CN104560003A - Organic boron zirconium crosslinking agent - Google Patents
Organic boron zirconium crosslinking agent Download PDFInfo
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- CN104560003A CN104560003A CN201410807656.4A CN201410807656A CN104560003A CN 104560003 A CN104560003 A CN 104560003A CN 201410807656 A CN201410807656 A CN 201410807656A CN 104560003 A CN104560003 A CN 104560003A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
- C09K8/685—Compositions based on water or polar solvents containing organic compounds containing cross-linking agents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/80—Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
Abstract
The invention provides an organic boron zirconium crosslinking agent, belonging to the technical field of oilfield fracturing fluids. In order to solve the problem that the existing organic boron zirconium crosslinking agent prepared from the expensive organic zirconium complex enhances the raw material cost of the organic boron zirconium crosslinking agent and lowers the economic benefit, the invention provides an organic boron zirconium crosslinking agent which comprises the following components in parts by weight: 1 part of inorganic zirconium salt, 2-4 parts of water, 3-6 parts of isopropanol, 0.4-1 part of inorganic boride, 4-20 parts of methanol, 2-4 parts of polyalcohol, 1-2 parts of sodium alpha-hydroxycarboxylate, 1-2 parts of triethanolamine and 0.5-1 part of tetrahydroxypropyl ethylenediamine. By using the cheap inorganic zirconium salt as the raw material, the organic boron zirconium crosslinking agent provided by the invention greatly saves the cost, and is beneficial to marketization of the organic boron zirconium crosslinking agent and wide application in the high-temperature-resistant fracturing fluid system.
Description
Technical field
The present invention relates to oil field fracturing fluid technology, be specifically related to a kind of organic boron zirconium cross linking agent for high temperature resistance fracturing fluid system.
Background technology
Oil field compression fracture technique is a major measure of well production increment, generally adopts in each oil field.It utilizes ground high-pressure pump group that fracturing liquid is pumped into stratum with the discharge capacity substantially exceeding formation absorption ability, in formation crack, stratum, improves the flow conductivity of hydrocarbon zone, thus reach volume increase object.
Fracturing liquid experienced by huge differentiation since nineteen forty-seven is first for fracture stimulation.Early stage fracturing liquid is in gasoline, add the viscous fluid being enough to press off and extend crack; Afterwards, along with the increase of well depth and the rising of well temperature, of the fracturing fluid viscosity was had higher requirement, and started to adopt melon glue and derivative base fracturing liquid thereof.
High temperature resistance fracturing fluid system is the gordian technique of fracturing reform high temperature low permeability reservoir.In hot environment, two principal elements affecting fracturing fluid gel network structure stability are the stability of main polymer chain and the stability of crosslinking functionality, and the main component therefore affecting its temperature resistant capability in high temperature resistance fracturing fluid system is viscosifying agent and linking agent.
More for the research of high temperature resistance fracturing fluid system is modifyed guar gum cross-linking system, mainly comprises: organo-metallic cross-linking system, organic boron cross-linking system and organic boron zirconium cross-linking system.Organo-metallic (titanium, zirconium) crosslinked fracturing fluid system has the advantages such as high temperature resistant, delay cross linking, but frozen glue mechano-degradation under high speed shear that this kind of linking agent is formed is serious, the ability of carrying propping agent is poor, and its frozen glue formed does not possess the ability of thoroughly broken glue, degraded in the short period of time, cause serious supporting crack flow conductivity injury; Organic borate cross-linker has the advantage such as good solubility, delay cross linking characteristic, but its temperature tolerance forming frozen glue exists certain limitation; Organic boron zirconium cross linking agent combines the advantage of organo-metallic crosslinker and organic borate cross-linker, effectively can promote the heatproof resistant to shearing ability of fracturing fluid system, cross-linking efficiency is high, consumption is few, also has delay cross linking effect simultaneously.
The organic boron zirconium cross linking agent of US Patent No. 5217632 invention is with alpha-hydroxy carboxylic acid compounds zirconiums such as zirconium lactates for raw material, and after polyol reaction for some time, more obtained after reacting for some time with Inorganic Boron and sodium hydroxide.The organic boron zirconium cross linking agent OBZ-1(of the exploitation such as Shengli Oil Field Zhang Wensheng opens literary composition victory, Qin Liping. fracturing liquid is with organic boron zirconium cross linking agent OBZ-1 [J]. oilfield chemistry, 1996, 13 (3): 210-212.) and organic boron zirconium cross linking agent Guo BA1-21(of the exploitation such as Southwest Petrol University Xin Jun build the spring, Xin Jun, Wang Shibin, Deng. abnormal high temperature guanidine gum fracturing fluid system Developing Application [J]. oil drilling technology, 2010, 32 (3): 64-67.) be under strict control reaction conditions, in organic boron, introduce zirconium complex obtain organic boron zirconium cross linking agent, organic boron colloidal particle is bonded together securely by zirconium ion, form larger colloidal particle, therefore improve cross-linking density and cross-link intensity.Zhongyuan Oil Field Wang Dong etc. has prepared high temperature retarding-type organic boron zirconium cross linking agent CZB-03(Wang Dong, Wang Junying, Liu Hongsheng, Deng. the preparation [J] of aqueous fracturing fluid high temperature retarding-type organic boron zirconium cross linking agent CZB-03. oilfield chemistry, 2004,21 (2): 113-115.), this linking agent is by organic boron and organic zirconium crosslinker is composite forms, and the fracturing fluid system temperature tolerance of formation is higher than 160 DEG C.The organic boron zirconium cross linking agent being applicable to 135 ~ 163 DEG C of reservoirs of US Patent No. 7683011 invention be after reacting with alkanolamine and zirconium complex again with water and hydroxy alkylidene diamine reactant, last reaction with boron compound obtains.
As can be seen from disclosed document above: organic boron zirconium cross linking agents a lot of is at present that raw material is prepared and forms with zirconium complex.But expensive due to zirconium complex, causes the raw materials cost of organic boron zirconium cross linking agent high, reduce further the economic benefit of oil field compression fracture.
In addition, at present in order to improve the heatproof resistant to shearing ability of organic boron zirconium cross linking agent in high temperature resistance fracturing fluid system, some organic boron zirconium cross linking agent usually needs strictly to control reaction conditions in the preparation, produces bring certain difficulty to the marketization of organic boron zirconium cross linking agent; Some organic boron zirconium cross linking agent needs preparation method to be divided into multiple step to carry out (such as in the preparation, compositely again after synthesizing organic borate cross-linker and organic zirconium crosslinker respectively obtain organic boron zirconium cross linking agent), and there is the sepn process of intermediate, loaded down with trivial details, the consuming time length of schedule of operation, production efficiency is low.
Summary of the invention
For solving the problem, the invention provides a kind of organic boron zirconium cross linking agent, raw material is cheap and easy to get, and preparation technology is simple, the organic boron zirconium cross linking agent obtained is applied in high temperature resistance fracturing fluid system, and the frozen glue of formation has good heatproof endurance of cutting more than 135 DEG C under high temperature.
The present invention adopts following technical scheme:
A kind of organic boron zirconium cross linking agent, it is characterized in that, described organic boron zirconium cross linking agent is made up of following formula:
Calculate by weight:
Inorganic zirconium salts 1 part; Water 2-4 part; Virahol 3-6 part; Inorganic compounds of boron 0.4-1 part; Methyl alcohol 4-20 part; Polyvalent alcohol 2-4 part; Alpha-hydroxy carboxylic acid compounds sodium 1-2 part; Trolamine 1-2 part; Tetrahydroxypropyl ethylenediamine 0.5-1 part.
As preferably, described inorganic zirconium salts is the combination of a kind of in zirconium oxychloride or zirconium tetrachloride or two kinds.
As preferably, described inorganic compounds of boron is the combination of a kind of in boric acid or borax or two kinds.
As preferably, described polyvalent alcohol is the combination of a kind of in glycerol or ethylene glycol or two kinds.
As preferably, described alpha-hydroxy carboxylic acid compounds sodium is the combination of a kind of in Sodium.alpha.-hydroxypropionate or Sunmorl N 60S or two kinds.
Further, the formula of described organic boron zirconium cross linking agent also can be:
Calculate by weight:
Zirconium oxychloride 1 part; 2 parts, water; Virahol 3 parts; Boric acid 0.4 part; Methyl alcohol 4 parts; Glycerol 2 parts; Sodium.alpha.-hydroxypropionate 1 part; Trolamine 1 part; Tetrahydroxypropyl ethylenediamine 0.5 part.
Further, the formula of described organic boron zirconium cross linking agent also can be:
Calculate by weight:
Zirconium oxychloride 1 part; 4 parts, water; Virahol 6 parts; Boric acid 0.5 part; Methyl alcohol 10 parts; Ethylene glycol 4 parts; Sodium.alpha.-hydroxypropionate 2 parts; Trolamine 2 parts; Tetrahydroxypropyl ethylenediamine 0.5 part.
Further, described organic boron zirconium cross linking agent is made by the following method:
In water, add inorganic zirconium salts and Virahol, after stirring, at 55-60 DEG C, pass into ammonia and back flow reaction 0.5-1 hour; And then add polyvalent alcohol, alpha-hydroxy carboxylic acid compounds sodium and alkanolamine, continue reaction after 2-4 hour, then add the B solution prepared by inorganic compounds of boron and methyl alcohol, continue reaction after 2-4 hour, obtain described organic boron zirconium cross linking agent.
The application of a kind of organic boron zirconium cross linking agent recited above in high temperature resistance fracturing fluid system.
The invention has the beneficial effects as follows:
(1) traditional organic boron zirconium cross linking agent is much form for raw material is prepared with the zirconium complex of costliness, and cost is high; And organic boron zirconium cross linking agent provided by the invention, utilize cheap inorganic zirconium salts for raw material, greatly saved cost, be conducive to the marketization of organic boron zirconium cross linking agent and the widespread use in high temperature resistance fracturing fluid system.
(2) organic boron zirconium cross linking agent provided by the invention, have the features such as cross-linking efficiency is high, consumption is few, the frozen glue formed with hydroxypropylguar gum has good temperature and shearing sustainability, effectively can promote the heatproof resistant to shearing ability of fracturing fluid system.In addition, organic boron zirconium cross linking agent provided by the invention also has delayed crosslinked effect, reduces of the fracturing fluid pumping frictional resistance; There is secondary crosslinking phenomenon in the frozen glue that organic boron zirconium cross linking agent provided by the invention and melon glue are formed, improve the ability that it is made seam and carries propping agent under shear at high temperature.
(3) organic boron zirconium cross linking agent provided by the invention, the low in raw material price in its formula, can adopt one kettle way prepare and obtain.That is: adopt formula provided by the invention, according to the timed interval provided by the invention, add reaction raw materials successively, under 55-60 DEG C of comparatively gentle temperature of reaction, carry out back flow reaction, without the need to separation of intermediates, can organic boron zirconium cross linking agent be obtained.Reaction raw materials price is low, and market-oriented prospect is large; Without intermediate separation in preparation process, preparation technology is simple, easy to operate.Compared with prior art, the organic boron zirconium complex that formula provided by the invention and preparation technology are formed is applied in high temperature resistance fracturing fluid system, under the frozen glue of the formation high temperature more than 135 DEG C, there is good heatproof endurance of cutting.
(4) utilize formula provided by the invention, temperature of reaction required when preparing organic boron zirconium cross linking agent be lower, mild condition, easy to control.If temperature of reaction is too high, inorganic zirconium salts (especially zirconium oxychloride) solubleness in Virahol can be reduced, accelerate the process that inorganic zirconium salts generates zirconium gel, if temperature is more than 80 DEG C, inorganic zirconium salts (especially zirconium oxychloride) solution can change gelatinous precipitate into rapidly under base catalysis, causes subsequent reactions difficulty; If temperature of reaction is too low, the complexing of inorganic zirconium salts, inorganic compounds of boron and organic ligand is insufficient, and in product, inorganics composition proportion is large, and product cross-linking effect is poor.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention 5 linking agent forms frozen glue at 140 DEG C, 170s
-1lower viscosity change curve;
Fig. 2 is that the embodiment of the present invention 6 linking agent forms frozen glue at 135 DEG C, 170s
-1lower viscosity change curve.
Embodiment
Below in conjunction with embodiment, the present invention is further described, but therefore protection scope of the present invention be not limited among scope of embodiments.
embodiment 1
A kind of organic boron zirconium cross linking agent, its formula is:
Calculate by weight:
Zirconium oxychloride 1 part; 2 parts, water; Virahol 3 parts; Boric acid 0.4 part; Methyl alcohol 4 parts; Glycerol 2 parts; Sodium.alpha.-hydroxypropionate 1 part; Trolamine 1 part; Tetrahydroxypropyl ethylenediamine 0.5 part.
This organic boron zirconium cross linking agent is prepared from by following steps:
(1) 10g zirconium oxychloride and 20g water and 30g Virahol are made into zirconium salt solution, add in flask, at 55 DEG C, in solution, pass into ammonia, back flow reaction 0.5 hour;
(2) in flask, add 20g glycerol successively, 10g Sodium.alpha.-hydroxypropionate, 10g trolamine, 5g tetrahydroxypropyl ethylenediamine, react 3 hours;
(3) in flask, add the B solution that 4g boric acid and 40g methyl alcohol are made into, react 3 hours, obtain faint yellow organic boron zirconium cross linking agent.
embodiment 2
A kind of organic boron zirconium cross linking agent, its formula is:
Calculate by weight:
Zirconium oxychloride 1 part; 4 parts, water; Virahol 6 parts; Borax 0.5 part; Methyl alcohol 10 parts; Ethylene glycol 4 parts; Sodium.alpha.-hydroxypropionate 2 parts; Trolamine 2 parts; Tetrahydroxypropyl ethylenediamine 0.5 part.
This organic boron zirconium cross linking agent is prepared from by following steps:
(1) 10g zirconium oxychloride and 40g part water and 60g Virahol are made into zirconium salt solution, add in flask, at 60 DEG C, in solution, pass into ammonia, back flow reaction 1 hour;
(2) in flask, add 40g ethylene glycol successively, 20g Sodium.alpha.-hydroxypropionate, 20g trolamine, 5g tetrahydroxypropyl ethylenediamine, react 2 hours;
(3) add to flask the B solution that 5g borax and 100g methyl alcohol is made into, react 2 hours, obtain faint yellow organic boron zirconium cross linking agent.
embodiment 3
A kind of organic boron zirconium cross linking agent, its formula is:
Calculate by weight:
Zirconium tetrachloride 1 part; 2 parts, water; Virahol 4 parts; Boric acid 0.8 part; Methyl alcohol 8 parts; Glycerol 4 parts; Sunmorl N 60S 1 part; Trolamine 1 part; Tetrahydroxypropyl ethylenediamine 1 part.
This organic boron zirconium cross linking agent is prepared from by following steps:
(1) 10g zirconium tetrachloride and 20g water and 40g Virahol are made into zirconium salt solution, add in flask, at 58 DEG C, in solution, pass into ammonia, back flow reaction 1 hour;
(2) in flask, add 40g glycerol successively, 10g Sunmorl N 60S, 10g trolamine, 10g tetrahydroxypropyl ethylenediamine, react 3 hours;
(3) in flask, add the B solution that 8g boric acid and 80g methyl alcohol are made into, react 2 hours, obtain faint yellow organic boron zirconium cross linking agent.
embodiment 4
A kind of organic boron zirconium cross linking agent, its formula is:
Calculate by weight:
Zirconium tetrachloride 1 part; 3 parts, water; Virahol 6 parts; Borax 1 part; Methyl alcohol 20 parts; Ethylene glycol 3 parts; Sunmorl N 60S 1.5 parts; Trolamine 1.5 parts; Tetrahydroxypropyl ethylenediamine 1 part.
This organic boron zirconium cross linking agent is prepared from by following steps:
(1) 10g zirconium tetrachloride and 30g water and 60g Virahol are made into zirconyl chloride solution, add in flask, at 59 DEG C, in solution, pass into ammonia, back flow reaction 0.8 hour;
(2) in flask, add 30g ethylene glycol successively, 15g Sunmorl N 60S, 15g trolamine, 10g tetrahydroxypropyl ethylenediamine, react 3 hours;
(3) in flask, add the B solution that 10g borax and 200g methyl alcohol are made into, react 4 hours, obtain faint yellow organic boron zirconium cross linking agent.
embodiment 5
In tap water, fracturing liquid base fluid (in this embodiment " % " all represents mass concentration) is configured: 0.55% viscosifying agent JK101(is: the hydroxypropylguar gum being produced in Kunshan Beijing-Kunming oilfield chemistry scientific and technological development company) according to following formula, 1% clay stabilizer KCl, 0.5% cleanup additive CF-5A(is produced in long celebrating down-hole oilfield additive limited liability company), 0.05% sterilant formaldehyde, 0.04%pH conditioning agent NaOH; In formula, each material has added and after stirring, has left standstill 4 hours.In the fracturing liquid base fluid configured, add the organic boron zirconium cross linking agent that 0.5% embodiment 1 is obtained, in 8 minutes, form the good frozen glue of hanging property.Haake MARS III rotational rheometer measure this frozen glue temperature be 140 DEG C, shearing rate is 170s
-1under heatproof endurance of cutting, its viscosity change curve is as shown in Figure 1.
As can be seen from Figure 1, there is secondary crosslinking phenomenon in this frozen glue under shear at high temperature, and after continuous shear stress 120min, the viscosity of frozen glue still remains on more than 50mPas.Illustrate that the organic boron zirconium cross linking agent cross-linking efficiency that embodiment 1 obtains is high, consumption is few, it is high that it makes the ability of stitching and carrying propping agent, under the high temperature of the frozen glue formed with hydroxypropylguar gum more than 140 DEG C, still there is good heatproof endurance of cutting, effectively can promote the heatproof resistant to shearing ability of fracturing fluid system.
embodiment 6
According to the recipe configuration fracturing liquid base fluid of example 5, in the fracturing liquid base fluid configured, add 0.5%(mass concentration) the obtained organic boron zirconium cross linking agent of embodiment 2, in 8 minutes, form the good frozen glue of hanging property.Haake MARS III rotational rheometer measure this frozen glue temperature be 135 DEG C, shearing rate is 170s
-1under heatproof endurance of cutting, its viscosity change curve is as shown in Figure 2.
There is secondary crosslinking phenomenon in this frozen glue, after continuous shear stress 120min, the viscosity of frozen glue still remains on more than 80mPas under shear at high temperature.Illustrate that the organic boron zirconium cross linking agent cross-linking efficiency that embodiment 2 obtains is high, consumption is few, it is high that it makes the ability of stitching and carrying propping agent, the frozen glue formed with hydroxypropylguar gum has good temperature and shearing sustainability, effectively can promote the heatproof resistant to shearing ability of fracturing fluid system.
Claims (9)
1. an organic boron zirconium cross linking agent, is characterized in that, described organic boron zirconium cross linking agent is made up of following formula:
Calculate by weight:
Inorganic zirconium salts 1 part; Water 2-4 part; Virahol 3-6 part; Inorganic compounds of boron 0.4-1 part; Methyl alcohol 4-20 part; Polyvalent alcohol 2-4 part; Alpha-hydroxy carboxylic acid compounds sodium 1-2 part; Trolamine 1-2 part; Tetrahydroxypropyl ethylenediamine 0.5-1 part.
2. a kind of organic boron zirconium cross linking agent according to claim 1, is characterized in that, described inorganic zirconium salts is the combination of a kind of in zirconium oxychloride or zirconium tetrachloride or two kinds.
3. a kind of organic boron zirconium cross linking agent according to claim 1, is characterized in that, described inorganic compounds of boron is the combination of a kind of in boric acid or borax or two kinds.
4. a kind of organic boron zirconium cross linking agent according to claim 1, is characterized in that, described polyvalent alcohol is the combination of a kind of in glycerol or ethylene glycol or two kinds.
5. a kind of organic boron zirconium cross linking agent according to claim 1, is characterized in that, described alpha-hydroxy carboxylic acid compounds sodium is the combination of a kind of in Sodium.alpha.-hydroxypropionate or Sunmorl N 60S or two kinds.
6. a kind of organic boron zirconium cross linking agent according to claim 1-5, is characterized in that, the formula of described organic boron zirconium cross linking agent also can be:
Calculate by weight:
Zirconium oxychloride 1 part; 2 parts, water; Virahol 3 parts; Boric acid 0.4 part; Methyl alcohol 4 parts; Glycerol 2 parts; Sodium.alpha.-hydroxypropionate 1 part; Trolamine 1 part; Tetrahydroxypropyl ethylenediamine 0.5 part.
7. a kind of organic boron zirconium cross linking agent according to claim 1-5, is characterized in that, the formula of described organic boron zirconium cross linking agent also can be:
Calculate by weight:
Zirconium oxychloride 1 part; 4 parts, water; Virahol 6 parts; Boric acid 0.5 part; Methyl alcohol 10 parts; Ethylene glycol 4 parts; Sodium.alpha.-hydroxypropionate 2 parts; Trolamine 2 parts; Tetrahydroxypropyl ethylenediamine 0.5 part.
8. a kind of organic boron zirconium cross linking agent according to claim 1, is characterized in that, described organic boron zirconium cross linking agent is made by the following method:
In water, add inorganic zirconium salts and Virahol, after stirring, at 55-60 DEG C, pass into ammonia and back flow reaction 0.5-1 hour; And then add polyvalent alcohol, alpha-hydroxy carboxylic acid compounds sodium and alkanolamine, continue reaction after 2-4 hour, then add the B solution prepared by inorganic compounds of boron and methyl alcohol, continue reaction after 2-4 hour, obtain described organic boron zirconium cross linking agent.
9. the application of organic boron zirconium cross linking agent in high temperature resistance fracturing fluid system described in an any one of claim 1-8.
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| CN106318367A (en) * | 2016-08-17 | 2017-01-11 | 富象油气技术服务有限公司 | Ultrahigh temperature fracturing solution organic borate-zirconate crosslinking agent and preparation method thereof |
| CN106800927A (en) * | 2017-01-05 | 2017-06-06 | 中国石油化工股份有限公司 | A kind of guanidine gum fracturing fluid crosslinking agent and preparation method and application |
| CN106867498A (en) * | 2017-02-08 | 2017-06-20 | 中国石油集团川庆钻探工程有限公司长庆井下技术作业公司 | A kind of utilization acid fracturing returns the fracturing fluid of discharge opeing preparation |
| WO2018176532A1 (en) * | 2017-03-27 | 2018-10-04 | 成都劳恩普斯科技有限公司 | Cross-linking agent, full suspension fracturing fluid and preparation method thereof |
| CN111663021A (en) * | 2020-06-12 | 2020-09-15 | 广州广钢新材料股份有限公司 | Corrosion-resistant deformed steel bar and preparation method thereof |
| CN112126420A (en) * | 2020-09-04 | 2020-12-25 | 四川省威沃敦化工有限公司 | Crosslinking agent for fracturing and preparation method thereof |
| CN116083069A (en) * | 2023-02-27 | 2023-05-09 | 中海油田服务股份有限公司 | Cross-linking agent for seawater-based fracturing fluid and preparation method thereof |
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| CN106800927A (en) * | 2017-01-05 | 2017-06-06 | 中国石油化工股份有限公司 | A kind of guanidine gum fracturing fluid crosslinking agent and preparation method and application |
| CN106867498A (en) * | 2017-02-08 | 2017-06-20 | 中国石油集团川庆钻探工程有限公司长庆井下技术作业公司 | A kind of utilization acid fracturing returns the fracturing fluid of discharge opeing preparation |
| CN106867498B (en) * | 2017-02-08 | 2020-02-07 | 中国石油集团川庆钻探工程有限公司长庆井下技术作业公司 | Fracturing fluid prepared from acidizing fracturing flow-back fluid |
| WO2018176532A1 (en) * | 2017-03-27 | 2018-10-04 | 成都劳恩普斯科技有限公司 | Cross-linking agent, full suspension fracturing fluid and preparation method thereof |
| CN111663021A (en) * | 2020-06-12 | 2020-09-15 | 广州广钢新材料股份有限公司 | Corrosion-resistant deformed steel bar and preparation method thereof |
| CN112126420A (en) * | 2020-09-04 | 2020-12-25 | 四川省威沃敦化工有限公司 | Crosslinking agent for fracturing and preparation method thereof |
| CN116083069A (en) * | 2023-02-27 | 2023-05-09 | 中海油田服务股份有限公司 | Cross-linking agent for seawater-based fracturing fluid and preparation method thereof |
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Application publication date: 20150429 |