CN102382331B - Solid high-temperature retarding agent for oil-well cement and preparation method thereof - Google Patents
Solid high-temperature retarding agent for oil-well cement and preparation method thereof Download PDFInfo
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- CN102382331B CN102382331B CN201110229274A CN201110229274A CN102382331B CN 102382331 B CN102382331 B CN 102382331B CN 201110229274 A CN201110229274 A CN 201110229274A CN 201110229274 A CN201110229274 A CN 201110229274A CN 102382331 B CN102382331 B CN 102382331B
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Abstract
The invention discloses a solid high-temperature retarding agent for oil-well cement and a preparation method thereof. The retarding agent is prepared by mixing the following components in percentage by mass: 60-70 percent of oxidized starch, 15-25 percent of organic phosphonic acid, 5-15 percent of zinc oxide and 1-10 percent of sodium borate. The retarding agent can be used for adjusting the thickening time of cement grout within the temperature range of 50-200 DEG C, does not influence the strength development of set cement, is not sensitive to dosage, and has high compatibility with other oil-well cement additives.
Description
Technical field
The present invention relates to a kind of retardant and preparation method thereof, especially oil well cement high temperature retarder and preparation method thereof.
Background technology
In oil gas well cementing job, in sleeve pipe, inject grout usually, grout returns out from annular space again, treat that it solidifies after, the annular space between the sealing borehole wall and sleeve pipe.Grout must keep good pumpability before reaching the desired position of sealing.In the well cementation process, along with the carrying out of grout hydration reaction, the mobile variation of grout, when the denseness of grout reached certain value, grout lost flowability and can't pumping.
Along with deepening continuously of oil field prospecting development, the deep well cementing situation is more and more.Along with the rising of bottom temperature, the setting rate of grout also can be accelerated, and using high temperature retarder is the effective means that prolongs cement slurry thickening time in the high temperature high pressure deep well well cementation process.
Several kinds of retardant systems at present commonly used have several kinds of sulfonated lignin, saccharide compound, derivatived cellulose and organophosphates; Be used for pyritous oil well cement retarder ubiquity Applicable temperature narrow range; Thermally sensitive shortcoming, most products are in the well temperature rise or when reducing by 10 ℃, and dosage can double above or reduce over half; Cement strength changes greatly, and well cementing operation safety is had a negative impact.Because deep-well interval isolation FT up and down differs bigger, the tiny difference of dosage can make grout not coagulate for a long time, causes serious consequence.
Summary of the invention
In order to solve the requirement that prolongs cement slurry thickening time in the deep well cementing operation, the present invention provides a kind of oil well cement that at high temperature uses with solid high temperature retarder and preparation method thereof.
The objective of the invention is to realize like this: a kind of oil well cement is used the solid high temperature retarder; Be to be that raw materials mix forms with Sumstar 190, organic phospho acid, zinc oxide and Sodium Tetraborate; The mass percent of each raw material is respectively: Sumstar 190 is 60%-70%; Organic phospho acid is 15%-25%, and zinc oxide is 5%-15%; Sodium Tetraborate is 1%-10%.
Described organic phospho acid is a kind of in solid HEDP, ATMP or the ethylenediamine tetramethylene phosphonic acid.
The preparation method of said Sumstar 190 comprises the steps: the starch water is made into the starch emulsion that mass percent concentration is 25%-30%, keeps not stopping to stir, and regulates pH to 9-10 with alkali; Keep 45-55 ℃ temperature of reaction, add oxygenant, reacted 2-3 hour; After reaction finished, standing demix removed supernatant liquid; Lower floor's emulsion is carried out drying, obtain Sumstar 190.
Said starch is a kind of of yam starch, W-Gum, tapioca(flour) or wheat starch.
Said oxygenant is that mass percent concentration is 30% aqueous hydrogen peroxide solution, and add-on is the 5%-15% of dry starch quality.
Said alkali is that mass percent concentration is 2% sodium hydroxide solution.
Above-mentioned oil well cement by adding after its per-cent weighing in the stirrer, stirs each raw material 30-40 minute under normal temperature condition with the preparation method of solid high temperature retarder, mixes.
Advantage of the present invention and characteristics:
1, Applicable temperature a wider range is generally about 50-200 ℃.
2, the strength development to grout does not influence.
3, dosage is insensitive, and there are good linear relationship the volume of retardant and thickening time, and multiviscosisty is short transit time, and tracing pattern is good.
4, good with other admixture compatiblenesies.
5, good with cement adaptability, to the not influence of other performances of grout.
Embodiment
Oil well cement of the present invention is used the solid high temperature retarder; Be to be that raw materials mix forms with Sumstar 190, organic phospho acid, zinc oxide and Sodium Tetraborate; The mass percent of each raw material is respectively: Sumstar 190 is 60%-70%, and organic phospho acid is 15%-25%, and zinc oxide is 5%-15%; Sodium Tetraborate is 1%-10%.
Described organic phospho acid is a kind of in HEDP, ATMP or the ethylenediamine tetramethylene phosphonic acid.
The preparation method of said Sumstar 190 comprises the steps: the starch water is made into the starch emulsion that mass percent concentration is 25%-30%, keeps not stopping to stir, and regulates pH to 9-10 with alkali; Keep 45-55 ℃ temperature of reaction, add oxygenant, reacted 2-3 hour; After reaction finished, standing demix removed supernatant liquid; Lower floor's emulsion is carried out drying, obtain Sumstar 190.
Said starch is a kind of of yam starch, W-Gum, tapioca(flour) or wheat starch.
Said oxygenant is that mass percent concentration is 30% aqueous hydrogen peroxide solution, and add-on is the 5%-15% of dry starch quality.
Said alkali is that mass percent concentration is 2% sodium hydroxide solution.
Above-mentioned oil well cement by adding after its per-cent weighing in the stirrer, stirs each raw material 30-40 minute under normal temperature condition with the preparation method of solid high temperature retarder, mixes.
Below in conjunction with specific embodiment the present invention is done further explain:
In order to understand the present invention, further specify the present invention with embodiment below, but do not limit the present invention.Said percentage ratio is mass percent.
Embodiment 1
At first prepare Sumstar 190.Prepare 30% yam starch breast, keep not stopping to stir, stirring velocity is 60r/min; Transfer pH to 9-10 with 2%NaOH solution, keeping temperature of reaction is 50 ℃, and the mass percent concentration that adds starch (butt) amount 15% is 30% superoxol; The generation of carboxyl causes the pH value to descend in the oxidising process; Should add 2%NaOH solution control pH value (9-10) in stable scope, react 2 hours, filtration, drying obtain Sumstar 190.
Get Sumstar 190 325g, HEDP 100g, zinc oxide 50g, Sodium Tetraborate 25g, four kinds of raw materials were stirred in stirrer 30 minutes, obtain solid high temperature retarder sample 1.
Embodiment 2
At first prepare Sumstar 190.Prepare 25% corn starch milk, transfer pH to 9-10, keeping temperature of reaction is 45 ℃, and the mass percent concentration that adds starch (butt) amount 8% is 30% superoxol.
Operate according to embodiment 1 described method, obtain Sumstar 190.
Get Sumstar 190 300g, ATMP 115g, zinc oxide 60g, Sodium Tetraborate 25g, four kinds of raw materials were stirred in stirrer 30 minutes, obtain solid high temperature retarder sample 2.
Embodiment 3
At first prepare Sumstar 190.Prepare 28% tapioca(flour) breast, transfer pH to 9-10, keeping temperature of reaction is 55 ℃, and the mass percent concentration that adds starch (butt) amount 12% is 30% superoxol.
Operate according to embodiment 1 described method, obtain Sumstar 190.
Get Sumstar 190 350g, ethylenediamine tetramethylene phosphonic acid 90g, zinc oxide 40g, Sodium Tetraborate 20g, four kinds of raw materials were stirred in stirrer 30 minutes, obtain solid high temperature retarder sample 3.
Embodiment 4
At first prepare Sumstar 190.Prepare 30% wheat starch breast, transfer pH to 9-10, keeping temperature of reaction is 55 ℃, and the mass percent concentration that adds starch (butt) amount 13% is 30% superoxol.
Operate according to embodiment 1 described method, obtain Sumstar 190.
Get Sumstar 190 310g, ethylenediamine tetramethylene phosphonic acid 120g, zinc oxide 55g, Sodium Tetraborate 15g, four kinds of raw materials were stirred in stirrer 30 minutes, obtain solid high temperature retarder sample 4.
Embodiment 5 oil well cement high temperature retarder performance evaluations of the present invention
According to the SY-T5504.1-2005 standard retardant is carried out performance evaluation.The grout prescription is: good magnificent G class g cement+35% silica flour+retardant+water, and wc is 0.55, the sample dosage all is benchmark with cement in the prescription.
Sample thief 1, with 120 ℃ be representative temperature, research retardant dosage and the relation of thickening time, the result is as shown in table 1.
The relation of table 1 retardant dosage and thickening time
Can be known that by table 1 data along with the increase of retardant volume, the thickening time prolongs, explain that there is good linear relationship volume and thickening time, the thickening time is adjustable, and volume does not have sensitive spot, and to the strength development of grout less than influencing.
Sample thief 2, with 120 ℃, 140 ℃, 160 ℃ be the representative temperature point, research temperature and the relation of thickening time, the result is as shown in table 2.
The relation of table 2 experimental temperature and thickening time
| Numbering | Volume % (BWOC) | Experimental temperature ℃ | Experimental pressure MPa | Initial consistency Bc | Thickening time min |
| 1 | 2 | 120 | 73.9 | 13.5 | 435 |
| 2 | 2 | 140 | 87.6 | 12.3 | 380 |
| 3 | 2 | 160 | 101.3 | 11.5 | 290 |
Can be known that by table 2 data temperature raises, the thickening time reduces, but still can satisfy the demand of well cementation, explains that this retardant heat resistance is good.
Above-described embodiment only is used to explain technological thought of the present invention and characteristics; Its purpose is to make those skilled in the art can understand content of the present invention and implements according to this; Can not only limit claim of the present invention with present embodiment; Be equal variation or the modification that all disclosed spirit is done, still drop in the claim of the present invention.
Claims (6)
1. an oil well cement is used the solid high temperature retarder; It is characterized in that, be to be that raw materials mix forms with Sumstar 190, organic phospho acid, zinc oxide and Sodium Tetraborate, and the mass percent of each raw material is respectively: Sumstar 190 is 60%-70%; Organic phospho acid is 15%-25%, and zinc oxide is 5%-15%; Sodium Tetraborate is 1%-10%; Described organic phospho acid is a kind of in solid HEDP, ATMP or the ethylenediamine tetramethylene phosphonic acid.
2. use the solid high temperature retarder according to the said oil well cement of claim 1, it is characterized in that, the preparation method of said Sumstar 190 comprises the steps: the starch water is made into the starch emulsion that mass percent concentration is 25%-30%, keeps not stopping to stir; Regulate pH to 9-10 with alkali, keep 45-55 ℃ temperature of reaction, add oxygenant; Reacted 2-3 hour, after reaction finishes, standing demix; Remove supernatant liquid, lower floor's emulsion is carried out drying, obtain Sumstar 190.
3. oil well cement according to claim 2 is used the solid high temperature retarder, it is characterized in that, said starch is a kind of of yam starch, W-Gum, tapioca(flour) or wheat starch.
4. oil well cement according to claim 2 is used the solid high temperature retarder, it is characterized in that, said oxygenant is that mass percent concentration is 30% aqueous hydrogen peroxide solution, and add-on is the 5%-15% of dry starch quality.
5. oil well cement according to claim 2 is used the solid high temperature retarder, it is characterized in that, said alkali is that mass percent concentration is 2% sodium hydroxide solution.
6. the described oil well cement of claim 1 is characterized in that with the preparation method of solid high temperature retarder, and each raw material by adding after its per-cent weighing in the stirrer, was stirred 30-40 minute under normal temperature condition, mixes.
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| CN105482796A (en) * | 2015-12-03 | 2016-04-13 | 高大元 | Preparation method of environmentally friendly oil well paraffin remover |
| KR20210096193A (en) * | 2018-11-26 | 2021-08-04 | 사우디 아라비안 오일 컴퍼니 | Cement slurry, hardened cement and method of making and using same |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101177459A (en) * | 2007-11-30 | 2008-05-14 | 四川大学 | High carbonyl content oxidation starch and method for making same |
| CN101368091A (en) * | 2007-08-16 | 2009-02-18 | 中国石油天然气集团公司 | Oil well cement inhibiting agent |
| CN101451061A (en) * | 2008-12-30 | 2009-06-10 | 山东大学 | Sand consolidation and water plugging profile control agent made by oil sand |
| CN101537663A (en) * | 2009-04-30 | 2009-09-23 | 辽河石油勘探局 | Preparation method of high temperature resisting cement grout |
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| DE10338825A1 (en) * | 2003-08-21 | 2005-03-24 | Daimlerchrysler Ag | Diagnostic device and diagnostic method for a multi-antenna system |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101368091A (en) * | 2007-08-16 | 2009-02-18 | 中国石油天然气集团公司 | Oil well cement inhibiting agent |
| CN101177459A (en) * | 2007-11-30 | 2008-05-14 | 四川大学 | High carbonyl content oxidation starch and method for making same |
| CN101451061A (en) * | 2008-12-30 | 2009-06-10 | 山东大学 | Sand consolidation and water plugging profile control agent made by oil sand |
| CN101537663A (en) * | 2009-04-30 | 2009-09-23 | 辽河石油勘探局 | Preparation method of high temperature resisting cement grout |
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Owner name: TIANJIN NINGSAI TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: TIANJIN KELIOIL ENGINEERING MATERIAL AND TECHNOLOGY CO., LTD. Effective date: 20130918 |
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Effective date of registration: 20130918 Address after: 301508 north side of satellite River Road, East Tuo Town, Ninghe County, Tianjin Patentee after: TIANJIN NINGSAI TECHNOLOGY CO., LTD. Address before: 301507, Tianjin County, Ninghe East spines Tuo Town West Tuo Tuo village 500 meters east Patentee before: Tianjin Kelioil Engineering Material and Technology Co., Ltd. |