CN108084361A - A kind of oil-well cement retarder and preparation method thereof - Google Patents
A kind of oil-well cement retarder and preparation method thereof Download PDFInfo
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- CN108084361A CN108084361A CN201711450299.0A CN201711450299A CN108084361A CN 108084361 A CN108084361 A CN 108084361A CN 201711450299 A CN201711450299 A CN 201711450299A CN 108084361 A CN108084361 A CN 108084361A
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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
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- 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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/165—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
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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
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention belongs to cement additive technical fields, disclose a kind of oil-well cement retarder and preparation method thereof, raw material includes：80 120 parts of maleic anhydride, 160 180 parts of p-aminobenzene sulfonic acid, 300 2600 parts of allyl alcohol polyoxyethylene ether, 60 80 parts of acrylamide, 70 90 parts of sodium hydroxide, 38 parts of initiator, 25 parts of chain-transferring agent.Product of the present invention is conducive to disperse at low temperature, and retarding effect is good under high temperature, can effectively extend the thickening time of cement mortar, it is ensured that the safety of cementing operation.
Description
Technical field
The invention belongs to cement additive technical fields, and in particular to a kind of oil-well cement retarder and its preparation side
Method.
Background technology
When oil-well cement is oil, natural gas exploration and exploitation, oil, the cement special kind of gas well cementing processing.In oil
In gas well cementing job, cement mortar is pumped into well by pumping, through slurry is replaced to replace cement mortar between pipe sleeve and wellbore
Annular space, achieve the purpose that packing oil, gas and water layer protection production layer and support protection sleeve pipe, cement sent to required
There should be good pumpability before position.With the progress of hydration reaction in cement, as soon as when cohesive force reaches timing, cement
It can lose flowability and construction operation can not be carried out.The thickening time of cement mortar be control well cementing operation, ensure construction safety and
The key parameter of cementing quality.Patent CN1513797A provides a kind of oil well cement retarder, containing gluconate, has
The reaction product of machine phosphonic acid and its salt and organic acid, the retarder heat resistance is poor, and temperature sensitive property is big.CN101368091A
A kind of oil-well cement retarder is disclosed wherein containing carboxylic acid group multiple copolymer, but must be with organic phospho acid and its esters
It is used in combination.
The content of the invention
The present invention is in view of the above-mentioned problems, provide a kind of heat resistance good retarder, in order to achieve the above objectives, the present invention adopts
With following technical scheme, a kind of oil-well cement retarder, by weight, raw material includes：It is 80-120 parts of maleic anhydride, right
160-180 parts of aminobenzenesulfonic acid, 300-2600 parts of allyl alcohol polyoxyethylene ether, 60-80 parts of acrylamide, sodium hydroxide 70-
90 parts, 3-8 parts of initiator, 2-5 parts of chain-transferring agent.
Preferably, the oil well cement retarder, including following chemical formula compound represented：
Wherein, R1For H or CH3, m is the integer more than or equal to 1, and n is the integer of 8-30.
The preparation method of above-mentioned oil well cement retarder, comprises the following steps：
(1) water and p-aminobenzene sulfonic acid are put into a kettle, is warming up to 50-65 DEG C, be added dropwise 30% sodium hydroxide it is molten
Liquid, and put into maleic anhydride in batches, solution keeps alkalescence when so that the maleic anhydride is not added.
(2) above-mentioned solution is warming up to 70-75 DEG C, it is molten that initiator solution, chain-transferring agent solution, acrylamide monomer is added dropwise
Liquid, allyl alcohol polyethenoxy ether monomer solution (or isobutene alcohol polyoxyethylene ether monomer solution) control initiator solution and chain
Transfer agent solution is later than monomer solution 5min and drips off.Near room temperature is to get the oil-well cement retarder after keeping the temperature 1h.
Preferably, the molecular weight of the allyl alcohol polyoxyethylene ether is between 400-2200.
Preferably, solution ph is between 8-10 when maleic anhydride does not add in step (1).
Preferably, in step (1) after last batch of maleic anhydride input, solution ph is between 6-8.
Initiator in the step (2) is redox system initiator, and wherein oxidant is ammonium ceric nitrate, dioxygen
One kind in water, sodium peroxydisulfate, potassium peroxydisulfate, ammonium persulfate, reducing agent is ascorbic acid, in sodium hypophosphite, ferrous sulfate
One kind.
Preferably, the initiator in the step (2) is made of ammonium ceric nitrate and ferrous sulfate.
The chain-transferring agent is thioacetic acid, one kind in mercaptopropionic acid, 2- acrylamido -2- methyl propane sulfonic acid sodium.
The functional groups such as carboxyl, sulfonic group, the amide groups of oil well retarder in cold stage, molecule can inhale in the present invention
Cement particle surface is attached to, forms adsorption layer, polyoxyethylene groups (- CH therein2CH2O-) there is space steric effect, can prevent
Cement particle agglomerates, and plays the role of scattered and slows down hydrated cementitious；With the rise of temperature, macromolecular progressively hydrolyzes, and is formed
It is multiple to contain carboxyl (- COO-), sulfonic group (- SO3-) etc. groups small molecule, amide group also hydrolyzing to form at high temperature
Carboxyl (- COO-), carboxyl (- COO-), sulfonic group (- SO in small molecule3-) can be combined with calcium, form unstable complexing
On the one hand object forms rich calcium protective layer, prevent contact of the water with cement particle, on the other hand the Ca in controllable liquid phase2+Ion
Concentration, generate deferred action；A large amount of sulfonic introducings make system have higher sulfonation degree, it is made both to be resistant to higher temperature
Degree, and with water-soluble and salt tolerance well.
The beneficial effects of the present invention are：Product of the present invention is conducive to disperse at low temperature, and amide group hydrolyzes under high temperature,
Retarding effect is good, can effectively extend the thickening time of cement mortar, it is ensured that the safety of cementing operation, and do not have to strength of cement development
Have an impact.
Specific embodiment
With reference to specific embodiment, the specific embodiment of the present invention is further described.Following embodiment is only used
In clearly illustrating technical scheme, the scope of the present invention is not limited to the embodiment of the present invention.
Embodiment 1
A kind of oil-well cement retarder, raw material include：80 parts of maleic anhydride, 160 parts of p-aminobenzene sulfonic acid, pi-allyl
800 parts of alcohol polyoxyethylene ether, 80 parts of acrylamide, 70 parts of sodium hydroxide, 5 parts of initiator, 3 parts of chain-transferring agent, the number are
Parts by weight.
The preparation method of above-mentioned oil well cement retarder, comprises the following steps：
(1) water and p-aminobenzene sulfonic acid are put into a kettle, are warming up to 50 DEG C, 30% sodium hydroxide solution is added dropwise,
And maleic anhydride is put into batches, solution keeps alkalescence when so that the maleic anhydride is not added.
(2) above-mentioned solution is warming up to 75 DEG C, initiator solution, chain-transferring agent solution, allyl alcohol polyethenoxy ether is added dropwise
Monomer solution and acrylamide monomer solution control initiator solution and chain-transferring agent solution to be later than monomer solution 5min and drip off.
Near room temperature is to get the oil-well cement retarder after keeping the temperature 1h.
The molecular weight of the allyl alcohol polyethenoxy ether is 400.
Initiator in the step (2) is redox system initiator, and wherein oxidant is hydrogen peroxide, and reducing agent is
Ascorbic acid.
The chain-transferring agent is thioacetic acid.
Embodiment 2
A kind of oil-well cement retarder, raw material include：120 parts of maleic anhydride, 180 parts of p-aminobenzene sulfonic acid, allyl
2400 parts of base alcohol polyoxyethylene ether, 60 parts of acrylamide, 90 parts of sodium hydroxide, 3 parts of initiator, 5 parts of chain-transferring agent, the number
For parts by weight.
The preparation method of above-mentioned oil well cement retarder, comprises the following steps：
(1) water and p-aminobenzene sulfonic acid are put into a kettle, are warming up to 65 DEG C, 30% sodium hydroxide solution is added dropwise,
And maleic anhydride is put into batches, solution keeps alkalescence when so that the maleic anhydride is not added.
(2) above-mentioned solution is warming up to 70-75 DEG C, initiator solution, chain-transferring agent solution, isobutene alcohol polyoxy second is added dropwise
Alkene ether monomer solution and acrylamide monomer solution control initiator solution and chain-transferring agent solution to be later than monomer solution 5min drops
It is complete.Near room temperature is to get the oil-well cement retarder after keeping the temperature 1h.
The molecular weight of the isobutene alcohol polyoxyethylene ether is 2200.
Initiator in the step (2) is redox system initiator, and wherein oxidant is sodium peroxydisulfate reducing agent
For sodium hypophosphite.
The chain-transferring agent is mercaptopropionic acid.
Embodiment 3
A kind of oil-well cement retarder, raw material include：100 parts of maleic anhydride, 170 parts of p-aminobenzene sulfonic acid, allyl
1200 parts of base alcohol polyoxyethylene ether, 70 parts of acrylamide, 80 parts of sodium hydroxide, 6 parts of initiator, 4 parts of chain-transferring agent, the number
For parts by weight.
The preparation method of above-mentioned oil well cement retarder, comprises the following steps：
(1) water and p-aminobenzene sulfonic acid are put into a kettle, are warming up to 55 DEG C, 30% sodium hydroxide solution is added dropwise,
And maleic anhydride is put into batches, solution keeps alkalescence when so that the maleic anhydride is not added.
(2) above-mentioned solution is warming up to 72 DEG C, initiator solution, chain-transferring agent solution, allyl alcohol polyethenoxy ether is added dropwise
Monomer solution and acrylamide monomer solution control initiator solution and chain-transferring agent solution to be later than monomer solution 5min and drip off.
Near room temperature is to get the oil-well cement retarder after keeping the temperature 1h.
The molecular weight of the allyl alcohol polyethenoxy ether is 1200.
Initiator in the step (2) is made of ammonium ceric nitrate and ferrous sulfate.
The chain-transferring agent is 2- acrylamido -2- methyl propane sulfonic acid sodium.
Embodiment 4
A kind of oil-well cement retarder, raw material include：110 parts of maleic anhydride, 162 parts of p-aminobenzene sulfonic acid, allyl
1800 parts of base alcohol polyoxyethylene ether, 72 parts of acrylamide, 78 parts of sodium hydroxide, 5 parts of initiator, 3 parts of chain-transferring agent, the number
For parts by weight.
Embodiment 5
A kind of oil-well cement retarder, including following chemical formula compound represented：
Wherein, R1For H or CH3, m is the integer more than or equal to 1, and n is the integer of 8-30.
Comparative example 1
A kind of oil-well cement retarder, raw material include：100 parts of maleic anhydride, 170 parts of p-aminobenzene sulfonic acid, propylene
70 parts of amide, 80 parts of sodium hydroxide, 6 parts of initiator, 4 parts of chain-transferring agent, the number are parts by weight.
The preparation method of above-mentioned oil well cement retarder, comprises the following steps：
(1) water and p-aminobenzene sulfonic acid are put into a kettle, are warming up to 55 DEG C, 30% sodium hydroxide solution is added dropwise,
And maleic anhydride is put into batches, solution keeps alkalescence when so that the maleic anhydride is not added.
(2) above-mentioned solution is warming up to 72 DEG C, it is molten that initiator solution, chain-transferring agent solution and acrylamide monomer is added dropwise
Liquid controls initiator solution and chain-transferring agent solution to be later than monomer solution 5min and drip off.Near room temperature is to get described after keeping the temperature 1h
Oil-well cement retarder.
Initiator in the step (2) is made of ammonium ceric nitrate and ferrous sulfate.
The chain-transferring agent is 2- acrylamido -2- methyl propane sulfonic acid sodium.
Comparative example 2
A kind of oil-well cement retarder, raw material include：100 parts of maleic anhydride, 170 parts of p-aminobenzene sulfonic acid, allyl
1200 parts of base alcohol polyoxyethylene ether, 70 parts of acrylamide, 80 parts of sodium hydroxide, 6 parts of initiator, 4 parts of chain-transferring agent, the number
For parts by weight.
The preparation method of above-mentioned oil well cement retarder, comprises the following steps：
(1) water and p-aminobenzene sulfonic acid are put into a kettle, is warming up to 55 DEG C, add in sodium hydroxide and maleic anhydride,
It is sufficiently stirred.
(2) above-mentioned solution is warming up to 72 DEG C, initiator solution, chain-transferring agent solution, allyl alcohol polyethenoxy ether is added dropwise
Monomer solution and acrylamide monomer solution control initiator solution and chain-transferring agent solution to be later than monomer solution 5min and drip off.
Near room temperature is to get the oil-well cement retarder after keeping the temperature 1h.
The molecular weight of the allyl alcohol polyethenoxy ether is 1200.
Initiator in the step (2) is made of ammonium ceric nitrate and ferrous sulfate.
The chain-transferring agent is 2- acrylamido -2- methyl propane sulfonic acid sodium.
Performance test
With retarder G will be added in by the 1.5% of cement quality to the oil-well cement obtained by embodiment 1-5 and comparative example 1-2
It is tested for the property in class g cement, the result is shown in the following table 1.
1 the performance test results of table
It should be noted that above-described embodiment is only the preferred embodiment of the present invention, it is not intended to limit the present invention, according to
The modification that is carried out according to the technical solution recorded in embodiment and equivalent substitution, improvement etc. are carried out to which part technical characteristic,
It should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of oil-well cement retarder, which is characterized in that by weight, raw material includes：80-120 parts of maleic anhydride,
160-180 parts of p-aminobenzene sulfonic acid, allyl alcohol polyoxyethylene ether/or 300-2600 parts of isobutene alcohol polyoxyethylene ether, propylene
60-80 parts of amide, 70-90 parts of sodium hydroxide, 3-8 parts of initiator, 2-5 parts of chain-transferring agent.
2. oil well cement retarder according to claim 1, which is characterized in that the oil-well cement is wrapped in retarder
Include following chemical formula compound represented：
Wherein, R1For H or CH3, m is the integer more than or equal to 1, and n is the integer of 8-30.
3. a kind of preparation method of claim 1-2 any one of them oil-well cement retarder, which is characterized in that including with
Lower step：
(1) water and p-aminobenzene sulfonic acid are put into a kettle, are warming up to 50-65 DEG C, 30% sodium hydroxide solution is added dropwise, and
Maleic anhydride is put into batches, and solution keeps alkalescence when so that the maleic anhydride is not added；
(2) above-mentioned solution is warming up to 70-75 DEG C, be added dropwise initiator solution, chain-transferring agent solution, acrylamide monomer solution,
Allyl alcohol polyethenoxy ether monomer solution/or isobutene alcohol polyoxyethylene ether monomer solution control initiator solution and chain tra nsfer
Agent solution is later than monomer solution 5min and drips off, and near room temperature is to get the oil-well cement retarder after keeping the temperature 1h.
4. the preparation method of oil-well cement retarder according to claim 3, which is characterized in that in the step (1)
Solution ph is between 8-10 when maleic anhydride does not add.
5. the preparation method of oil-well cement retarder according to claim 3, which is characterized in that in the step (1)
After last batch of maleic anhydride input, solution ph is between 6-8.
6. the preparation method of oil-well cement retarder according to claim 3, which is characterized in that the initiator is oxygen
Change reduction system initiator, wherein oxidant is one in ammonium ceric nitrate, hydrogen peroxide, sodium peroxydisulfate, potassium peroxydisulfate, ammonium persulfate
Kind, reducing agent is ascorbic acid, one kind in sodium hypophosphite, ferrous sulfate.
7. the preparation method of oil-well cement retarder according to claim 6, which is characterized in that the initiator is by nitre
Sour cerium ammonium and ferrous sulfate composition.
8. the preparation method of oil-well cement retarder according to claim 3, which is characterized in that the chain tra nsfer
Agent is thioacetic acid, one kind in mercaptopropionic acid, 2- acrylamido -2- methyl propane sulfonic acid sodium.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114057958A (en) * | 2021-12-29 | 2022-02-18 | 成都欧美克石油科技股份有限公司 | Weak-dispersion early-strength retarder for oil well cement and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114057958A (en) * | 2021-12-29 | 2022-02-18 | 成都欧美克石油科技股份有限公司 | Weak-dispersion early-strength retarder for oil well cement and preparation method thereof |
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Application publication date: 20180529 |