CN109852352A - A kind of organic phospho acid polymer fluid loss agent and its preparation method and application - Google Patents
A kind of organic phospho acid polymer fluid loss agent and its preparation method and application Download PDFInfo
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Abstract
This application provides a kind of organic phospho acid polymer fluid loss agents and its preparation method and application, the preparation method the following steps are included: by isopropylene and phosphonic acid monomer, acrylamide monomers and the monomer of carboxy-containing acid group initiator effect under carry out polymerization reaction, obtain organic phospho acid polymer fluid loss agent；The acrylamide monomers are selected from acrylamide, 2- Methacrylamide, N methacrylamide, N- ethyl acrylamide or N, N- dimethylacrylamide；The monomer of the carboxy-containing acid group is selected from acrylic acid or 2- methacrylic acid.Organic phospho acid polymer fluid loss agent provided by the invention includes: the first repetitive unit with 1 structure of formula, the second repetitive unit with 2 structure of formula and the third repeating unit with 3 structure of formula, can be used for preparing drilling fluid；It can be suitable for drilling fluid system with high salt with better saline-alkaline tolerance well, and preparation is easy.Formula 1Formula 2
Description
Technical field
The invention belongs to oilfield chemistry additive for drilling fluid technical field, it is related to a kind of drilling fluid filtrate reducer and its preparation
A kind of method, and in particular to organic phospho acid polymer fluid loss agent and its preparation method and application.
Background technique
In recent years, extensive with oil-gas exploration and development region, developed oil-gas Layer position is deeper and deeper, and geological conditions is more
Complexity, this proposes new challenge to the exploitation of additive for drilling fluid.Wherein, filtrate reducer for drilling fluid is dosage in drilling process
One of maximum inorganic agent occupies core position in all additive for drilling fluid, high to maintenance stabilizing mud properties, safety
Effect drilling well has important role.
In order to reduce drilling fluid leak-off water into stratum, guarantee chemistry used in property of drilling fluid and stabilizing borehole
Product are fluid loss additive or fluid loss agent.In the 1970s and 1980s in last century, foreign countries have developed intermediate molecular weight resistant to high temperatures poly- third
Olefin(e) acid salt fluid loss additive, polyacrylate better heat stability, but to use tolerance to high valence ion as fluid loss additive
Degree is poor.
Then, it develops in succession both at home and abroad with vinyl sulfonic acid monomer such as 2- acrylamide-2-methyl propane sulfonic (AMPS),
It is resistant to high temperatures, salt resistance calcium characteristic for the multiple copolymer of monomer with acrylamide, alkyl acrylamide, ethylene vinyl amide etc.
Polymer filtrate reducer.It is generally comprised in this quasi polymer fluid loss agent structure: n-vinyl-2-pyrrolidone, 2- acryloyl
The function monomers such as amido -2- methyl-propane sulfonic acid, show good polymerization activity and stability.But in complexity such as calcium with high salt
Operation block, still show many deficiencies, filtrate-loss control energy index is difficult to meet construction requirement.
Summary of the invention
In view of this, the application provides a kind of organic phospho acid polymer fluid loss agent and its preparation method and application, this hair
The organic phospho acid polymer fluid loss agent of bright offer has better saline-alkaline tolerance, can be suitable for wellbore fluid with high salt well
System.
The present invention provides a kind of organic phospho acid polymer fluid loss agent, including the first repetitive unit, tool with 1 structure of formula
There are the second repetitive unit of 2 structure of formula and the third repeating unit with 3 structure of formula:
In formula 1, R1Selected from hydrogen or methyl；In formula 2, R2And R3Independently selected from hydrogen, methyl or ethyl；Described first repeats
The molar ratio of unit, the second repetitive unit and the third repeating unit is (0.05~0.55): (0.2~0.8): (0.1~0.5).
Preferably, the pH value of the organic phospho acid polymer fluid loss agent is 7.5~8.5.
The present invention provides a kind of preparation method of organic phospho acid polymer fluid loss agent, comprising the following steps:
Isopropyl alkenyl phosphoric acid monomer, acrylamide monomers and the monomer of carboxy-containing acid group are gathered under initiator effect
Reaction is closed, organic phospho acid polymer fluid loss agent is obtained；
The acrylamide monomers are selected from acrylamide, 2- Methacrylamide, N methacrylamide, N- ethyl third
Acrylamide or N, N- dimethylacrylamide；The monomer of the carboxy-containing acid group is selected from acrylic acid or 2- methacrylic acid.
Preferably, the molar ratio of the isopropylene and phosphonic acid monomer, acrylamide monomers and the monomer of carboxy-containing acid group is
(0.1~0.5): (0.2~0.8): (0.05~0.55).
Preferably, the polymerization reaction initiator effect under carry out in water, the initiator be selected from ammonium persulfate or
Potassium peroxydisulfate.
Preferably, the quality of the initiator is the isopropylene and phosphonic acid monomer, acrylamide monomers and contains carboxylic acid group
The 0.1%~1.0% of monomer three's gross mass of group.
Preferably, the preparation method specifically:
Isopropylene and phosphonic acid monomer, acrylamide monomers and the monomer of carboxy-containing acid group are mixed, water is re-dissolved in, obtains list
Body aqueous solution；
It will be mixed after monomer solution heating with initiator solution, carry out polymerization reaction, neutralize after reaction
System to pH value is 7.5~8.5, obtains organic phospho acid polymer fluid loss agent.
Preferably, the temperature of the polymerization reaction is 80 DEG C~100 DEG C, and the time is 1~6 hour.
Preferably, the polymerization reaction carries out in the presence of protective gas, and the protective gas is argon gas.
The present invention also provides organic phospho acid polymer fluid loss agents as described above to prepare the application in drilling fluid.
Compared with prior art, the present invention provides a kind of organic phospho acid polymer fluid loss agent comprising shown in formula 1
The third repeating unit shown in second repetitive unit shown in one repetitive unit, formula 2 and formula 3.Organic phospho acid of the present invention is poly-
In the molecular structure for closing object fluid loss agent, the complexing power of phosphonic acid base and calcium ion is stronger, and product is enable to have stronger anticalcium
Power, it is more preferable to the applicability of drilling fluid system with high salt.
In addition, the preparation of organic phospho acid polymer fluid loss agent of the present invention is easy, it is suitable for industrial application.
Detailed description of the invention
Fig. 1 is the structural characterization result of 1 products therefrom of the embodiment of the present invention.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention provides a kind of organic phospho acid polymer fluid loss agent, including with 1 structure of formula the first repetitive unit,
The second repetitive unit with 2 structure of formula and the third repeating unit with 3 structure of formula:
In formula 1, R1Selected from hydrogen or methyl；In formula 2, R2And R3Independently selected from hydrogen, methyl or ethyl；Described first repeats
The molar ratio of unit, the second repetitive unit and the third repeating unit is (0.05~0.55): (0.2~0.8): (0.1~0.5).
Polymer fluid loss agent provided by the invention has better saline-alkaline tolerance, and existing drilling fluid drop can be overcome to lose
Aqua is the problem of high calcium system stability is strong, salt resistant character is poor, cannot be suitable for drilling fluid system with high salt well.
The molecular structure of polymer fluid loss agent provided by the invention include: the first repetitive unit with 1 structure of formula and
The second repetitive unit with 2 structure of formula.Contain carboxylic acid group (- COOH) in 1 structure of formula；In formula 1, R1Selected from hydrogen (H) or first
Base (CH3).In formula 2, R2And R3Independently selected from hydrogen (H), methyl (CH3) or ethyl (CH2CH3)。
Polymer fluid loss agent provided by the invention includes the third repeating unit with 3 structure of formula, includes in 3 structure of formula
Phosphorus oxygen double bond (P=O) and C-P key can be formed the structure by organic phospho acid.Organic phospho acid generally refers to have P-C bond structure
Organic phosphine oxygen acid, it, can be with Ca as a kind of strong electronic ligand for containing phosphorus oxygen double bond (P=O)2+、Mg2+、Al3+Plasma
Survivable strong chelate structure is formed at high temperature, and organic phosphonate generally has good water solubility, it can be very big
It avoids being precipitated in aqueous solution in degree, so as to improve the type additive for drilling fluid to the tolerance energy of high volence metal ion
Power.Secondly, organic phospho acid group is directly connected with C-P key with high molecular main chain or side chain compared with inorganic phosphate, overcome
Inorganic phosphate corrosivity is strong, is easy the shortcomings that being lost.Relative to sulfonic acid monomer common in additive for drilling fluid, organic phospho acid list
C-P key in body is stronger compared with C-S key, its intensity is at least suitable with C-C bond strength.Also, C-P key has very strong anti-oxidant
And hydrolysis resistance, it is even more more stable than C-C key in this respect.Therefore, organic phospho acid polymer fluid loss agent of the present invention
Molecular structure in, the complexing power of phosphonic acid base and calcium ion is stronger, product have stronger anticalcium ability.
In the present invention, the molar ratio of first repetitive unit, the second repetitive unit and the third repeating unit is (0.05
~0.55): (0.2~0.8): (0.1~0.5).In an embodiment of the present invention, the knot of the organic phospho acid polymer fluid loss agent
Structure formula can are as follows:
In formula 4, m, n, o are respectively the molal quantity of above-mentioned repetitive unit, m:n:o=(0.05~0.55): (0.2~0.8):
(0.1~0.5).Wherein, the present invention not connection type between the above-mentioned repetitive unit of particular determination.In some realities of the invention
It applies in example, the pH value of the organic phospho acid polymer fluid loss agent can be 7.5~8.5, if pH value is 8.
Meanwhile the present invention provides a kind of preparation methods of organic phospho acid polymer fluid loss agent, comprising the following steps: will
Isopropylene and phosphonic acid monomer, acrylamide monomers and the monomer of carboxy-containing acid group carry out polymerization reaction under initiator effect, obtain
To organic phospho acid polymer fluid loss agent；
The acrylamide monomers are selected from acrylamide, 2- Methacrylamide, N methacrylamide, N- ethyl third
Acrylamide or N, N- dimethylacrylamide；The monomer of the carboxy-containing acid group is selected from acrylic acid or 2- methacrylic acid.
The present invention is based on isopropylene and phosphonic acid (IPPA) monomers to pass through polymerization reaction, forms organic phospho acid high molecular material.Tool
Body, the present invention polymerize anti-using isopropylene and phosphonic acid, acrylamides and the compound of carboxy-containing acid group as monomer
It answers.Wherein, the acrylamide monomers are selected from acrylamide, 2- Methacrylamide, N methacrylamide, N- ethyl third
Acrylamide or N, N- dimethylacrylamide；The monomer of the carboxy-containing acid group is selected from acrylic acid or 2- methacrylic acid.At this
In invention, molar ratio (the i.e. amount of substance of the isopropylene and phosphonic acid monomer, acrylamide monomers and the monomer of carboxy-containing acid group
The ratio of n) preferably (0.1~0.5): (0.2~0.8): (0.05~0.55)；Also referred to as 10%~50%:20%~
80%:5%~55%.The amount of substance is used herein as unified unit；Cause polymerization can be obtained different molecular weight model later
The mixture enclosed.
Polymerization reaction of the present invention carries out under initiator effect, and the initiator is preferably ammonium persulfate or persulfuric acid
Potassium.Preferably, the quality that the initiator is added is the isopropylene and phosphonic acid monomer, acrylamide monomers and contains carboxylic acid group
The 0.1%~1.0% of monomer three's gross mass of group, more preferably 0.15%~0.9%.
In a preferred embodiment of the invention, the solvent of above-mentioned polymerization reaction is water.The polymerization reaction is preferably being protected
It is carried out in the presence of gas, the protective gas can be argon gas.The temperature of the polymerization reaction is preferably 80 DEG C~100 DEG C, the time
It can be 1 hour~6 hours.
The present invention is not particularly limited the charging sequence of reaction；The preparation method is preferred specifically: by isopropyl alkene phosphine
Acid monomers, acrylamide monomers and the mixing of the monomer of carboxy-containing acid group, are re-dissolved in water, obtain monomer (mixture) aqueous solution；
The monomer solution is mixed with initiator solution, polymerization reaction is carried out, obtains organic phospho acid polymer fluid loss agent.
Wherein, the embodiment of the present invention mixes three kinds of monomers according to the mass ratio of the material example, and gained monomer mixture is dissolved in
Water can be made into the monomer solution that mass fraction is 10%~50%.Also, will account for monomer mixture gross mass be 0.1%~
1.0% initiator is made into 2.0% initiator solution.Reaction kettle can be added in monomer mixture solution by the embodiment of the present invention
In, the air being passed through in argon gas emptying system, and it is warming up to initial temperature.The embodiment of the present invention is by the monomer solution liter
Temperature adds initiator solution after being preferably warming up to 50 DEG C~80 DEG C；Reaction kettle is added portionwise in the initiator solution
In, speed is added and is subject to temperature of reaction kettle no more than 90 DEG C.After to be triggered dose of aqueous solution adds, system temperature is warming up to 80
DEG C~100 DEG C react 1~6 hour.
After reaction, the present invention can be by system alkali neutralization, until pH value is 7.5~8.5, obtained product is by drying
Dry, crushing is to get drilling fluid filtrate reducer.The embodiment of the present invention is prepared by control group ratio and reaction condition etc.
Organic phospho acid polymer fluid loss agent, can meet the wellbore construction requirement on calcium stratum with high salt.
In addition, the present invention also provides organic phospho acid polymer fluid loss agents as described above in preparing drilling fluid
Using.
A certain amount of synthesized polymer can be added in the present invention in base slurry, and high-speed stirred 5min is put into height after placing 6h
In 120 DEG C, 135 DEG C of rolling aging 16h in warm roller furnace, then takes out, be down to room temperature, high-speed stirred 5min, according to GB/T
Filter pressing loss in the room temperature of the regulation measurement drilling fluid of 16783.1-20067.2,24 DEG C ± 3 DEG C of temperature, pressure 690KPa.Its
In, the base slurry can be the compound salt slurries of this field routine；And synthesized polymer dosage can be 1%~2% (this field
" dosage " concept known to technical staff).In addition, type, dosage etc. of the present invention to other inorganic agents in the drilling fluid of preparation
It is not particularly limited.
According to measurement result, organic phospho acid polymer drilling fluid fluid loss additive of the invention is in compound salt-water drilling fluid
In, after 120 DEG C/16h, 135 DEG C/16h aging, significant filtrate reducing effect is shown, anticalcium ability is excellent.
For a further understanding of the application, dehydration is dropped to organic phospho acid polymer provided by the present application below with reference to embodiment
Agent and its preparation method and application is specifically described.
Embodiment 1
It is 10% according to the mass ratio of the material by isopropylene and phosphonic acid (IPPA) and acrylamide (AM) and acrylic acid (AA):
70%:20% mixing is made into the monomer mixture aqueous solution that mass fraction is 30%；Monomer mixture gross mass, which will be accounted for, is
0.3% potassium peroxydisulfate is made into 2.0% initiator solution.
The monomer mixture solution is added in reaction kettle, the air being passed through in argon gas emptying system, and is warming up to 60
℃；The initiator solution is added portionwise in the reaction kettle, speed is added and is subject to temperature of reaction kettle no more than 90 DEG C；To
After initiator solution adds, system temperature is warming up to 80 DEG C and is reacted 2 hours, after reaction, in sodium hydroxide and body
System to pH value is 8, and obtained product, to get drilling fluid filtrate reducer containing phosphine, is white powder by drying, crushing.
By products therefrom through IR Characterization, as a result as shown in Figure 1.3334cm in Fig. 1-1It is-CONH2Group vibration peak,
3186cm-1It is-OH group vibration peak, 2937cm-1It is-CH2Group vibration peak, 1659cm-1It is that-C=O group stretching vibration is inhaled
Receive peak, 1048cm-1It is-P=O group stretching vibration absworption peak；According to above each absorption peak and analysis, the production of synthesis can be determined
Object is target product.
Embodiment 2~9
According to the method for embodiment 1, organic phospho acid polymer fluid loss agent is prepared respectively；Different formulas and condition
It is shown in Table 1:
The substance dosage and reaction condition of polymerization reaction in 1 embodiment 2~9 of table
Comparative example
By acrylamide (AM) monomer and acrylic acid (AA) monomer, the amount proportion according to substance is 70%:30% mixing, and
It is made into 30% monomer mixture aqueous solution of mass fraction；The initiator ammonium persulfate for accounting for monomer gross mass 0.2% is made into 10%
Aqueous solution.
Reaction kettle is warming up to 65 DEG C, the reaction kettle is added portionwise in above-mentioned monomer mixture solution and initiator solution
In, speed is added and is subject to temperature of reaction kettle no more than 80 DEG C, after monomer mixture aqueous solution and initiator solution add,
System is warming up to 90 DEG C of reaction 5h, after reaction, in sodium hydroxide and system to pH value be 8, obtain sticky shape product,
P (AA/AM) drilling fluid fluid loss agent is obtained after dried, crushed.
Embodiment 10
Filtrate reducing effect assessment is carried out to above-described embodiment and comparative example products obtained therefrom, evaluation is starched with base and method is as follows:
(1) compound salt slurries are prepared
It measures 350mL distilled water to be placed in cup, 16.0g sodium chloride, 2.6g anhydrous calcium chloride, 6.9g magnesium chloride is added, to
52.5g calcium bentonite (calcium bentonite meets GB/T20973-2007 standard) and 3.15g natrium carbonicum calcinatum is added in it after dissolving, high
Speed stirring 20min, at least during the stop two times, to scrape clay adhered to the wall of the container, the curing in airtight condition at 24 DEG C ± 3 DEG C
For 24 hours, as compound salt slurries.
(2) drilling fluid filtration is tested
A certain amount of synthesized polymer is added into the slurry of base obtained by (1), high-speed stirred 5min is put into height after placing 6h
In 120 DEG C, 135 DEG C of rolling aging 16h in warm roller furnace, then takes out, be down to room temperature, high-speed stirred 5min, according to GB/T
Filter pressing loss in the room temperature of the regulation measurement drilling fluid of 16783.1-20067.2,24 DEG C ± 3 DEG C of temperature, pressure 690KPa.
(3) evaluation result is shown in Table 2.
Result after 2. drilling fluid room temperature of table and high temperature ageing
From measurement result as can be seen that organic phospho acid polymer drilling fluid fluid loss additive of the invention is in complex salt water drilling
In well liquid, significant filtrate reducing effect is shown after 120 DEG C/16h, 135 DEG C/16h aging, result is better than comparative example
Acrylic acid and acrylamide bipolymer drilling fluid fluid loss agent, show good anticalcium ability.
The above is only a preferred embodiment of the present invention, it is noted that for making the professional technique of the art
Personnel are that by various modifications to these embodiments without departing from the technical principles of the invention, and these
Modification also should be regarded as the range that the present invention should protect.
Claims (10)
1. a kind of organic phospho acid polymer fluid loss agent, including with 1 structure of formula the first repetitive unit, with 2 structure of formula
Second repetitive unit and the third repeating unit with 3 structure of formula:
In formula 1, R1Selected from hydrogen or methyl；In formula 2, R2And R3Independently selected from hydrogen, methyl or ethyl；First repetitive unit,
The molar ratio of second repetitive unit and the third repeating unit is (0.05~0.55): (0.2~0.8): (0.1~0.5).
2. organic phospho acid polymer fluid loss agent according to claim 1, which is characterized in that the organic phospho acid polymer
The pH value of fluid loss agent is 7.5~8.5.
3. a kind of preparation method of organic phospho acid polymer fluid loss agent, comprising the following steps:
Isopropylene and phosphonic acid monomer, acrylamide monomers and the monomer of carboxy-containing acid group polymerize instead under initiator effect
It answers, obtains organic phospho acid polymer fluid loss agent；
The acrylamide monomers are selected from acrylamide, 2- Methacrylamide, N methacrylamide, N- ethyl propylene acyl
Amine or N, N- dimethylacrylamide；The monomer of the carboxy-containing acid group is selected from acrylic acid or 2- methacrylic acid.
4. preparation method according to claim 3, which is characterized in that the isopropylene and phosphonic acid monomer, acrylic amide list
The molar ratio of body and the monomer of carboxy-containing acid group is (0.1~0.5): (0.2~0.8): (0.05~0.55).
5. preparation method according to claim 3, which is characterized in that the polymerization reaction initiator effect under in water
It carries out, the initiator is selected from ammonium persulfate or potassium peroxydisulfate.
6. preparation method according to claim 5, which is characterized in that the quality of the initiator is the isopropylene and phosphonic acid
The 0.1%~1.0% of monomer, acrylamide monomers and the monomer of carboxy-containing acid group three's gross mass.
7. preparation method according to claim 5, which is characterized in that the preparation method specifically:
Isopropylene and phosphonic acid monomer, acrylamide monomers and the monomer of carboxy-containing acid group are mixed, water is re-dissolved in, obtains monomer water
Solution；
It will be mixed after monomer solution heating with initiator solution, carry out polymerization reaction, neutralize system after reaction
It is 7.5~8.5 to pH value, obtains organic phospho acid polymer fluid loss agent.
8. the preparation method according to any one of claim 3~7, which is characterized in that the temperature of the polymerization reaction is
80 DEG C~100 DEG C, the time is 1~6 hour.
9. the preparation method according to any one of claim 3~7, which is characterized in that the polymerization reaction is in protection gas
It is carried out in the presence of body, the protective gas is argon gas.
10. as appointed in organic phospho acid polymer fluid loss agent according to any one of claims 1 to 2 or claim 3~9
The organic phospho acid polymer fluid loss agent that preparation method described in one obtains is preparing the application in drilling fluid.
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| CN115322283A (en) * | 2022-09-23 | 2022-11-11 | 爱森（中国）絮凝剂有限公司 | Preparation method of anti-scaling, anti-drag and thickening integrated fracturing emulsion |
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| CN114437290A (en) * | 2020-11-03 | 2022-05-06 | 中石化石油工程技术服务有限公司 | Low-viscosity organic phosphonic acid polymer fluid loss agent, preparation method and application thereof |
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| CN115322283A (en) * | 2022-09-23 | 2022-11-11 | 爱森（中国）絮凝剂有限公司 | Preparation method of anti-scaling, anti-drag and thickening integrated fracturing emulsion |
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