thereof - Google Patents

A kind of organic zirconium crosslinker and preparation method thereof Download PDF

Info

Publication number
CN105018057B
CN105018057B CN201510383977.0A CN201510383977A CN105018057B CN 105018057 B CN105018057 B CN 105018057B CN 201510383977 A CN201510383977 A CN 201510383977A CN 105018057 B CN105018057 B CN 105018057B
Authority
CN
China
Prior art keywords
solution
water
zirconium
revs
crosslinker
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.)
Active
Application number
CN201510383977.0A
Other languages
Chinese (zh)
Other versions
CN105018057A (en
Inventor
罗跃
杨欢
苏高申
罗霄
张黄鹤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yangtze University
Original Assignee
Yangtze University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Yangtze University filed Critical Yangtze University
Priority to CN201510383977.0A priority Critical patent/CN105018057B/en
Publication of CN105018057A publication Critical patent/CN105018057A/en
Application granted granted Critical
Publication of CN105018057B publication Critical patent/CN105018057B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

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
    • C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
    • C09K8/504—Compositions based on water or polar solvents
    • C09K8/506—Compositions based on water or polar solvents containing organic compounds
    • C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
    • C09K8/512—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
    • 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
    • C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
    • C09K8/504—Compositions based on water or polar solvents
    • C09K8/506—Compositions based on water or polar solvents containing organic compounds
    • C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
    • C09K8/5083—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The present invention relates to a kind of preparation method and application of the New Organo-Zirconium crosslinking agent for deep profile controlling transfer drive, belongs to oilfield chemistry and improves oil recovery factor technical field.It is to be synthesized with eight water oxygen zirconium chlorides, citric acid and ethylenediamine etc. for base stock, can realize effective control of delay crosslinking time and viscosity, and can be with salinity 40000mgL‑1Hereinafter, 0-600mgL of calcium ions and magnesium ions content‑1Various sewage are with poly-, 35 DEG C -70 DEG C oil reservoirs of Applicable temperature.In deep profile controlling transfer drive system, clear water can be replaced with sewage with poly-, as a kind of function admirable and the green non-pollution crosslinking agent harmless to reservoir, improves oil recovery factor.Solve that conventional cross-linking agent ground adaptability is poor, and salt-resistance is poor, be only suitable for clear water compatibility, pollution weight, it is big to reservoir damage the problems such as.Site test results of the present invention show that the cross linker system can be with live sewage compatibility, and plastic effect is preferable, beneficial to environmental protection.

Description

A kind of organic zirconium crosslinker and preparation method thereof
Technical field
The present invention relates to a kind of New Organo-Zirconium crosslinking agent and preparation method thereof, belongs to chemical flooding and improves oil recovery factor technology Field.
Background technology
Oil-water well water plugging and profile controlling is heterogeneous reservoir water and oil control, the important technical for improving waterflood efficiency.China's oil Field is most to enter High water cut or after the ultra-high water-containing productive life, and since water filling interval difference is big, high permeability zone water absorbing capacity is strong, is formed Water stream channel, non-available water circulation, and less permeable layer is noted and not intake, in order to improve the swept volume of injection water and injection water drive oil Efficiency, high permeability zone is blocked using profile control agent, is finally reached the purpose of balanced intake profile.Due to conventional water plugging and profile controlling skill Art has been unable to meet oil field production requirement, the research and application of deep profile correction technology etc. and achieves many new developments, high improving Remarkable result is obtained in terms of aqueous oil reservoir water flooding effectiveness.
The crosslinking agent that country's water plugging and profile controlling uses at present mainly includes：Organic aluminum crosslinker, phenolic crosslinkers, Organic Chromium The systems such as crosslinking agent.But since the ground adaptability of organo-aluminium and phenolic crosslinkers is poor, salt-resistance is poor, is only suitable for matching somebody with somebody with clear water 5；And current most popular organic chrome cross linker, adaptability is very strong, can be resistant to the temperature and pH conditions of relative broad range, Adapt to different crosslinkings（Plastic）The requirement of time, but hexavalent chromium has serious harm to underground water and reservoir, even if making Cr VI is replaced with trivalent chromium, the potential hazard to reservoir can be still caused by oxidation.CN86108877 proposes a kind of zirconium The preparation method of crosslinked gel plugging aqua, crosslinking agent therein are inorganic zirconium compound zirconium oxychloride, zirconium chloride, zirconium sulfate, nitric acid Zirconium etc. forms, and the system closing time which forms is short, is unfavorable for on-site construction operations；Effective viscosity is low, it is difficult to meets Contraction in Site requirement.102559159 A of CN have invented a kind of high-temperature resistant phenolic resin weak gel profile control plugging agent, wherein Crosslinking agent be heat safe phenolic resin, although can resisting temperature up to more than 90 DEG C, total ore deposit higher with water quality requirement needed for poly- Change degree is not higher than 8500mgL-1.103937474 A of CN provide a kind of environment protection type high-strength profile-controlling and plugging agent and its preparation side Method, crosslinking agent therein is polyethyleneimine, of high cost, and preparation process is complicated, and popularization rate is low, is not applied to.CN 101613456 B proposes a kind of coating type crosslinker and its preparation method and application, and for the crosslinking agent with Toluene-2,4-diisocyanate, 4- diisocyanate is oil Soluble monomers, atoleine are oil phase, and ethylenediamine is water-soluble monomer, using chromium of organic acid aqueous solution as core, octyl phenol Polyoxyethylene (10) ether and sorbitan monostearate are made for emulsifying agent, and chromium of organic acid therein is poisonous and harmful, not only Reservoir is injured it is also possible to polluted underground water source.
As oil field deep profile control scale constantly expands, clear water resource day needed for polymer solution preparation is becoming tight, country The further of environmental protection is paid attention to, meanwhile, the particularly high saline sewage of the large amount of sewage separated in oil well produced liquid is difficult to locate Reason.To be recycled oil field high-salt sewage, a kind of function admirable and harmless to reservoir is researched and developed, can be replaced with sewage clearly Water, which prepares deep profile controlling transfer drive cross linker system, has great economy and social effect.
The content of the invention
It is an object of the present invention to provide effective control of a kind of achievable delay crosslinking time and viscosity, and can use Sewage instead of clear water prepare, suitable for deep profile controlling transfer drive system, function admirable is harmless to reservoir, green non-pollution it is new Organic zirconium crosslinker and preparation method thereof, greatly improves oil recovery factor.The prior art is solved to stratum bad adaptability, uses clear water Prepare, consume water resource；And underground water and reservoir are seriously endangered, it is unfavorable for environmental protection problem.
The present invention is to realize above-mentioned purpose by the following technical solutions
A kind of New Organo-Zirconium crosslinking agent for depth profile control transfer drive and preparation method thereof, it is characterised in that：This is new Organic zirconium crosslinker is made of the raw material of following weight parts：
Eight 2~5 parts of zirconium oxychlorides of hydration；
1~3 part of citric acid；
2~5 parts of sodium thiosulfate；
7~10 parts of ethylenediamine；
0.03~0.05 part of potassium chloride；
0.5~1 part of ammonium nitrate；
50~60 parts of deionized water；
The preparation process of the New Organo-Zirconium crosslinking agent is as follows：
（1）Zirconium oxychloride, citric acid and sodium thiosulfate are hydrated by eight at room temperature and deionized water is prepared, with 20-50 Rev/min it is stirred to obtain mixed transparent solution A；
（2）Potassium chloride is added in solution A, is stirred evenly under 20 revs/min, obtains solution B；
（3）Above-mentioned solution B is poured into stir under 100-200 revs/min in three-necked flask, and is heated under 80 DEG C of water-baths, React 20min；
（4）After 20min, ethylenediamine is slowly added to, reaction time 5h, obtains semi-finished product solution C；
（5）Stop addition ammonium nitrate after reaction filters to mix with semi-finished product solution C, that is, obtain New Organo-Zirconium crosslinking Agent；
（6）In above-mentioned reaction, in the mixed transparent solution A eight hydration zirconium oxychlorides, citric acid, sodium thiosulfate and Deionized water in mass ratio 5:1.2:3:50—6:1.44:6.27:60 prepare；The potassium chloride concentration of addition is 3-5wt%；Second two Amine is 1 according to weight ratio with solution B:10—1:7 ratio addition；Ammonium nitrate is 1 according to mass ratio with semi-finished product solution C: 70—1:60 ratio addition；Above steps carries out under normal pressure.
The beneficial effect of the present invention compared with prior art is
The preparation process of the New Organo-Zirconium crosslinking agent and preparation method thereof is simple, easy to operate, can save a large amount of personnel And operating expenses；The New Organo-Zirconium crosslinking agent can directly with salinity 40000mgL-1Below, calcium-magnesium content for 0- 600mg·L-1Various sewage with poly-；The cross-linked polymer formed using the New Organo-Zirconium crosslinking agent and aqueous solutions of polymers System can effectively control viscosity, the delayed cross-linking time, strong in 12-70h, plastic suitable for 35 DEG C-70 DEG C oil reservoirs, gelation time Degree can reach E-G；The New Organo-Zirconium crosslinking agent is harmless to reservoir, and green pollution-free, greatly improves oil recovering Rate.The prior art is solved perfectly to stratum bad adaptability, is prepared with clear water, consumes water resource；And seriously endanger underground water And reservoir, the problem of being unfavorable for environmental protection.
Embodiment
The New Organo-Zirconium crosslinking agent can be described as citric acid ethylenediamine organic zirconium crosslinker again.Ethylenediamine is as organic ligand With the Zr in inorganic zirconium salts4+Synthesize organic zirconium crosslinker, while add citric acid can be hindered by chemical action it is hydrolyzed The progress of journey, and the O in-COOH therein has lone pair electrons also can be with the metal zirconium ion unoccupied orbital phase in inorganic zirconium salts Combine to form complex so that product has chelating ring structure, forms a kind of stable comple of co-ordinate covalent bond.It is thio Sodium sulphate can be such that the product of synthesis more stablizes as a kind of stabilizer.Potassium chloride and ammonium nitrate are added as protective agent, can It is poly- to match somebody with somebody for different quality.Gelation reaction is realized by ligand exchange, hinders what is hydrolyzed since citric acid has during this Effect, the rock-steady structure of chelate ring, causes metal Zr4+Dissociate the speed come from complex compound to substantially reduce, so as to fulfill prolonging Retarded crosslinking.
Embodiment 1
Precise raw material：5.36 kilogram of eight hydration zirconium oxychloride, 1.44 kilograms of citric acids, 6.27 kilograms of thiosulfuric acids Sodium, 50 kilograms of deionized waters, 6.72 kilograms of ethylenediamines, 0.03 kilogram of potassium chloride.
Preparation method：Zirconium oxychloride, citric acid and sodium thiosulfate is hydrated by eight at room temperature to prepare with deionized water, with 20-50 revs/min are stirred to obtain mixed transparent solution A；Potassium chloride is added in solution A again, is stirred under 20 revs/min Uniformly, solution B is obtained；Above-mentioned solution B is poured into three-necked flask with stirring under 100-200 revs/min and under 80 DEG C of water-baths plus Heat, reacts 20min；After 20min, ethylenediamine is slowly added to, reaction time 5h, obtains semi-finished product solution C；Stop reaction filtering To product.
Embodiment 2
Precise raw material：5.36 kilogram of eight hydration zirconium oxychloride, 1.44 kilograms of citric acids, 6.27 kilograms of thiosulfuric acids Sodium, 50 kilograms of deionized waters, 7.84 kilograms of ethylenediamines, 0.04 kilogram of potassium chloride.
Preparation method：Zirconium oxychloride, citric acid and sodium thiosulfate is hydrated by eight at room temperature to prepare with deionized water, with 20-50 revs/min are stirred to obtain mixed transparent solution A；Potassium chloride is added in solution A again, is stirred under 20 revs/min Uniformly, solution B is obtained；Above-mentioned solution B is poured into three-necked flask with stirring under 100-200 revs/min and under 80 DEG C of water-baths plus Heat, reacts 20min；After 20min, ethylenediamine is slowly added to, reaction time 5h, obtains semi-finished product solution C；Stop reaction filtering To product.
Embodiment 3
Precise raw material：5.36 kilogram of eight hydration zirconium oxychloride, 1.3 kilograms of citric acids, 6.27 kilograms of thiosulfuric acids Sodium, 50 kilograms of deionized waters, 7.84 kilograms of ethylenediamines, 0.04 kilogram of potassium chloride.
Preparation method：Zirconium oxychloride, citric acid and sodium thiosulfate is hydrated by eight at room temperature to prepare with deionized water, with 20-50 revs/min are stirred to obtain mixed transparent solution A；Potassium chloride is added in solution A again, is stirred under 20 revs/min Uniformly, solution B is obtained；Above-mentioned solution B is poured into three-necked flask with stirring under 100-200 revs/min and under 80 DEG C of water-baths plus Heat, reacts 20min；After 20min, ethylenediamine is slowly added to, reaction time 5h, obtains semi-finished product solution C；Stop reaction filtering To product.
Embodiment 4
Precise raw material：5.36 kilogram of eight hydration zirconium oxychloride, 1.2 kilograms of citric acids, 4 kilograms of sodium thiosulfate, 50 Kilogram deionized water, 7.84 kilograms of ethylenediamines, 0.05 kilogram of potassium chloride.
Preparation method：Zirconium oxychloride, citric acid and sodium thiosulfate is hydrated by eight at room temperature to prepare with deionized water, with 20-50 revs/min are stirred to obtain mixed transparent solution A；Potassium chloride is added in solution A again, is stirred under 20 revs/min Uniformly, solution B is obtained；Above-mentioned solution B is poured into three-necked flask with stirring under 100-200 revs/min and under 80 DEG C of water-baths plus Heat, reacts 20min；After 20min, ethylenediamine is slowly added to, reaction time 5h, obtains semi-finished product solution C；Stop reaction filtering To product.
Embodiment 5
Precise raw material：5.36 kilogram of eight hydration zirconium oxychloride, 1.2 kilograms of citric acids, 3 kilograms of sodium thiosulfate, 50 Kilogram deionized water, 7.84 kilograms of ethylenediamines, 0.04 kilogram of potassium chloride.
Preparation method：Zirconium oxychloride, citric acid and sodium thiosulfate is hydrated by eight at room temperature to prepare with deionized water, with 20-50 revs/min are stirred to obtain mixed transparent solution A；Potassium chloride is added in solution A again, is stirred under 20 revs/min Uniformly, solution B is obtained；Above-mentioned solution B is poured into three-necked flask with stirring under 100-200 revs/min and under 80 DEG C of water-baths plus Heat, reacts 20min；After 20min, ethylenediamine is slowly added to, reaction time 5h, obtains semi-finished product solution C；Stop reaction filtering To product.
Embodiment 6
Precise raw material：5.36 kilogram of eight hydration zirconium oxychloride, 1.2 kilograms of citric acids, 3 kilograms of sodium thiosulfate, 50 Kilogram deionized water, 7.84 kilograms of ethylenediamines, 0.04 kilogram of potassium chloride, 0.7 kilogram of ammonium nitrate.
Preparation method：Zirconium oxychloride, citric acid and sodium thiosulfate is hydrated by eight at room temperature to prepare with deionized water, with 20-50 revs/min are stirred to obtain mixed transparent solution A；Potassium chloride is added in solution A again, is stirred under 20 revs/min Uniformly, solution B is obtained；Above-mentioned solution B is poured into three-necked flask with stirring under 100-200 revs/min and under 80 DEG C of water-baths plus Heat, reacts 20min；After 20min, ethylenediamine is slowly added to, reaction time 5h, obtains semi-finished product solution C；Stop reaction filtering Afterwards, ammonium nitrate is added to be mixed with obtaining product.
Embodiment 7
Organic zirconium crosslinker in one of embodiment of the present invention 1~6 is mixed with the aqueous solution of polymer poly acrylamide The polymeric cross-linked systems of formation are used for Water in Water Shutoff in Oil Field profile control or transfer drive；Polymer concentration is in the cross-linking polymer system 0.1wt%, crosslinker concentration 0.38wt%.Gelation time is 42-70h at 35 DEG C, and gelling strength reaches G grades.With polymer Polyacrylamide is salinity 5000mgL with poly- water quality-1—20000mg·L-1。
Embodiment 8
Organic zirconium crosslinker in one of embodiment of the present invention 1~6 is mixed with the aqueous solution of polymer poly acrylamide The polymeric cross-linked systems of formation are used for Water in Water Shutoff in Oil Field profile control or transfer drive；Polymer concentration is in the cross-linking polymer system 0.15wt%, crosslinker concentration 0.4wt%.Gelation time is 22-50h at 50 DEG C, and gelling strength reaches F grades.With polymer Polyacrylamide is salinity 5000mgL with poly- water quality-1—20000mg·L-1, calcium ions and magnesium ions content 100mgL-1— 200mg·L-1。
Embodiment 9
Organic zirconium crosslinker in one of embodiment of the present invention 1~6 is mixed with the aqueous solution of polymer poly acrylamide The polymeric cross-linked systems of formation are used for Water in Water Shutoff in Oil Field profile control or transfer drive；Polymer concentration is in the cross-linking polymer system 0.15wt%, crosslinker concentration 0.5wt%.Gelation time is 12-20h at 70 DEG C, and gelling strength reaches E grades.With polymer Polyacrylamide is salinity 10000mgL with poly- water quality-1—30000mg·L-1, calcium ions and magnesium ions content 200mgL-1— 400mg·L-1。
Embodiment 10
Organic zirconium crosslinker in one of embodiment of the present invention 1~6 is mixed with the aqueous solution of polymer poly acrylamide The polymeric cross-linked systems of formation are used for Water in Water Shutoff in Oil Field profile control or transfer drive；Polymer concentration is in the cross-linking polymer system 0.2wt%, crosslinker concentration 0.7wt%, gelation time is 15-50h at 50 DEG C, and gelling strength reaches E grades.With polymer Polyacrylamide is salinity 10000mgL with poly- sewage quality-1—40000mg·L-1, calcium ions and magnesium ions content 200mg L-1—600mg·L-1。
Embodiment 11
The polymeric cross-linked systems that organic zirconium crosslinker prepared by the embodiment of the present invention 3 is formed with polyacrylamide are in Xinjiang 10 well groups of block such as red 18 wellblock in oil field, red 29 wellblock, 21 wellblock of heath, 81 wellblocks have carried out deep profile controlling field test, Injected respectively by slug：Polymer concentration 0.15wt%, crosslinker concentration 0.5wt%；Polymer concentration 0.15wt%, Crosslinker concentration is 0.4wt%；Polymer concentration 0.1wt%, crosslinker concentration 0.38wt%.By organic zirconium of the present invention The cross-linking polymer system that crosslinking agent is prepared is continuously injected into 100 days, and average individual-well injection rate is 5870m3, add up injection rate 58700m3, closing well 5~7 days after injection, result of the test shows：The crosslinking prepared using organic zirconium crosslinker of the present invention In polymeric system injection process, well head pressure is stablized；After the cross-linking polymer system is injected into stratum, injection well pressure is obvious Rise, Hall Curve slope steep, average individual well pressure rises 2.5MPa, and high permeability formation has obtained effective closure, corresponding oil well contains Underwater drop, day oil level rise, and the 6 months statistical average individual well groups that take effect have a net increase of 1000 tons of oil, and recovery ratio improves 0.62%.Mesh The preceding corresponding oil well effect of tracking is still notable.
Embodiment 12：
The New Organo-Zirconium crosslinking agent and aqueous solutions of polymers are prepared to form cross-linking polymer system, its preparation method is such as Under：
Step 1：Take and match somebody with somebody polywater sample, be placed on electric mixer, adjust agitator speed after opening power supply, make liquid level vortex As deep as 1cm or so, weigh polyacrylamide and be slowly added in water, 2-3h of stirring to uniform, standing 40-60min of curing, The polyacrylamide solution that mass fraction is 0.15wt% -0.3wt% is made.
Step 2：Above-mentioned New Organo-Zirconium crosslinking agent is taken in proportion, and stirring is added to step 1）Obtained 0.15wt%- In 0.3wt% polyacrylamide solutions, it is uniformly mixed up to cross-linking polymer system.
The cross-linking polymer system that the New Organo-Zirconium crosslinking agent is formed with aqueous solutions of polymers is used for Water in Water Shutoff in Oil Field profile control Or transfer drive；The polymer is the HENGFLOC 50820 of the permanent poly- Chemical Group responsibility Co., Ltd in Beijing, the cross-linked polymeric Polymer concentration is 0.15wt% -0.3wt% in objects system, which is 0.5wt% -0.7wt%, energy Enough and salinity 40000mgL-1Below, 0-600mgL of calcium-magnesium content-1Various sewage are with poly-, Applicable temperature 35 DEG C -70 DEG C oil reservoir, gelation time is 12-70h, and gelling strength reaches E-G grades.
The above is the embodiment of the invention, and the example above illustrates not form the substantive content of the present invention Limitation, person of an ordinary skill in the technical field can repair above-mentioned embodiment after this specification has been read Change or deform, without departing from the spirit and scope of the invention.

Claims (1)

  1. A kind of 1. organic zirconium crosslinker, it is characterised in that：The organic zirconium crosslinker is made of the raw material of following weight parts：
    The preparation process of the organic zirconium crosslinker is as follows：
    (1) zirconium oxychloride, citric acid and sodium thiosulfate are hydrated by eight at room temperature and deionized water is prepared, with 20-50 revs/min It is stirred to obtain mixed transparent solution A；
    (2) potassium chloride is added in solution A, is stirred evenly under 20 revs/min, obtain solution B；
    (3) above-mentioned solution B is poured into stir under 100-200 revs/min in three-necked flask, and is heated under 80 DEG C of water-baths, reacted 20min；
    (4) after 20min, ethylenediamine is slowly added to, reaction time 5h, obtains semi-finished product solution C；
    (5) stop addition ammonium nitrate after reaction filters to mix with semi-finished product solution C, that is, obtain the organic zirconium crosslinker；
    (6) in above-mentioned reaction, in the mixed transparent solution A eight hydration zirconium oxychlorides, citric acid, sodium thiosulfate and go from Sub- water in mass ratio 5:1.2:3:50—6:1.44:6.27:60 prepare；The potassium chloride concentration of addition is 3-5wt%；Ethylenediamine With solution B according to weight ratio be 1:10—1:7 ratio addition；Ammonium nitrate is 1 according to mass ratio with semi-finished product solution C:70— 1:60 ratio addition；Above steps carries out under normal pressure.
CN201510383977.0A 2015-07-03 2015-07-03 A kind of organic zirconium crosslinker and preparation method thereof Active CN105018057B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510383977.0A CN105018057B (en) 2015-07-03 2015-07-03 A kind of organic zirconium crosslinker and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510383977.0A CN105018057B (en) 2015-07-03 2015-07-03 A kind of organic zirconium crosslinker and preparation method thereof

Publications (2)

Publication Number Publication Date
CN105018057A CN105018057A (en) 2015-11-04
CN105018057B true CN105018057B (en) 2018-04-13

Family

ID=54408368

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510383977.0A Active CN105018057B (en) 2015-07-03 2015-07-03 A kind of organic zirconium crosslinker and preparation method thereof

Country Status (1)

Country Link
CN (1) CN105018057B (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007095367A2 (en) * 2006-02-14 2007-08-23 E. I. Du Pont De Nemours And Company Cross-linking composition and method of use
CN101633840A (en) * 2009-07-08 2010-01-27 中国石油天然气股份有限公司 Hydrophobic group graft modified guar gum fracturing fluid gel
CN102206484A (en) * 2011-04-07 2011-10-05 中国石油天然气股份有限公司 Acidic hydrophobic association compound fracturing fluid
CN103484097A (en) * 2012-06-11 2014-01-01 中国石油化工股份有限公司 Ground crosslinked acid crosslinking agent and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007095367A2 (en) * 2006-02-14 2007-08-23 E. I. Du Pont De Nemours And Company Cross-linking composition and method of use
CN101633840A (en) * 2009-07-08 2010-01-27 中国石油天然气股份有限公司 Hydrophobic group graft modified guar gum fracturing fluid gel
CN102206484A (en) * 2011-04-07 2011-10-05 中国石油天然气股份有限公司 Acidic hydrophobic association compound fracturing fluid
CN103484097A (en) * 2012-06-11 2014-01-01 中国石油化工股份有限公司 Ground crosslinked acid crosslinking agent and preparation method thereof

Also Published As

Publication number Publication date
CN105018057A (en) 2015-11-04

Similar Documents

Publication Publication Date Title
CN105368423B (en) One kind is recovered the oil and uses Chrome-free compound resin gel-like profile control agent and preparation method and purposes
CN101928366B (en) Method for preparing viscosity breaking agent for drilling fluid
CN104926167B (en) Method for consolidating waste incineration fly ash heavy metal through microorganism cement mineralization
CN109735315B (en) Environment-friendly delayed crosslinking profile control agent for oil extraction and preparation method and application thereof
CN104192918B (en) Sewage treatment agent and preparation method and application thereof
CN105199706A (en) Organic zirconium crosslinking agent applicable to polymer fracturing fluid system and preparation method of organic zirconium crosslinking agent
CN104927816A (en) Environmental-friendly organic profile control agent and preparation method and use thereof
CN110256275A (en) A kind of preparation method of salt-resistant type amphoteric ion hydrophobic associated polymer and the application on fracturing fluid
CN102391436A (en) High temperature resistant and compound salt resistant viscosity reduction agent for drilling fluid and preparation method thereof
CN106433590A (en) Casing damage leakage well high-efficiency phenolic resin water plugging agent and application thereof
CN104357026A (en) Treating agent for zwitter-ion inorganic-organic monomer polymer drilling fluid and preparation method of treating agent
CN106589257A (en) Preparation method of lignin grafted and copolymerized polymer flocculation type profile modifying/water plugging agent
CN102503295A (en) Non-sintered brick prepared from river and lake silt and preparation process thereof
CN106867498B (en) Fracturing fluid prepared from acidizing fracturing flow-back fluid
CN105018057B (en) A kind of organic zirconium crosslinker and preparation method thereof
CN102993356A (en) Preparation process of leak protection plugging agent along with drilling based on control of dosage of filling agent
CN112778990B (en) Sewage mixing temporary plugging agent for oilfield water injection well and preparation method thereof
CN104611549A (en) Method of using ferric sulfate solution to perform acid leaching on laterite-nickel ore for extracting nickel and cobalt
CN109294540B (en) High-salinity-resistant profile control agent for deep oil reservoir and preparation method thereof
CN106517852B (en) A kind of modified aluminate cement retarder and preparation method thereof of the pre- aluminum ions AMPS copolymer of chelating and borate compounding
CN106477997B (en) A kind of method using emulsified asphalt to solidify saline soil
CN103183406A (en) Preparation method of high-concentration PAM-aluminum, zinc iron composite water treatment agent
CN104293330B (en) A kind of high temperature LOW PERMEABILITY RESERVOIR CO2Gas drive envelope alters agent
CN106634910A (en) Profile control agent and preparation method thereof
CN109679641B (en) Fracturing fluid prepared from high-salinity salt lake water and preparation method thereof

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