CN105018057A - Novel organic zirconium cross-linking agent and preparation method thereof - Google Patents
Novel organic zirconium cross-linking agent and preparation method thereof Download PDFInfo
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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
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- 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
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- 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
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Abstract
The invention relates to a preparation method of a novel organic zirconium cross-linking agent used for deep profile controlling and flooding as well as an application, which belongs to the technical field of oil field chemical increasing crude oil recovery efficiency. The organic zirconium cross-linking agent is synthesized by taking zirconylchloride octahydrate, citric acid and ethene diamine as basic raw materials, crosslinking time and viscosity can be delayed with effective control, various sewage with mineralization degree being 40000mg.L<-1> and calcium and magnesium ions content being 0-600mg.L<-1> can be cooperated, and a formed crosslinking polymer system is suitable for oil reservoir at temperature of 35-70 DEG C. In a deep profile controlling and flooding system, sewage can be used for substituting clear water, and can be a green no-pollution cross-linking agent with excellent performance and no harm on a reservoir layer, and the crude oil recovery efficiency can be increased. Problems of poor stratum adaptability, poor salt resistance, only compatibility with clear water, heavy pollution and large damage on the reservoir layer of a traditional cross-linking agent can be solved. The on-site test result shows that the cross-linking agent system enables compatibility with on-site sewage, has good gelling effect, and is benefit for environmental protection.
Description
Technical field
The present invention relates to a kind of New Organo-Zirconium linking agent and preparation method thereof, belong to chemical flooding and improve oil recovery factor technical field.
Background technology
Oil and water well water plugging and profile controlling is heterogeneous reservoir water and oil control, the important technical improving waterflood efficiency.China's oil field majority enters High water cut or after the ultra-high water-containing productive life, because water filling interval difference is large, most permeable zone water-retaining capacity is strong, form water stream channel, non available water circulates, and low permeability layer is noted and do not intake, in order to improve the swept volume that injects water and inject oil-water displacement efficiency, adopt amendment to carry out shutoff most permeable zone, finally reach the object of balanced intake profile.Because the water plugging and profiling technology of routine can not meet field produces demand, the Study and appliance etc. of deep profile correction technology achieves many new developments, obtains unusual effect improving in high water-cut reservoir water flooding effectiveness.
The linking agent that current domestic water plugging and profile controlling adopts mainly comprises: the systems such as organoaluminum linking agent, phenolic crosslinkers, organic chrome cross linker.But because the ground adaptability of organoaluminum and phenolic crosslinkers is poor, salt resistance is poor, be only suitable for and clear water compatibility; And current most popular organic chrome cross linker, adaptability is very strong, temperature and the pH condition of relative broad range can be tolerated, the requirement of different crosslinked (plastic) time can be adapted to, but hexavalent chromium has serious harm to underground water and reservoir, even if use trivalent chromium to replace sexavalent chrome, the potential hazard to reservoir still oxidizedly can be caused.CN86108877 proposes a kind of preparation method of Zirconium gel water sealing agent, and linking agent is wherein inorganic zirconium compound zirconium oxychloride, zirconium tetrachloride, zirconium sulfate, the compositions such as zirconium nitrate, and the system closing time that this linking agent is formed is short, is unfavorable for on-site construction operations; Virtual viscosity is low, is difficult to meet Contraction in Site requirement.CN 102559159 A has invented a kind of high-temperature resistant phenolic resin weak gel profile control plugging agent, and linking agent is wherein resistant to elevated temperatures resol, although resisting temperature can reach more than 90 DEG C, it is higher to join poly-required water quality requirement, and total mineralization is not higher than 8500mgL
-1.CN 103937474 A provides a kind of environment protection type high-strength profile-controlling and plugging agent and preparation method thereof, and linking agent is wherein polymine, and cost is high, complicated process of preparation, and popularization rate is low, inapplicable.CN 101613456 B proposes a kind of coating type crosslinker and its preparation method and application, this linking agent is with Toluene-2,4-diisocyanate, 4-vulcabond is oil-soluble monomer, whiteruss is oil phase, quadrol is water-soluble monomer, and with the chromium of organic acid aqueous solution for core, octyl phenol polyoxyethylene (10) ether and sorbitan monostearate are that emulsifying agent obtains, chromium of organic acid poisonous and harmful wherein, not only injures reservoir also likely polluted underground water source.
Along with oil field deep profile control scale constantly expands, clear water resource day needed for polymer solution preparation is becoming tight, the further attention of country to environmental protection, and meanwhile, the large amount of sewage separated in oil well produced liquid particularly high saline sewage is difficult to process.For making oil field height salt sewage obtain recycle, researching and developing a kind of excellent property and harmless to reservoir, clear water can be replaced to prepare deep profile controlling transfer drive cross linker system with sewage and there is great economy and social effect.
Summary of the invention
The object of the invention is to, a kind of effective control realizing delay cross linking time and viscosity is provided, and available sewage replaces clear water preparation, be applicable to deep profile controlling transfer drive system, excellent property, harmless to reservoir, New Organo-Zirconium linking agent of green non-pollution and preparation method thereof, improves oil recovery factor greatly.Solve prior art formation bad adaptability, with clear water preparation, consume water resources; And serious harm underground water and reservoir, be unfavorable for environmental protection problem.
The present invention realizes above-mentioned purpose by the following technical solutions
A kind of New Organo-Zirconium linking agent for depth profile control transfer drive and preparation method thereof, is characterized in that: this New Organo-Zirconium linking agent is made up of the raw material of following weight parts:
Eight hydration zirconium oxychlorides 2 ~ 5 parts;
Citric acid 1 ~ 3 part;
2 ~ 5 parts, Sulfothiorine;
Quadrol 7 ~ 10 parts;
0.03 ~ 0.05 part, Repone K;
0.5 ~ 1 part, ammonium nitrate;
Deionized water 50 ~ 60 parts;
The preparation process of this New Organo-Zirconium linking agent is as follows:
(1) under room temperature, eight hydration zirconium oxychlorides, citric acid and Sulfothiorine and deionized water are prepared, be uniformly mixed with 20-50 revs/min and obtain mixed transparent solution A;
(2) Repone K is joined in solution A, stir under 20 revs/min, obtain solution B;
(3) above-mentioned solution B is poured in there-necked flask and stir under 100-200 revs/min, and heat under 80 DEG C of water-baths, reaction 20min;
(4) after 20min, slowly add quadrol, reaction times 5h, obtain semi-finished product solution C;
(5) add ammonium nitrate after stopped reaction suction filtration to mix with semi-finished product solution C, namely obtain this New Organo-Zirconium linking agent;
(6) in above-mentioned reaction, the 5:1.2:3:50-6:1.44:6.27:60 preparation in mass ratio of eight hydration zirconium oxychlorides, citric acid, Sulfothiorine and deionized water in described mixed transparent solution A; The potassium chloride concentration added is 3-5wt%; Quadrol and solution B are added according to the ratio that weight ratio is 1:10-1:7; Ammonium nitrate and semi-finished product solution C add according to the ratio that mass ratio is 1:70-1:60; Above steps is carried out all at ambient pressure.
The present invention's beneficial effect is compared with prior art
The preparation technology of this New Organo-Zirconium linking agent and preparation method thereof is simple, easy to operate, can save a large amount of personnel and executive cost; This New Organo-Zirconium linking agent can directly and salinity 40000mgL
-1below, calcium-magnesium content is 0-600mgL
-1various sewage join poly-; The cross-linking polymer system adopting this New Organo-Zirconium linking agent and aqueous solutions of polymers to be formed effectively can control viscosity, the delayed cross-linking time, and be applicable to 35 DEG C of-70 DEG C of oil reservoirs, gelation time is at 12-70h, and gelling strength all can reach E-G; This New Organo-Zirconium linking agent is harmless to reservoir, and environmental protection is pollution-free, greatly improves oil recovery factor.Solve prior art formation bad adaptability perfectly, with clear water preparation, consume water resources; And serious harm underground water and reservoir, be unfavorable for the problem of environment protection.
Embodiment
This New Organo-Zirconium linking agent can be described as again citric acid quadrol organic zirconium crosslinker.Quadrol is as the Zr in organic ligand and inorganic zirconium salts
4+synthesis organic zirconium crosslinker, the citric acid simultaneously added by chemical action to hinder the carrying out of hydrolytic process, and the O in-COOH wherein has lone-pair electron also can to combine with the metal zirconium ion unoccupied orbital in inorganic zirconium salts formation coordination compound, make product have chelate ring structure, form a kind of stable comple of coordinate-covalent bond.Sulfothiorine can make the product of synthesis more stable as a kind of stablizer.Repone K and ammonium nitrate add as protective material, can join poly-for different quality.Realize gelation reaction by ligand exchange, because citric acid has the effect hindering hydrolysis in this process, the rock steady structure of chelate ring, causes metallic Z r
4+the speed of dissociating out from complex compound reduces greatly, thus realizes delayed cross-linking.
Embodiment 1
Precise raw material: 5.36 kilogram of eight hydration zirconium oxychloride, 1.44 kilograms of citric acids, 6.27 kilograms of Sulfothiorine, 50 kilograms of deionized waters, 6.72 kilograms of quadrols, 0.03 kilogram of Repone K.
Preparation method: by eight hydration zirconium oxychlorides under room temperature, citric acid and Sulfothiorine and deionized water are prepared, and be uniformly mixed obtain mixed transparent solution A with 20-50 revs/min; Again Repone K is joined in solution A, stir under 20 revs/min, obtain solution B; Above-mentioned solution B is poured into stir under 100-200 revs/min and to heat under 80 DEG C of water-baths in there-necked flask, reaction 20min; After 20min, slowly add quadrol, reaction times 5h, obtain semi-finished product solution C; Stopped reaction suction filtration obtains product.
Embodiment 2
Precise raw material: 5.36 kilogram of eight hydration zirconium oxychloride, 1.44 kilograms of citric acids, 6.27 kilograms of Sulfothiorine, 50 kilograms of deionized waters, 7.84 kilograms of quadrols, 0.04 kilogram of Repone K.
Preparation method: by eight hydration zirconium oxychlorides under room temperature, citric acid and Sulfothiorine and deionized water are prepared, and be uniformly mixed obtain mixed transparent solution A with 20-50 revs/min; Again Repone K is joined in solution A, stir under 20 revs/min, obtain solution B; Above-mentioned solution B is poured into stir under 100-200 revs/min and to heat under 80 DEG C of water-baths in there-necked flask, reaction 20min; After 20min, slowly add quadrol, reaction times 5h, obtain semi-finished product solution C; Stopped reaction suction filtration obtains product.
Embodiment 3
Precise raw material: 5.36 kilogram of eight hydration zirconium oxychloride, 1.3 kilograms of citric acids, 6.27 kilograms of Sulfothiorine, 50 kilograms of deionized waters, 7.84 kilograms of quadrols, 0.04 kilogram of Repone K.
Preparation method: by eight hydration zirconium oxychlorides under room temperature, citric acid and Sulfothiorine and deionized water are prepared, and be uniformly mixed obtain mixed transparent solution A with 20-50 revs/min; Again Repone K is joined in solution A, stir under 20 revs/min, obtain solution B; Above-mentioned solution B is poured into stir under 100-200 revs/min and to heat under 80 DEG C of water-baths in there-necked flask, reaction 20min; After 20min, slowly add quadrol, reaction times 5h, obtain semi-finished product solution C; Stopped reaction suction filtration obtains product.
Embodiment 4
Precise raw material: 5.36 kilogram of eight hydration zirconium oxychloride, 1.2 kilograms of citric acids, 4 kilograms of Sulfothiorine, 50 kilograms of deionized waters, 7.84 kilograms of quadrols, 0.05 kilogram of Repone K.
Preparation method: by eight hydration zirconium oxychlorides under room temperature, citric acid and Sulfothiorine and deionized water are prepared, and be uniformly mixed obtain mixed transparent solution A with 20-50 revs/min; Again Repone K is joined in solution A, stir under 20 revs/min, obtain solution B; Above-mentioned solution B is poured into stir under 100-200 revs/min and to heat under 80 DEG C of water-baths in there-necked flask, reaction 20min; After 20min, slowly add quadrol, reaction times 5h, obtain semi-finished product solution C; Stopped reaction suction filtration obtains product.
Embodiment 5
Precise raw material: 5.36 kilogram of eight hydration zirconium oxychloride, 1.2 kilograms of citric acids, 3 kilograms of Sulfothiorine, 50 kilograms of deionized waters, 7.84 kilograms of quadrols, 0.04 kilogram of Repone K.
Preparation method: by eight hydration zirconium oxychlorides under room temperature, citric acid and Sulfothiorine and deionized water are prepared, and be uniformly mixed obtain mixed transparent solution A with 20-50 revs/min; Again Repone K is joined in solution A, stir under 20 revs/min, obtain solution B; Above-mentioned solution B is poured into stir under 100-200 revs/min and to heat under 80 DEG C of water-baths in there-necked flask, reaction 20min; After 20min, slowly add quadrol, reaction times 5h, obtain semi-finished product solution C; Stopped reaction suction filtration obtains product.
Embodiment 6
Precise raw material: 5.36 kilogram of eight hydration zirconium oxychloride, 1.2 kilograms of citric acids, 3 kilograms of Sulfothiorine, 50 kilograms of deionized waters, 7.84 kilograms of quadrols, 0.04 kilogram of Repone K, 0.7 kilogram of ammonium nitrate.
Preparation method: by eight hydration zirconium oxychlorides under room temperature, citric acid and Sulfothiorine and deionized water are prepared, and be uniformly mixed obtain mixed transparent solution A with 20-50 revs/min; Again Repone K is joined in solution A, stir under 20 revs/min, obtain solution B; Above-mentioned solution B is poured into stir under 100-200 revs/min and to heat under 80 DEG C of water-baths in there-necked flask, reaction 20min; After 20min, slowly add quadrol, reaction times 5h, obtain semi-finished product solution C; After stopped reaction suction filtration, add ammonium nitrate and be mixed to get product with it.
Embodiment 7
The polymeric cross-linked systems that the aqueous solution of the organic zirconium crosslinker in one of embodiment of the present invention 1 ~ 6 and polymer poly acrylamide is formed is used for Water in Water Shutoff in Oil Field profile control or transfer drive; In described cross-linking polymer system, polymer concentration is 0.1wt%, and crosslinker concentration is 0.38wt%.At 35 DEG C, gelation time is 42-70h, and gelling strength reaches G level.Joining poly-water quality with polymer poly acrylamide is salinity 5000mgL
-1-20000mgL
-1.
Embodiment 8
The polymeric cross-linked systems that the aqueous solution of the organic zirconium crosslinker in one of embodiment of the present invention 1 ~ 6 and polymer poly acrylamide is formed is used for Water in Water Shutoff in Oil Field profile control or transfer drive; In described cross-linking polymer system, polymer concentration is 0.15wt%, and crosslinker concentration is 0.4wt%.At 50 DEG C, gelation time is 22-50h, and gelling strength reaches F level.Joining poly-water quality with polymer poly acrylamide is salinity 5000mgL
-1-20000mgL
-1, calcium ions and magnesium ions content 100mgL
-1-200mgL
-1.
Embodiment 9
The polymeric cross-linked systems that the aqueous solution of the organic zirconium crosslinker in one of embodiment of the present invention 1 ~ 6 and polymer poly acrylamide is formed is used for Water in Water Shutoff in Oil Field profile control or transfer drive; In described cross-linking polymer system, polymer concentration is 0.15wt%, and crosslinker concentration is 0.5wt%.At 70 DEG C, gelation time is 12-20h, and gelling strength reaches E level.Joining poly-water quality with polymer poly acrylamide is salinity 10000mgL
-1-30000mgL
-1, calcium ions and magnesium ions content 200mgL
-1-400mgL
-1.
Embodiment 10
The polymeric cross-linked systems that the aqueous solution of the organic zirconium crosslinker in one of embodiment of the present invention 1 ~ 6 and polymer poly acrylamide is formed is used for Water in Water Shutoff in Oil Field profile control or transfer drive; In described cross-linking polymer system, polymer concentration is 0.2wt%, and crosslinker concentration is 0.7wt%, and at 50 DEG C, gelation time is 15-50h, and gelling strength reaches E level.Joining poly-sewage quality with polymer poly acrylamide is salinity 10000mgL
-1-40000mgL
-1, calcium ions and magnesium ions content 200mgL
-1-600mgL
-1.
Embodiment 11
Organic zirconium crosslinker prepared by the embodiment of the present invention 3 and the polymeric cross-linked systems that polyacrylamide is formed have carried out deep profile controlling test in place at block 10 well groups such as red 18 wellblocks of Xinjiang Oilfield, red 29 wellblocks, heath 21 wellblock, 81 wellblocks, press slug respectively to inject: polymer concentration 0.15wt%, crosslinker concentration is 0.5wt%; Polymer concentration 0.15wt%, crosslinker concentration is 0.4wt%; Polymer concentration 0.1wt%, crosslinker concentration is 0.38wt%.The cross-linking polymer system of organic zirconium crosslinker preparation of the present invention is injected 100 days continuously, and average individual-well injection rate is 5870m
3, accumulative injection rate 58700m
3, closing well 5 ~ 7 days after injection, test-results shows: in the cross-linking polymer system injection process using organic zirconium crosslinker of the present invention to prepare, and wellhead pressure is stablized; After this cross-linking polymer system is injected into stratum, injection well pressure obviously rises, Hall Curve slope steep, average individual well pressure increase 2.5MPa, high permeability formation obtains effective shutoff, corresponding well water declines, day oil level rising, 6 months statistical average individual well groups that take effect have a net increase of oil 1000 tons, and recovery ratio improves 0.62%.The corresponding oil well effect of current tracking is still remarkable.
Embodiment 12:
This New Organo-Zirconium linking agent and aqueous solutions of polymers are prepared and form cross-linking polymer system, its preparation method is as follows:
Step 1: get and join polywater sample, be placed on electric mixer, agitator speed is regulated after opening power, liquid level vortex is made deeply to reach about 1cm, take polyacrylamide it is slowly added to the water, stir 2-3h to evenly, leave standstill slaking 40-60min, make the polyacrylamide solution that massfraction is 0.15wt%-0.3wt%.
Step 2: get above-mentioned New Organo-Zirconium linking agent in proportion, stirs and joins in the obtained 0.15wt%-0.3wt% polyacrylamide solution of step 1), mix and obtain cross-linking polymer system.
The cross-linking polymer system that this New Organo-Zirconium linking agent and aqueous solutions of polymers are formed is used for Water in Water Shutoff in Oil Field profile control or transfer drive; Described polymkeric substance is the HENGFLOC 50820 of the poly-Chemical Group responsibility company limited of Beijing perseverance, in described cross-linking polymer system, polymer concentration is 0.15wt%-0.3wt%, this New Organo-Zirconium crosslinker concentration is 0.5wt%-0.7wt%, can with salinity 40000mgL
-1below, calcium-magnesium content 0-600mgL
-1various sewage is joined poly-, and the oil reservoir that Applicable temperature is 35 DEG C-70 DEG C, gelation time is 12-70h, and gelling strength all reaches E-G level.
The above is the embodiment of this invention, above-mentioned illustrating is not construed as limiting flesh and blood of the present invention, person of an ordinary skill in the technical field can make an amendment above-mentioned embodiment or be out of shape after having read this specification sheets, and does not deviate from the spirit and scope of the invention.
Claims (1)
1. New Organo-Zirconium linking agent and preparation method thereof, is characterized in that: this New Organo-Zirconium linking agent is made up of the raw material of following weight parts:
Eight hydration zirconium oxychlorides 2 ~ 5 parts;
Citric acid 1 ~ 3 part;
2 ~ 5 parts, Sulfothiorine;
Quadrol 7 ~ 10 parts;
0.03 ~ 0.05 part, Repone K;
0.5 ~ 1 part, ammonium nitrate;
Deionized water 50 ~ 60 parts;
The preparation process of this New Organo-Zirconium linking agent is as follows:
(1) under room temperature, eight hydration zirconium oxychlorides, citric acid and Sulfothiorine and deionized water are prepared, be uniformly mixed with 20-50 revs/min and obtain mixed transparent solution A;
(2) Repone K is joined in solution A, stir under 20 revs/min, obtain solution B;
(3) above-mentioned solution B is poured in there-necked flask and stir under 100-200 revs/min, and heat under 80 DEG C of water-baths, reaction 20min;
(4) after 20min, slowly add quadrol, reaction times 5h, obtain semi-finished product solution C;
(5) add ammonium nitrate after stopped reaction suction filtration to mix with semi-finished product solution C, namely obtain this New Organo-Zirconium linking agent;
(6) in above-mentioned reaction, the 5:1.2:3:50-6:1.44:6.27:60 preparation in mass ratio of eight hydration zirconium oxychlorides, citric acid, Sulfothiorine and deionized water in described mixed transparent solution A; The potassium chloride concentration added is 3-5wt%; Quadrol and solution B are added according to the ratio that weight ratio is 1:10-1:7; Ammonium nitrate and semi-finished product solution C add according to the ratio that mass ratio is 1:70-1:60; Above steps is carried out all at ambient pressure.
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| 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 |
-
2015
- 2015-07-03 CN CN201510383977.0A patent/CN105018057B/en active Active
Patent Citations (4)
| 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 |
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