CN104926991B - A kind of preparation method of drilling fluid amphoteric ion copolymer - Google Patents

A kind of preparation method of drilling fluid amphoteric ion copolymer Download PDF

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CN104926991B
CN104926991B CN201410100622.1A CN201410100622A CN104926991B CN 104926991 B CN104926991 B CN 104926991B CN 201410100622 A CN201410100622 A CN 201410100622A CN 104926991 B CN104926991 B CN 104926991B
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salt
sulfonic acid
propane sulfonic
vinylpridine
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CN104926991A (en
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杨超
鲁娇
陈楠
张志智
尹泽群
刘全杰
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China Petroleum and Chemical Corp
Sinopec Fushun Research Institute of Petroleum and Petrochemicals
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China Petroleum and Chemical Corp
Sinopec Fushun Research Institute of Petroleum and Petrochemicals
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Abstract

The present invention provides a kind of preparation method of drilling fluid amphoteric ion copolymer, and N, N dimethyl-allyl propane sulfonic acid salt and 4 vinylpyridine propane sulfonic acid inner salts are respectively synthesized first;Proportionally by N, N dimethyl-allyl propane sulfonic acid salt, acrylamide and 4 vinylpyridine propane sulfonic acid inner salts are passed through N after adding solvent dissolving2Deoxygenation is reacted, and obtains gelatinous solid after then adding initiator for reaction, white depositions are obtained with acetone precipitation;Obtained sediment is crushed after drying, final to obtain amphoteric ion copolymer.The polymer that the inventive method is obtained can heatproof be up to 210 DEG C, anti-NaCl saturations, anti-CaCl2Saturation, and reduce with the filtrate reducing amount of the increase polymer of salt amount, while also having superior shale inhibition energy.

Description

A kind of preparation method of drilling fluid amphoteric ion copolymer
Technical field
It is more particularly to a kind of to bore the present invention relates to drilling fluid polymer and preparation method thereof is used in Process of Oil Well Drilling The preparation method of well liquid amphoteric ion copolymer.
Background technology
Species complexity that polymer for drilling fluid is related to is various, Various Functions, but fluid loss additive therein is mostly important, is The maximum polymer treatment agent of consumption.Fluid loss additive is to ensure stabilizing mud properties, reduces harmful liquid invaded formation, And ensure hole diameter rule, the important additive for drilling fluid of stabilizing borehole.As drilling strata is increasingly sophisticated, and exceptional well, Increasing for ultradeep well and Holes of Complicated Wells quantity, higher requirement is proposed to filtrate reducer for drilling fluid, to meet salt tolerance(NaCl is dense Degree is more than 10%, CaCl2Concentration is more than 5%)And temperature tolerance(Temperature is higher than 150 DEG C)New demand.Gelatinized starch, carboxymethyl are fine It is all the filtrate reducer for drilling fluid used earliest to tie up element, lignite etc..With research deepen continuously and drilling strata increasingly Complexity, the need for existing natural and natural modified fluid loss additive can not meet drilling condition, so as to promote people The research and development of work synthesized polymer species fluid loss additive.
Due to both containing the cation group with absorption and aquation double action in amphoteric ion polymer, again containing big The aquation group of amount, can form the hydrated sheath of densification around clay particle, prevent and delay hydrone to be connect with surface of clay Touch, play a part of preventing clay particle hydration swelling;Cation group and anionic group are ionized in water not by outside heating Influence, it is also possible to prevent the hydrolysis of amide groups, therefore amphoteric ion polymer also has the advantages that temperature-resistant anti-salt, it is studied Just progressively it is being taken seriously with development and application.Yang little Hua uses MAOPS, AM and AA to synthesize amphoteric ion sulphonate polymer CPS- 2000, be respectively provided with various drilling fluid systems stronger filtrate reducing, carry it is glutinous cut ability and inhibition effect, also with stronger Resistance to gentle salt resistance, anticalcium ability.Yang Jinrong has synthesized amphion using redox system as initiator using aqueous solution polymerization Quadripolymer:Polyacrylamide-dimethyl diallyl ammonium chloride -2- acrylamide-2-methylpro panesulfonic acids sodium-methyl Acrylic acid(PADAM), with stronger drop dehydration ability and inhibition, preferable salt tolerance and temperature tolerance.Zheng Haihong is with propylene Acid amides(AM), 2- acrylamide-2-methyl propane sulfonics(AMPS), dimethyl diallyl ammonium chloride(DMDAAC)With maleic two Acid anhydrides(MA)For monomer, using aqueous solution polymerization method, synthesized by initiator of ammonium persulfate/sodium hydrogensulfite both sexes from Sub- polymer filtrate reducer PA-1, heat endurance is good, and filtrate reducing ability and temperature resistance ability are strong.Yang Wen is with dimethyl diallyl chlorine Change ammonium(DMDAAC), 2- acrylamide-2-methylpro panesulfonic acids(AMPS), maleic anhydride(MA), acrylamide(AM)For monomer, Redox system is initiator, and amphoteric ion polymer fluid loss additive PMADA has been synthesized using water solution polymerization process.He Aimin The AEDMAC/AM/AA ampholyte copolymer fluid loss additives synthesized using aqueous solution polymerization method, with good filtrate reducing, are prevented Collapse, reservoir protec-tion performance, temperature resistance, salt-resistance are preferable.Chinese patent CN2008100472416 is with acrylamide 2- acrylamides Base -2- methyl propane sulfonic acids are monomer, and a kind of amphoteric ion polymer fluid loss additive, temperature resistance salt tolerant have been synthesized using aqueous solution polymerization Property is stronger.
But the preparation of above-mentioned amphoteric ion polymer is obtained by anions and canons monomer copolymerization.Due to by cation Anion-content is significantly larger than cations in the limitation of monomer reactivity and reactivity ratio, copolymer, causes in copolymer The quantity of positive and negative charge is unequal, does not reach preferable " anti-polyelectrolyte " effect, and polymer anti-calcium and anti-salt performance is limited.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of preparation method of drilling fluid amphoteric ion copolymer.This The polymer that inventive method is obtained can heatproof be up to 210 DEG C, anti-NaCl saturations, anti-CaCl2Saturation, and polymerize with the increase of salt amount The filtrate reducing amount of thing reduces, while also having superior shale inhibition energy.
The structure of drilling fluid amphoteric ion copolymer prepared by the present invention is as follows:
The preparation method of drilling fluid amphoteric ion copolymer of the present invention comprises the following steps:
(1)It is 2 to weigh mol ratio respectively first:1~8:1 N, N- DMAA and PS, And to N, PS is added in N- DMAAs, 0.5~4h is then reacted at a temperature of 10~60 DEG C, Eventually pass filter, extracting, dry obtained N, N- dimethyl-allyl propane sulfonic acid salt;
(2)It is 1 according to mol ratio:1.1~1:1.3 weigh 4-vinylpridine and PS respectively, then Weigh organic solvent and auxiliary agent, the total mass ratio of organic solvent and 4-vinylpridine and PS is 2:1~8: 1, the total mass ratio of auxiliary agent and 4-vinylpridine, PS and organic solvent is 0.001~0.01, then will be had Machine solvent is divided into three parts, is mixed respectively with 4-vinylpridine, PS, auxiliary agent dissolving, by obtain three Plant mixed solution and sequentially add reactor, 1~10h is reacted under the conditions of 20 DEG C~90 DEG C, then through filtering, washing, dry system Obtain 4-vinylpridine propane sulfonic acid inner salt;
(3)According to(4~3):(5~6):(0.5~1)Mol ratio weigh step respectively(1)Obtained N, N- dimethyl Pi-allyl propane sulfonic acid salt, acrylamide and step(2)4-vinylpridine propane sulfonic acid inner salt is obtained, is led to after adding solvent dissolving Enter N20.5~1h of deoxygenation, while addition 4~6h of initiator for reaction after 50~70 DEG C, 5~10min of constant temperature is warming up to, after reaction To gelatinous solid, white depositions are obtained with acetone precipitation;
(4)By step(3)Obtained sediment is dried after 16~24h at 100~120 DEG C and crushed, final both sexes from Sub- copolymer.
In the inventive method, step(1)The mol ratio of middle N, N- DMAA and PS is 3:1 ~5:1.
In the inventive method, step(1)Middle PS is added drop-wise in N, N- DMAAs or straight Connect and be disposably added in N, N- DMAAs, be preferably directly added into mode.Weighed during using directly disposable addition N, N- DMAAs and PS mol ratio are 5:1~8:1.Using N, N- dimethyl during the mode of dropwise addition Allyl amine and PS mol ratio are 2:1~5:1, PS can be heated and melted before dropwise addition.
In the inventive method, step(1)Reaction condition be at a temperature of 20~55 DEG C react 1~3h.
In the inventive method, step(1)Middle extraction solvent select methanol or ethanol, preferred alcohol, extraction times be 1~ 3h.The drying is that 10~20h is dried under the conditions of 30~50 DEG C.
In the inventive method, step(2)Described in organic solvent be benzene, toluene, ethyl acetate, acetone, cyclohexanone, carbonic acid Any of propylene.
In the inventive method, step(2)Described in auxiliary agent be hydroxylamine compound and nitrobenzene compounds, wherein azanol Class compound is dimethyl hydroxylamine, diethyl hydroxylamine, dipropyl azanol, isopropylhydroxyla, dibutylhydroxylamine, methyl ethylhydroxylamine Any of;Nitrobenzene compounds are 1,2- dinitro benzenes, 1,3- dinitro benzenes, 1,4- dinitro benzenes, the nitre of 1,3,5- tri- Any of base benzene.
In the inventive method, step(2)Described in filter operation be transferred in funnel for obtained product will be reacted and filter Remove solvent and unreacted raw material, it is preferable to use Buchner funnel carries out decompression suction filtration.
In the inventive method, step(2)Described in washing operation to use step(2)Described in organic solvent washing 2~5 It is secondary.
In the inventive method, step(2)Described in dry be at 40~60 DEG C dry 10~20h.
In the inventive method, step(3)Described in solvent be deionized water or salt solution, add solvent after monomer gross mass Concentration is 20%~40%, and the NaCl concentration added in the salt solution is 0~0.5mol/L.
In the inventive method, step(3)The middle initiator used is any in potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate Kind;The initiator amount accounts for the 0.9%~1.3% of monomer gross mass.
Compared with prior art, the inventive method advantage is as follows:
(1)PS is added in excessive N, N- DMAAs by the inventive method, excessive N, N- DMAA act not only as raw material and participate in reaction, and can play a part of solvent, it is to avoid often Use poisonous acetone to be solvent in rule method, be a kind of green synthetic method.
(2)The inventive method is by controlling PS and N, and N- DMAAs mole when feed intake Mode, solves PS and N, when N- DMAAs are conventionally directly reacted(Typically It is that equimolar ratio reacts), it is impossible to the problem of obtaining monomer N, N- dimethyl-allyl propane sulfonic acid salt.
(3)The inventive method causes the 4-vinylpridine propane sulfonic acid inner salt that synthesis is obtained by adding auxiliary agent, not only Product yield is high, up to more than 90%, and needs not move through re-crystallization step and directly obtain high purity product, and product is powder Shape, product purity >=95%.The inventive method has the reaction time short, simple to operate, reacts post-reactor not kiss-coating, it is easy to clear Maintenance is washed, is conducive to industrialized production, suitable for commercial Application.
(4)Amphoteric ion copolymer prepared by the inventive method, N, N- dimethyl-allyl propane sulfonic acid salt and 4- vinyl Pyridine propane sulfonic acid inner salt is macromolecular polymeric monomer, and the polymer that its copolymerization is obtained has long-chain branch.In aqueous by In the presence of long-chain branch, add the steric hindrance of polymer, increase the hydrodynamic volume of polymer, cause polymer by The trend of temperature influence fracture hydrolysis is reduced, so as to improve the performance of its heatproof, heatproof is up to 210 DEG C.
(5)Salt form amphoteric ion polymer in amphoteric ion copolymer category prepared by the inventive method, with traditional both sexes from Unlike sub- polymer, it is intermolecular due to electrostatic attraction effect in fresh water, shows as strand and curls.And in high salt In high calcium solution, due to the presence of small molecule salt, intermolecular association is shielded, intermolecular electrostatic attraction is changed For electrostatic repulsion forces so that strand is more unfolded.Obvious " anti-polyelectrolyte " effect that it is shown makes the property of polymer Can gradually it strengthen with the increase of salt amount.Can anti-NaCl saturations and CaCl2Saturation, this is current almost all of zwitterion polymerization The anti-calcium and anti-salt performance that thing does not possess.Also contain substantial amounts of quaternary ammonium in amphoteric ion copolymer structure prepared by the inventive method Cation group, enables polymer to have superior shale inhibition.
Embodiment
The effect and effect of the inventive method are illustrated with reference to embodiment, but following examples are not constituted to this The limitation of scheme of the invention.
Embodiment 1
Prepare N, N- DMAA propane sulfonic acid salt
Weigh 430g N, N- DMAAs(DA)Pour into reactor, be then placed in thermostat water bath, heat And start stirring.122g1,3-N-morpholinopropanesulfonic acid lactone are weighed again(PS), it is added directly into DA, reaction temperature is 45 DEG C, and stirring is anti- Answer and N is obtained after 3h, N- dimethyl-allyl propane sulfonic acid salt(DAPS)Crude product.DAPS crude products are transferred in large stretch of filter paper Wrap, be positioned in Soxhlet extraction device, the use of ethanol is solvent extraction 3h, filter paper bag is placed on drying box by extracting after finishing In, dried at 50 DEG C, finally give pure DAPS monomers, yield is 93.7%.
Comparative example 1(Directly react)
According to stoichiometric proportion DA:PS is 1:1 reaction.Weigh 85gDA to pour into reactor, be then placed in thermostat water bath In, heat and start stirring.122gPS is weighed again, is added directly into DA, and reaction temperature is 20 DEG C, after stirring reaction 0.5h To mass polymerization product, without DAPS monomers, yield is 0.During according to stoichiometric reaction, substantial amounts of hot nothing is produced in reaction Method disperses in time, and temperature moment steeply rises, and causes raw material DA and product DAPS all to polymerize.
Comparative example 2(Conventional method, using acetone as solvent reaction)
Weigh 90gDA to pour into reactor, be then placed in thermostat water bath, heat and start stirring.Weigh again 122gPS is dissolved in 650g acetone, and mixed solution is added directly into DA, and reaction temperature is 60 DEG C, obtains after stirring reaction 4h DAPS crude product.DAPS crude products are transferred in large stretch of filter paper and wrapped, are positioned in Soxhlet extraction device, are using ethanol Filter paper bag is placed in drying box by solvent extraction 2h, extracting after finishing, and is dried at 35 DEG C, is finally given pure DAPS mono- Body, yield is 81.5%.
Embodiment 2
Prepare 4-vinylpridine propane sulfonic acid inner salt(VPPS)
(1)105g 4-vinylpridine is weighed respectively(4-VP), 125g PS(PS), 500g has The diethyl hydroxylamine of machine solvent benzol, 0.75g;
(2)Organic solvent-benzene is divided into three parts, respectively with 4-vinylpridine, PS, auxiliary agent two Ethylhydroxyl amine dissolving mixing;
(3)Obtain three kinds of mixed solutions are sequentially added into reactor, 2h is reacted at 70 DEG C, then through depressurizing suction filtration, Then washed 2~3 times using benzene, 15h is dried at 50 DEG C, 4-vinylpridine propane sulfonic acid inner salt is made(VPPS), through meter Calculation finally gives faint yellow solid powdery product 2136g.
Embodiment 3
72gDAPS, 42g acrylamides are weighed respectively(AM), 11gVPPS adds to be transferred to instead after a certain amount of deionized water dissolving Device is answered, total monomer is 25%.It is passed through N2Deoxygenation 1h, while being warming up to 65 DEG C, keeps adding 1.3g potassium peroxydisulfates after 30min, Gelatinous solid is obtained after reaction 6h, white depositions are obtained with acetone precipitation.Dry after 24h and crush at 110 DEG C, it is final to obtain two Property ionic copolymer.
Embodiment 4
Weigh and be transferred to after 82gDAPS, 35gAM, 22gVPPS, 13gNaCl, plus a certain amount of deionized water dissolving instead respectively Device is answered, total monomer is 40%.It is passed through N2Deoxygenation 1h, while being warming up to 55 DEG C, keeps adding 1.8g ammonium persulfates after 30min, Gelatinous solid is obtained after reaction 5h, white depositions are obtained with acetone precipitation.Dry after 24h and crush at 110 DEG C, it is final to obtain two Property ionic copolymer.
Comparative example 3
Traditional zwitterionic monomer A, AMPS/AM/DMDAAC terpolymers synthetic method presses document《AM / AMPS / DMDAAC copolymers are synthesized and its filtrate loss controllability research》(Wang Chunhua, 2012《Shandong chemical industry》)It is prepared by report method.
Comparative example 4
Traditional zwitterionic monomer B, AMPS/AM/AA/ cationic monomer quadripolymer synthetic method press document《Anti- height The research of warm resistant to sea water fluid loss additive and performance evaluation》(Wang Zhongguang, 2010《Drilling and completion fluids》)It is prepared by report method.
Above-described embodiment and comparative example evaluate filtrate loss controllability using the base slurry of saliferous calcic, and specific evaluation method is as follows:
Fresh water-based slurry is prepared:40g calcium bentonites and 5g sodium carbonate, high-speed stirred 20min, room temperature are added in 1000mL water It is lower to place maintenance 24h, obtain fresh water-based slurry.
The water base slurry of saturated salt:Add people 36%NaCl, high-speed stirred 20min in 1000mL fresh water-based slurrys, conserve at room temperature 24h, obtains the water base slurry of saturated salt.
Anti-salt property evaluation method:350mL fresh water-based slurry is measured, a certain amount of NaCl, high-speed stirred 5min is first added, then Filter pressing loss in being surveyed after the amphoteric ion copolymer of addition 1.5%, high-speed stirred 5min, normal temperature maintenance 24h.By investigating light NaCl amount is continuously increased in water base slurry, the change of filtrate reducing amount is determined.Wherein filtrate reducing amount is more low better.
Anticalcium method of evaluating performance:The 350mL water base slurry of saturated salt is measured, a certain amount of CaCl is first added2, high-speed stirred 5min, add 2.0% amphoteric ion copolymer, high-speed stirred 5min, normal temperature maintenance 24h after survey in filter pressing loss.In saturation CaCl is continuously increased in brine mud2Amount, determine filtrate reducing amount change.
The different amphoteric ion polymer anti-salt property contrast tables of table 1
The different amphoteric ion polymer anticalcium performance comparison tables of table 2
The different amphoteric ion polymer heat-resisting property contrast tables of table 3
Aging temperature/DEG C 3 filter losses of embodiment/mL 4 filter losses of embodiment/mL 3 filter losses of comparative example/mL 4 filter losses of comparative example/mL
180 28 21 126 47
210 36 27 210 86

Claims (18)

1. a kind of preparation method of drilling fluid amphoteric ion copolymer, it is characterised in that:The preparation method includes following step Suddenly:
(1)It is 2 to weigh mol ratio respectively first:1~8:1 N, N- DMAA and PS, and to PS is added in N, N- DMAA, 0.5~4h is then reacted at a temperature of 10~60 DEG C, finally Through filtering, extracting, dry obtained N, N- dimethyl-allyl propane sulfonic acid salt;
(2)It is 1 according to mol ratio:1.1~1:1.3 weigh 4-vinylpridine and PS respectively, then weigh The total mass ratio of organic solvent and auxiliary agent, organic solvent and 4-vinylpridine and PS is 2:1~8:1, help The total mass ratio of agent and 4-vinylpridine, PS and organic solvent is 0.001~0.01, then will be organic molten Agent is divided into three parts, is mixed respectively with 4-vinylpridine, PS, auxiliary agent dissolving, mixed by obtain three kinds Close solution and sequentially add reactor, 1~10h is reacted under the conditions of 20 DEG C~90 DEG C, then through filtering, washing, dry obtained 4- Vinylpyridine propane sulfonic acid inner salt;
(3)According to(4~3):(5~6):(0.5~1)Mol ratio weigh step respectively(1)Obtained N, N- dimethallyl Base propane sulfonic acid salt, acrylamide and step(2)Obtained 4-vinylpridine propane sulfonic acid inner salt, is passed through after adding solvent dissolving N20.5~1h of deoxygenation, while being warming up to addition 4~6h of initiator for reaction after 50~70 DEG C, 5~10min of constant temperature, is obtained after reaction Gelatinous solid, white depositions are obtained with acetone precipitation;
(4)By step(3)Obtained sediment is dried after 16~24h at 100~120 DEG C and crushed, final that amphion is total to Polymers.
2. in accordance with the method for claim 1, it is characterised in that:Step(1)Middle N, N- DMAA and 1,3- third The mol ratio of sultones is 3:1~5:1.
3. in accordance with the method for claim 1, it is characterised in that:Step(1)Middle PS is added drop-wise to N, N- bis- In methacrylic amine or directly disposably it is added in N, N- DMAAs.
4. according to the method described in claim 1 or 3, it is characterised in that:Step(1)Middle PS is directly disposable It is added in N, N- DMAAs.
5. in accordance with the method for claim 3, it is characterised in that:The N weighed during using directly disposable addition, N- dimethyl Allyl amine and PS mol ratio are 5:1~8:1.
6. in accordance with the method for claim 3, it is characterised in that:Using be added dropwise mode when N, N- DMAAs and 1, 3-N-morpholinopropanesulfonic acid lactone mol ratio is 2:1~5:1.
7. in accordance with the method for claim 1, it is characterised in that:Step(1)Reaction condition be in 20~55 DEG C of temperature 1~3h of lower reaction.
8. in accordance with the method for claim 1, it is characterised in that:Step(1)Described in extraction solvent select methanol or ethanol.
9. in accordance with the method for claim 1, it is characterised in that:Step(1)Described in extraction times be 1~3h.
10. in accordance with the method for claim 1, it is characterised in that:Step(1)Described in dry be at 30~50 DEG C dry 10~20h.
11. in accordance with the method for claim 1, it is characterised in that:Step(2)Described in organic solvent be benzene, toluene, acetic acid Any of ethyl ester, acetone, cyclohexanone, propene carbonate.
12. in accordance with the method for claim 1, it is characterised in that:Step(2)Described in auxiliary agent be hydroxylamine compound and nitre Base benzene-like compounds, wherein hydroxylamine compound are dimethyl hydroxylamine, diethyl hydroxylamine, dipropyl azanol, isopropylhydroxyla, two Any of butylhydroxylamine, methyl ethylhydroxylamine;Nitrobenzene compounds be 1,2- dinitro benzenes, 1,3- dinitro benzenes, 1, Any of 4- dinitro benzenes, 1,3,5- trinitrobenzens.
13. in accordance with the method for claim 1, it is characterised in that:Step(2)Described in washing operation to use step(2)In The organic solvent washing 2~5 times.
14. in accordance with the method for claim 1, it is characterised in that:Step(2)Described in dry be at 40~60 DEG C dry 10~20h.
15. in accordance with the method for claim 1, it is characterised in that:Step(3)Described in solvent be deionized water or salt The NaCl concentration added in water, the salt solution is 0~0.5mol/L.
16. in accordance with the method for claim 1, it is characterised in that:Step(3)Monomer gross mass concentration is after middle addition solvent 20%~40%.
17. in accordance with the method for claim 1, it is characterised in that:Step(3)The middle initiator used is potassium peroxydisulfate, mistake It is any in sodium sulphate, ammonium persulfate.
18. in accordance with the method for claim 1, it is characterised in that:The initiator amount account for monomer gross mass 0.9%~ 1.3%。
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