CN118240536A - High-temperature-resistant oilfield cementing fluid loss agent and preparation method thereof - Google Patents
High-temperature-resistant oilfield cementing fluid loss agent and preparation method thereof Download PDFInfo
- Publication number
- CN118240536A CN118240536A CN202410334507.4A CN202410334507A CN118240536A CN 118240536 A CN118240536 A CN 118240536A CN 202410334507 A CN202410334507 A CN 202410334507A CN 118240536 A CN118240536 A CN 118240536A
- Authority
- CN
- China
- Prior art keywords
- fluid loss
- unsaturated
- resistant
- acid
- high temperature
- 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.)
- Pending
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 claims abstract description 20
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 claims abstract description 20
- OFNISBHGPNMTMS-UHFFFAOYSA-N 3-methylideneoxolane-2,5-dione Chemical compound C=C1CC(=O)OC1=O OFNISBHGPNMTMS-UHFFFAOYSA-N 0.000 claims abstract description 20
- CYUZOYPRAQASLN-UHFFFAOYSA-N 3-prop-2-enoyloxypropanoic acid Chemical compound OC(=O)CCOC(=O)C=C CYUZOYPRAQASLN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 150000008040 ionic compounds Chemical class 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- 239000000178 monomer Substances 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000003999 initiator Substances 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 39
- 229920000642 polymer Polymers 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 21
- 229960000892 attapulgite Drugs 0.000 claims description 17
- 229910052625 palygorskite Inorganic materials 0.000 claims description 17
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 16
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims description 16
- 239000000654 additive Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 13
- 230000000996 additive effect Effects 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 229910021389 graphene Inorganic materials 0.000 claims description 10
- ZIYVHBGGAOATLY-UHFFFAOYSA-N methylmalonic acid Chemical compound OC(=O)C(C)C(O)=O ZIYVHBGGAOATLY-UHFFFAOYSA-N 0.000 claims description 10
- XLPJNCYCZORXHG-UHFFFAOYSA-N 1-morpholin-4-ylprop-2-en-1-one Chemical compound C=CC(=O)N1CCOCC1 XLPJNCYCZORXHG-UHFFFAOYSA-N 0.000 claims description 8
- CFRFHWQYWJMEJN-UHFFFAOYSA-N 9h-fluoren-2-amine Chemical compound C1=CC=C2C3=CC=C(N)C=C3CC2=C1 CFRFHWQYWJMEJN-UHFFFAOYSA-N 0.000 claims description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 8
- 239000012986 chain transfer agent Substances 0.000 claims description 8
- ZSZRUEAFVQITHH-UHFFFAOYSA-N 2-(2-methylprop-2-enoyloxy)ethyl 2-(trimethylazaniumyl)ethyl phosphate Chemical compound CC(=C)C(=O)OCCOP([O-])(=O)OCC[N+](C)(C)C ZSZRUEAFVQITHH-UHFFFAOYSA-N 0.000 claims description 7
- 239000007795 chemical reaction product Substances 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- WQAQPCDUOCURKW-UHFFFAOYSA-N butanethiol Chemical compound CCCCS WQAQPCDUOCURKW-UHFFFAOYSA-N 0.000 claims description 3
- 150000001767 cationic compounds Chemical class 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 2
- 230000003213 activating effect Effects 0.000 claims description 2
- 150000001718 carbodiimides Chemical class 0.000 claims description 2
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 2
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- XFTALRAZSCGSKN-UHFFFAOYSA-M sodium;4-ethenylbenzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=C(C=C)C=C1 XFTALRAZSCGSKN-UHFFFAOYSA-M 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims 1
- 239000004568 cement Substances 0.000 abstract description 28
- 238000004062 sedimentation Methods 0.000 abstract description 15
- 239000000126 substance Substances 0.000 abstract description 6
- 238000012546 transfer Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 9
- 239000003921 oil Substances 0.000 description 9
- 239000007789 gas Substances 0.000 description 6
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 5
- 239000004575 stone Substances 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 229920001577 copolymer Polymers 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 3
- 229910052901 montmorillonite Inorganic materials 0.000 description 3
- 239000003129 oil well Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- 239000008186 active pharmaceutical agent Substances 0.000 description 2
- 238000010668 complexation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 125000003983 fluorenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000005465 channeling Effects 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000138 intercalating agent Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 230000037048 polymerization activity Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention provides a high-temperature-resistant oilfield cementing fluid loss agent and a preparation method thereof, wherein the fluid loss agent comprises the following raw materials: 2-acrylamido-2-methylpropanesulfonic acid, beta- (acryloyloxy) propionic acid, itaconic anhydride, unsaturated ionic compounds, unsaturated high temperature resistant monomers, initiators, chain transfer agents, complex inorganic substances and deionized water. The fluid loss agent has excellent high temperature resistance and good sedimentation stability, can improve the mechanical properties of cement, and has good market prospect.
Description
Technical Field
The invention belongs to the technical field of oil and gas well cementing additives, and particularly relates to a high-temperature-resistant oilfield cementing fluid loss agent and a preparation method thereof.
Background
With the rapid development of the economy in China, the demand for petroleum and natural gas resources is increasing, and the great energy demand is urgent to develop petroleum resources of deep stratum. Well cementation operation is an important link in oil and gas exploration, and as the process of exploring and exploiting oil and gas fields is continued, exploration and development face totally new challenges and difficulties. In the well cementation operation, water loss phenomenon is very easy to occur, and serious problems such as the rising of cement slurry density and the deterioration of cement slurry rheological property in the cement injection stage are caused; the displacement pressure breaks through the weak stratum to generate lost circulation phenomenon; bridge plugging of the annular space, mutual channeling of hydrocarbon reservoirs and the like.
At present, the oil gas exploration and development of China gradually advances towards deep and ultra-deep stratum, and severe stratum conditions such as ultra-high temperature, high pressure and the like provide serious challenges for the water loss reduction performance and sedimentation stability of well cementation cement paste. Under the ultra-high temperature environment, the well cementation cement slurry system has a serious dilution viscosity-reducing effect, and a large amount of cement particles are settled while free liquid is separated out.
Chinese patent CN 113651931A relates to an ultra-high temperature modified polymer type well cementation fluid loss agent, a preparation method and application thereof. The fluid loss agent provided by the invention has the advantages of stable performance, strong temperature resistance, excellent salt resistance and fluid loss reduction performance, strong adaptability, obvious improvement of mechanical properties of cement stones and the like. However, the obtained fluid loss agent has weak adsorptivity, and the influence on the mechanical properties of the cement stone is not disclosed.
Chinese patent CN 106977651B relates to a polymer/intercalated montmorillonite composite fluid loss agent and a preparation method thereof, wherein the fluid loss agent has a composite structure that a polymer is loaded in the intercalation of montmorillonite, and 2-acrylamide-2-methylpropanesulfonic acid, N-dimethylacrylamide and maleic anhydride are polymerized to form the polymer in the presence of an intercalating agent, water, a pH regulator, a defoaming agent, a molecular weight regulator, an anti-metal ion interfering agent and an initiator and are loaded in the intercalation of montmorillonite. However, the patent is not concerned with the study of the comprehensive properties of the high-temperature cement slurry at 80 ℃ or higher, and the degree of the temperature resistance is to be studied.
Therefore, there is a need for an oilfield cementing fluid loss agent, which has the characteristics of high temperature resistance and good sedimentation stability, so as to solve the problem of water loss in cementing operation in a higher oilfield environment.
Disclosure of Invention
Aiming at the prior art, the invention aims to provide the high-temperature-resistant oilfield cementing fluid loss agent and the preparation method thereof, and the fluid loss agent has excellent high temperature resistance and good sedimentation stability, can improve the mechanical property of cement, improves the compressive strength of the cement, and has good application value.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
The invention provides a high-temperature-resistant oilfield cementing fluid loss additive, which comprises the following raw materials: 2-acrylamido-2-methylpropanesulfonic acid, beta- (acryloyloxy) propionic acid, itaconic anhydride, unsaturated ionic compounds, unsaturated high temperature resistant monomers, initiators, chain transfer agents, complex inorganic substances and deionized water.
The reaction mechanism and action of the invention are as follows:
1. According to the fluid loss agent, the unsaturated ionic compound and the unsaturated high-temperature resistant monomer are introduced to strengthen the molecular structure of the copolymer, so that the performance of the fluid loss agent is strengthened by using a composite inorganic substance. The unsaturated high-temperature resistant monomer with high polymerization activity is adopted to replace the traditional amide monomer, the unsaturated ionic compound is introduced to improve the adsorptivity of the polymer, the unsaturated ionic compound has a synergistic effect with 2-acrylamido-2-methylpropanesulfonic acid, the stability of the polymer at high temperature is ensured, meanwhile, according to the idea of synergistic effect of dicarboxylic acid, beta- (acryloyloxy) propionic acid and itaconic anhydride are introduced, the adsorption efficiency of the polymer on the surface of cement particles and the adaptability of the polymer to materials are improved, and the mechanical strength of cement stone is not influenced while the adsorption and water loss reduction are realized; in addition, the chain transfer agent is added into the polymer, so that the molecular structure of the polymer can be reformed, and the molecular weight of the polymer is controlled, so that the fluid loss agent has the excellent properties of no thickening at low temperature and weak dispersion at high temperature.
2. The composite inorganic matter provided by the invention is formed by mixing modified graphene oxide and attapulgite. The applicant synergistically improves the high temperature resistance and the sedimentation stability of the fluid loss agent by regulating and controlling the proportion between the two.
On one hand, carboxyl on methylmalonic acid and amino of 2-aminofluorene are subjected to esterification reaction, carboxyl and hydroxyl are further utilized for dehydration and combination, and the esterification reaction product is grafted to the surface of graphene oxide through carboxyl on the other side of methylmalonic acid, so that the modified graphene oxide contains a fluorene ring structure, and the fluorene ring structure inhibits the thermal movement and internal rotation of a polymer chain segment, so that the polymer is endowed with higher rigidity, the thermal decomposition activation energy is further improved, and the polymer has good high temperature resistance. The modified graphene oxide is introduced into the molecular structure of the polymer, so that the influence of the 2-acrylamide-2-methylpropanesulfonic acid polymer on the cement hydration process can be obviously reduced, and the mechanical strength and durability of the cement-based material can be improved by regulating and controlling the pore structure, interface combination and other modes; meanwhile, the modified graphene oxide can improve the temperature resistance of the polymer fluid loss agent and the capability of controlling the fluid loss under the high-temperature and ultra-high-temperature conditions.
On the other hand, the organic copolymer is polymerized among the chain lamellar structures of the attapulgite, so that metal ions in the attapulgite and the polymer are subjected to electrostatic adsorption or complexation, the molecular chain conformation of the organic polymer is changed, the organic copolymer is better suspended and dispersed in cement paste along with the attapulgite, and good sedimentation stability of the fluid loss agent is provided; meanwhile, metal cations can have chelation reaction with carboxyl groups in the polymer, so that the high-temperature adaptability of the polymer is improved.
In some embodiments, the unsaturated ionic compound is an unsaturated cationic compound that is 2-methacryloyloxyethyl phosphorylcholine.
In some embodiments, the unsaturated high temperature resistant monomer is any one or more of N-vinyl pyrrolidone, sodium p-styrenesulfonate, and 4-acryloylmorpholine.
In some embodiments, the mass ratio of 2-acrylamido-2-methylpropanesulfonic acid, β - (acryloyloxy) propionic acid, itaconic anhydride, unsaturated ionic compound, and unsaturated high temperature resistant monomer is (25-40): (2-8): (3-8): (5-15): (2-6).
In some embodiments, the composite inorganic substance is modified graphene oxide and attapulgite in an amount of 0.2-0.5% of the total mass of 2-acrylamido-2-methylpropanesulfonic acid, beta- (acryloyloxy) propionic acid, itaconic anhydride, unsaturated ionic compound, and unsaturated high temperature resistant monomer.
Preferably, the mass ratio of the modified graphene oxide to the attapulgite is (1-2.5): 1.
Further preferably, the mass ratio of the modified graphene oxide to the attapulgite is 2:1.
In some embodiments, the method for preparing graphene oxide comprises the steps of:
(1) Adding methylmalonic acid and deionized water into a container, stirring to obtain a mixed solution 1, adding 2-aminofluorene and ethanol into the container, and stirring to obtain a mixed solution 2;
(2) Adding the mixed solution 1 and the mixed solution 2 obtained in the step (1) into a reaction kettle, adding a carbodiimide condensing agent and an activating agent, stirring, and reacting for 5-6h to obtain a reaction product;
(3) Adding graphene oxide and N, N-dimethylacetamide into a reaction kettle, stirring, adding concentrated sulfuric acid, reacting for 5-6 hours at 80-100 ℃, adding the reaction product obtained in the step (2), heating to 110-120 ℃, reacting for 3-4 hours, cooling, centrifuging, washing for 3-4 times with ethanol and water in sequence, and drying for 10-12 hours to obtain the modified graphene oxide.
In some embodiments, the molar ratio of methylmalonic acid to 2-aminofluorene in step (1) is 1: (1.05-1.8).
In some embodiments, the chain transfer agent is any one or more of hypophosphorous acid, n-butanethiol, n-dodecanethiol, 3-mercaptopropionic acid, and 2-mercaptoethanol in an amount of 0.05 to 0.8% of the total mass of 2-acrylamido-2-methylpropanesulfonic acid, β - (acryloyloxy) propionic acid, itaconic anhydride, unsaturated ionic compounds, and unsaturated high temperature resistant monomers.
In some embodiments, the initiator is any one or more of ammonium persulfate, potassium persulfate, and azobisiso Ding Mi, and is used in an amount of 0.4 to 0.8% of the total mass of 2-acrylamido-2-methylpropanesulfonic acid, β - (acryloyloxy) propionic acid, itaconic anhydride, unsaturated ionic compound, and unsaturated high temperature resistant monomer.
The invention also provides a preparation method of the high-temperature-resistant oilfield cementing fluid loss additive, which comprises the following steps:
s1, placing the composite inorganic matters into partial deionized water, and performing ultrasonic treatment for 30-60min to obtain a dispersion liquid;
S2, adding 2-acrylamido-2-methylpropanesulfonic acid, beta- (acryloyloxy) propionic acid, itaconic anhydride and the rest deionized water into a reaction kettle, stirring for 30-45min, regulating the pH to 5-6, adding an unsaturated ionic compound and an unsaturated high temperature resistant monomer, stirring for 50-70min, heating to 55-60 ℃, adding a chain transfer agent and an initiator, stirring for 20-30min, heating to 75-85 ℃, and reacting for 2-3h to obtain a polymer solution;
S3, adding the dispersion liquid obtained in the step S1 into the polymer solution obtained in the step S2, heating to 75-85 ℃, reacting for 40-50min, and cooling to room temperature to obtain the fluid loss agent.
Compared with the prior art, the invention has the following beneficial effects:
1. The fluid loss agent has excellent high temperature resistance and good sedimentation stability, and can improve the mechanical property of cement and the compressive strength of the cement.
2. The invention improves the integral performance of the polymerization product by synergistic dicarboxylic acid, effective introduction of high temperature resistant groups, intervention of unsaturated ionic compounds and optimization of molecular weight by using a chain transfer agent.
3. The composite inorganic matter is formed by mixing modified graphene oxide and attapulgite. The applicant can cooperatively improve the high temperature resistance and the sedimentation stability of the fluid loss agent by regulating and controlling the proportion between the two, and reduce the problems of pit shaft collapse, flow collapse and the like, thereby improving the production efficiency and the safety of an oil field.
Detailed Description
The invention will be described below in connection with specific embodiments. The following examples are illustrative of the present invention and are not intended to limit the present invention. Other combinations and various modifications within the spirit of the invention may be made without departing from the spirit or scope of the invention.
The fluid loss additives were prepared according to the ratios and the production methods of the respective raw materials specified in the following examples and comparative examples.
To facilitate the practice of the present invention by those skilled in the art, some of the raw material manufacturers of the examples and comparative examples will now be described as follows:
graphene oxide: purchased from wuhank biomedical technologies limited;
Other raw materials are available in the market without special description.
Preparation example 1
The preparation method of the modified graphene oxide A comprises the following steps:
(1) Adding 10g of methylmalonic acid and 10ml of deionized water into a container, stirring to obtain a mixed solution 1, adding 21.5g of 2-aminofluorene and 16ml of ethanol into the container, and stirring to obtain a mixed solution 2;
(2) Adding the mixed solution 1 and the mixed solution 2 obtained in the step (1) into a reaction kettle, adding 5g of (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 3g N-hydroxysuccinimide, stirring, and reacting for 5 hours to obtain a reaction product;
(3) Adding 5g of graphene oxide and 500ml of N, N-dimethylacetamide into a reaction kettle, stirring, adding 50ml of concentrated sulfuric acid, reacting for 5.5 hours at 90 ℃, adding the reaction product obtained in the step (2), heating to 120 ℃, reacting for 4 hours, cooling to room temperature, centrifuging, washing for 4 times sequentially with ethanol and water, and drying for 10 hours at 110 ℃ to obtain the modified graphene oxide A.
Preparation example 2
The preparation method of the modified graphene oxide B is the same as that of preparation example 1, except that 38.4g of 2-aminofluorene and 25ml of ethanol are added into a container in the step (1), and stirred to obtain a mixed solution 2.
Example 1
A high temperature resistant oilfield cementing fluid loss agent comprises the following raw materials: 32.5g of 2-acrylamido-2-methylpropanesulfonic acid, 5g of beta- (acryloyloxy) propionic acid, 5.5g of itaconic anhydride, 10g of 2-methacryloyloxyethyl phosphorylcholine, 4g of 4-acryloylmorpholine, 0.242g of ammonium persulfate, 0.342g of 2-mercaptoethanol, 0.13g of modified graphene oxide A, 0.07g of attapulgite and 228g of deionized water.
The preparation method of the oilfield cementing fluid loss agent comprises the following steps:
S1, placing modified graphene oxide A and attapulgite in part (accounting for 40% of the total mass of deionized water) of deionized water, and performing ultrasonic treatment for 45min to obtain a dispersion liquid;
S2, adding 2-acrylamido-2-methylpropanesulfonic acid, beta- (acryloyloxy) propionic acid, itaconic anhydride and the rest deionized water (accounting for 60% of the total mass of deionized water) into a reaction kettle, stirring for 40min, adjusting the pH to 6, adding 2-methacryloyloxyethyl phosphorylcholine and 4-acryloylmorpholine, stirring for 60min, heating to 60 ℃, adding 2-mercaptoethanol and ammonium persulfate, stirring for 25min, heating to 80 ℃, and reacting for 3h to obtain a polymer solution;
S3, adding the dispersion liquid obtained in the step S1 into the polymer solution obtained in the step S2, heating to 80 ℃, reacting for 45min, and cooling to room temperature to obtain the fluid loss agent.
Example 2
A high temperature resistant oilfield cementing fluid loss agent comprises the following raw materials: 25g of 2-acrylamido-2-methylpropanesulfonic acid, 2g of beta- (acryloyloxy) propionic acid, 3g of itaconic anhydride, 5g of 2-methacryloyloxyethyl phosphorylcholine, 2g of 4-acryloylmorpholine, 0.019g of ammonium persulfate, 0.148g of 2-mercaptoethanol, 0.037g of modified graphene oxide A, 0.037g of attapulgite and 148g of deionized water.
The preparation method of the oilfield cementing fluid loss additive is the same as that of the embodiment 1.
Example 3
A high temperature resistant oilfield cementing fluid loss agent comprises the following raw materials: 40g of 2-acrylamido-2-methylpropanesulfonic acid, 8g of beta- (acryloyloxy) propionic acid, 8g of itaconic anhydride, 15g of 2-methacryloyloxyethyl phosphorylcholine, 6g of 4-acryloylmorpholine, 0.616g of ammonium persulfate, 0.616g of 2-mercaptoethanol, 0.275g of modified graphene oxide A, 0.11g of attapulgite and 308g of deionized water.
The preparation method of the oilfield cementing fluid loss additive is the same as that of the embodiment 1.
Example 4
A high temperature resistant oilfield cementing fluid loss agent comprises the following raw materials: 28g of 2-acrylamido-2-methylpropanesulfonic acid, 10g of beta- (acryloyloxy) propionic acid, 2g of itaconic anhydride, 9g of 2-methacryloyloxyethyl phosphorylcholine, 8g of 4-acryloylmorpholine, 0.242g of ammonium persulfate, 0.348 g of 2-mercaptoethanol, 0.13g of modified graphene oxide A, 0.07g of attapulgite and 228g of deionized water.
The preparation method of the oilfield cementing fluid loss additive is the same as that of the embodiment 1.
Example 5
The concrete implementation mode of the high-temperature-resistant oilfield cementing fluid loss agent is the same as example 1, and the difference is that the modified graphene oxide A prepared by replacing the equivalent amount of commercially available graphene oxide.
Example 6
The specific implementation mode of the high-temperature-resistant oilfield cementing fluid loss agent is the same as example 1, and the difference is that the modified graphene oxide A is replaced by the equivalent modified graphene oxide B.
Comparative example 1
A high temperature resistant oilfield cementing fluid loss agent comprises the following raw materials: 32.5g of 2-acrylamido-2-methylpropanesulfonic acid, 9g of beta- (acryloyloxy) propionic acid, 5.5g of itaconic anhydride, 10g of 4-acryloylmorpholine, 0.242g of ammonium persulfate, 0.348 g of 2-mercaptoethanol, 0.13g of modified graphene oxide A, 0.07g of attapulgite and 228g of deionized water.
The preparation method of the oil field well cementation fluid loss agent of the comparative example is the same as that of example 1.
Comparative example 2
The concrete implementation mode of the high-temperature-resistant oilfield cementing fluid loss agent is the same as example 1, wherein 0.2g of modified graphene oxide A is used for replacing 0.13g of modified graphene oxide A and 0.07g of attapulgite.
The preparation method of the oil field well cementation fluid loss agent of the comparative example is the same as that of example 1.
Effect evaluation:
The lubricating oils prepared in examples 1 to 6 and comparative examples 1 to 2 above were subjected to API water loss, sedimentation stability and 72-hour compressive strength test analysis, and the specific results are shown in Table 1.
Performance test:
(1) According to the oil and gas industry standard SY/T5504.2-2013, part 2 of the evaluation method of oil well Cement Admixture: the fluid loss agent and the fluid loss agent of 5% bwoc # (note: # represents mass fraction of cement) are added according to the relevant regulations in national standard GB/T19139-2012 "oil well cement test method", and the API fluid loss and sedimentation stability of cement paste are tested at different test temperatures.
(2) According to the relevant regulations in oil and gas industry standard SY/T6466-2016 'oil well cement stone performance test method', the influence of the compressive strength of cement stone obtained after curing for 72 hours at 240 ℃ and 20MPa is examined.
Table 1 performance test
As shown in the results of Table 1, the fluid loss additives of examples 1 to 3 have excellent high temperature resistance and good sedimentation stability, and can improve the mechanical properties of cement and the compressive strength of cement.
Example 4 changed the mass ratio of five monomers, so that the overall performance of the fluid loss agent was greatly reduced. The modified graphene oxide A prepared by substituting the commercially available graphene oxide in the composite inorganic matter of the embodiment 5 lacks the introduction of a compound, so that the dispersibility of the graphene oxide in a system is reduced, the high temperature resistance and the sedimentation stability of the fluid loss agent are poor, and the mechanical property of cement is also reduced. Example 6 for the preparation of modified graphene oxide the molar ratio of methylmalonic acid to 2-aminofluorene was 1:2.5, the carboxyl on the methylmalonic acid is excessively reacted, and is difficult to combine with graphene oxide subsequently to enhance the compatibility of the methylmalonic acid, so that the high temperature resistance and the sedimentation stability of the fluid loss agent are reduced.
The comparative example 1 was free of the addition of an unsaturated ionic compound, which deteriorated the adsorptivity of the fluid loss agent, affected the sedimentation stability thereof, and further affected the high temperature resistance thereof. The inorganic substance in comparative example 2 is modified graphene oxide alone, and no attapulgite is added, so that electrostatic adsorption or complexation of the inorganic substance and the polymer is affected, and the sedimentation stability and the high temperature resistance of the fluid loss agent are also affected.
While the application has been described with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the application.
Claims (10)
1. The high-temperature-resistant oilfield cementing fluid loss agent is characterized by comprising the following raw materials: 2-acrylamido-2-methylpropanesulfonic acid, beta- (acryloyloxy) propionic acid, itaconic anhydride, unsaturated ionic compounds, unsaturated high temperature resistant monomers, initiator, chain transfer agent, composite inorganic matters and deionized water.
2. The high temperature resistant oilfield cementing fluid loss additive of claim 1, wherein the unsaturated ionic compound is an unsaturated cationic compound, and the unsaturated cationic compound is 2-methacryloyloxyethyl phosphorylcholine.
3. The high temperature resistant oilfield cementing fluid loss additive according to claim 1, wherein the unsaturated high temperature resistant monomer is any one or more of N-vinyl pyrrolidone, sodium p-styrenesulfonate and 4-acryloylmorpholine.
4. The high temperature resistant oilfield cementing fluid loss additive according to claim 1, wherein the mass ratio of the 2-acrylamido-2-methylpropanesulfonic acid, beta- (acryloyloxy) propionic acid, itaconic anhydride, unsaturated ionic compound and unsaturated high temperature resistant monomer is (25-40): (2-8): (3-8): (5-15): (2-6).
5. The high-temperature-resistant oilfield cementing fluid loss agent according to claim 1, wherein the composite inorganic matter is modified graphene oxide and attapulgite, and the dosage of the composite inorganic matter is 0.2-0.5% of the total mass of 2-acrylamido-2-methylpropanesulfonic acid, beta- (acryloyloxy) propionic acid, itaconic anhydride, unsaturated ionic compounds and unsaturated high-temperature-resistant monomers.
6. The high temperature resistant oilfield cementing fluid loss additive of claim 5, wherein the preparation method of the modified graphene oxide comprises the following steps:
(1) Adding methylmalonic acid and deionized water into a container, stirring to obtain a mixed solution 1, adding 2-aminofluorene and ethanol into the container, and stirring to obtain a mixed solution 2;
(2) Adding the mixed solution 1 and the mixed solution 2 obtained in the step (1) into a reaction kettle, adding a carbodiimide condensing agent and an activating agent, stirring, and reacting for 5-6h to obtain a reaction product;
(3) Adding graphene oxide and N, N-dimethylacetamide into a reaction kettle, stirring, adding concentrated sulfuric acid, reacting for 5-6 hours at 80-100 ℃, adding the reaction product obtained in the step (2), heating to 110-120 ℃, reacting for 3-4 hours, cooling, centrifuging, washing for 3-4 times with ethanol and water in sequence, and drying for 10-12 hours to obtain the modified graphene oxide.
7. The high temperature resistant oilfield cementing fluid loss additive of claim 6, wherein the molar ratio of the methylmalonic acid to the 2-aminofluorene in the step (1) is 1: (1.05-1.8).
8. The high-temperature-resistant oilfield cementing fluid loss additive according to claim 1, wherein the chain transfer agent is any one or more of hypophosphorous acid, n-butyl mercaptan, n-dodecyl mercaptan, 3-mercaptopropionic acid and 2-mercaptoethanol, and the amount of the chain transfer agent is 0.05-0.8% of the total mass of 2-acrylamido-2-methylpropanesulfonic acid, beta- (acryloyloxy) propionic acid, itaconic anhydride, unsaturated ionic compounds and unsaturated high-temperature-resistant monomers.
9. The high-temperature-resistant oilfield cementing fluid loss agent according to claim 1, wherein the initiator is any one or more of ammonium persulfate, potassium persulfate and azodiiso Ding Mi hydrochloride, and the dosage of the initiator is 0.4-0.8% of the total mass of 2-acrylamido-2-methylpropanesulfonic acid, beta- (acryloyloxy) propionic acid, itaconic anhydride, unsaturated ionic compounds and unsaturated high-temperature-resistant monomers.
10. A method for preparing the high-temperature-resistant oilfield cementing fluid loss additive according to any one of claims 1-9, which is characterized by comprising the following steps:
s1, placing the composite inorganic matters into partial deionized water, and performing ultrasonic treatment for 30-60min to obtain a dispersion liquid;
S2, adding 2-acrylamido-2-methylpropanesulfonic acid, beta- (acryloyloxy) propionic acid, itaconic anhydride and the rest deionized water into a reaction kettle, stirring for 30-45min, regulating the pH to 5-6, adding an unsaturated ionic compound and an unsaturated high temperature resistant monomer, stirring for 50-70min, heating to 55-60 ℃, adding a chain transfer agent and an initiator, stirring for 20-30min, heating to 75-85 ℃, and reacting for 2-3h to obtain a polymer solution;
S3, adding the dispersion liquid obtained in the step S1 into the polymer solution obtained in the step S2, heating to 75-85 ℃, reacting for 40-50min, and cooling to room temperature to obtain the fluid loss agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410334507.4A CN118240536A (en) | 2024-03-22 | 2024-03-22 | High-temperature-resistant oilfield cementing fluid loss agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410334507.4A CN118240536A (en) | 2024-03-22 | 2024-03-22 | High-temperature-resistant oilfield cementing fluid loss agent and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN118240536A true CN118240536A (en) | 2024-06-25 |
Family
ID=91550458
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410334507.4A Pending CN118240536A (en) | 2024-03-22 | 2024-03-22 | High-temperature-resistant oilfield cementing fluid loss agent and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN118240536A (en) |
-
2024
- 2024-03-22 CN CN202410334507.4A patent/CN118240536A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111875758B (en) | Preparation method of environment-friendly ultra-high temperature resistant filtrate reducer for water-based drilling fluid | |
| CN110204667B (en) | Polymer modified carbon microsphere and preparation method and application thereof | |
| CN108059697B (en) | Preparation method of polycarboxylate superplasticizer with regular sequence structure | |
| CN108715624B (en) | Ultrahigh-temperature-resistant composite-salt-resistant zwitterionic hydrophobically-associating polymer fluid loss agent and preparation method thereof | |
| CN111303846B (en) | Oil-gas well cementing brine high-density cement slurry | |
| CN113651931A (en) | Ultra-high temperature modified polymer cementing fluid loss agent and preparation method and application thereof | |
| CN111978001B (en) | Silane-containing polymer oil well cement dispersant, and preparation method and application thereof | |
| CN105601787A (en) | Method for preparing cement dispersant with both high water reduction effect and viscosity reduction effect | |
| CN114835850B (en) | Polymeric ionic liquid inhibitor and preparation method and application thereof | |
| CN113736016A (en) | High-temperature-resistant polymerization suspension stabilizer cement slurry for oil well cement and preparation method thereof | |
| CN114989351A (en) | Low-molecular-weight high-temperature-resistant saturated-salt-resistant filtrate reducer for water-based drilling fluid and preparation method and application thereof | |
| CN113563508B (en) | High-temperature-resistant low-viscosity filtrate reducer | |
| CN110818838B (en) | Drilling fluid treating agent and preparation method thereof | |
| CN112300346A (en) | Amphoteric ion grafted copolymer fluid loss agent and preparation method and application thereof | |
| CN118240536A (en) | High-temperature-resistant oilfield cementing fluid loss agent and preparation method thereof | |
| CN114773539B (en) | High-temperature-resistant high-salt-resistant micro-crosslinking hydrophobic association tackifying filtrate reducer for water-based drilling fluid and preparation method thereof | |
| CN114835848A (en) | Temperature-resistant salt-resistant fluid loss agent for well cementation and preparation method and application thereof | |
| CN112778990B (en) | Sewage mixing temporary plugging agent for oilfield water injection well and preparation method thereof | |
| CN114591464B (en) | Preparation method of filtrate reducer for drilling fluid and filtrate reducer | |
| CN114685734A (en) | Polymer-based nano-composite early strength agent and preparation method and application thereof | |
| CN116253832B (en) | Polymer for ultra-high temperature retarder, preparation method and ultra-high temperature retarder | |
| CN115505069B (en) | Low-molecular-weight ultrahigh-temperature well cementation fluid loss agent and preparation method and application thereof | |
| CN116284570B (en) | High-temperature-resistant high-salt-resistant filtrate reducer for water-based drilling fluid and preparation method and application thereof | |
| CN109824823B (en) | Temperature self-adaptive high-temperature retarder suitable for oil-gas well cementation, preparation method thereof and well cementation cement slurry | |
| CN113943401B (en) | Oil well cement dispersant and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication |