CN103396775B - A kind of resistant, toughened retardant - Google Patents
A kind of resistant, toughened retardant Download PDFInfo
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- CN103396775B CN103396775B CN201310307297.1A CN201310307297A CN103396775B CN 103396775 B CN103396775 B CN 103396775B CN 201310307297 A CN201310307297 A CN 201310307297A CN 103396775 B CN103396775 B CN 103396775B
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- sepiolite
- borax
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- boric acid
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Abstract
The invention discloses a kind of resistant, toughened retardant, be prepared as follows: sepiolite is pulverized by (1), through water soaking, stir clarification, refilter, clean, dry, pulverize, levigately to sieve; Sepiolite powder is added in nitric acid, sulfuric acid or hydrochloric acid soln, after stirring 3 ~ 8h, with deionized water wash to neutral, filters; At 100 ~ 200 DEG C after roasting 2 ~ 4h, at 600 DEG C, calcine 2 ~ 3h again; (2) borax is mixed with the mass ratio of boric acid according to 1.2 ~ 4:6 ~ 8.8, be slowly poured into water, stir 5 ~ 15min; (3) sepiolite after process is joined in the mixing solutions of borax and boric acid, stir 2 ~ 4h, make sepiolite-boric acid, borax mixed solution; (4) spraying dry.Slow releasing delayed coagulation composition of the present invention, reduces cement to the sensitivity of retardant, has good mechanical property, still can play delayed coagulation and on mechanical property without impact under high temperature under making Behavior of Hardened Cement Paste low temperature.
Description
Technical field
The present invention relates to for the toughness reinforcing retardant of the one of oil gas well cementing operation in petroleum natural gas exploration, this retardant improves Mechanical Behavior of Hardened Cement Paste while regulating the cement thickening time.
Background technology
Along with petroleum exploration and development is constantly to hot hole, deep-well and ultra deep well future development, grout in well cementing process is required to have good heat-resisting property and pumpability, depend merely on the basic skills changing cement clinker chemical composition and mineral composition thereof, be difficult to tackle and adapt to, therefore in hot hole, deep-well and ultra deep well well cementing operation in order to prevent pumps water mud quick multiviscosisty and condensation in whole pumping procedure, must add suitable retardant with make cementing job safety carry out smoothly.And the exploitation along with various hot hole, deep-well, ultra deep well and Holes of Complicated Wells also needs Behavior of Hardened Cement Paste to have good mechanical property.In existing retardant ubiquity, under low temperature, retarding effect is good but be not suitable for hot conditions, affect cement strength and the high shortcoming of susceptibility, therefore develops resistant, toughened retardant significant.
At present, reported in literature is had to utilize metakaolin-slag base geological polymer (200810020859.3), the high temperature retarder of the polymkeric substance such as AMPS (200810160489.3) and the preparation such as organism and mixture of inorganic substance (200910229271.3), improve the grout thickening time at high temperature, make the safe pumping of grout.But and have no the relevant report improving the mechanical property of Behavior of Hardened Cement Paste while improving the grout high temperature thickening time, regulating the susceptibility of retardant dosage.
Boric acid and borax are that retardant commonly used by oil well cement, have good delayed coagulation to oil well cement, but the dosage of boric acid and thickening time are broken line or exponential relationship, and dosage sensitivity is very high; Just lose its delayed coagulation when borax uses in hot environment and do not possess toughening effect.Sepiolite is a kind of fibrous rich magnesium silicate mineral, belongs to sepiolite-palygorskite clay mineral race.In the sepiolite (α-type sepiolite) that threadiness exists, there is great potential specific surface area and pore volume, high adsorption capacity, Heat stability is good, good salt resistance, rheological and catalytic performance and become of many uses, Application Areas expansion one of mineral products more rapidly in modern age.Be combined with boric acid and borax by sepiolite, maximize favourable factors and minimize unfavourable ones, thus prepare high temperature resistant, sensitivity is moderate and have the retardant of toughening effect.
Summary of the invention
The object of the present invention is to provide a kind of resistant, toughened retardant, this retardant has slow releasing delayed coagulation composition, reduce cement to the sensitivity of retardant, thickening time is more easily regulated, under the toughness reinforcing composition of high temperature resistance simultaneously contained in retardant makes Behavior of Hardened Cement Paste low temperature, there is good mechanical property, still can play delayed coagulation under hot environment and on the mechanical property of high temperature without impact.
For reaching above technical purpose, the invention provides following technical scheme.
A kind of resistant, toughened retardant, prepare as follows:
(1) process of sepiolite
Screening: sepiolite is pulverized, through water soaking, remove sand setting after stirring clarification, refilter, clean, dry, pulverize, levigately to sieve, making order number is 300 order ~ 1300 object sepiolite powders.
Acid activation process: be added to by sepiolite powder in nitric acid, sulfuric acid or the hydrochloric acid soln that concentration is 0.4 ~ 2.0mol/L, low whipping speed is after stirring 3 ~ 8h under the condition of 120 ~ 150r/min, with deionized water wash to neutral, filters.
Roasting: be take out after roasting 2 ~ 4h under the condition of 100 ~ 200 DEG C in temperature, (heat-up rate is 10 ~ 15 DEG C/min) calcines 2 ~ 3h at 600 DEG C again, and obtained sepiolite is stand-by.
The sepiolite that the present invention selects is chemical constitution content of MgO is 19.0 ~ 30.0 quality %, SiO
2content is 57.0 ~ 70.0 quality %, Al
2o
3content is the hot-liquid type sepiolite of a kind of macrofiber shape of 0.2 ~ 7.9 quality %, i.e. α-type sepiolite.The hardness of sepiolite is 2.2 ~ 2.5, and relative density is 2.1 ~ 2.6.
(2) preparation of borax and boric acid mixing solutions
Borax is mixed with the mass ratio of boric acid according to 1.2 ~ 4:6 ~ 8.8, opens low-speed agitator and under the rotating speed of 1200r/min, it is slowly poured into water, stir 5 ~ 15min, be mixed with the solution that concentration is 10000 ~ 11340mg/L.
(3) adsorption process
Sepiolite 25 ~ 30g after process is joined in the mixing solutions of 450 ~ 600mL borax and boric acid, under the condition of 100 ~ 200r/min, stirs 2 ~ 4h, make sepiolite-boric acid, borax mixed solution.
(4) spraying dry
Sepiolite-boric acid, borax mixed solution are placed in spray drying device, and drying temperature is 150 ~ 250 DEG C, takes out, obtain resistant, toughened retardant after process 1.5s.
The above material is commercially available.
Compared with prior art, the present invention has following beneficial effect: this retardant has slow releasing slow setting composition, certain toughening effect is had to Behavior of Hardened Cement Paste while at high temperature still delayed coagulation can being played to grout, stable performance, its preparation method technique is simple, easy to operate, with low cost, production controllability is strong, good product consistency.The cement slurry thickening time obtained with this retardant is adjustable, sedimentation stability good, good fluidity, fluid loss are less, and after high temperature, intensity does not fail.
Embodiment
The preparation and property test of resistant, toughened retardant, cement paste for well cementation
Embodiment 1:
In the preparation process of resistant, toughened retardant, correlation parameter is as follows:
Sepiolite order number (order): 300
Concentration of nitric acid (mol/L): 0.4
Sepiolite acid activation stirring velocity (r/min): 120
Sepiolite acid activation time (h): 3
Sepiolite maturing temperature (DEG C): 110
Sepiolite roasting time (h): 2
Borax quality (g): 12
Boric acid quality (g): 88
Absorption sepiolite quality (g): 25
Absorption boric acid-borax soln volume (mL): 450
Adsorption time (h): 2
Spray drying temperature (DEG C): 150
Prepare cement paste for well cementation: take 100 weight part oil well cements, 40 weight part quartz sands, 3 weight part Natvosols are dry mixed as dry powder, measure 61 parts of water, and the resistant, toughened retardant of 0.4 ~ 2 weight part, 0.1 weight part dimethyl silicone oil is soluble in water.Then, put by the aqueous solution in the mixing container, agitator rotates with low speed (4000 ± 200r/min), and in 15 seconds, add the dry powder taking mixing, covers the lid of agitator, and continues stirring 35 seconds under high speed (12000 ± 500r/min).
After preparing cementing slurry according to API specification, test its engineering property.Thickening time test condition is: 200 DEG C × 150MPa.Behavior of Hardened Cement Paste curing condition is: low temperature 50 DEG C × 0.1MPa × 72h, high temperature 315 DEG C × 21MPa × 168h.
The Performance Detection of this grout and Behavior of Hardened Cement Paste is in table 1 and table 2.
Embodiment 2:
In the preparation process of resistant, toughened retardant, correlation parameter is as follows:
Sepiolite order number (order): 500
Concentration of nitric acid (mol/L): 1.5
Sepiolite acid activation stirring velocity (r/min): 120
Sepiolite acid activation time (h): 3.5
Sepiolite maturing temperature (DEG C): 115
Sepiolite roasting time (h): 2
Borax quality (g): 30
Boric acid quality (g): 70
Absorption sepiolite quality (g): 26
Absorption boric acid-borax soln volume (mL): 500
Adsorption time (h): 2
Spray drying temperature (DEG C): 180
Prepare cement paste for well cementation: take 100 weight part oil well cements, 40 weight part slags, 2.5 weight part Natvosols are dry mixed as dry powder, measure 60 parts of water, and the resistant, toughened retardant of 0.4 ~ 2.5 weight part, 0.2 weight part dimethyl silicone oil is soluble in water.Then, put by the aqueous solution in the mixing container, agitator rotates with low speed (4000 ± 200r/min), and in 15 seconds, add the dry powder taking mixing, covers the lid of agitator, and continues stirring 35 seconds under high speed (12000 ± 500r/min).
After preparing cementing slurry according to API specification, test its engineering property.Thickening time test condition is: 200 DEG C × 150MPa.Behavior of Hardened Cement Paste curing condition is: low temperature 50 DEG C × 0.1MPa × 72h, high temperature 315 DEG C × 21MPa × 168h.
The Performance Detection of this grout and Behavior of Hardened Cement Paste is in table 3 and table 4.
Embodiment 3:
In the preparation process of resistant, toughened retardant, correlation parameter is as follows:
Sepiolite order number (order): 800
Concentration of nitric acid (mol/L): 0.6
Sepiolite acid activation stirring velocity (r/min): 130
Sepiolite acid activation time (h): 5
Sepiolite maturing temperature (DEG C): 140
Sepiolite roasting time (h): 2.5
Borax quality (g): 36
Boric acid quality (g): 64
Absorption sepiolite quality (g): 28
Absorption boric acid-borax soln volume (mL): 550
Adsorption time (h): 2.5
Spray drying temperature (DEG C): 200
Prepare cement paste for well cementation: take 100 weight part oil well cements, 30 weight parts of fine coal ashes, 1.5 weight part Natvosols are dry mixed as dry powder, measure 60 parts of water, and the resistant, toughened retardant of 0.4 ~ 2.5 weight part, 0.1 weight part dimethyl silicone oil is soluble in water.Then, put by the aqueous solution in the mixing container, agitator rotates with low speed (4000 ± 200r/min), and in 15 seconds, add the dry powder taking mixing, covers the lid of agitator, and continues stirring 35 seconds under high speed (12000 ± 500r/min).
After preparing cementing slurry according to API specification, test its engineering property.Thickening time test condition is: 200 DEG C × 150MPa.Behavior of Hardened Cement Paste curing condition is: low temperature 50 DEG C × 0.1MPa × 72h, high temperature 315 DEG C × 21MPa × 168h.
The Performance Detection of this grout and Behavior of Hardened Cement Paste is in table 5 and table 6.
Embodiment 4:
In the preparation process of resistant, toughened retardant, correlation parameter is as follows:
Sepiolite order number (order): 1250
Concentration of nitric acid (mol/L): 1.0
Sepiolite acid activation stirring velocity (r/min): 140
Sepiolite acid activation time (h): 6.5
Sepiolite maturing temperature (DEG C): 170
Sepiolite roasting time (h): 2.5
Borax quality (g): 30
Boric acid quality (g): 70
Absorption sepiolite quality (g): 30
Absorption boric acid-borax soln volume (mL): 600
Adsorption time (h): 2.5
Spray drying temperature (DEG C): 230
Prepare cement paste for well cementation: take 100 weight part oil well cements, 35 weight part quartz sands, 2.0 weight part Natvosols are dry mixed as dry powder, measure 60 parts of water, and the resistant, toughened retardant of 0.2 ~ 2.5 weight part, 0.15 weight part dimethyl silicone oil is soluble in water.Then, put by the aqueous solution in the mixing container, agitator rotates with low speed (4000 ± 200r/min), and in 15 seconds, add the dry powder taking mixing, covers the lid of agitator, and continues stirring 35 seconds under high speed (12000 ± 500r/min).
After preparing cementing slurry according to API specification, test its engineering property.Thickening time test condition is: 200 DEG C × 150MPa.Behavior of Hardened Cement Paste curing condition is: low temperature 50 DEG C × 0.1MPa × 72h, high temperature 315 DEG C × 21MPa × 168h.
The Performance Detection of this grout and Behavior of Hardened Cement Paste is in table 7 and table 8.
Table 1 cement paste for well cementation engineering property test result (embodiment 1)
Table 2 is cemented the well with Mechanical Behavior of Hardened Cement Paste test result (embodiment 1)
Table 3 cement paste for well cementation engineering property test result (embodiment 2)
Table 4 is cemented the well with Mechanical Behavior of Hardened Cement Paste test result (embodiment 2)
Table 5 cement paste for well cementation engineering property test result (embodiment 3)
Table 6 is cemented the well with Mechanical Behavior of Hardened Cement Paste test result (embodiment 3)
Table 7 cement paste for well cementation engineering property test result (embodiment 4)
Table 8 is cemented the well with Mechanical Behavior of Hardened Cement Paste test result (embodiment 4)
Can be found out by table 1 ~ table 8, while this resistant, toughened retardant can effectively improve the cement thickening time, reduce the fragility of well-cementing cement, and do not affect the intensity after Behavior of Hardened Cement Paste high temperature.
Claims (1)
1. a resistant, toughened retardant, prepare as follows:
(1) sepiolite is pulverized, through water soaking, removes sand setting after stirring clarification, refilter, clean, dry, pulverize, levigately to sieve, making order number is 300 order ~ 1300 object sepiolite powders; Be added to by sepiolite powder in nitric acid, sulfuric acid or the hydrochloric acid soln that concentration is 0.4 ~ 2.0mol/L, low whipping speed is after stirring 3 ~ 8h under the condition of 120 ~ 150r/min, with deionized water wash to neutral, filters; Be take out after roasting 2 ~ 4h under the condition of 100 ~ 200 DEG C in temperature, at 600 DEG C, calcine 2 ~ 3h again;
(2) borax is mixed with the mass ratio of boric acid according to 1.2 ~ 4:6 ~ 8.8, open low-speed agitator and under the rotating speed of 1200r/min, it is slowly poured into water, stir 5 ~ 15min, be mixed with the solution that concentration is 10000 ~ 11340mg/L;
(3) the sepiolite 25 ~ 30g after process is joined in the mixing solutions of 450 ~ 600mL borax and boric acid, under the condition of 100 ~ 200r/min, stir 2 ~ 4h, make sepiolite-boric acid, borax mixed solution;
(4) sepiolite-boric acid, borax mixed solution are placed in spray drying device, drying temperature is 150 ~ 250 DEG C, takes out, obtain resistant, toughened retardant after process 1.5s.
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| CN103396775B true CN103396775B (en) | 2015-10-14 |
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| CN105368418B (en) * | 2015-12-11 | 2018-01-23 | 西南石油大学 | A kind of coconut carbon fibre toughener for being used to improve well-cementing cement mechanical property |
| CN112635099B (en) * | 2020-12-08 | 2021-10-26 | 重庆大学 | Insulating material for manufacturing mineral insulated cable and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401421A (en) * | 2002-09-24 | 2003-03-12 | 武汉理工大学 | Hydrogen-storage sepiolite mineral material and preparing process thereof |
| CN101321712A (en) * | 2005-10-25 | 2008-12-10 | 普拉德研究及开发股份有限公司 | Versatile additives for well cementing applications |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401421A (en) * | 2002-09-24 | 2003-03-12 | 武汉理工大学 | Hydrogen-storage sepiolite mineral material and preparing process thereof |
| CN101321712A (en) * | 2005-10-25 | 2008-12-10 | 普拉德研究及开发股份有限公司 | Versatile additives for well cementing applications |
Non-Patent Citations (2)
| Title |
|---|
| 活化海泡石吸附性能研究;侯立臣等;《污染防治技术》;19990331;第12卷(第01期);40-42 * |
| 海泡石的酸改性对其吸附性能的影响;杨翠英等;《山东科技大学学报(自然科学版)》;20050930;第24卷(第03期);97-100 * |
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