CN105601853B - A kind of oil-well cement drag reducer and preparation method thereof - Google Patents
A kind of oil-well cement drag reducer and preparation method thereof Download PDFInfo
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- CN105601853B CN105601853B CN201510718976.7A CN201510718976A CN105601853B CN 105601853 B CN105601853 B CN 105601853B CN 201510718976 A CN201510718976 A CN 201510718976A CN 105601853 B CN105601853 B CN 105601853B
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Abstract
The invention discloses a kind of oil-well cement drag reducer and preparation method thereof, oil-well cement is made up of with drag reducer phenol, formaldehyde, acetone and sodium sulfite；Preparation method comprises the following steps：(1) sodium sulfite is dissolved in distilled water；(2) phenol is dissolved in sodium sulfite solution；(3) pH of the solution obtained in step (2) is adjusted to 11-12；(4) formaldehyde is added dropwise for the first time, is added dropwise to material color and is changed into faint yellow；(5) acetone is added in the material that step (4) obtains, after addition, material color is changed into crocus from faint yellow, then is changed into reddish brown from crocus；(6) second formaldehyde is added dropwise, obtains red solid powder by reaction product is spray-dried.The well cement tolerance blocking that the present invention obtains, compared with prior art, drag-reduction effect is notable, and high temperature resistant, and cement mortar flow pattern is preferable, good with other oil well cement additive compatibilities.
Description
Technical field
The present invention relates to oilfield chemistry additive.More particularly, to a kind of oil-well cement drag reducer and its preparation side
Method.
Background technology
In recent years, with the development of reinforcing oil well technology, requirement to cement slurry property used in well cementation also more and more higher.Mesh
Preceding use oil well cement additive is to improve slurry flowing performance-changing, improves the most effectual way of cementing quality.Oil-well cement subtracts
Resist is highly important one kind in oil well cement additive, and the wider well cement tolerance blocking of application mainly has beta-naphthalenesulfonic-acid first
Aldehyde condensate and sulfonated acetone formaldehyde condensation products.Beta-naphthalenesulfonic-acid formaldehyde condensation compound be using naphthalene as raw material, by sulfonation, condensation, in
With etc. step synthesize to obtain, there is good dispersibility, shortcoming is the sodium sulfate byproduct generated containing neutralisation of sulphuric acid, and
Sodium sulphate can corrode Behavior of Hardened Cement Paste again, cause the decline of cementing quality；Another kind of sulfonated acetone formaldehyde condensation products are current domestic cities
More product is used on field, the composition principle of such a drag reducer is, as obtained from after acetone sulfonation with the polycondensation of formaldehyde,
Dispersion effect is good, but its temperature in use has certain limitations to it, and high temperature drag-reduction effect is not notable.
The content of the invention
It is an object of the present invention to provide a kind of high oil-well cement drag reducer of temperature in use, and provide this oil
The preparation method of well cement drag reducer.
To reach above-mentioned purpose, the present invention uses following technical proposals：
A kind of oil-well cement drag reducer, is made up of phenol, formaldehyde, acetone and sodium sulfite.
Above-mentioned oil-well cement drag reducer, phenol, formaldehyde, the weight ratio of acetone and sodium sulfite are 1-2:16-20:5-8:
6-10.Preferred value point is 1：17.5：6.6：8, although above raw material can be reacted in the number range provided,
In the presence of a kind of " wooden pail effect ", i.e., various raw material must just can guarantee that the abundant progress of reaction in suitable scope.
A kind of preparation method of oil-well cement drag reducer, comprises the following steps：
(1) sodium sulfite is dissolved in distilled water, obtains sodium sulfite solution；
(2) phenol is dissolved in sodium sulfite solution；
(3) pH of the solution obtained in step (2) is adjusted to 11-12；
(4) formaldehyde is added dropwise for the first time：Formaldehyde is added dropwise in the solution obtained to step (3), stirs, rear material face is added dropwise
Discoloration is faint yellow；
(5) acetone is added in the material that step (4) obtains, stirring, after addition, material color is changed into from faint yellow
Crocus, then reddish brown is changed into from crocus；
(6) second of dropwise addition formaldehyde：Residual formaldehyde is added drop-wise in the material that step (5) obtains and reacted, is stirred, i.e.,
Reaction product, obtain red solid powder by reaction product is spray-dried.
The preparation method of above-mentioned oil-well cement drag reducer, in step (4)：The amount that formaldehyde is added dropwise is formaldehyde gross weight
29%-31%, preferable numerical point are 30%；In step (6)：The amount that formaldehyde is added dropwise is the 69%-71% of formaldehyde gross weight,
Preferable numerical point is 70%.
The preparation method of above-mentioned oil-well cement drag reducer, in step (5)：Controlling reaction temperature at 45-52 DEG C because
Acetone highly volatile, when temperature is too high, reaction is insufficient, and the product dispersion effect finally given is bad, and constant temperature keeps 40min.
The preparation method of above-mentioned oil-well cement drag reducer, in step (6)：Controlling reaction temperature 95-100 DEG C with,
Temperature is too high strict to production equipment requirement, and production technology is difficult to control, and the too low reaction product degree of polymerization of temperature is low, drag-reduction effect
Not significantly, constant temperature keeps 3h.
The preparation method of above-mentioned oil-well cement drag reducer, in step (1)：The quality of distilled water is sodium sulfite quality
3-6 times, distilled water is too little or too much can all influence synthesis drag reducer dispersion effect, become the rheological property of cement mortar
Difference.
The preparation method of above-mentioned oil-well cement drag reducer, in step (3)：With the pH of NaOH regulation solution for 11-
12, reaction must be carried out in the basic conditions, when pH not in this range when, be unfavorable for the progress of synthetic reaction.
The preparation method of above-mentioned oil-well cement drag reducer, dropwise addition duration when being added dropwise formaldehyde for the first time for 15-
30min, the time that control formaldehyde is added dropwise is actually the rate of addition for controlling formaldehyde, is furtherly to control the temperature of reaction
Degree；It is actually control first that dropwise addition duration during second of dropwise addition formaldehyde controls the time of formaldehyde dropwise addition for 15-30min
The rate of addition of aldehyde, it is furtherly to control the temperature of reaction.
The preparation method of above-mentioned oil-well cement drag reducer, in step (4), (5) and (6)：Use magnetic stirring apparatus, magnetic
The speed of power stirring is 800r/min.
Beneficial effects of the present invention are as follows：
1st, the drag-reduction effect of oil-well cement drag reducer provided by the invention is good, particularly shows in high temperature section drag-reduction effect
Write, temperature in use adds this product up to 200 DEG C in oil well cement paste, and cement mortar flow pattern is more superior than other drag reducers.
2nd, the synthesis technique of oil-well cement drag reducer of the invention is simple, and reaction condition is gentle, and the reaction time is short, simultaneously
Preparation method is low for equipment requirements.
3rd, when oil-well cement drag reducer dosage provided by the invention is 0.3-0.5wt% (BWOC), you can to reach very
Good dispersion effect.
4th, oil-well cement drag reducer provided by the invention and other cement additive compatibilities are good, are obtained with of the invention
To the oil-well cement of drag reducer (dosage is the 0.5wt% of cement dosage) and our company with fluid loss agent G310, (dosage is water
The 5wt% of mud amount) and oil-well cement with retarder GH-9 (time solidified as needed is added) compatible use, its API
Dehydration can be controlled in 30ml or so, and cement mortar is good without sedimentation, fluidity.Oil-well cement drag reducer of the present invention, oil
Well cement is added in oil well cement paste together with fluid loss agent G310, oil-well cement with retarder GH-9：API dehydrations can be controlled
System is in 30ml or so, and cement mortar is good without sedimentation, fluidity；Illustrate that drag reducer of the present invention discloses out with our company in the market
The product oil-well cement fluid loss agent G310 (dosage is the 5wt% of cement amount) and oil-well cement retarder GH-9 compatibilities sold
It is functional, and in the market other drag reducers cannot realize so excellent compatibility.
5th, the present invention is in the prior art on the basis of sulfonated acetone formaldehyde condensation products, introduces benzene in the polymer
Ring, drag reducer temperature in use produced by the present invention is improved, expands the scope of application of sulfonated acetone formaldehyde condensation products, and
And the cement mortar flow pattern that with the addition of drag reducer of the present invention is fine, guarantee is provided for well cementation safe construction.Solves Vehicles Collected from Market master
The drag reducer high temperature section led in use, dispersion effect (quality of dispersion effect typically represents that n values are that fluidity refers to n values and K values
Number, reflection be cement mortar flow pattern quality, n values are the bigger the better；K values are consistency coefficients, reflection be cement mortar sticky journey
Degree, therefore K values are the smaller the better) bad, the problem of cement mortar flow pattern is unstable.
Embodiment
In order to illustrate more clearly of the present invention, with reference to preferred embodiment, the present invention is described further.Ability
Field technique personnel should be appreciated that following specifically described content is illustrative and be not restrictive, and this should not be limited with this
The protection domain of invention.
Embodiment 1
70g sodium sulfites are completely dissolved in 300g distilled water, 12g phenol is weighed and is completely dissolved in sodium sulfite solution,
Appropriate NaOH is taken to adjust pH value to 11.
Weigh 48g formaldehyde to be slowly dropped in above-mentioned material, and be stirred continuously【Use magnetic stirring apparatus, magnetic agitation speed
Degree is 800r/min】, rear material color is added dropwise and is changed into faint yellow.
Weigh 60g acetone to be slowly dropped in above-mentioned material, using magnetic stirring apparatus, magnetic stirring speed is 800r/
Min, after being added dropwise, material color is changed into crocus from faint yellow, then is changed into reddish brown, controlling reaction temperature from crocus
Below 52 DEG C, constant temperature stirring keeps 40min.
112g formalins are weighed, are slowly dropped in above-mentioned material, using magnetic stirring apparatus, magnetic stirring speed is
Be added dropwise in 800r/min, 20min, after being added dropwise, temperature of charge is upgraded to 92 DEG C, insulated and stirred reaction 3h both it is of the invention
Product.
Red solid powder, as oil-well cement drag reducer are obtained by above reaction product is spray-dried.
Embodiment 2
(1) 90g sodium sulfites are completely dissolved in 400g distilled water, weigh 15g phenol and be completely dissolved in sodium sulfite solution
In, take appropriate NaOH to adjust pH value to 12.
(2) weigh 54g formaldehyde to be slowly dropped in above-mentioned material, and be stirred continuously【Use magnetic stirring apparatus, magnetic agitation
Speed is 800r/min】, rear material color is added dropwise and is changed into faint yellow.
(3) weigh 70g acetone to be slowly dropped in above-mentioned material, using magnetic stirring apparatus, magnetic stirring speed is 800r/
Min, after being added dropwise, material color is changed into crocus from faint yellow, then is changed into reddish brown, controlling reaction temperature from crocus
Below 52 DEG C, constant temperature stirring keeps 40min.
(4) 126g formalins are weighed, are slowly dropped in above-mentioned material, use magnetic stirring apparatus, magnetic stirring speed
It is 800r/min, is added dropwise in 25min, after being added dropwise, temperature of charge is upgraded to 95 DEG C, and insulated and stirred reacts 3h both get Ben Fa
Bright product.
(5) red solid powder, as oil-well cement drag reducer are obtained by above reaction product is spray-dried.
The cement slurry property experimental result such as following table of oil-well cement drag reducer obtained by two embodiments：
The cement slurry property such as following table of the oil-well cement drag reducer of embodiment 1
| Sample dosage, wt% | Temperature, DEG C | N values | K values | Thickening time, min | 24h intensity, MPa |
| 0 | 85 | 0.431 | 1.563 | 76 | 16.3 |
| 0.3 | 85 | 0.716 | 0.129 | 80 | 14.9 |
| 0.5 | 85 | 0.845 | 0.050 | 83 | 15.6 |
The cement slurry property such as following table of the oil-well cement drag reducer of embodiment 2
| Sample dosage, wt% | Temperature, DEG C | N values | K values | Thickening time, min | 24h intensity, MPa |
| 0 | 85 | 0.457 | 1.270 | 78 | 15.8 |
| 0.3 | 85 | 0.770 | 0.088 | 81 | 15.0 |
| 0.5 | 85 | 0.858 | 0.044 | 86 | 16.2 |
Note：N values-liquidity index, K values-consistency coefficient, sample dosage are the addition of oil-well cement drag reducer.
Cement used is oil well G class g cements, and cement mortar, the ratio of mud 0.44 are prepared by API standard.
Comparative example
Comparative example 1
The present embodiment is the comparative example of embodiment 1, and specific production technology difference is as follows：Phenol is not added, remaining
Material dosage and processing step are identical.
(cement used is oil well G class g cements to the cement slurry property of test the present embodiment drag reducer, and water is prepared by API standard
Mud, the ratio of mud 0.44), experimental result such as following table：
| Sample dosage, wt% | Temperature, DEG C | N values | K values | Thickening time, min | 24h intensity, MPa |
| 0 | 85 | 0.431 | 1.563 | 76 | 16.3 |
| 0.3 | 85 | 0.521 | 0.986 | 82 | 14.5 |
| 0.5 | 85 | 0.597 | 0.863 | 85 | 15.1 |
Comparative example 2
The present embodiment is the comparative example of embodiment 2, and specific production technology difference is as follows：All formaldehyde and acetone are same
When add, remaining material dosage and processing step are identical.
(cement used is oil well G class g cements to the cement slurry property of test the present embodiment drag reducer, and water is prepared by API standard
Mud, the ratio of mud 0.44), experimental result such as following table：
| Sample dosage, wt% | Temperature, DEG C | N values | K values | Thickening time, min | 24h intensity, MPa |
| 0 | 85 | 0.457 | 1.270 | 78 | 15.8 |
| 0.3 | 85 | 0.568 | 0.675 | 81 | 14.8 |
| 0.5 | 85 | 0.603 | 0.384 | 85 | 16.0 |
Comparative example 3
The present embodiment is the comparative example of embodiment 2, and specific production technology difference is as follows：When adding formaldehyde for the first time
All formaldehyde are added simultaneously, remaining material dosage and processing step are identical.
(cement used is oil well G class g cements to the cement slurry property of test the present embodiment drag reducer, and water is prepared by API standard
Mud, the ratio of mud 0.44), experimental result such as following table：
| Sample dosage, wt% | Temperature, DEG C | N values | K values | Thickening time, min | 24h intensity, MPa |
| 0 | 85 | 0.457 | 1.270 | 78 | 15.8 |
| 0.3 | 85 | 0.520 | 0.763 | 82 | 14.7 |
| 0.5 | 85 | 0.598 | 0.421 | 88 | 16.1 |
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is extended out still in protection scope of the present invention.
Claims (8)
1. a kind of preparation method of oil-well cement drag reducer, it is characterised in that comprise the following steps：
(1) sodium sulfite is dissolved in distilled water, obtains sodium sulfite solution；
(2) phenol is dissolved in sodium sulfite solution；
(3) pH of the solution obtained in step (2) is adjusted to 11-12；
(4) formaldehyde is added dropwise for the first time：Formaldehyde is added dropwise in the solution obtained to step (3), stirs, rear material color is added dropwise and becomes
To be faint yellow；
(5) acetone is added in the material that step (4) obtains, stirring, after addition, material color is changed into orange from faint yellow
Color, then reddish brown is changed into from crocus；
(6) second of dropwise addition formaldehyde：Residual formaldehyde is added drop-wise in the material that step (5) obtains and reacted, is stirred, is produced anti-
Product is answered, obtains red solid powder by reaction product is spray-dried；
Phenol, formaldehyde, the weight ratio of acetone and sodium sulfite are 1-2:16-20:5-8:6-10.
2. the preparation method of oil-well cement drag reducer according to claim 1, it is characterised in that in step (4)：Drop
The amount for adding formaldehyde is the 29%-31% of formaldehyde gross weight；In step (6)：The amount that formaldehyde is added dropwise is the 69%- of formaldehyde gross weight
71%.
3. the preparation method of oil-well cement drag reducer according to claim 1, it is characterised in that in step (5)：Control
For reaction temperature processed at 45-52 DEG C, constant temperature keeps 40min.
4. the preparation method of oil-well cement drag reducer according to claim 1, it is characterised in that in step (6)：Control
For reaction temperature processed at 95-100 DEG C, constant temperature keeps 3h.
5. the preparation method of oil-well cement drag reducer according to claim 1, it is characterised in that in step (1)：Steam
The quality of distilled water is 3-6 times of sodium sulfite quality.
6. the preparation method of oil-well cement drag reducer according to claim 1, it is characterised in that in step (3)：With
The pH of NaOH regulation solution is 11-12.
7. the preparation method of oil-well cement drag reducer according to claim 1, it is characterised in that formaldehyde is added dropwise for the first time
When the dropwise addition duration be 15-30min；Dropwise addition duration during second of dropwise addition formaldehyde is 15-30min.
8. the preparation method of oil-well cement drag reducer according to claim 1, it is characterised in that in step (4), (5)
(6) in：Using magnetic stirring apparatus, magnetic stirring speed is 800r/min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186459A (en) * | 2007-12-04 | 2008-05-28 | 北京工业大学 | Method for preparing aliphatic high efficiency water reducing agent by using industrial by-product and application thereof |
| CN104293324A (en) * | 2014-05-30 | 2015-01-21 | 中国石油化工集团公司 | Ultrahigh-temperature drilling fluid filtrate reducer and its preparation method |
| CN104531113A (en) * | 2014-12-24 | 2015-04-22 | 廊坊古莱特石油技术有限公司 | Drag reducer for oil-well cement |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186459A (en) * | 2007-12-04 | 2008-05-28 | 北京工业大学 | Method for preparing aliphatic high efficiency water reducing agent by using industrial by-product and application thereof |
| CN104293324A (en) * | 2014-05-30 | 2015-01-21 | 中国石油化工集团公司 | Ultrahigh-temperature drilling fluid filtrate reducer and its preparation method |
| CN104531113A (en) * | 2014-12-24 | 2015-04-22 | 廊坊古莱特石油技术有限公司 | Drag reducer for oil-well cement |
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