CN106699989A - Preparation method of temperature-adaptive retarder - Google Patents
Preparation method of temperature-adaptive retarder Download PDFInfo
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- CN106699989A CN106699989A CN201710040751.XA CN201710040751A CN106699989A CN 106699989 A CN106699989 A CN 106699989A CN 201710040751 A CN201710040751 A CN 201710040751A CN 106699989 A CN106699989 A CN 106699989A
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- temperature
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- preparation
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- trimethyl ammonium
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- 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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- 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
- C04B2103/20—Retarders
- C04B2103/22—Set retarders
Abstract
The invention relates to a preparation method of a temperature-adaptive retarder, and belongs to the technical field of cement admixtures for oil wells. The preparation method comprises the following steps: weighing sodium p-styrenesulfonate, itaconic acid, methacryloyloxyethyl trimethyl ammonium chloride and methylallyl polyethenoxy ether according to a mass ratio of (20-25):(5-10):(3-5):(1-3), dissolving the former three monomers and half of an initiator into water, dropwise adding the remaining initiator and the fourth monomer while stirring under the conditions that the temperature is 65 DEG C and nitrogen is inflated, and reacting for 3-4 hours to obtain the temperature-adaptive retarder product. The temperature-adaptive retarder is low in temperature sensitivity, has a good retarding effect at high temperature, has a small influence on the compressive strength of the top of a cement column, and has good compatibility with other admixtures.
Description
Technical field
The present invention relates to a kind of preparation method of temperature self-adaptation type retarder, belong to oil well cement additive technical field.
Background technology
As exploration and development technology is constantly goed deep into deep-well, ultradeep well, the big temperature difference low pressure of long cementing interval can be often run into easy
Leakage cementing operation, due to sealing segment length, to ensure the construction safety under hot conditions, is usually added into a large amount of retarder.But low
The lower deferred action of temperature cannot be eliminated in time, easily cause cement mortar in well section top low temperature region compression strength slower development, or even
Cannot condense, so as to influence cementing quality and Oil/gas Well safety.Retarder conventional both at home and abroad mainly has lignin sulfonic acid at present
Salt and its derivative, hydroxycarboxylic acid and its salt（Tartaric acid, citric acid etc.）, cellulose derivative, saccharide compound, organic phosphoric acid
Salt, synthetic polymer etc., but existing retarder can not be completely eliminated influence of the altitude temperature difference effect to cement strength, easily cause water
Mud is in well section top low temperature region compression strength slower development, or even cannot condense, and has a strong impact on cementing quality and subsequently applies
Work progress.
Therefore, need badly and develop a kind of high temperature resistant retarder suitable for big temperature difference oil well, to meet high temperature deep well envelope long
Gu Behavior of Hardened Cement Paste early anti pressured intension develops fast requirement under slow setting, low temperature under the big temperature difference well cementation high temperature of section.
The content of the invention
It is an object of the invention to：There is provided a kind of temperature sensitive property small, it is right at high temperature with good deferred action
Concrete column top compression strength influences the preparation side of small and good with other additive compatibilities temperature self-adaptation type retarder
Method.
What the present invention was realized in：
A kind of preparation method of temperature self-adaptation type retarder, it is characterised in that it is comprised the following steps：
1）, sodium p styrene sulfonate, itaconic acid, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride be dissolved in deionized water, and
Stir, obtain solution A；
2）, methyl allyl polyoxyethylene ether is dissolved in deionized water, obtain solution B；
3）, quantitatively weigh 2 parts of potassium peroxydisulfates, 1 part is dissolved in solution A, and another 1 part is dissolved in solution B；
4）, solution A is placed in the four-hole boiling flask equipped with agitator and logical nitrogen device, be warming up to 65 DEG C, be stirred continuously condition
Under, during solution B dropped into solution liquid using constant pressure funnel, rate of addition is that 30~40 drops are per minute, after completion of dropping
Continue to react 3~4 hours, obtain, temperature self-adaptation type retarder product.
Described sodium p styrene sulfonate, itaconic acid, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, methacrylic gather
The mass ratio of oxygen vinethene is 20~25:5~10:1~3:1~3.
The total monomer concentration is 25%~35%.（Total monomer refers specifically to sodium p styrene sulfonate, itaconic acid, metering system
Acyloxyethyl trimethyl ammonium chloride, methyl allyl polyoxyethylene ether）
The initiator concentration is the 0.3%~0.5% of monomer total amount（Initiator is potassium peroxydisulfate）.
The advantage of the invention is that：
1st, retarding performance is strong；Contain anion and cation group on the slow setting agent molecule simultaneously, anionic group is adsorbed in water
Change the part of cement particle surface positively charged, cation group is adsorbed in the electronegative part of hydrated cement particle surface, dual
Suction-operated increased the retarding performance of retarder.
2nd, the zwitterion group in slow setting agent molecule assigns its molecular structure temperature response characteristics, in low temperature environment, point
Subchain is curled, and adsorption group is in bound state, reduces the absorption to cement granules, and retarding performance weakens.And in hot conditions
Lower, strand is unfolded, and exposes more adsorption groups, retarding performance enhancing.Also, this process is reversible, so that
Big temperature difference well cementation environment is suitable for, the problem of the low heat cement post extra retarded set that conventional retarder causes is overcome.
3rd, temperature sensitive monomer TPEG is contained in slow setting agent molecule, under low temperature, side base ether chain long is with hydrone in hydrogen bond mode
Bonding so that molecule side base is unfolded, the steric hindrance effect of long-chain, hinders absorption of the zwitterion in cement particle surface,
So as to weaken the deferred action under low temperature.Under high temperature, temperature effect causes that molecular thermalmotion aggravates, the hydrogen of ehter bond and hydrone
Key declines, so that molecule side base collapse, steric hindrance effect reduction so that zwitterion is more easy to be adsorbed in cement granules table
Face, retardation capability enhancing, so as to realize the big temperature characteristic of retarder.
Specific embodiment
Embodiment 1：
20g sodium p styrene sulfonates, 5g itaconic acids, 3g MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides, 0.05g mistakes are weighed successively
Potassium sulfate is dissolved in 50ml deionized waters, is designated as A liquid；1g methyl allyl polyoxyethylene ethers, 0.05g potassium peroxydisulfates is weighed to be dissolved in
In 30ml deionized waters, B liquid is designated as；A liquid is placed in the four-hole boiling flask equipped with agitator and logical nitrogen device, 65 DEG C are warming up to,
Under constant agitation, in B drops being added into A liquid using constant pressure funnel, rate of addition is that 30~40 drops are per minute, drop
To add continue after finishing and react 3 hours, you can obtain temperature self-adaptation type retarder sample, its solid content is 26.4%, is designated as sample
1。
Embodiment 2：
22g sodium p styrene sulfonates, 8g itaconic acids, 2g MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides, 0.06g mistakes are weighed successively
Potassium sulfate is dissolved in 50ml deionized waters, is designated as A liquid；2g methyl allyl polyoxyethylene ethers, 0.06g potassium peroxydisulfates is weighed to be dissolved in
In 30ml deionized waters, B liquid is designated as；A liquid is placed in the four-hole boiling flask equipped with agitator and logical nitrogen device, 65 DEG C are warming up to,
Under constant agitation, in B drops being added into A liquid using constant pressure funnel, rate of addition is that 30~40 drops are per minute, drop
To add continue after finishing and react 3 hours, you can obtain temperature self-adaptation type retarder sample, its solid content is 28.9%, is designated as sample
2。
Embodiment 3
25g sodium p styrene sulfonates, 10g itaconic acids, 3g MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides, 0.05g are weighed successively
Potassium peroxydisulfate is dissolved in 60ml deionized waters, is designated as A liquid；Weigh 3g methyl allyl polyoxyethylene ethers, 0.05g potassium peroxydisulfates molten
In 30ml deionized waters, B liquid is designated as；A liquid is placed in the four-hole boiling flask equipped with agitator and logical nitrogen device, 65 are warming up to
DEG C, under constant agitation, during B drops are added into A liquid using constant pressure funnel, rate of addition is 30~40 every point of drops
Clock, continues to react 3 hours after completion of dropping, you can obtain temperature self-adaptation type retarder sample, and its solid content is 30.3%, note
It is sample 3.
Embodiment 4
20g sodium p styrene sulfonates, 5g itaconic acids, 1g MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides, 0.05g mistakes are weighed successively
Potassium sulfate is dissolved in 50ml deionized waters, is designated as A liquid；1g methyl allyl polyoxyethylene ethers, 0.05g potassium peroxydisulfates is weighed to be dissolved in
In 30ml deionized waters, B liquid is designated as；A liquid is placed in the four-hole boiling flask equipped with agitator and logical nitrogen device, 65 DEG C are warming up to,
Under constant agitation, in B drops being added into A liquid using constant pressure funnel, rate of addition is that 30~40 drops are per minute, drop
To add continue after finishing and react 3 hours, you can obtain temperature self-adaptation type retarder sample, its solid content is 25.2%, is designated as sample
4。
For temperature self-adaptation type retarder properties of product prepared by the detection present invention；According to SY/T 5504.1-2013《Oil
Well cement additive evaluation method part 1：Retarder》Thickening time evaluation, foundation are carried out to the sample 1~4 in example
GB19139-2003 is investigated after compression strength, i.e. cement mortar are with slurry at the top of Behavior of Hardened Cement Paste using high temperature dynamic prefabrication system and is loaded high temperature
High pressure multiviscosity meter, constant temperature zone is entered by thickening testing program, and top static temperature is down to after constant temperature 60min, splits out multiviscosity meter slurry
Cup, goes oil processing, and then molding is put into curing temperature and conserves to age.With simulated field execution conditions as far as possible, obtain most true
Real cement slurry property.The investigation of the compression strength of Behavior of Hardened Cement Paste under hot conditions, cement mortar correspondence in HTHP maintenance axe
High-temperature temperature under conserved, after reaching curing age, test Behavior of Hardened Cement Paste compression strength.
Cement mortar basic recipe is：Good+1% fluid loss agent of silica sand of China G class g cements+35%+retarder, water-solid ratio is 0.44.
By 1~table of table 4 as can be seen that the retarder sample in example influences not on Behavior of Hardened Cement Paste compression strength under hot conditions
Greatly, the strength development and to top Behavior of Hardened Cement Paste does not have harmful effect, and in 60 DEG C, 90 DEG C, top cement strength also can
Very fast development, reaches more than 14MPa, meets construction requirement, can also overcome " big altitude temperature difference effect " to high-temperature cement slurry system
The problem of " extra retarded set " that brings.
Claims (3)
1. a kind of preparation method of temperature self-adaptation type retarder, it is characterised in that it is comprised the following steps：
1）, sodium p styrene sulfonate, itaconic acid, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride be dissolved in deionized water, and
Stir, obtain solution A；
2）, methyl allyl polyoxyethylene ether is dissolved in deionized water, obtain solution B；
3）, quantitatively weigh 2 parts of potassium peroxydisulfates, 1 part is dissolved in solution A, and another 1 part is dissolved in solution B；
4）, solution A is placed in the four-hole boiling flask equipped with agitator and logical nitrogen device, be warming up to 65 DEG C, be stirred continuously condition
Under, during solution B dropped into solution liquid using constant pressure funnel, rate of addition is that 30~40 drops are per minute, after completion of dropping
Continue to react 3~4 hours, obtain, temperature self-adaptation type retarder product；
Described sodium p styrene sulfonate, itaconic acid, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, methacrylic polyoxy second
The mass ratio of alkene ether is 20~25:5~10:1~3:1~3.
2. the preparation method of a kind of temperature self-adaptation type retarder according to claim 1, it is characterised in that described to benzene
Vinyl sulfonic acid sodium, itaconic acid, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, the monomer concentration of methyl allyl polyoxyethylene ether
It is 25%~35%.
3. a kind of preparation method of temperature self-adaptation type retarder according to claim 1, it is characterised in that the over cure
Sour potassium concn is the 0.3%~0.5% of monomer total amount.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710040751.XA CN106699989A (en) | 2017-01-20 | 2017-01-20 | Preparation method of temperature-adaptive retarder |
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| CN201710040751.XA CN106699989A (en) | 2017-01-20 | 2017-01-20 | Preparation method of temperature-adaptive retarder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109824823A (en) * | 2019-01-28 | 2019-05-31 | 中国石油大学(华东) | Temperature self-adaptation type high temperature retarder suitable for oil gas well cementing operation and preparation method thereof and cementing slurry |
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| CN101570412A (en) * | 2009-05-31 | 2009-11-04 | 上海三瑞化学有限公司 | Polycarboxylic acid gypsum water reducing agent and preparation method thereof |
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Cited By (2)
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| CN109824823A (en) * | 2019-01-28 | 2019-05-31 | 中国石油大学(华东) | Temperature self-adaptation type high temperature retarder suitable for oil gas well cementing operation and preparation method thereof and cementing slurry |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170524 |
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| RJ01 | Rejection of invention patent application after publication |