CN107974246A - A kind of high temperature resistant crosslinking acid system, preparation method and application - Google Patents
A kind of high temperature resistant crosslinking acid system, preparation method and application Download PDFInfo
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- CN107974246A CN107974246A CN201610919687.8A CN201610919687A CN107974246A CN 107974246 A CN107974246 A CN 107974246A CN 201610919687 A CN201610919687 A CN 201610919687A CN 107974246 A CN107974246 A CN 107974246A
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- 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
- C09K8/72—Eroding chemicals, e.g. acids
- C09K8/74—Eroding chemicals, e.g. acids combined with additives added for specific purposes
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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
- C09K8/72—Eroding chemicals, e.g. acids
- C09K8/725—Compositions containing polymers
Abstract
The invention discloses a kind of high temperature resistant crosslinking acid system, preparation method and application.System is prepared by the raw material including following components, and each component is by weight percentage：Sour 10.0wt% 20.0wt%；Polymer thickening agent 1.0wt% 2.0wt%；Organic zirconium crosslinker 0.5wt% 4.0wt%；Corrosion inhibiter 1.0wt% 4.0wt%；Surplus is water；Polymer thickening agent is 2 vinyl methyl propanesulfonate quadripolymer of acrylamide/Methacrylamide/MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride/2 acryloyl-oxy.The high temperature resistant acid fracturing of the present invention, up to 50~70mPa.s, is applicable to temperature up to 160 DEG C of carbonate reservoir acid fracturing stimulation work with crosslinking acid system viscosity at 160 DEG C.
Description
Technical field
The present invention relates to oilfield reservoir renovation technique field, further say, be related to a kind of high temperature resistant crosslinking acid system,
Preparation method and application.
Background technology
Acid-fracture technology is to release Carbonate Reservoir and the blocking of sandstone oil reservoir oil/gas well near wellbore zone, expand or extend
Oil gas flow channel, recovery improve in-place permeability, the important technique measure of increasing yield and injection.From the 1950s to control
Regular hydrochloric acid acid fluid system based on acid liquid corrosion is starting point, former later as depth of reservoirs continues to increase, temperature is higher and higher
Acid solution has been unable to meet the needs of reservoir reconstruction, and then has developed some unconventional acid fluid systems, main crosslinking acid, thickening
Acid, emulsified acid and foamed acid etc..Cross-linked acid is by the crosslinking to thickening agent, forms solid netted chain, reduces hydrochlorate reaction speed
A large amount of leak-offs of degree and acid solution, overcome the acid fracturing method acid etchings such as emulsified acid acid fracturing, viscous acid acid fracturing, foamed acid acid fracturing seam length
Deficiency, by forming slit, improves acid fracturing effect.Cross-linked acid has become the hot technology of reservoir reconstruction in recent years.
With the continuous improvement of deep acidizing technical requirements, crosslinked acidic can have been unable to meet the need of deep Reservoir Acidization pressure break
Ask, show more heat resistance it is poor, by shear inference is big, acid solution tackifying ability is weak, the extemporaneous preparation time is long, thickening agent dissolves speed
Spend the shortcomings of slow.
Wang Dongmei etc. (oil drilling technology, 2006,27,64-65) is made with acrylamide and other 2 kinds of temperature-resistant anti-salt monomers
The apparent viscosity of thickening agent TP-1,4%TP-1 in 20%HCl acid solutions, 90 DEG C, which is prepared, for synthon reaches 46mPas,
Apparent viscosity 27mPas at 120 DEG C.Dai Leiyang etc. (Speciality Petrochemicals is in progress, 2014,15,32-35) uses non-ionic monomer
Acrylamide (AM), cationic monomer MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (DMC), anionic monomer AMPS make raw material
Synthesize amphion terpolymer AM/AMPS/DMC acidifying thickening agents, thickening acid solution and the water flooding of preparation have
Good compatibility ability and retardative property, 90 DEG C of apparent viscosity is less than 25mPas in the acid solution containing 1% thickening agent.Patent CN
103525393 A disclose the viscous acid that a kind of instant capacity gelling agent for acid fluid is mixed with hydrochloric acid, and thickening agent raw material composition is poly-
200 50~55 parts of ethylene glycol, 35~40 parts of polymer (MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride or polyoxyethylene), point
2~5 parts of powder.Viscosity loss velocity of the thickening agent viscosity in more than 50mPas, 90 DEG C is less than 10%.Patent CN
104073237 disclose a kind of high temperature resistant ground surface crosslinking acid and preparation method, which is 15~28% acid,
0.4~1.0% polyacrylamide polymer, 0.1~0.5% aldehyde crosslinking agent, 0.05~0.25% Phenolic crosslinkers,
0.005~0.1% crosslinking accelerator, 0.5%~2.0% corrosion inhibiter, 0.5%~2.0% ferrous stability, 0.01~
0.1% ammonium persulfate, surplus are water.Cross-linked acid is in 120 DEG C, 170s-1Viscosity is 113.3mPa after condition down cut 120min
s.Patent CN 102352235A disclose a kind of cross-linked acid acidizing and fracturing fluid, form as 10~30% hydrochloric acid, 0.4~0.8% thick
Agent, 1.0~2.0% crosslinking agents, 1.0~2.0% corrosion inhibiter, surplus are water.Viscosity is after 80 DEG C of shearing 60min of the crosslinking agent
88mPa·s.104403658 A of patent CN disclose a kind of high temperature resistant crosslinking acid fluid system, form as 20% hydrochloric acid, 1.0%
Polymer thickening agent, 0.3% chelating titanium crosslinkers, surplus is water, and the high temperature resistant cross-linked acid acid solution of preparation is handed under strong acid environment
Connection forms the frozen glue hung, is resistant to 190 DEG C of high temperature, increases production available for 160-190 DEG C of Carbonate Oil gas reservoir acid fracturing.Patent US
4225445 disclose a kind of acid thickening agent, and the thickening agent is by triethylene ammonio methacrylate, tetraene ammonium chloride, tetraene chlorination piperazine
Piperazine (tetraallylpiperazinium chloride) or N, N, N ', N '-tetraene-N, N '-dimethyl hexamethylene ammonium chloride exists
On divinyl alkyl dimethyl ammonium chloride molecule grafting into etc., its molecular weight is up to millions of, is 15% and 28% in concentration
1% thickening agent viscosity is respectively 21.5 and 33.0mPas in HCl solution, and 1% thickening agent exists after being preserved 6h and 2.8 day at 65 DEG C
Viscosity in 15% hydrochloric acid is respectively 15.0 and 14.5mPas, shows that the thickening agent hydrochloric acid solution can keep good at 65 DEG C
Stability.
It can be seen that the temperature resistance scarce capacity of the thickening agent product in document causes cross-linked acid generally existing heatproof, resistance to
The characteristics of cutting performance is poor, can not meet the requirement that more than 160 DEG C reservoir acid fracturings are constructed to cross-linked acid.
The content of the invention
To solve produced problem in the prior art, the present invention provides a kind of high temperature resistant crosslinking acid system, preparation method
And application.It is the frozen glue that can be hung that the high temperature resistant that the present invention prepares, which is crosslinked acid solution under strong acid environment, in 160 DEG C of shear rates
170s-1Lower 120 minutes apparent viscosities are kept at 50~70mPas, available for 160 DEG C of Carbonate Oil gas reservoir acid fracturings
Stimulation work.
An object of the present invention is to provide a kind of high temperature resistant crosslinking acid system.
The cross-linked acid is prepared by the raw material including following components, and each component is by weight percentage：
Sour 10.0wt%-20.0wt%；Preferably 15.0wt%-20.0wt%；
Polymer thickening agent 1.0wt%-2.0wt%；Preferably 1.0wt%-1.5wt%；
Organic zirconium crosslinker 0.5wt%-4.0wt%；Preferably 1.5wt%-3.0wt%；
Corrosion inhibiter 1.0wt%-4.0wt%；Preferably 1.0wt%-2.0wt%；
Surplus is water.
The acid is hydrochloric acid, formic acid, acetic acid, one kind in hydrofluoric acid or combination；
The polymer thickening agent is acrylamide/Methacrylamide/methylacryoyloxyethyl trimethyl ammonia chloride
Ammonium/2- acryloyl-oxy -2- vinyl methyl propanesulfonate quadripolymers, monomer weight ratio is (20~65):(5~15):(5
~18):(15~55)；Preferably (25~45):(7~12):(5~10):(20~40) present invention uses redox legal system
Standby polymer thickening agent product dissolution velocity is fast, and cost is low, and stability is good, places occur without precipitation for a long time.
The preparation method of thickening agent is with reference to patent (patent of 201610802354.7 inventor of Application No. in preceding application).
Thickening agent is preferably prepared according to the following steps：(1) by the acrylamide, Methacrylamide, methacryloxypropyl of the dosage
Ethyl-trimethyl salmiac, 2- acryloyl-oxies -2- vinyl methyls propanesulfonate and molecular weight regulator under agitation according to
Secondary be separately added into fills being placed in the reactor of water bath with thermostatic control of water, adds pH adjusting agent to control the pH value of polymerization system to exist
6.0~10.0；(2) lead to nitrogen deoxygenation 10~30min of stir about, polymeric solution temperature is risen to 20~50 DEG C, then add and draw
Agent is sent out, continues to logical nitrogen gas stirring about 15~30min；(3) reaction vessel of built-in polymer jelly is placed in thermostatted water
Constant temperature polymerisation 6-12h in bath, takes out shear granulation, drying, to obtain the final product crushing, high temperature resistant acid fracturing polymer.
The crosslinking agent is triethanolamine zirconium, zirconium lactate or gluconic acid zirconium；
The corrosion inhibiter is polyethylene glycol, imidazoline pyridine, benzotriazole, monoethanolamine, diethanol amine, dodecyl three
One kind in ammonio methacrylate, amide imidazoline quaternary ammonium salt, thiocarbamide.
The second object of the present invention is to provide a kind of preparation method of high temperature resistant crosslinking acid system.
Including：
Acid is diluted to the concentration with water first, then polymer thickening agent is added in acid, after stirring and dissolving is uniform,
Corrosion inhibiter, crosslinking agent are added, the high temperature resistant crosslinking acid system is made after stirring.
It is wherein preferred：
Polymer thickening agent is added in acid, at the uniform velocity stirs 5~10min；
2-5min is stirred after adding corrosion inhibiter, crosslinking agent.
Following steps can specifically be used：
Quantitative polymer thickening agent is slowly added into a certain concentration hydrochloric acid solution in whipping process at normal temperatures, is stirred
Mix 5~10min and obtain uniform viscous fluid, continuously add corrosion inhibiter, added after stirring 5min and quantify organic zirconium crosslinker, stirring 2~
5min, obtains the faint yellow cross-linked acid frozen glue that can be hung.
The third object of the present invention is to provide a kind of high temperature resistant and is crosslinked acid system more than 160 DEG C in carbonate reservoir
Using.
The high temperature resistant acid fracturing of the present invention, up to 50~70mPa.s, is applicable to temperature with crosslinking acid system viscosity at 160 DEG C
Up to 160 DEG C of carbonate reservoir acid fracturing stimulation work.
Brief description of the drawings
Fig. 1 is that the high temperature resistant of embodiment 3 is crosslinked 160 DEG C of acid system, 170s-1Under the conditions of high temperature rheological curve；
Embodiment
With reference to embodiment, the present invention is further illustrated.
Embodiment 1：
The present embodiment provides a kind of high temperature resistant ground surface crosslinking acid acid solution, which includes following component：
Hydrochloric acid 17wt%100g, polymer thickening agent 1.2g, imidazoline pyridine 1.5g, triethanolamine zirconium 1.5g.
The high temperature resistant ground surface crosslinking acid acid solution of the present embodiment is to be prepared by the following method to obtain：
The preparation of polymer thickening agent：By 20g acrylamides, 5g Methacrylamides, 15g methylacryoyloxyethyls three
75% solution of ammonio methacrylate, 28g 2- acryloyl-oxies -2- vinyl methyls propanesulfonates 300r/min rotating speeds stirring under according to
Secondary add fills being placed in the reactor of water bath with thermostatic control of 160ml water, is stirring evenly and then adding into molecular weight regulator polyoxyethylene
Diacrylate 0.05g, the pH value that polymerization system is adjusted with 20% sodium hydrate aqueous solution is 7, leads to nitrogen deoxygenation stir about
30min, 45 DEG C are risen to by polymeric solution temperature, are then respectively adding each 0.15g of potassium peroxydisulfate, sodium sulfite and are triggered polymerization, after
It is continuous to maintain logical nitrogen about 20min；The constant temperature polymerisation 8h in water bath with thermostatic control, take out shear granulation, drying, crushing, up to poly-
Compound thickening agent.
The preparation of base fluid：The hydrochloric acid 100g of 17wt% is added in a reservoir, is slowly added to 1.2g thickening agents, is continued after adding
5min is stirred, thickening agent is fully dissolved；
The preparation of cross-linked acid：1.5g imidazolines pyridine, 1.5g triethanolamine zirconiums are sequentially added in a reservoir, are stirred evenly,
Obtain cross-linked acid acid solution.
High temperature resistant ground surface crosslinking acid acid solution obtained by the present embodiment is as clear as crystal, substantially without residue.
Embodiment 2：
The present embodiment provides a kind of high temperature resistant ground surface crosslinking acid acid solution, which includes following component：
Hydrochloric acid 18wt%100g, polymer thickening agent 1.2g, benzotriazole 1.7g, zirconium lactate 1.2g.
The high temperature resistant ground surface crosslinking acid acid solution of the present embodiment is to be prepared by the following method to obtain：
The preparation of polymer thickening agent：By 30g acrylamides, 10g Methacrylamides, 8g acrylyl oxy-ethyl-trimethyls
75% solution of ammonium chloride, 20g 2- acryloyl-oxies -2- vinyl methyls propanesulfonates add successively under the stirring of 300r/min rotating speeds
Enter to fill being placed in the reactor of water bath with thermostatic control for 175ml water, be stirring evenly and then adding into two propylene of molecular weight regulator ethylene glycol
Acid esters 0.075g, the pH value that polymerization system is adjusted with 20% potassium hydroxide aqueous solution is 8, leads to nitrogen deoxygenation stir about 25min, will
Polymeric solution temperature rises to 35 DEG C, is then respectively adding each 0.25g of potassium peroxydisulfate, sodium sulfite and triggers polymerization, continues to lead to
Nitrogen about 25min；The constant temperature polymerisation 9h in water bath with thermostatic control, takes out shear granulation, drying, to obtain the final product crushing, polymer thickening
Agent.
The preparation of base fluid：The hydrochloric acid 100g of 18wt% is added in a reservoir, is slowly added to 1.2g thickening agents, is continued after adding
5min is stirred, thickening agent is fully dissolved；
The preparation of cross-linked acid：1.7g benzotriazole, 1.2g zirconium lactates are sequentially added in a reservoir, are stirred evenly, are obtained
Cross-linked acid acid solution.
High temperature resistant ground surface crosslinking acid acid solution obtained by the present embodiment is as clear as crystal, substantially without residue.
Embodiment 3：
The present embodiment provides a kind of high temperature resistant ground surface crosslinking acid acid solution, which includes following component：
Formic acid 20wt%100g, polymer thickening agent 1.5g, amide imidazoline quaternary ammonium salt 3.0g, gluconic acid zirconium 1.5g.
The high temperature resistant ground surface crosslinking acid acid solution of the present embodiment is to be prepared by the following method to obtain：
The preparation of polymer thickening agent：By 35g acrylamides, 8g Methacrylamides, 8g dimethyl diallyl chlorinations
70% solution of ammonium, 32g 2- acryloyl-oxies -2- vinyl methyls propanesulfonates sequentially add Sheng under the stirring of 300r/min rotating speeds
There is being placed in the reactor of water bath with thermostatic control for 180ml water, be stirring evenly and then adding into molecular weight regulator butanediol diacrylate
0.28g, the pH value that polymerization system is adjusted with 20% sodium hydrate aqueous solution is 9, leads to nitrogen deoxygenation stir about 30min, will polymerize
Solution temperature rises to 50 DEG C, is then respectively adding each 0.23g of potassium peroxydisulfate, sodium sulfite and triggers polymerization, continues to logical nitrogen
About 20min；The constant temperature polymerisation 10h in water bath with thermostatic control, takes out shear granulation, drying, to obtain the final product crushing, polymer thickening agent.
The preparation of base fluid：The formic acid 100g of 20wt% is added in a reservoir, is slowly added to thickening agent, is continued to stir after adding
5min, makes thickening agent fully dissolve；
The preparation of cross-linked acid：3.0g amide imidazolines quaternary ammonium salt, 1.5g gluconic acid zirconiums are sequentially added in a reservoir, are stirred
3 minutes, stir evenly, obtain cross-linked acid acid solution.
High temperature resistant ground surface crosslinking acid acid solution obtained by the present embodiment is as clear as crystal, substantially without residue.
Embodiment 4：
The present embodiment provides a kind of high temperature resistant ground surface crosslinking acid acid solution, which includes following component：
Acetic acid 16wt%100g, polymer thickening agent 1.2g, thiocarbamide 2.0g, triethanolamine zirconium 1.5g.
The high temperature resistant ground surface crosslinking acid acid solution of the present embodiment is to be prepared by the following method to obtain：
The preparation of polymer thickening agent：By 40g acrylamides, 8g Methacrylamides, 10g methylacryoyloxyethyls three
75% solution of ammonio methacrylate, 25g 2- acryloyl-oxies -2- vinyl methyls propanesulfonates 300r/min rotating speeds stirring under according to
Secondary add fills being placed in the reactor of water bath with thermostatic control of 150ml water, is stirring evenly and then adding into molecular weight regulator neopentyl glycol
Diacrylate 0.3g, the pH value that polymerization system is adjusted with 20% sodium hydrate aqueous solution is 9.5, leads to nitrogen deoxygenation stir about
20min, 35 DEG C are risen to by polymeric solution temperature, are then respectively adding each 0.28g of potassium peroxydisulfate, sodium sulfite and are triggered polymerization, after
It is continuous to maintain logical nitrogen about 30min；The constant temperature polymerisation 12h in water bath with thermostatic control, take out shear granulation, drying, crushing, up to poly-
Compound thickening agent.
The preparation of base fluid：The acetic acid of 100mL 16wt% is added in a reservoir, is slowly added to 1.2g thickening agents, is added follow-up
Continuous stirring 5min, makes thickening agent fully dissolve；
The preparation of cross-linked acid：2.0g thiocarbamides, 1.5g triethanolamine zirconiums are sequentially added in a reservoir, is stirred 2 minutes, and stirring is equal
It is even, obtain cross-linked acid acid solution.
High temperature resistant ground surface crosslinking acid acid solution obtained by the present embodiment is as clear as crystal, substantially without residue.
Embodiment 5：
The present embodiment provides a kind of high temperature resistant ground surface crosslinking acid acid solution, which includes following component：
Hydrofluoric acid 20wt%100g, polymer thickening agent 1.2g, dodecyl trimethyl ammonium chloride 3.0g, zirconium lactate
1.5g。
The high temperature resistant ground surface crosslinking acid acid solution of the present embodiment is to be prepared by the following method to obtain：
The preparation of polymer thickening agent：By 38g acrylamides, 8g Methacrylamides, 10g methylacryoyloxyethyls three
75% solution of ammonio methacrylate, 40g 2- acryloyl-oxies -2- vinyl methyls propanesulfonates 300r/min rotating speeds stirring under according to
Secondary add fills being placed in the reactor of water bath with thermostatic control of 160ml water, is stirring evenly and then adding into molecular weight regulator tetrol dipropyl
Olefin(e) acid ester 0.35g, the pH value that polymerization system is adjusted with 20% sodium hydrate aqueous solution is 8.5, leads to nitrogen deoxygenation stir about
30min, 30 DEG C are risen to by polymeric solution temperature, are then respectively adding each 0.2g of potassium peroxydisulfate, sodium sulfite and are triggered polymerization, continue
Maintain logical nitrogen about 20min；The constant temperature polymerisation 10h in water bath with thermostatic control, takes out shear granulation, drying, to obtain the final product crushing, polymerization
Thing thickening agent.
The preparation of base fluid：The hydrofluoric acid of 100mL 20wt% is added in a reservoir, 1.2g thickening agents is slowly added to, after adding
Continue to stir 10min, thickening agent is fully dissolved；
The preparation of cross-linked acid：3.0g dodecyl trimethyl ammonium chloride, 1.5g zirconium lactates are sequentially added in a reservoir, are stirred
5 minutes, stir evenly, obtain cross-linked acid acid solution.
High temperature resistant ground surface crosslinking acid acid solution obtained by the present embodiment is as clear as crystal, substantially without residue.
The viscosity data of crosslinking acid solution prepared by embodiment 1-5 the results are shown in Table 1.
Table 1
Claims (6)
1. a kind of high temperature resistant is crosslinked acid system, it is characterised in that the system is prepared by the raw material including following components, respectively
Component is by weight percentage：
The acid is hydrochloric acid, formic acid, acetic acid, one kind in hydrofluoric acid or combination；
The polymer thickening agent is acrylamide/Methacrylamide/MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride/2-
Acryloyl-oxy -2- vinyl methyl propanesulfonate quadripolymers, monomer weight ratio are (20~65):(5~15):(5~18):
(15~55)；
The crosslinking agent is triethanolamine zirconium, zirconium lactate or gluconic acid zirconium；
The corrosion inhibiter is polyethylene glycol, imidazoline pyridine, benzotriazole, monoethanolamine, diethanol amine, trimethyl
One kind in ammonium chloride, amide imidazoline quaternary ammonium salt, thiocarbamide.
2. high temperature resistant as claimed in claim 1 is crosslinked acid system, it is characterised in that：
3. high temperature resistant as claimed in claim 1 is crosslinked acid system, it is characterised in that：
Thickening agent is acrylamide/Methacrylamide/MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride/2- acryloyl-oxies -2-
Vinyl methyl propanesulfonate quadripolymer；
Monomer weight ratio is (25~45):(7~12):(5~10):(20~40).
A kind of 4. preparation method of high temperature resistant crosslinking acid system as described in one of claims 1 to 3, it is characterised in that the side
Method includes：
Acid is diluted to the concentration with water first, then polymer thickening agent is added in acid, after stirring and dissolving is uniform, is added
Corrosion inhibiter, crosslinking agent, are made the high temperature resistant crosslinking acid system after stirring.
A kind of 5. preparation method of high temperature resistant crosslinking acid system as claimed in claim 4, it is characterised in that：
Polymer thickening agent is added in acid, at the uniform velocity stirs 5~10min；
2~5min is stirred after adding corrosion inhibiter, crosslinking agent.
6. a kind of high temperature resistant crosslinking acid system as described in one of claims 1 to 3 is in formation temperature up to 160 DEG C of carbonate rock
Application in reservoir.
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| CN111171802A (en) * | 2018-11-13 | 2020-05-19 | 中国石油化工股份有限公司 | Preparation method of acid liquor system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108822827A (en) * | 2018-07-21 | 2018-11-16 | 东营市宝泽能源科技有限公司 | A kind of superhigh temperature cross-linked acid |
| CN111117590A (en) * | 2018-11-01 | 2020-05-08 | 中国石油化工股份有限公司 | Crosslinked emulsified acid, preparation method and application |
| CN111171800A (en) * | 2018-11-13 | 2020-05-19 | 中国石油化工股份有限公司 | Preparation method of crosslinked acid |
| CN111171802A (en) * | 2018-11-13 | 2020-05-19 | 中国石油化工股份有限公司 | Preparation method of acid liquor system |
| CN111171797A (en) * | 2018-11-13 | 2020-05-19 | 中国石油化工股份有限公司 | Cross-linking agent and preparation method thereof |
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