CN103319650A - Phosphoaluminate cement system fluid loss additive and preparation method thereof - Google Patents
Phosphoaluminate cement system fluid loss additive and preparation method thereof Download PDFInfo
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- CN103319650A CN103319650A CN2013100701825A CN201310070182A CN103319650A CN 103319650 A CN103319650 A CN 103319650A CN 2013100701825 A CN2013100701825 A CN 2013100701825A CN 201310070182 A CN201310070182 A CN 201310070182A CN 103319650 A CN103319650 A CN 103319650A
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Abstract
The invention discloses a phosphoaluminate cement system fluid loss additive and a preparation method thereof. The fluid loss additive comprises four raw materials of acrylamide (AM), 2-acrylamide-2-methyl propanesulfonic acid (AMPS), dimethyl diallyl ammonium chloride (DMDAAC) and itaconic acid (IA), and the mass ratio of the four raw materials is 45-55:25-35:10-15:10. An initiator is an ammonium persulfate-sodium bisulfite redox system, and synthesized by employing a free radical solution polymerization method. The fluid loss additive can help to control the fluid loss rate of a phosphoaluminate cement mortar system at 50 mL/30 min or less, is excellent in high temperature resistance ( greater than 110 DEG C) and stable in performance, and has no adverse influence to comprehensive properties of cement mortar.
Description
Technical field
The present invention relates to a kind of reinforcing oil well with phosphor aluminate cement system water retaining and preparation method, belong to oilfield chemistry and oil gas well cementing operation field.
Background technology
CO
2One of associated gas that generates as oil gas is prevalent in all kinds of hydrocarbon-bearing pools.In recent years, CO
2Bury and CO
2The development need of the technology such as the displacement of reservoir oil is injected a large amount of CO in the stratum
2, can greatly improve CO in the stratum like this
2Concentration.CO
2Corrosion to cementing concrete stone can cause sleeve water mudstone forfeiture sealing performance, so final generation CO
2Bury unsuccessfully, the serious consequence such as rate of oil and gas recovery reduction.The CO of sleeve water mudstone
2Anticorrosion Problems is one of significant problem of needing to be resolved hurrily of casing and cementing technician.Chinese scholars is to CO
2Ultimate principle and the influence factor thereof of corrosion silicate cement mudstone are studied, and have proposed some anti-corrosion measures.These anti-corrosion measures are normally carried out modification to the silicate cement commonly used of cementing the well, and as improving cement slurry density, reduce Behavior of Hardened Cement Paste porosity and permeability etc., but these methods can not fundamentally solve the corrosion-prone problem of silicate cement.Abroad begin one's study and improve the antiseptic power of cementing concrete stone by the mineral composition that changes cement, the ThermaLock of Halliburton oil company has developed anti-CO
2The special cement system of corrosion, this cement system has good anti-CO
2The performance of corrosion, but its resistance to crocking is very poor, and cost is higher.
Its main hydration products of phosphor aluminate cement (PALC) is different types of apatite mineral, has more excellent anti-CO
2Corrodibility, but the drated calcium aluminate in the hydrated product is subject to CO
2Corrosion is by adding the carbon dioxide corrosion resistant ability that extra material SHP can further improve phosphor aluminate cement in phosphor aluminate cement.The phosphor aluminate cement hydration rate is fast, and denseness will rapid growth within the time at the several minutes of with slurry, and seminar selects the compound system of sodium lignosulfonate and boric acid to satisfy the well cementing operation demand as retardant for this reason, thereby develops novel anti-CO
2Corrosion cement system-phosphor aluminate cement system, this cement system has good corrosion resistance nature after tested.
Except the basic demand of satisfying the thickening time, in the situation of the higher water cement ratio of maintenance, also need to satisfy the requirement of the low dehydration of cement in the well cementing operation process.If grout a large amount of " dehydrations ", the density of grout, thickening time, rheological property change thereupon, in addition become can not pumping, cause cementing the well unsuccessfully; A large amount of filtrate enters the stratum and also can cause reservoir injury in various degree simultaneously, reduces the oil gas production capacity.Phosphor aluminate cement is starched fluid loss only can reach 1500ml/30min, does not satisfy the requirement of casing and cementing far away, needs to add the performance that water retaining is regulated mortar architecture.
At present, the oil-well cement filtrate reducer of existing numerous species is used for the cementing job of silicate cement.Commonly used have cellulose ethers (Natvosol, carboxymethyl cellulose and carboxymethyl hydroxyethyl cellulose etc.), polyvinyl alcohol, polyacrylamide, poly-2-acrylamide-2-methyl propane sulfonic (AMPS) class.Because the difference of phosphor aluminate cement system Mineral Component and silicate cement composition, through the traditional oil-well cement filtrate reducer of in-house laboratory investigation to the dehydration controllability of phosphor aluminate cement system a little less than or fall dehydration effect and can not reach needs of cementing operations.
Summary of the invention
The object of the invention is to provides a kind of phosphor aluminate cement system water retaining and preparation method thereof for the deficiencies in the prior art.
Water retaining functional group the most important thing is that good adsorption and hydration will be arranged.Play adsorbing functional group and select the quaternaries cation group; From hydration, carboxyl, sulfonic group, amide group have preferably hydratability; From anti-salt angle quaternaries cation, sulfonic acid group has preferably salt tolerance.Consider the functional group that quaternaries cation, carboxyl, sulfonic group, amide group can be used as phosphor aluminate cement system water retaining.
It is raw material that the present invention selects acrylamide (AM), 2-acrylamide-2-methylpro panesulfonic acid (AMPS), dimethyl diallyl ammonium chloride (DMDAAC), four kinds of monomers of methylene-succinic acid (IA), adopts the free radical solution polymerization method to synthesize.
Phosphor aluminate cement system water retaining, its structural formula is as follows:
The invention provides a kind of preparation method of phosphor aluminate cement system water retaining, described preparation method is:
According to following quality than four kinds of monomers of weighing: acrylamide (AM): 2-acrylamide-2-methylpro panesulfonic acid (AMPS): dimethyl diallyl ammonium chloride (DMDAAC): methylene-succinic acid (IA)=45～55:25～35:10～15:10; With IA and deionized water in mass ratio 1:15～1:10 be dissolved in the reaction vessel, under cooling conditions, regulating pH value with sodium hydroxide is 6～8, add AMPS in reaction vessel, the AM that the adding water dissolves in advance is in reaction vessel, slowly stir, be warming up to 50～60 ℃, rear adding DMDAAC stirs, logical nitrogen 30min, drip the initiator initiation reaction of water in advance dissolving, described initiator is the in mass ratio redox system of 1:1 composition of what sodium bisulfite of ammonium persulphate, and the initiator dosage is 0.15%～0.25% of four kinds of monomer total masses; Stop to stir after dripping initiator, reaction 4～7h, the final thick liquid that gets is purified with dehydrated alcohol, gets white flocks, repeatedly pulverizes to get powdery copolymer with the absolute ethanol washing post-drying.
Described preparation method, the total concn of four kinds of monomers in reaction vessel is 25wt%～35wt%.
Compared with prior art, the present invention has the following advantages:
(1) on molecular chain, introduces simultaneously cation group and anionic group.Cation group mainly plays adsorption, firmly be adsorbed on cement particle surface, overcome the shortcoming of anionic group in the difficult absorption in phosphor aluminate cement surface, anionic group mainly plays aquation, fetter a large amount of free water, form the hydration shell of one deck densification at cement particle surface, reduce the filter cake perviousness, have and well fall the dehydration effect.
(2) synthetic water retaining stable chemical performance has no adverse effects to over-all propertieies such as phosphor aluminate cement system slurry multiviscosisty performance, slurry stability, strength developments, can use with multiple admixture compatibility.
(3) simple synthetic method is feasible, easy handling, and productive rate is higher.
Description of drawings
Fig. 1 is the infrared spectrogram (sample 2) of polymkeric substance.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Feed composition comprises: acrylamide (AM) 21.43g, 2-acrylamide-2-methylpro panesulfonic acid (AMPS) 12.858g, dimethyl diallyl ammonium chloride (DMDAAC) 4.286g, methylene-succinic acid (IA) 4.286g, deionized water 100g, ammonium persulphate 0.043g, sodium bisulfite 0.043g.The preparation method is: IA and 50g is water-soluble in there-necked flask, under cooling conditions, regulating pH value with soda-lye is 7, takes by weighing AMPS and joins in the there-necked flask, add with the water-soluble AM of 20g in there-necked flask, be warming up to 60 ℃ in the situation that slowly stir, rear adding DMDAAC stirs, logical nitrogen 30min, drip and use in advance the initiation reaction of the water-soluble ammonium persulfate-sodium bisulfite system of 30g, stop to stir reaction 5h, the final thick liquid that gets after dripping initiator.Purify with dehydrated alcohol, get white flocks, repeatedly pulverize to get powdery copolymer with the absolute ethanol washing post-drying.Code name is sample 1.
Embodiment 2
Feed composition comprises: acrylamide (AM) 19.287g, 2-acrylamide-2-methylpro panesulfonic acid (AMPS) 15.001g, dimethyl diallyl ammonium chloride (DMDAAC) 4.286g, methylene-succinic acid (IA) 4.286g, deionized water 100g, ammonium persulphate 0.054g, sodium bisulfite 0.054g.The preparation method is: IA and 50g is water-soluble in there-necked flask, under cooling conditions, regulating pH value with soda-lye is 7, takes by weighing AMPS and joins in the there-necked flask, add with the water-soluble AM of 20g in there-necked flask, be warming up to 60 ℃ in the situation that slowly stir, rear adding DMDAAC stirs, logical nitrogen 30min, drip and use in advance the initiation reaction of the water-soluble ammonium persulfate-sodium bisulfite system of 30g, stop to stir reaction 5h, the final thick liquid that gets after dripping initiator.Purify with dehydrated alcohol, get white flocks, repeatedly pulverize to get powdery copolymer with the absolute ethanol washing post-drying.Code name is sample 2.Such as Fig. 1, be the infrared spectrogram of sample 2,3421.14cm-1 and 1664.29cm-1 are amide group in the AM chain link-CONH characteristic absorbance, and wherein 1664.29cm-1 is the stretching vibration of C=O key in the amide group, and 3421.14cm-1 is-stretching vibration of NH2.Wave number be 1193.74cm-1 and 1042.78cm-1 be the AMPS chain link characteristic absorbance wherein 1193.74cm-1 be the stretching vibration of C=O key in the AMPS chain, 1041cm-1 is the stretching vibration of S=O among sulfonic group-SO3-, and the 630.62cm-1 place is C-S stretching vibration absorption peak.3207.09cm-1 be among the AMPS-the stretching vibration absorption peak of NH-.2360.48cm-1 be five-ring stretching vibration absorption peak, 1193.74cm-1,1301.74cm-1 are the C-N key stretching vibration absorption peak of quaternary ammonium salt.1544.73cm-1 locate unsymmetrically and the symmetrical stretching vibration band for-COO-with the 1454.09cm-1 place; 2921.68cm-1 be-the CH3 absorption peak; 771.39cm-1 be the flexural vibration absorption peak of C-H on the long carbochain skeleton, and the stretching vibration absorption peak of the two keys of C=C do not occur between 1620-1650cm-1, illustrate that four kinds of monomers have participated in reaction, synthetic polymer is target product.
The filtrate-loss control of phosphor aluminate cement system water retaining of the present invention can be estimated:
The pulvis sample 1 and the sample 2 that add certain mass percentage ratio (take cement quality as benchmark) in the phosphor aluminate cement system are 0.5 grout by the standby water cement ratio of GB10238-88 standard system, and the density of grout is 1.84g/cm
3, by the fluid loss of the oil and gas industry standard SY/T5960-94 of the People's Republic of China (PRC) " oil-well cement filtrate reducer evaluation method " working sample 1 and sample 2, the filtrate-loss control energy of evaluation sample 1 and sample 2.
Evaluate according to the method described above the dehydration effect that falls of sample 1 and 2 pairs of phosphor aluminate cements of sample, the results are shown in Table 1.Experimental result shows, the present invention is used for the phosphor aluminate cement system good effect, and during dosage 2wt%, dehydration is satisfied the requirement of anti-gas channeling at 50mL/30min.110 ℃ with interior rising with temperature, the cement slurry water loss that is added with water retaining changes little, and good heat-resisting property is arranged, and the content of grout free liquid is 0, illustrates that the present invention has good filtrate-loss control energy, is applicable to the phosphor aluminate cement system.
Table 1 cement slurry water loss amount performance table
Should be understood that, for those of ordinary skills, can be improved according to the above description or conversion, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (3)
1. the preparation method of a phosphor aluminate cement system water retaining is characterized in that, described preparation method is:
According to following quality than four kinds of monomers of weighing: acrylamide (AM): 2-acrylamide-2-methylpro panesulfonic acid (AMPS): dimethyl diallyl ammonium chloride (DMDAAC): methylene-succinic acid (IA)=45～55:25～35:10～15:10; With IA and deionized water in mass ratio 1:15～1:10 be dissolved in the reaction vessel, under cooling conditions, regulating pH value with sodium hydroxide is 6～8, add AMPS in reaction vessel, the AM that the adding water dissolves in advance is in reaction vessel, slowly stir, be warming up to 50～60 ℃, rear adding DMDAAC stirs, logical nitrogen 30min, drip the initiator initiation reaction of water in advance dissolving, described initiator is the in mass ratio redox system of 1:1 composition of what sodium bisulfite of ammonium persulphate, and the initiator dosage is 0.15%～0.25% of four kinds of monomer total masses; Stop to stir after dripping initiator, reaction 4～7h, the final thick liquid that gets is purified with dehydrated alcohol, gets white flocks, repeatedly pulverizes to get powdery copolymer with the absolute ethanol washing post-drying.
2. preparation method according to claim 1 is characterized in that, the total concn of four kinds of monomers in reaction vessel is 25wt%～35wt%.
3. the phosphor aluminate cement system water retaining of preparation method according to claim 1 and 2 preparation.
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Cited By (6)
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| CN104178094A (en) * | 2014-08-26 | 2014-12-03 | 山东聚鑫化工有限公司 | Composite-type oil well cement filtrate reducer and preparation method thereof |
| CN105349127A (en) * | 2015-12-16 | 2016-02-24 | 中国石油大学(华东) | Pre-chelated aluminate base cement fluid loss additive and preparation method thereof as well as cement paste containing same |
| CN106966648A (en) * | 2017-03-10 | 2017-07-21 | 陕西省石油化工研究设计院 | A kind of anti-CO2、H2S corrodes cementing slurry |
| CN110054730A (en) * | 2019-05-05 | 2019-07-26 | 天津科力奥尔工程材料技术有限公司 | It is a kind of with anti-fluid loss agent for being thickened projecting performance and preparation method thereof and purposes |
| CN111153624A (en) * | 2020-01-10 | 2020-05-15 | 中国石油集团渤海钻探工程有限公司 | Oil well cement fluid loss additive for solving problem of cement paste thickening core-spun and preparation method thereof |
| CN113416277A (en) * | 2021-08-24 | 2021-09-21 | 中国石油大学(华东) | Non-foaming oil well cement latex fluid loss agent, preparation method and application |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104178094A (en) * | 2014-08-26 | 2014-12-03 | 山东聚鑫化工有限公司 | Composite-type oil well cement filtrate reducer and preparation method thereof |
| CN105349127A (en) * | 2015-12-16 | 2016-02-24 | 中国石油大学(华东) | Pre-chelated aluminate base cement fluid loss additive and preparation method thereof as well as cement paste containing same |
| CN105349127B (en) * | 2015-12-16 | 2018-07-31 | 中国石油大学(华东) | A kind of pre- chelating aluminate-base cement water reducer and preparation method and the cement mortar comprising it |
| CN106966648A (en) * | 2017-03-10 | 2017-07-21 | 陕西省石油化工研究设计院 | A kind of anti-CO2、H2S corrodes cementing slurry |
| CN106966648B (en) * | 2017-03-10 | 2021-09-03 | 陕西省石油化工研究设计院 | CO prevention2、H2S corrosion well cementation cement slurry |
| CN110054730A (en) * | 2019-05-05 | 2019-07-26 | 天津科力奥尔工程材料技术有限公司 | It is a kind of with anti-fluid loss agent for being thickened projecting performance and preparation method thereof and purposes |
| CN110054730B (en) * | 2019-05-05 | 2021-01-19 | 天津科力奥尔工程材料技术有限公司 | Fluid loss agent with thickening-prevention and hanging-over-prevention performance and preparation method and application thereof |
| CN111153624A (en) * | 2020-01-10 | 2020-05-15 | 中国石油集团渤海钻探工程有限公司 | Oil well cement fluid loss additive for solving problem of cement paste thickening core-spun and preparation method thereof |
| CN113416277A (en) * | 2021-08-24 | 2021-09-21 | 中国石油大学(华东) | Non-foaming oil well cement latex fluid loss agent, preparation method and application |
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Application publication date: 20130925 |