CN104531110B - A kind of preparation method of the oil well cement additive of anti-hydrogen sulfide corrosion - Google Patents
A kind of preparation method of the oil well cement additive of anti-hydrogen sulfide corrosion Download PDFInfo
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- CN104531110B CN104531110B CN201410755763.7A CN201410755763A CN104531110B CN 104531110 B CN104531110 B CN 104531110B CN 201410755763 A CN201410755763 A CN 201410755763A CN 104531110 B CN104531110 B CN 104531110B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
- C04B22/08—Acids or salts thereof
- C04B22/10—Acids or salts thereof containing carbon in the anion
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/0068—Ingredients with a function or property not provided for elsewhere in C04B2103/00
- C04B2103/0078—Sorbent materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/60—Agents for protection against chemical, physical or biological attack
- C04B2103/61—Corrosion inhibitors
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/32—Anticorrosion additives
Abstract
The present invention relates to a kind of preparation method of the oil well cement additive of anti-hydrogen sulfide corrosion, is comprised the following steps successively：(1) process of meerschaum；(2) in ZnCl2Isopropanol, Deca Na are added in solution2CO3Solution, adds Dodecyl trimethyl ammonium chloride, reaction to cool down after 23 hours, and washing, sucking filtration, drying obtain a nanometer basic zinc carbonate；(3) take during a nanometer basic zinc carbonate is added to NaOH solution and form basic carbonate zinc solution；(4) basic carbonate zinc solution is placed in electrolytic cell anode pond, meerschaum is placed in the cathode pool containing HCl solution, be powered, after 10 30 minutes, take out meerschaum solution, filtering drying grinds to form 500 800 mesh powder, as oil well cement additive.The present invention is easy to operate, and raw material is easy to get, and product yield is higher, can effectively improve the anti-H of Behavior of Hardened Cement Paste2The ability of S corrosion, can be used at high temperature, and salt tolerance is strong, and cement mortar engineering property is had no adverse effect.
Description
Technical field
The present invention relates to during Cementing the oil well cement additive of anti-hydrogen sulfide corrosion preparation method, it is main to use
In the oil gas well cementing operation slurry design of high sulfur-bearing, the anti-H of Behavior of Hardened Cement Paste is improved2S corrosive powers.
Background technology
With continuing to increase for oil and gas development degree, the quantity of high sulfur crude gas well is more and more, H2S is produced as natural gas
In associated gas be present in stratum.In Gas field 80% be sour natural gas, H in natural gas2S contents are mostly in 1%-
Between 13%, 35% is reached as high as.China H2S acid gas fields containing highest are North China Zhao Lanzhuan oil gas fields, and content reaches as high as
92%.H2The presence of S reduces the alkalescence of Behavior of Hardened Cement Paste, causes the corrosion of the corrosion failure and production tube of cement sheath and sleeve pipe to break
Split.With the increase of extent of corrosion, in Behavior of Hardened Cement Paste, cementing properties component is reduced, and pore structure destruction, permeability become big, comprcssive strength
Reduce even completely losing, and other down-hole accidents may be induced.It is high to contain H2The acidic materials such as S are to Behavior of Hardened Cement Paste seriously corroded, ring
Easily there is has channeling after forming etching channels in empty cement sheath, occur that well head annular space is with pressure, and the safety in production of oil supply gas well brings sternness
Challenge, greatly destruction is caused to life around, property and environment.Cement sheath can cause the corrosion of sleeve pipe after being corroded, plus
Finish the service life of other metal tools of the down-hole such as sleeve pipe soon, thus also bring huge economic loss, China in 2012
Petroleum industry is every year due to corroding the loss for causing more than 40,000,000,000 yuan.
Micro- silicon, flyash, slag are used equally to improve Behavior of Hardened Cement Paste decay resistance, but the addition of these extra materials is to water
The etch-proof long-term effect of mudstone is unsatisfactory.The organic polymer such as TH resins of anti-hydrogen sulfide corrosion mortar architecture also by with
In raising Behavior of Hardened Cement Paste decay resistance, but this cement slurry ties up to matter property shakiness under high salty formation and hot conditionss
It is fixed, corrosion-resisting function can be lost.
In order to improve Behavior of Hardened Cement Paste in H2Long term structural integrity and sealing under S media, is badly in need of exploitation new
Corrosion Proof Cement System, solves the long-term anticorrosive problem of cement sheath, realizes the safety in production of gas well and extends the gas well life-span.This
Invention provides a kind of anti-H2The preparation method of the oil well additive of S corrosion, the additive energy and H2S reacts the protection to form densification
Layer prevents H2S is further to Behavior of Hardened Cement Paste diffusion inside.The corrosion resistance of hardened oilwell cement is improved, it is abundant in high temperature and stratum water
Under conditions of can also play a role, and then reach the purpose of safe and efficient production.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the oil well cement additive of anti-hydrogen sulfide corrosion, principle can
Lean on, easy to operate, raw material is easy to get, and product yield is higher, and the additive of preparation is added in oil well cement paste, effectively improves water
The anti-H of mudstone2The ability of S corrosion, can use under 130 DEG C of hot conditionss, and salt tolerance is strong, and to cement mortar engineering property invariably
Profit affects.
To reach above technical purpose, the present invention provides technical scheme below.
A kind of preparation method of the oil well cement additive of anti-hydrogen sulfide corrosion, is comprised the following steps successively：
(1) process of meerschaum
Meerschaum is added in the water of 10 times of volumes, is stirred 20 minutes, meerschaum takes upper liquid in the suspension of upper strata,
Sucking filtration and with distilled water wash after, be placed under the conditions of 140 DEG C of baking oven and be vacuum dried 3 hours, smash into 500 mesh powder, by the powder
End is added in reactor with the water of 20 times of volumes, is stirred 1 hour at 120-220 DEG C, is separated drying, use 2-5 matter then at 60 DEG C
After the hydrochloric acid of amount % carries out activation processing 1 hour, 140 DEG C of Jing is drying to obtain Activated Sepiolite, calcines 1 hour at 600 DEG C.
(2) preparation of nanometer basic zinc carbonate
By 100mL, ZnCl of the concentration for 2moL/L2Solution is poured in 500mL there-necked flasks, while adding the isopropyl of 50mL
Alcohol, is stirred and heated to 70 DEG C, by 100mL, Na of the concentration for 2moL/L2CO3Solution Deca is in there-necked flask, and adds 10g
Dodecyl trimethyl ammonium chloride, cools down after reaction 2-3 hours, with distilled water wash, sucking filtration, is subsequently placed in 110 DEG C of vacuum and does
It is dried in dry case, obtains final product a nanometer basic zinc carbonate.
(3) prepare basic carbonate zinc solution
Take 20g nanometer basic zinc carbonates and be added to 100mL, concentration is to stir 10-30 in the NaOH solution of 5-10 mass %
Minute, form basic carbonate zinc solution.
(4) Zn is made using electrophoretic techniquess2+Uniform adsorption is in meerschaum surface and hole
Basic carbonate zinc solution is placed in electrolytic cell anode pond, then the meerschaum for processing is placed in containing 3-5 matter
In the cathode pool of the HCl solution of amount %, ion permeability film UNICOM is used in the middle of electrolyzer, is powered, electric current is 10mA, 10-30 point
After clock take out meerschaum solution, after filtration in 140 DEG C of baking ovens vacuum drying 2 hours, grind to form 500-800 mesh powder, as
Oil well cement additive.
Above-mentioned substance commercially has sale.
The above-mentioned process to meerschaum makes meerschaum have more preferable distribution of pores and an adsorptivity, and isopropanol is acted on
In the dispersibility for improving solution, the effect of Dodecyl trimethyl ammonium chloride is the degree of crystallinity for reducing basic zinc carbonate, and adjustable
Section pH value is conducive to the formation of basic zinc carbonate.
Additive favorable dispersibility in cement mortar, with H2S reacts the protective layer prevention H to form densification2S further to
Behavior of Hardened Cement Paste diffusion inside.And the additive of this special handling is avoided and H2There is fierce reaction in S, can play for a long time
Effect, improves the Corrosion Protection of oil-well cement, and the present invention still has effect at a high temperature of certain in addition.
Compared with prior art, production process of the invention is easy to operate, with low cost, and effect is substantially, and compatibility is good,
It is easy to engineer applied.After the additive is added in oil-well cement, Mechanical Behavior of Hardened Cement Paste and pore structure are improved：
(1) little is affected on Behavior of Hardened Cement Paste early stage comprcssive strength, highest reduces by 6%, can meet engine request；
(2) after Behavior of Hardened Cement Paste corrosion, strength ratio starches intensity height only, is up to 2.7 times of net pulp-water mudstone；
(3) the Behavior of Hardened Cement Paste permeability after corroding added with the additive is obvious lower than the Behavior of Hardened Cement Paste for not adding the additive, highest
Reduce 35.71%.
Specific embodiment
Below according to embodiment, the present invention is further illustrated.
Below if no special instructions, the percent of each material is mass percent, and number is mass parts.
Embodiment 1
Process for preparation parameter：
Meerschaum and water mixed volume ratio：1:10；
Meerschaum mixed liquor mixing time：20 minutes；
Meerschaum drying temperature：140℃；
Meerschaum drying time：3 hours；
Mesh number after meerschaum smashing：500 mesh；
Meerschaum heating-up temperature in a kettle.：120℃；
Meerschaum mixing time in a kettle.：1 hour；
Concentration of hydrochloric acid：2%；
Activation temperature：60℃；
Meerschaum calcination time：1 hour；
Meerschaum calcining heat：600℃；
Isopropanol dosage：50mL；
Agitating heating temperature：70℃；
Dodecyl trimethyl ammonium chloride dosage：10g；
Zinc chloride and sodium carbonate response time：2 hours；
Basic carbonate baking temperature：110℃；
Electrolyte HCl solution concentration：3%；
Conduction time：10 minutes；
Size of current is：10mA；
Meerschaum drying temperature and time after electrophoresis：140 DEG C, 2 hours；
Product mesh number：500 mesh.
Cement mortar basic components：100 parts of good China G class g cements, fluid loss agent (blue moral petrochemical iy produced 2- acrylamido -2-
Dimethyl propylene sulphonic acids polymer) 5 parts, liquid-solid ratio 0.44.It is with slurry according to 10 standards of API, compare the cement without additive
Slurry, and the mortar architecture containing 0.5%, 1%, 3%, 5% additive forms the Corrosion Protection of Behavior of Hardened Cement Paste respectively.
The cement mortar for preparing is poured in the annular die of ready Φ 25.4mm × 25.4mm, 90 DEG C of sheet glass is covered
Conserve 48 hours in lower water-bath, the demoulding.Simultaneously a part of cement mortar is poured in the Fang Mo of 5mm × 5mm × 5mm in curing autoclave
In coring after maintenance 48 hours at 90 DEG C.Behavior of Hardened Cement Paste sample is put in high temperature pressure corrosion instrument together and is corroded 21 days.Test 90
℃、H2With 130 DEG C, H under the conditions of S partial pressure 1MPa stagnation pressure 3MPa2Comprcssive strength before and after corroding under the conditions of S partial pressure 1MPa stagnation pressure 3MPa
With the change of permeability, 1 and table 2 are the results are shown in Table.
Embodiment 2
Process for preparation parameter：
Meerschaum and water mixed volume ratio：1:10；
Meerschaum mixed liquor mixing time：20 minutes；
Meerschaum drying temperature：140℃；
Meerschaum drying time：3 hours；
Mesh number after meerschaum smashing：500 mesh；
Meerschaum heating-up temperature in a kettle.：160℃；
Meerschaum mixing time in a kettle.：1 hour；
Concentration of hydrochloric acid：3%；
Activation temperature：60℃；
Meerschaum calcination time：1 hour；
Meerschaum calcining heat：600℃；
Isopropanol dosage：50mL；
Agitating heating temperature：70℃；
Dodecyl trimethyl ammonium chloride dosage：10g；
Zinc chloride and sodium carbonate response time：2.5 hour；
Basic carbonate baking temperature：110℃；
Electrolyte HCl solution concentration：4%；
Conduction time：20 minutes；
Size of current is：10mA；
Meerschaum drying temperature and time after electrophoresis：140 DEG C, 2 hours；
Product mesh number：600 mesh.
Basic cement-slurry method：100 parts of good China G class g cements, fluid loss agent (blue moral petrochemical iy produced 2- acrylamido -2-
Dimethyl propylene sulphonic acids polymer) 5 parts, liquid-solid ratio 0.44.It is with slurry according to 10 standards of API, compare the cement without additive
Slurry, and the mortar architecture containing 0.5%, 1%, 3%, 5% additive forms the Corrosion Protection of Behavior of Hardened Cement Paste respectively.
The cement mortar for preparing is poured in the annular die of ready Φ 25.4mm × 25.4mm, 90 DEG C of sheet glass is covered
Conserve 48 hours in lower water-bath, the demoulding.Simultaneously a part of cement mortar is poured in the Fang Mo of 5mm × 5mm × 5mm in curing autoclave
In coring after maintenance 48 hours at 90 DEG C.Behavior of Hardened Cement Paste sample is put in high temperature pressure corrosion instrument together and is corroded 21 days.Test 90
℃、H2With 130 DEG C, H under the conditions of S partial pressure 1MPa stagnation pressure 3MPa2Comprcssive strength before and after corroding under the conditions of S partial pressure 1MPa stagnation pressure 3MPa
With the change of permeability, 3 and table 4 are the results are shown in Table.
Embodiment 3
Process for preparation parameter：
Meerschaum and water mixed volume ratio：1:10；
Meerschaum mixed liquor mixing time：20 minutes；
Meerschaum drying temperature：140℃；
Meerschaum drying time：3 hours；
Mesh number after meerschaum smashing：500 mesh；
Meerschaum heating-up temperature in a kettle.：220℃；
Meerschaum mixing time in a kettle.：1 hour；
Concentration of hydrochloric acid：5%；
Activation temperature：60℃；
Meerschaum calcination time：1 hour；
Meerschaum calcining heat：600℃；
Isopropanol dosage：50mL；
Agitating heating temperature：70℃；
Dodecyl trimethyl ammonium chloride dosage：10g；
Zinc chloride and sodium carbonate response time：3 hours；
Basic carbonate baking temperature：110℃；
Electrolyte HCl solution concentration：5%；
Conduction time：10 minutes；
Size of current is：10mA；
Meerschaum drying temperature and time after electrophoresis：140 DEG C, 2 hours；
Product mesh number：800 mesh.
Basic cement-slurry method：100 parts of good China G class g cements, fluid loss agent (blue moral petrochemical iy produced 2- acrylamido -2-
Dimethyl propylene sulphonic acids polymer) 5 parts, liquid-solid ratio 0.44.It is with slurry according to 10 standards of API, compare the cement without additive
Slurry, and the mortar architecture containing 0.5%, 1%, 3%, 5% additive forms the Corrosion Protection of Behavior of Hardened Cement Paste respectively.
The cement mortar for preparing is poured in the annular die of ready Φ 25.4mm × 25.4mm, 90 DEG C of sheet glass is covered
Conserve 48 hours in lower water-bath, the demoulding.Simultaneously a part of cement mortar is poured in the Fang Mo of 5mm × 5mm × 5mm in curing autoclave
In coring after maintenance 48 hours at 90 DEG C.Behavior of Hardened Cement Paste sample is put in high temperature pressure corrosion instrument together and is corroded 21 days.Test 90
℃、H2With 130 DEG C, H under the conditions of S partial pressure 1MPa stagnation pressure 3MPa2Comprcssive strength before and after corroding under the conditions of S partial pressure 1MPa stagnation pressure 3MPa
With the change of permeability, 5 and table 6 are the results are shown in Table.
1 embodiment 1 (comprcssive strength and permeability variation before and after Behavior of Hardened Cement Paste corrosion under the conditions of 90 DEG C) of table
2 embodiment 1 (comprcssive strength and permeability variation before and after Behavior of Hardened Cement Paste corrosion under the conditions of 130 DEG C) of table
3 embodiment 2 (comprcssive strength and permeability variation before and after Behavior of Hardened Cement Paste corrosion under the conditions of 90 DEG C) of table
4 embodiment 2 (comprcssive strength and permeability variation before and after Behavior of Hardened Cement Paste corrosion under the conditions of 130 DEG C) of table
5 embodiment 3 (comprcssive strength and permeability variation before and after Behavior of Hardened Cement Paste corrosion under the conditions of 90 DEG C) of table
6 embodiment 3 (comprcssive strength and permeability variation before and after Behavior of Hardened Cement Paste corrosion under the conditions of 130 DEG C) of table
By the data of table 1- tables 6, it can be seen that：Behavior of Hardened Cement Paste added with anticorrosion additive and plus anticorrosion is additional
The Behavior of Hardened Cement Paste of agent has different degrees of corrosion, but added with anti-H2The cement strength fading rate of S corrosion additives is little, fine and close
Property it is good, and when anticorrosion additive dosage be 3% when, the anti-H of Behavior of Hardened Cement Paste2The effect of S corrosion is best.
Claims (1)
1. a kind of preparation method of the oil well cement additive of anti-hydrogen sulfide corrosion, is comprised the following steps successively：
(1) during meerschaum to be added the water of 10 times of volumes, stir 20 minutes, meerschaum takes upper liquid in the suspension of upper strata, takes out
Filter and with distilled water wash after, be placed under the conditions of 140 DEG C of baking oven and be vacuum dried 3 hours, smash into 500 mesh powder, by the powder
Add in reactor with the water of 20 times of volumes, stir 1 hour at 120-220 DEG C, separate drying, then at 60 DEG C with 2-5 mass %
Hydrochloric acid carry out activation processing 1 hour after, 140 DEG C of Jing is drying to obtain Activated Sepiolite, 600 DEG C calcine 1 hour；
(2) by 100mL, ZnCl of the concentration for 2moL/L2Solution is poured in there-necked flask, while the isopropanol of 50mL is added, stirring
And 70 DEG C are heated to, by 100mL, Na of the concentration for 2moL/L2CO3Solution Deca is in there-necked flask, and adds 10g dodecanes
Base trimethylammonium bromide, cools down after reaction 2-3 hours, with distilled water wash, sucking filtration, is subsequently placed in 110 DEG C of vacuum drying ovens
It is dried, obtains final product a nanometer basic zinc carbonate；
(3) 20g nanometer basic zinc carbonates are taken and is added to 100mL, concentration is divided for 10-30 is stirred in the NaOH solution of 5-10 mass %
Clock, forms basic carbonate zinc solution；
(4) basic carbonate zinc solution is placed in electrolytic cell anode pond, then the meerschaum for processing is placed in containing 3-5 mass %
HCl solution cathode pool in, in the middle of electrolyzer use ion permeability film UNICOM, be powered, electric current is 10mA, after 10-30 minutes
Take out meerschaum solution, after filtration in 140 DEG C of baking ovens vacuum drying 2 hours, grind to form 500-800 mesh powder, as oil well
Cement additive.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010701A (en) * | 2009-09-04 | 2011-04-13 | 中国石油化工股份有限公司 | Oil-well cement additive for preventing corrosion of hydrogen sulfide as well as preparation method and application thereof |
| CN102145989A (en) * | 2010-02-08 | 2011-08-10 | 四川嘉华企业（集团）股份有限公司 | Corrosion resistant cement system and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| DE10104302A1 (en) * | 2001-01-30 | 2002-08-22 | Henkel Kgaa | Electrochemical production of nanoscale metal (mixed) oxides |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010701A (en) * | 2009-09-04 | 2011-04-13 | 中国石油化工股份有限公司 | Oil-well cement additive for preventing corrosion of hydrogen sulfide as well as preparation method and application thereof |
| CN102145989A (en) * | 2010-02-08 | 2011-08-10 | 四川嘉华企业（集团）股份有限公司 | Corrosion resistant cement system and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 纳米粘土矿物海泡石;韩炜等;《矿产保护与利用》;20031231(第6期);第19－25页 * |
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Inventor after: Cheng Xiaowei Inventor after: Wang Shengzheng Inventor after: Guo Xiaoyang Inventor after: Li Zaoyuan Inventor after: Duan Yi Inventor after: Gu Tao Inventor after: Long Dan Inventor after: Wei Tingcong Inventor before: Cheng Xiaowei Inventor before: Wang Shengzheng Inventor before: Guo Xiaoyang Inventor before: Li Zaoyuan Inventor before: Gu Tao Inventor before: Long Dan Inventor before: Wei Tingcong |
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