CN102225988B - Dispersant used in polymer cement mortar for oil field cementing, and preparation method thereof - Google Patents
Dispersant used in polymer cement mortar for oil field cementing, and preparation method thereof Download PDFInfo
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- CN102225988B CN102225988B CN 201110071969 CN201110071969A CN102225988B CN 102225988 B CN102225988 B CN 102225988B CN 201110071969 CN201110071969 CN 201110071969 CN 201110071969 A CN201110071969 A CN 201110071969A CN 102225988 B CN102225988 B CN 102225988B
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Abstract
The invention relates to a dispersant used in polymer cement mortar for oil field cementing. The dispersant is prepared through the following steps that: a. the following three substances, which are methoxy polyethylene glycol methacrylate (MPEG-MA), [alpha]-methacrylic acid, and 2-acrylamide-2-methylpro panesulfonic acid, with a total amount of 20 to 40 parts by weight, are mixed according to a weight ratio of 1:0.05 to 0.3:0.1 to 0.4; the mixture is dissolved with 10 to 20 parts by weight of water, and a mercapto chain transferring agent with an amount of 0.2 to 1.6% by weight of the three substances is added into the solution, such that a material A is obtained; b. a persulfate initiator with an amount of 0.5 to 4% by weight of the three substances is dissolved with 10 to 20 parts by weight of water, such that a material B is obtained; c. when a temperature in a reaction vessel is 88 DEG C to 92 DEG C, the material A and the material B are simultaneously dropped in the reaction vessel for carrying out a polymerization reaction; the reaction temperature is controlled at 88 DEG C to 92 DEG C, and the reaction time is controlled at 3 to 5 hours; d. when the polymerization reactionis finished, the PH value of the reaction resultant is regulated to 5 to 6, and an obtained material is the dispersant. The invention also relates to the preparation method of the dispersant.
Description
Invention field
The present invention relates to a kind of dispersion agent, especially for the dispersion agent of reinforcing oil well polymer water mud, the invention still further relates to the preparation method of described dispersion agent for reinforcing oil well polymer water mud.
Background technology
The main purpose of well cementing operation is to replace open hole section mud, and makes grout and sleeve pipe and formation cementation good.Displacement efficiency increases with discharge capacity and improves, and may press Lou stratum but replace under high discharge capacity.Add dispersion agent (also claiming flow improver) in the grout and can improve its flowing property, dispersed grout has lower viscosity, can be issued to turbulent flow in low pump pressure, to reduce leakage.
Cementing slurry is the interactional complex system of cement-water-admixture, and wherein admixture mainly comprises dispersion agent, short solidifying or retardant, water retaining.Dispersion agent can be subject to the impact of other admixture and cement minerals on the improvement effect of the degree of mobilization of grout.At present, the multipolymer take 2-acrylamide-2-methylpro panesulfonic acid monomer (AMPS) as main monomer is because anti-salt, temperature resistance and to fall dehydration effect good etc. are widely used as the reinforcing oil well water retaining, and form the polymer water mud system with this.
No. 4557763 patent disclosures of US in the oil well cement dispersants such as well cementation sulfonated lignin (CLS) commonly used, naphthalene sulfonic salt (PNS), acetone-formaldehyde condenses (AFS), low molecular carboxylic acid (as: citric acid), the poly-polysaccharide of hydroxyl, often be the AFS dispersion agent with AMPS is that the grout of water retaining is used.Yet, find that in the grout formulating of recipe it is not obvious that the AFS dispersion agent is regulated the effect of grout degree of mobilization, and dosage often makes the cement slurry water loss amount increase when too much.
In addition, CN 101234866A patent disclosure the preparation method of a kind of the reinforcement of concrete polycarboxylic acids dehydragent (in reinforcing oil well, being called dispersion agent), it adopts the carboxylic monomers such as polyethylene glycol monomethyl ethermethacrylic acid esters (MPEG-MA) and α-methacrylic acid or vinylformic acid to carry out copolyreaction and generates polycarboxylic acids dehydragent.This polycarboxylic acids dehydragent also can adopt the carboxylic monomer copolymerizations such as allyl polyglycol (APEG) and toxilic acid or vinylformic acid to form that (polycarboxylate water-reducer functional group and molecular structure affect the research of cement initial stage aquation slurry temperature rise, silicate journal, 2008,27 (2): 415-419).Polycarboxylic acids dehydragent is the pectination water soluble surfactant active of a class take polyoxyethylene groups as side chain, take carboxyl as anchoring group, is widely applied in concrete at present.But such water reducer is less as the report of reinforcing oil well dispersion agent, particularly yet there are no report for the application in the cementing slurry take AMPS as water retaining.And, research finds that there is larger delayed coagulation in these the reinforcement of concrete polycarboxylate water-reducers, if it is directly applied in the polymer water mud system, because its delayed coagulation will make the difficult adjusting of grout pumping time, and if the adding setting accelerator tends to make the cement slurry property variation or make mortar architecture too complicated.
Therefore, be necessary to provide a kind of dispersion agent that is used for reinforcing oil well polymer water mud and preparation method thereof of better performances.
Summary of the invention
The purpose of this invention is to provide a kind of dispersion agent for reinforcing oil well polymer water mud.
Another object of the present invention provides a kind of preparation method of the dispersion agent for reinforcing oil well polymer water mud.
The present invention relates to a kind of dispersion agent for reinforcing oil well polymer water mud, it is characterized in that, it prepares by following step:
A. be following three kinds of materials of 20～40 parts with gross weight, be that polyethylene glycol monomethyl ethermethacrylic acid esters, α-methacrylic acid, 2-acrylamide-2-methylpro panesulfonic acid mix with 1: 0.05～0.3: 0.1～0.4 weight ratio, and with the water dissolution of 10～20 weight parts, 0.2～1.6% the sulfydryl class chain-transfer agent that then adds the gross weight that accounts for described three kinds of materials makes material A;
0.5～4% the persulfuric acid salt initiator of gross weight that b. will account for described three kinds of materials with the water dissolution of 10～20 weight parts to make material B;
C. when the temperature of reactor is 88 ℃～92 ℃, drip simultaneously described material A and described material B in the described reactor to carry out polyreaction, the temperature of described polyreaction is controlled at 88 ℃～92 ℃, and the reaction times is controlled at 3～5 hours;
D. after described polyreaction finishes, the pH value of resultant of reaction is adjusted to 5～6, discharging namely gets described dispersion agent.
Preferably, the gross weight of wherein said three kinds of materials is 30 parts, and weight ratio is 1: 0.1: 0.2, sulfydryl class chain-transfer agent account for described three kinds of materials gross weight 0.8%, persulfuric acid salt initiator account for described three kinds of materials gross weight 2%.And wherein sulfydryl class chain-transfer agent comprises mercaptoethanol, Thiovanic acid, thiohydracrylic acid, is preferably mercaptoethanol.Persulfuric acid salt initiator is preferably ammonium persulphate.The molecular weight of polyethylene glycol monomethyl ethermethacrylic acid esters is more than 1000, to be preferably 2000.
The invention still further relates to a kind of preparation method of the dispersion agent for reinforcing oil well polymer water mud, it is characterized in that it comprises the steps:
A. be following three kinds of materials of 20～40 parts with gross weight, be that polyethylene glycol monomethyl ethermethacrylic acid esters, α-methacrylic acid, 2-acrylamide-2-methylpro panesulfonic acid mix with 1: 0.05～0.3: 0.1～0.4 weight ratio, and with the water dissolution of 10～20 weight parts, 0.2～1.6% the sulfydryl class chain-transfer agent that then adds the gross weight that accounts for described three kinds of materials makes material A;
0.5～4% the persulfuric acid salt initiator of gross weight that b. will account for described three kinds of materials with the water dissolution of 10～20 weight parts to make material B;
C. when the temperature of reactor is 88 ℃～92 ℃, drip simultaneously described material A and described material B in the described reactor to carry out polyreaction, the temperature of described polyreaction is controlled at 88 ℃～92 ℃, and the reaction times is controlled at 3～5 hours;
D. after described polyreaction finishes, the pH value of resultant of reaction is adjusted to 5～6, discharging namely gets described dispersion agent.
Preferably, wherein in step c, the temperature of described polyreaction is controlled at 90 ℃, and the time for adding of material A is 3 hours, and the time for adding of material B is 3.5 hours.Be deionized water for the water that dissolves described three kinds of materials or persulfuric acid salt initiator wherein.Wherein water consumption is 40 weight parts at the bottom of the still of reactor.After polyreaction finishes, be incubated 1 hour, when the temperature of reactor is down to 55～65 ℃, with alkali lye the pH value of resultant of reaction be adjusted to 5～6, alkali lye can be selected alkali hydroxide soln.
Dispersion agent for reinforcing oil well polymer water mud of the present invention has good performance at polymer water mud, particularly has good performance at the water solubility copolymer take 2-acrylamide-2-methylpro panesulfonic acid and other monomers in the grout of water retaining.Particularly, the present invention is used for the good dispersion property of the dispersion agent of reinforcing oil well polymer water mud.With respect to aldehyde-ketone condensate class dispersion agent, dispersion agent of the present invention has preferably suitability in the grout take the 2-acrylamide-2-methylpro panesulfonic acid as water retaining, and with seawater prepared bentonite drilling fluid be mixed with in the grout of SILICA FUME and have equally preferably suitability, and be suitable for preparing high-density cement mortar.In addition, because dispersion agent of the present invention has adopted the large polyethylene glycol monomethyl ethermethacrylic acid esters of side chain molecular weight, and has introduced sulfonic group monomer 2-acrylamide-2-methylpro panesulfonic acid, thereby improved the delayed coagulation that polycarboxylic acid dispersant exists.
Performance evaluation
The below carries out performance evaluation to the dispersion agent F45L that makes among the following embodiment.
Cement slurry property is estimated
To the dispersion agent F45L of the present invention preparation, test according to the regulation of API RP10B " oil-well cement test recommendation way " the 22nd edition 1997.Cement is selected API G class g cement (company limited produces by the good magnificent enterprise stock in Sichuan), with slurry water is tap water, water retaining is selected G84L (AMPS copolymer analog water retaining, taking chemical company by Tianjin CNOOC produces), retardant selects CH40L (to contain carboxylic acid polyalcohol class retardant, Weihui City, effluent south chemical industry company limited produces), defoamer is selected X601L (the alcohol ether defoamer takes chemical company by Tianjin CNOOC and produces).According to the prescription in the table 1, preparation grout A, B, C, D, E, F, G.Wherein grout A does not add dispersion agent, and grout B, C, D add aldehyde-ketone condensate class dispersion agent (F40L), and grout E, F, G add the dispersion agent F45L of the present invention's preparation.The Evaluation results of each grout sees Table 1.Can find that from table 1 the dispersion agent F45L of the present invention's preparation has preferably suitability in the grout take AMPS as water retaining.
Table 1 1.95S.G grout prescription and performance evaluation
Annotate: 1.X601L is alcohol ether defoamer (taking chemical company by Tianjin CNOOC produces); G84L is AMPS copolymer analog water retaining (taking chemical company by Tianjin CNOOC produces); F40L is aldehyde-ketone condensate class dispersion agent (taking chemical company by Tianjin CNOOC produces); F45L is the dispersion agent that the present invention prepares; CH40L is for containing carboxylic acid polyalcohol class retardant (Weihui City, effluent south chemical industry company limited produces).
2. rheological, free liquid, API fluid loss, thickening time and ultrasonic intensity are tested according to the relevant regulations of API RP10B " oil-well cement test recommendation way " the 22nd edition (1997).
With seawater prepared bentonite drilling fluid and the cement slurry property evaluation when being mixed with SILICA FUME
To the dispersion agent F45L of the present invention's preparation, continue to estimate its performance in the polymer water mud system when replacing the fresh water with slurry with seawater and being mixed with SILICA FUME.According to the prescription in the table 2, preparation grout H, I, J, K.Wherein grout H, I are with seawater prepared bentonite drilling fluid, and grout J, K are mixed with SILICA FUME.The Evaluation results of each grout sees Table 2.Can find that from table 2 the F45L dispersion agent of the present invention preparation is with seawater prepared bentonite drilling fluid be mixed with in the grout of SILICA FUME and have equally preferably suitability.
Table 2 seawater prepared bentonite drilling fluid, be mixed with grout prescription and the performance evaluation of SILICA FUME
Annotate: G80L is AMPS copolymer analog anti-salt type water retaining (taking chemical company by Tianjin CNOOC produces), and seawater is taken from Seawater of Bohai Bay, divalent cation＜1600mg/L, total mineralization＜31600mg/L.
Preparation high-density cement mortar performance evaluation
To the dispersion agent F45L of the present invention's preparation, continue to estimate its performance when the preparation high-density cement mortar.According to the prescription in the table 3, preparation grout L, M, N, O, P, Q.The Evaluation results of each grout sees Table 3.As can be found from Table 3, the F45L dispersion agent of the present invention's preparation is applicable to prepare high-density cement mortar.
Table 3 2.30S.G grout prescription and performance evaluation
Annotate: CD20 is 1200 order pure iron breezes (taking chemical company by Tianjin CNOOC produces); PC-81 is 800 order silica powders (taking chemical company by Tianjin CNOOC produces); GS12L is unformed shape silicon-dioxide silicon slurry (taking chemical company by Tianjin CNOOC produces).
Embodiment
Embodiment
The method that the preparation solid content is about 30% the dispersion agent that is used for reinforcing oil well polymer water mud is: with polyethylene glycol monomethyl ethermethacrylic acid esters (the polyglykol MA2000 of about 23 weight parts, produced by Clarint company), α-methacrylic acid (the technical grade of about 2.3 weight parts, market is bought) and the 2-acrylamide-2-methylpro panesulfonic acid (technical grade of about 4.6 weight parts, market is bought) mix, and with the deionized water dissolving of 15 weight parts, then the mercaptoethanol (technical grade, market is bought) that adds 0.24 weight part is for subsequent use as material A; The ammonium persulphate (analytical pure is produced by traditional Chinese medicines group) of 0.6 weight part is for subsequent use as material B with the deionized water dissolving of 15 weight parts; Then the deionized water and the heating that in the reactor that mechanical stirring device and nitrogen tamping unit are housed, add 40 weight parts, under temperature of reaction kettle is 90 ℃ and condition in nitrogen protection, drip simultaneously material A and material B to carry out polyreaction, expect that wherein A drips 3 hours, material B drips 3.5 hours, and temperature of reaction is controlled at 90 ℃; After reaction finishes, be incubated 1 hour, when the temperature of reactor was down to 60 ℃, being 30% alkali lye with concentration was adjusted to 5～6 with the pH value of resultant of reaction, and discharging namely gets solid content and is about 30% the dispersion agent F45L for reinforcing oil well polymer water mud.
Claims (10)
1. dispersion agent that is used for reinforcing oil well polymer water mud is characterized in that it prepares by following step:
A. be following three kinds of materials of 20～40 parts with gross weight, be that polyethylene glycol monomethyl ethermethacrylic acid esters, α-methacrylic acid, 2-acrylamide-2-methylpro panesulfonic acid mix with 1: 0.05～0.3: 0.1～0.4 weight ratio, and with the water dissolution of 10～20 weight parts, 0.2～1.6% the sulfydryl class chain-transfer agent that then adds the gross weight that accounts for described three kinds of materials makes material A;
0.5～4% the persulfuric acid salt initiator of gross weight that b. will account for described three kinds of materials with the water dissolution of 10～20 weight parts to make material B;
C. when the temperature of reactor is 88 ℃～92 ℃, drip simultaneously described material A and described material B in the described reactor to carry out polyreaction, the temperature of described polyreaction is controlled at 88 ℃～92 ℃, and the reaction times is controlled at 3～5 hours;
D. after described polyreaction finishes, the pH value of resultant of reaction is adjusted to 5～6, discharging namely gets described dispersion agent.
2. the dispersion agent for reinforcing oil well polymer water mud as claimed in claim 1, the weight ratio of wherein said three kinds of materials is 1: 0.1: 0.2, described sulfydryl class chain-transfer agent account for described three kinds of materials gross weight 0.8%, described persulfuric acid salt initiator account for described three kinds of materials gross weight 2%.
3. the dispersion agent for reinforcing oil well polymer water mud as claimed in claim 1, the gross weight of wherein said three kinds of materials is 30 parts.
4. the dispersion agent for reinforcing oil well polymer water mud as claimed in claim 1, wherein said sulfydryl class chain-transfer agent comprises mercaptoethanol, Thiovanic acid, thiohydracrylic acid.
5. the dispersion agent for reinforcing oil well polymer water mud as claimed in claim 1, wherein said persulfuric acid salt initiator is ammonium persulphate.
6. the dispersion agent for reinforcing oil well polymer water mud as claimed in claim 1, the molecular weight of wherein said polyethylene glycol monomethyl ethermethacrylic acid esters is more than 1000.
7. the dispersion agent for reinforcing oil well polymer water mud as claimed in claim 6, the molecular weight of wherein said polyethylene glycol monomethyl ethermethacrylic acid esters is 2000.
8. the dispersion agent for reinforcing oil well polymer water mud as claimed in claim 1, the time for adding of wherein said material A is 3 hours, the time for adding of described material B is 3.5 hours.
9. the dispersion agent for reinforcing oil well polymer water mud as claimed in claim 1, the temperature of wherein said polyreaction is controlled at 90 ℃.
10. the preparation method of the dispersion agent for reinforcing oil well polymer water mud claimed in claim 1 is characterized in that it comprises the steps:
A. be following three kinds of materials of 20～40 parts with gross weight, be that polyethylene glycol monomethyl ethermethacrylic acid esters, α-methacrylic acid, 2-acrylamide-2-methylpro panesulfonic acid mix with 1: 0.05～0.3: 0.1～0.4 weight ratio, and with the water dissolution of 10～20 weight parts, 0.2～1.6% the sulfydryl class chain-transfer agent that then adds the gross weight that accounts for described three kinds of materials makes material A;
0.5～4% the persulfuric acid salt initiator of gross weight that b. will account for described three kinds of materials with the water dissolution of 10～20 weight parts to make material B;
C. when the temperature of reactor is 88 ℃～92 ℃, drip simultaneously described material A and described material B in the described reactor to carry out polyreaction, the temperature of described polyreaction is controlled at 88 ℃～92 ℃, and the reaction times is controlled at 3～5 hours;
D. after described polyreaction finishes, the pH value of resultant of reaction is adjusted to 5～6, discharging namely gets described dispersion agent.
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| CN103387640A (en) * | 2013-08-09 | 2013-11-13 | 卫辉市化工有限公司 | Method for preparing oil-well cement dispersing agent |
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| CN104745160B (en) * | 2015-03-17 | 2018-02-02 | 中国海洋石油总公司 | A kind of high-performance Oil/gas Well cement dispersants and preparation method thereof |
| CN108794696A (en) * | 2017-04-27 | 2018-11-13 | 中国石油天然气集团公司 | A kind of drag reducer, preparation method and applications |
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Address after: 100010 Chaoyangmen North Street, Dongcheng District, Dongcheng District, Beijing Co-patentee after: China Oilfield Services Limited Patentee after: China Offshore Oil Group Co., Ltd. Address before: 100010 Chaoyangmen North Street, Dongcheng District, Dongcheng District, Beijing Co-patentee before: China Oilfield Services Limited Patentee before: China National Offshore Oil Corporation |
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