CN113583642B - Modified nano-silica early strength coagulant for oil well cement, preparation method and application thereof - Google Patents
Modified nano-silica early strength coagulant for oil well cement, preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a modified nano-silica early strength coagulant for oil well cement, a preparation method and application thereof, wherein the modified nano-silica early strength coagulant comprises the following components: anhydrous sodium metasilicate, calcium nitrate tetrahydrate, sodium hydroxide solution with the mass fraction of 40%, formaldehyde aqueous solution with the mass fraction of 36% -37%, welan gum, nano titanium dioxide and softened water. The invention adopts a chemical sedimentation method to artificially synthesize nano-scale hydrated silicon dioxide, can accelerate the hydration reaction of cement by utilizing the in-situ growth effect of the hydrated silicon dioxide, improve the mechanical strength development of the set cement, and simultaneously avoid the damage of external harmful ions to the body structure of the set cement. The coagulant is a milky white uniform fluid in appearance and does not settle after long-term storage.
Description
Technical Field
The invention relates to the technical field of oil field chemical additives. In particular to a modified nano-silica early strength coagulant for oil well cement, a preparation method and application thereof.
Background
In shallow well or surface casing cementing operation, although cement slurry can meet pumping requirements, the problems of long thickening time, slow strength development and the like are often caused, the drilling footage and the well cementation quality are seriously influenced, and therefore, a coagulant is required to be added to change the performance of the cement slurry so as to meet the requirements of well cementation operation. The accelerator is an additive added in the process which can reduce the setting time of the cement slurry.
Currently, the common oil well cement set accelerators are mainly calcium chloride, sulfates (sodium sulfate, etc.) and organic amines (triethanolamine, etc.). Calcium chloride is a good coagulation accelerating early strength agent, but the thickening is serious, and chloride ions have strong corrosivity to metal materials such as sleeves and the like, and a plurality of blocks are forbidden to use in the open; the low-temperature early strength effect of the sulfate early strength agent is poor, and the organic amine is too sensitive (easily causes ultra-retardation), so that the application of the sulfate early strength agent in low-temperature well cementation is limited.
With the continuous and deep research of the hydration mechanism of oil well cement, the nano-silica material is found to have the low-temperature coagulation promoting effect, but the nano-silica has high specific surface area, so that the cement slurry is obviously thickened, the slurry flow is influenced, and the nano-silica material is not beneficial to shallow surface cementing with low stratum fracture pressure. Therefore, the modification of nano-silica is needed to prepare the modified nano-silica early strength coagulant for oil well cement.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide the modified nano-silica early strength coagulant for oil well cement, which has moderate coagulation promoting effect and improves the mechanical strength development of set cement, and the preparation method and the application thereof.
In order to solve the technical problems, the invention provides the following technical scheme:
the modified nano-silica early strength coagulant for oil well cement comprises the following components: anhydrous sodium metasilicate, calcium nitrate tetrahydrate, sodium hydroxide solution with the mass fraction of 40%, formaldehyde water solution with the mass fraction of 36% -37%, welan gum, nano titanium dioxide and softened water.
The modified nano-silica early strength coagulant for oil well cement comprises the following components in parts by weight: 120 portions of anhydrous sodium metasilicate, 120 portions of calcium nitrate tetrahydrate, 7 to 11.4 portions of sodium hydroxide solution with the mass fraction of 40 percent, 8 to 9 portions of formaldehyde solution with the mass fraction of 36 to 37 percent, 0.5 to 1.0 portion of welan gum, 0.1 to 0.2 portion of nano titanium dioxide and 780 portions of softened water.
The modified nano-silica early strength coagulant for oil well cement is R-type nano-titania.
The preparation method of the modified nano-silica early strength coagulant for oil well cement comprises the following steps:
(1) weighing anhydrous sodium metasilicate, dissolving in softened water of 70 deg.C, and cooling to 30 + -5 deg.C;
(2) weighing welan gum, 36-37% by mass of formaldehyde water solution and titanium dioxide for later use;
(3) weighing the rest softened water, putting into a three-neck glass flask, and stirring;
(4) putting calcium nitrate tetrahydrate into a three-neck glass flask and continuously stirring;
(5) adjusting the pH value of the material to 9-10 by using a sodium hydroxide solution with the mass fraction of 40%;
(6) dropwise adding the anhydrous sodium metasilicate solution prepared in the step (1) into a three-neck flask while keeping stirring;
(7) reducing the stirring speed, adding welan gum, 36-37% by mass of formaldehyde aqueous solution and nano titanium dioxide, then increasing the stirring speed to react, and obtaining milky uniform fluid which is the modified nano silicon dioxide early strength coagulant for oil well cement after the reaction is finished.
In the step (1), 200 parts by weight of softened water is used to dissolve anhydrous sodium metasilicate to obtain a sodium metasilicate solution.
In the preparation method of the modified nano-silica early strength coagulant for oil well cement, in the step (3), the stirring speed of stirring is started to be 1000 r/min; in step (4), calcium nitrate tetrahydrate is added and stirring is continued for 20 min.
In the step (6), the material change is observed during the process to prevent the material from caking, and the dropping time of the anhydrous sodium metasilicate solution is 2-2.5 h.
In the step (7), the stirring speed is reduced to 600r/min, welan gum, formaldehyde and titanium dioxide are added, the stirring speed is increased to 1200r/min, the timing is started, the reaction is finished after 10 hours of reaction, the stirring is stopped, and milky uniform fluid, namely the modified nano-silica early strength coagulant for oil well cement, is obtained.
The application of the modified nano-silica early strength coagulant for oil well cement.
The modified nano-silica early-strength coagulant is applied to the oil well cement, and the addition amount of the modified nano-silica early-strength coagulant is 3-5% of the mass of the oil well cement.
The technical scheme of the invention achieves the following beneficial technical effects:
1. the invention adopts a chemical sedimentation method to artificially synthesize nano-scale hydrated silicon dioxide, utilizes the in-situ growth effect of the hydrated silicon dioxide on the basis of producing the hydrated silicon dioxide by hydrating cement, further accelerates the rapid hydration reaction of the cement, improves the development of the mechanical early strength of the set cement, and avoids the damage of introducing foreign harmful ions to the body structure of the set cement. The coagulant is a milky homogeneous fluid in appearance and does not settle for long term storage.
2. In the application, anhydrous sodium metasilicate is taken as a silicon source, calcium nitrate tetrahydrate is taken as a calcium source, a formaldehyde water solution, welan gum and nano titanium dioxide are taken as modifiers, and a sodium hydroxide solution with the mass fraction of 40% is used for adjusting the pH of a system to 9-10, so that the coagulation-promoting but thickening-free nano hydrated silicon dioxide is artificially synthesized.
The modifier in the application enables the prepared early strength coagulant to be uniformly and stably dispersed on one hand, and enables the cement to have the characteristics of coagulation acceleration, early strength and no thickening on the other hand.
Welan gum has suspending and dispersing functions and can be used as a suspending and thickening agent;
on one hand, the nano titanium dioxide has good dispersion effect and can increase the permeability of the product; on the other hand, the product has the functions of stain resistance and self cleaning, and can react with redundant formaldehyde in the later product storage process, so that the product is more environment-friendly.
Under the condition of pH 9-10, it has strong dispersion and promotion effect on suspended nano particles.
3. Through the matching use of the components, the prepared early strength coagulant can be stored for a long time without sedimentation, and the cement can be early strength coagulated but not thickened.
Drawings
FIG. 1 is a graph showing the effect of the addition of the modified nano-silica early strength coagulant on the thickening time;
FIG. 2 shows the temperature and compressive strength influence curve of the modified nano-silica early strength coagulant of the present invention.
Detailed Description
Example 1
In this example, the components were as follows by weight: 100kg of anhydrous sodium metasilicate, 100kg of calcium nitrate tetrahydrate, 11.4kg of sodium hydroxide solution with the mass fraction of 40%, 8kg of formaldehyde solution with the mass fraction of 36-37%, 0.5kg of welan gum, 0.1kg of nano titanium dioxide and 780kg of softened water.
The preparation method is as follows:
1. weighing 100kg anhydrous sodium metasilicate, dissolving in 200kg softened water of 70 deg.C, and cooling to 30 + -5 deg.C;
2. weighing 0.5kg of welan gum for later use;
3. weighing 8kg of formaldehyde water solution with the mass fraction of 36-37% for later use;
4. weighing 580kg of residual softened water, putting into a reaction kettle, starting stirring and keeping the stirring speed at 1000 r/min;
5. putting 100kg of calcium nitrate tetrahydrate into a reaction kettle and stirring for 20 minutes;
6. adjusting the pH value of the material to 9-10 by using about 11.4kg of sodium hydroxide solution with the mass fraction of 40%;
7. dropwise adding anhydrous sodium metasilicate solution into the reaction kettle, keeping the stirring state, observing the material change to prevent the material from agglomerating, and finishing the adding within 2-2.5 hours;
8. reducing the stirring speed to 600r/min, adding 0.5kg of welan gum, 8kg of formaldehyde aqueous solution with the mass fraction of 36% -37% and 0.1kg of nano titanium dioxide, increasing the stirring speed to 1200r/min, starting timing, and stopping stirring after reacting for 10 hours;
9. the obtained milk white uniform fluid is the modified nano-silica early strength coagulant for oil well cement.
Example 2
In the present example, the weight of each component is as follows: 100kg of anhydrous sodium metasilicate, 120kg of calcium nitrate tetrahydrate, 7kg of sodium hydroxide solution with the mass fraction of 40%, 9kg of formaldehyde solution with the mass fraction of 36-37%, 1kg of welan gum, 0.2kg of nano titanium dioxide and 780kg of softened water.
The preparation method is as follows:
1. weighing 100kg anhydrous sodium metasilicate, dissolving in 200kg70 deg.C softened water, and cooling to 30 + -5 deg.C;
2. weighing 1kg of welan gum for later use;
3. weighing 9kg of formaldehyde water solution with the mass fraction of 36-37% for later use;
4. weighing 580kg of residual softened water, putting into a reaction kettle, starting stirring and keeping the stirring speed at 1000 r/min;
5. putting 120kg of calcium nitrate tetrahydrate into a reaction kettle and stirring for 20 minutes;
6. adjusting the pH value of the material to 9-10 by using about 7kg of sodium hydroxide solution with the mass fraction of 40%;
7. dropwise adding anhydrous sodium metasilicate solution into the reaction kettle, keeping stirring state, observing material change, preventing material agglomeration, and finishing adding within 2-2.5 hours;
8. reducing the stirring speed to 600r/min, adding 1kg of welan gum, 9kg of 36-37% formaldehyde aqueous solution and 0.2kg of nano titanium dioxide, increasing the stirring speed to 1200r/min, starting timing, and stopping stirring after reacting for 10 hours;
9. the obtained milky uniform fluid is the modified nano silicon dioxide early strength coagulant for oil well cement.
The modified nano-silica early strength accelerating agent for oil well cement prepared in example 1 and example 2 was evaluated for performance.
1. EXAMPLES results of benchmarking evaluation according to Accelerator industry standards
According to the oil well cement admixture evaluation method part 4 in the oil and gas industry Standard of the people's republic of China (SY/T5504.4-2019): accelerator "requirements were evaluated.
The specific implementation process is as follows:
example 1 base recipe: 792G +/-0.5G of Jiahua cement (G level high resistance), 349G +/-0.5G of water (including water in liquid coagulant), 5% of the cement mass in example 1, and the density of 1.91G/cm prepared by the method specified in GB/T19139 3 ±0.02g/cm 3 。
Example 2 base recipe: 792G +/-0.5G of Jiahua cement (G-level high-resistance), 349G +/-0.5G of water (including water in liquid coagulant), which accounts for 4 percent of the mass of the cement, of example 2 is prepared into the cement with the density of 1.91G/cm according to the method specified in GB/T19139 3 ±0.02g/cm 3 。
The performance comparison is shown in table 1.
TABLE 1
In example 1, the overall stability of the product was high due to the low contents of the calcium source and the silicon source, but the cost was increased due to the low content of the raw materials and the low content of the effective components of the product, which is an intangible ratio product. The addition amount is recommended to be 4-5% (W/C).
In example 2, the addition amount is recommended to be 3% -4% (W/C) for the optimized optimal solution.
2. The modified nano-silica early strength coagulant prepared in the example 2 is adopted to carry out application test on site.
The basic formula is as follows: the cement is prepared from Sichuan Jiahua cement (G-level high-resistance), G311 (AMPS copolymer produced by Weihui chemical Co., Ltd.) accounting for 3% of the mass of the cement, a nano early strength coagulant accounting for 3% of the mass of the cement and tap water (0.38W/C) accounting for 38% of the mass of the cement at 50 ℃.
Table 2 is a data comparison table of the modified nano-silica early strength coagulant prepared in example 2 and the composite early strength agent G209 produced by waihui chemical limited company of the applicant.
TABLE 2
Rheology and non-thixotropic property of cement paste show that the early strength coagulant does not thicken, and has no influence on the rheology of the cement paste, and blank and thickening time of nano early strength agent at 50 ℃ are compared, thereby powerfully showing the excellent effect of the early strength coagulant at a medium and low temperature section. (thickening and set-accelerating differ in this application, thickening being the thickening of the cement paste and set-accelerating being the early compressive strength of the cement paste)
As the addition of the modified nanosilica early strength coagulant increased, the thickening time decreased, as shown in table 3.
TABLE 3
| Addition amount (%) | Thickening time (min) |
| 0 | 113 |
| 1 | 100.3 |
| 2 | 86.5 |
| 3 | 69.2 |
| 4 | 66.2 |
It can be seen that the cement hydration reaction can be accelerated with the addition of the modified nano-silica early strength coagulant, so that the cement paste thickening time is substantially linearly shortened, as shown in fig. 1.
At the same addition, the cement slurry thickening time is also linear in temperature. With increasing temperature, the thickening time decreased (fig. 2), as shown in table 4.
TABLE 4
| Temperature (. degree.C.) | Thickening time (min) |
| 35 | 100.4 |
| 45 | 69.2 |
| 55 | 59.3 |
The effect of adding the early strength set accelerator on the 8 hour compressive strength of the set cement is shown in table 5 and figure 2.
TABLE 5
Figure 2 shows that the compressive strength of set cement at 8 hours after addition of the early strength set accelerator increases significantly and linearly with increasing temperature compared to the strength without addition of the nano early strength accelerator.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This need not be, nor should it be exhaustive of all embodiments. And obvious variations or modifications are possible which remain within the scope of the appended claims.
Claims (5)
1. The modified nano-silica early strength coagulant for oil well cement is characterized by comprising the following components: anhydrous sodium metasilicate, calcium nitrate tetrahydrate, sodium hydroxide solution with the mass fraction of 40%, formaldehyde water solution with the mass fraction of 36% -37%, welan gum, nano titanium dioxide and softened water;
the weight ratio of each component is as follows: 120 portions of anhydrous sodium metasilicate, 120 portions of calcium nitrate tetrahydrate, 7 to 11.4 portions of sodium hydroxide solution with the mass fraction of 40 percent, 8 to 9 portions of formaldehyde water solution with the mass fraction of 36 to 37 percent, 0.5 to 1.0 portion of welan gum, 0.1 to 0.2 portion of nano titanium dioxide and 780 portions of softened water; the nano titanium dioxide is R-type nano titanium dioxide;
the preparation method comprises the following steps:
(1) weighing anhydrous sodium metasilicate, dissolving in softened water of 70 deg.C, and cooling to 30 + -5 deg.C;
(2) weighing welan gum, 36-37% of formaldehyde water solution and titanium dioxide for later use;
(3) weighing the rest softened water, putting into a three-neck glass flask, and stirring;
(4) putting calcium nitrate tetrahydrate into a three-neck glass flask and continuously stirring;
(5) adjusting the pH value of the material to 9-10 by using a sodium hydroxide solution with the mass fraction of 40%;
(6) dropwise adding the anhydrous sodium metasilicate solution prepared in the step (1) into a three-neck flask while keeping stirring;
(7) reducing the stirring speed, adding welan gum, 36-37% by mass of formaldehyde aqueous solution and nano titanium dioxide, then increasing the stirring speed to react, and obtaining milky uniform fluid which is the modified nano silicon dioxide early strength coagulant for oil well cement after the reaction is finished;
in the step (6), the material change is observed during the process to prevent the material from agglomerating, and the dripping time of the anhydrous sodium metasilicate solution is 2-2.5 h;
in the step (7), the stirring speed is reduced to 600r/min, welan gum, formaldehyde and titanium dioxide are added, then the stirring speed is increased to 1200r/min, timing is started, after the reaction lasts for 10 hours, the reaction is finished, and the stirring is stopped, so that milky uniform fluid, namely the modified nano-silica early strength coagulant for oil well cement, is obtained.
2. The preparation method of the modified nano-silica early strength coagulant for oil well cement of claim 1 is characterized by comprising the following steps:
(1) weighing anhydrous sodium metasilicate, dissolving in softened water of 70 deg.C, and cooling to 30 + -5 deg.C;
(2) weighing welan gum, 36-37% by mass of formaldehyde water solution and titanium dioxide for later use;
(3) weighing the rest softened water, putting into a three-neck glass flask, and stirring;
(4) putting calcium nitrate tetrahydrate into a three-neck glass flask and continuously stirring;
(5) adjusting the pH value of the material to 9-10 by using a sodium hydroxide solution with the mass fraction of 40%;
(6) dropwise adding the anhydrous sodium metasilicate solution prepared in the step (1) into a three-neck flask while keeping stirring;
(7) reducing the stirring speed, adding welan gum, 36-37% by mass of formaldehyde aqueous solution and nano titanium dioxide, then increasing the stirring speed to react, and obtaining milky uniform fluid which is the modified nano silicon dioxide early strength coagulant for oil well cement after the reaction is finished;
in the step (6), the material change is observed during the process to prevent the material from agglomerating, and the dripping time of the anhydrous sodium metasilicate solution is 2-2.5 h;
in the step (7), the stirring speed is reduced to 600r/min, welan gum, formaldehyde and titanium dioxide are added, then the stirring speed is increased to 1200r/min, timing is started, after the reaction lasts for 10 hours, the reaction is finished, and the stirring is stopped, so that milky uniform fluid, namely the modified nano-silica early strength coagulant for oil well cement, is obtained.
3. The method for preparing the modified nano-silica early strength coagulant according to claim 2, wherein in the step (1), the anhydrous sodium metasilicate is dissolved with 200 parts by weight of the softened water to obtain the sodium metasilicate solution.
4. The method for preparing the modified nano-silica early strength coagulant for oil well cement according to claim 2, wherein in the step (3), the stirring speed of starting stirring is 1000 r/min; in step (4), calcium nitrate tetrahydrate is added and stirring is continued for 20 min.
5. The application of the modified nano-silica early strength coagulant for oil well cement as claimed in claim 1, wherein the addition amount of the modified nano-silica early strength coagulant is 3% -5% of the mass of the oil well cement.
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| US9567262B2 (en) * | 2010-02-25 | 2017-02-14 | Construction Research & Technology Gmbh | Hardening accelerator composition containing dispersants |
| ES2745743T3 (en) * | 2011-05-26 | 2020-03-03 | Saint Gobain Weber | Hydraulic binder comprising an accelerator, its use and preparation procedure for a construction material |
| WO2013083627A1 (en) * | 2011-12-05 | 2013-06-13 | Sika Technology Ag | Process for producing hardening accelerators for mineral binder compositions |
| WO2020019070A1 (en) * | 2018-07-24 | 2020-01-30 | Trican Well Service Ltd | Cement compositions and methods of making the same |
| CN110423315A (en) * | 2019-08-13 | 2019-11-08 | 重庆三圣实业股份有限公司 | A kind of nanometer of C-S-H gel super instant coagulant and preparation method thereof |
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| WO2011026723A1 (en) * | 2009-09-02 | 2011-03-10 | Construction Research & Technology Gmbh | Sulphonic acid and aromatic groups containing hardening accelerator compositions |
| CN109095807A (en) * | 2018-10-17 | 2018-12-28 | 武汉三源特种建材有限责任公司 | A kind of concrete liquid super instant coagulant and preparation method thereof |
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