CN105567196A - Toughness enhancing latex additive with weak slow setting and water loss controlling effects and preparation method of latex additive - Google Patents
Toughness enhancing latex additive with weak slow setting and water loss controlling effects and preparation method of latex additive Download PDFInfo
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- 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
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F279/00—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00
- C08F279/02—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00 on to polymers of conjugated dienes
Abstract
The invention discloses a toughness enhancing latex additive with weak slow setting and water loss controlling effects and a preparation method of the latex additive. The preparation method comprises the following steps of 1, taking polybutadiene rubber latex, styrene, sodium dodecyl sulfate, neopelex or sodium abietate, cumene hydroperoxide, and ethylenediamine tetracetic acid or sodium pyrophosphate; adding the materials into a reaction container; uniformly stirring the materials to obtain a mixed solution; continuously stirring the mixed solution; 2, taking and putting 2-acrylamido-2-methyl propane sulfonic acid or sodium p-styrenesulfonate, N,N-dimethyl acrylamide or acrylamide, crylic acid and water into a container; performing stirring to dissolve the materials; adding glucose and iron vitriol; stirring to dissolve the materials; 3, dripping the solution obtained in the second step into the mixed solution obtained in the first step, and reacting after the dripping completion. The latex additive has the advantages that the multiple effects of toughness enhancement, weak slow setting and water loss controlling are achieved; the integral performance is good; the applicability is wide; the production method is simple; the cost is lower.
Description
Technical field
The present invention relates to a kind of latex admixture and preparation method, belong to cementing concrete toughner field.
Background technology
The extraction of crude oil is a complex process, needs to solve the problems such as drilling well, well cementation, perforation in this complex process.Wherein, cementing quality directly affects the exploitation of Oil/gas Well and the exploitation of oil-gas field.Well-cementing cement belongs to hard brittle material, and tensile property is poor, and under lower tensile deformation, Behavior of Hardened Cement Paste just can produce tiny crack.When plus load reaches certain value, tiny crack will be expanded into macroscopic fracture rapidly, and cement mantle can be caused time serious to lose sealing function, causes oil gas interval to alter groove, and taping the latent power to the exploitation after perforation and transformation brings very large impact.Therefore, need in cement, to add a certain amount of toughner to improve hardened oilwell cement mechanical property, to alleviate the extent of injury that breaks that cement mantle causes at the stress concentration of the masterpiece used time that is hit.
In addition, in grout pumping procedure, there will be the phenomenon of excessive dehydration (API fluid loss can reach 1,500 one 2000mL/30min), multiviscosisty and condensation fast, in order to ensure that construction safety carries out smoothly, also needing the fluid loss and the thickening time that control grout.
Latex is the common name for describing a kind of Emulgating polymers, adds the mortar architecture after latex and is called as latex cement slurry system.As far back as 1958, latex cement slurry system was just used in the middle of oil well cementing engineering.Prior art discloses the preparation method of multiple cementing slurry latex admixture.As CN101328401A high temperature toughcementing carboxyl butadiene-styrene latex additive, disclose a kind of preparation method of grout toughner, this invention carboxylic styrene butadiene latex is as cementing concrete toughner, its Behavior of Hardened Cement Paste formed has toughness, good cementing quality can be ensured, but this preparation method's complex process, cost is higher.CN101759825A carboxylated styrene-butadiene rubber latex special for oil and gas field cementing well, disclose the carboxylic styrene butadiene latex being used as water retaining in a kind of oil-gas field well cementing operation, although this invention carboxylic styrene butadiene latex can control fluid loss effectively, it is not investigated performances such as latex cement stone intensity, thickening times.
So the latex admixture that the prior art being representative with above-mentioned patent documentation is synthesized can only solve some shortcoming of oil well cement.The latex of these patents synthesis also must add other admixture to solve other problem of oil well cement in Cementing application, and this not only can increase the cost of well cementation, also likely occurs the problem that between admixture, compatibleness is bad.Therefore, the latex being badly in need of developing a kind of excellent combination property carrys out the problem of large, the excessive dehydration of disposable solution oil well cement brittleness and multiviscosisty fast.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide one can effectively improve oil-gas field cementing quality, reservoir protec-tion, improve recovery ratio, reduce the toughness reinforcing latex admixture having weak slow setting and control dehydration effect concurrently of well cementation cost.
Second object of the present invention is to provide a kind of toughness reinforcing preparation method having the latex admixture of weak slow setting and control dehydration effect concurrently.
Technical scheme of the present invention is summarized as follows:
The toughness reinforcing preparation method having the latex admixture of weak slow setting and control dehydration effect concurrently, comprises the steps:
(1) get that 32-100 mass parts particle diameter is 100-300nm, solid content is 37.5% polybutadiene latex, 30-10 mass parts vinylbenzene, 1.2-5 mass parts sodium lauryl sulphate, Sodium dodecylbenzene sulfonate or sodium abietate, 0.1-0.54 mass parts hydrogen phosphide cumene, 0.2-1.2 mass parts ethylenediamine tetraacetic acid (EDTA) or trisodium phosphate, join in reaction vessel, 50-80 DEG C, under rotating speed is the condition of 150-350r/min, stir, obtain mixed solution, continue to stir;
(2) get 6-2 mass parts 2-acrylamide-2-methylpro panesulfonic acid or Sodium styrene sulfonate, 4-6 mass parts N,N-DMAA or acrylamide, 2-4 mass parts vinylformic acid and 126-75 mass parts water put into a container, be stirred to dissolve; Add 0.3-1.0 mass parts glucose, 0.3-0.9 mass parts iron vitriol, is stirred to dissolve;
(3) solution obtained in step (2) is added drop-wise in the mixed solution that step (1) obtains, and after dripping, reaction 2-4h, obtains the toughness reinforcing latex admixture having weak slow setting and control dehydration effect concurrently.
Step (1) is preferably: get that 96 mass parts particle diameters are 100-300nm, solid content is 37.5% polybutadiene latex, the vinylbenzene of 12 mass parts, 3.6-4.8 part sodium lauryl sulphate or sodium abietate, 0.18-0.36 mass parts hydrogen phosphide cumene, 0.4-0.8 mass parts ethylenediamine tetraacetic acid (EDTA), join in reaction vessel, 60-70 DEG C, under rotating speed is the condition of 200-300r/min, stir, obtain mixed solution, continue to stir.
Step (2) is preferably: the water getting the 2-acrylamide-2-methylpro panesulfonic acid of 4 mass parts, the N,N-DMAA of 5 mass parts, the vinylformic acid of 3 mass parts and 75 mass parts puts into a container, is stirred to dissolve; Add the glucose of 0.3-1.0 mass parts, the iron vitriol of 0.3-0.6 mass parts, is stirred to dissolve.
Step (3) reaction times is 3h.
The toughness reinforcing latex admixture having weak slow setting and control dehydration effect concurrently prepared by method.
Advantage of the present invention:
(1) the present invention adopts redox system initiator, and reactive grafting efficiency is high, can greatly reduce temperature of reaction and reaction times.
(2) invention introduces function monomer 2-acrylamide-2-methylpro panesulfonic acid, being added on macromolecular chain of 2-acrylamide-2-methylpro panesulfonic acid introduces sulfonic group, form thicker hydration layer, heatproof and salt resistant character can be brought to polymkeric substance, reduce the susceptibility of reaction system to pH.
(3) invention introduces function monomer N,N-DMAA, N, being added on macromolecular chain of N-DMAA introduces amide group, anti-salt and control dehydration effect good, form hyperconjugation system between nitrogen, carbonyl, double bond, Heat stability is good.
(4), when the toughness reinforcing latex admixture having weak slow setting and control dehydration effect concurrently of the present invention is used as cementing extra-agent, there is the multiple effect of toughness reinforcing, weak slow setting and control dehydration.
(5) the present invention adopts polybutadiene latex as soft monomer, and need not lead to N during reaction
2protection gas, method is simple, and cost is low, easily realizes suitability for industrialized production.
Latex admixture of the present invention has the multiple effect of toughness reinforcing, weak slow setting and control dehydration concurrently, and over-all properties is good, and suitability is wide, can be used alone in well cementing process, and its production technique is simple, and cost is lower, is easy to realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the toughness reinforcing latex admixture infrared spectrogram having weak slow setting and control dehydration effect concurrently prepared by embodiment 1;
Fig. 2 is the toughness reinforcing latex admixture hot weightless picture having weak slow setting and control dehydration effect concurrently prepared by embodiment 1;
Fig. 3 is the impact that the toughness reinforcing latex admixture having weak slow setting and control dehydration effect concurrently of embodiment 1 preparation develops cement strength;
The toughness reinforcing latex admixture having weak slow setting and control dehydration effect concurrently that Fig. 4 is prepared by embodiment 1 under different dosage on the impact of Behavior of Hardened Cement Paste crumbly coefficient;
Fig. 5 is the scanning electron microscope (SEM) photograph of plain cement;
Fig. 6 is the toughness reinforcing latex admixture Behavior of Hardened Cement Paste scanning electron microscope (SEM) photograph having weak slow setting and control dehydration effect concurrently prepared by embodiment 1;
Fig. 7 is the toughness reinforcing multiviscosisty curve of latex admixture grout at 80 DEG C having weak slow setting and control dehydration effect concurrently prepared by embodiment 1;
The toughness reinforcing latex admixture grout having weak slow setting and control dehydration effect concurrently that Fig. 8 is prepared by embodiment 1, at 80 DEG C, adds the multiviscosisty curve after 10% Industrial Salt.
Embodiment:
Polybutadiene latex manufacturer is: Dajie Chemical Co., Ltd., Tianjin
Below by specific embodiment, the present invention is further illustrated.Embodiments of the invention are to understand the present invention better, but do not impose any restrictions the present invention.
Embodiment 1
The toughness reinforcing preparation method having the latex admixture of weak slow setting and control dehydration effect concurrently, comprises the steps:
(1) get that 96g particle diameter is 100nm, solid content is 37.5% polybutadiene latex, 12g vinylbenzene, 3.6g sodium lauryl sulphate, 0.18g hydrogen phosphide cumene, 0.4g ethylenediamine tetraacetic acid (EDTA), join in reaction vessel, 70 DEG C, under rotating speed is the condition of 200r/min, stir, obtain mixed solution, continue to stir;
(2) get 4g2-acrylamide-2-methylpro panesulfonic acid, 5gN, N-DMAA, 3g vinylformic acid and 75g water and put into a container, be stirred to dissolve; Add 0.3g glucose, 0.3g iron vitriol, is stirred to dissolve;
(3) solution obtained in step (2) is added drop-wise in the mixed solution that step (1) obtains, and after dripping, reaction 3h, obtains the toughness reinforcing latex admixture having weak slow setting and control dehydration effect concurrently.
The toughness reinforcing cement slurry property that have the latex admixture (be called for short latex admixture) of weak slow setting and control dehydration effect obtained containing embodiment 1 is tested as shown in table 1.
Table 1
Note: the cement that the present invention uses is for praising magnificent cement in Sichuan.Water In The Experiment mud prescription is: 600g cement, and the add-on of latex admixture is equivalent to the 0-16% of cement quality, water cement ratio 0.44.
Latex admixture infrared spectrogram prepared by the present embodiment is shown in Fig. 1,3440cm
-1for the stretching vibration absorption peak of the N-H in 2-acrylamide-2-methylpro panesulfonic acid, 1250cm
-1and 1104cm
-1be respectively symmetry and the asymmetrical stretching vibration absorption peak of S=O in the sulfonic group of 2-acrylamide-2-methylpro panesulfonic acid, 1639cm
-1for the stretching vibration peak of C=O in the amide group of 2-acrylamide-2-methylpro panesulfonic acid and N,N-DMAA; 1548cm
-1and 1402cm
-1for the asymmetric of carboxyl in vinylformic acid and symmetrical stretching vibration peak; 698cm
-1and 754cm
-1be respectively formation vibration peak and the C-H face bending features absorption peak of phenyl ring, 2849cm
-1~ 3025cm
-1place is-CH in polybutadiene latex
3with-CH
2stretching vibration absorption peak.Can find that five kinds of monomers all participate in reaction by infrared spectrum, the latex admixture of synthesis is target product.
Latex admixture hot weightless picture prepared by the present embodiment is shown in Fig. 2, can be found out by thermal weight loss collection of illustrative plates, and the heat decomposition temperature of the latex admixture of synthesis, higher than 400 DEG C, has good high-temperature stability.
Latex admixture prepared by the present embodiment is 8% at dosage, curing temperature is the cement strength progress curve under 80 DEG C of conditions, see Fig. 3, can be found out by curve, before 8h, latex cement stone does not almost have intensity, illustrates that latex admixture plays certain delayed coagulation, after 8h, intensity develops rapidly, can play the effect of supporting sleeve in well cementing process, and the intensity added after latex admixture is significantly less than the intensity of plain cement, decreases the brittleness of Behavior of Hardened Cement Paste to a certain extent.
Latex admixture prepared by the present embodiment on the impact of Behavior of Hardened Cement Paste crumbly coefficient, is shown in Fig. 4 under different dosage.Can be found out by curve, along with its crumbly coefficient of increase of latex admixture dosage reduces rapidly, when latex admixture dosage to 8% time crumbly coefficient minimum, its value becomes again large but the crumbly coefficient numerical value adding the Behavior of Hardened Cement Paste of latex admixture is all less than the numerical value of plain cement subsequently, and toughening effect is obvious.
Embodiment 2
The toughness reinforcing preparation method having the latex admixture of weak slow setting and control dehydration effect concurrently, comprises the steps:
(1) 96g particle diameter is 300nm, solid content is 37.5% polybutadiene latex, 12g vinylbenzene, 4.8g sodium lauryl sulphate is got, 0.36g hydrogen phosphide cumene, 0.8g ethylenediamine tetraacetic acid (EDTA), join in reaction vessel, 60 DEG C, under rotating speed is the condition of 300r/min, stir, obtain mixed solution, continue to stir;
(2) get 4g2-acrylamide-2-methylpro panesulfonic acid, 5gN, N-DMAA, 3g vinylformic acid and 75g water and put into a container, be stirred to dissolve; Add 1.0g glucose, 0.6g iron vitriol, is stirred to dissolve;
(3) solution obtained in step (2) is added drop-wise in the mixed solution that step (1) obtains, and after dripping, reaction 3h, obtains the toughness reinforcing latex admixture having weak slow setting and control dehydration effect concurrently.
Embodiment 3
The toughness reinforcing preparation method having the latex admixture of weak slow setting and control dehydration effect concurrently, comprises the steps:
(1) 32g particle diameter is 100nm, solid content is 37.5% polybutadiene latex, 30g vinylbenzene, 1.2g sodium abietate is got, 0.1g hydrogen phosphide cumene, 0.2g ethylenediamine tetraacetic acid (EDTA), join in reaction vessel, 50 DEG C, under rotating speed is the condition of 150r/min, stir, obtain mixed solution, continue to stir;
(2) get 2g Sodium styrene sulfonate, 6gN, N-DMAA, 4g vinylformic acid and 126g water and put into a container, be stirred to dissolve; Add 0.3g glucose, 0.3g iron vitriol, is stirred to dissolve;
(3) solution obtained in step (2) is added drop-wise in the mixed solution that step (1) obtains, and after dripping, reaction 4h, obtains the toughness reinforcing latex admixture having weak slow setting and control dehydration effect concurrently.
Embodiment 4
The toughness reinforcing preparation method having the latex admixture of weak slow setting and control dehydration effect concurrently, comprises the steps:
(1) 100g particle diameter is 300nm, solid content is 37.5% polybutadiene latex, 10g vinylbenzene, 5g Sodium dodecylbenzene sulfonate is got, 0.54g hydrogen phosphide cumene, 1.2g trisodium phosphate, join in reaction vessel, 80 DEG C, under rotating speed is the condition of 350r/min, stir, obtain mixed solution, continue to stir;
(2) get 6g2-acrylamide-2-methylpro panesulfonic acid, 4g acrylamide, 2g vinylformic acid and 75g water and put into a container, be stirred to dissolve; Add 1.0g glucose, 0.9g iron vitriol, is stirred to dissolve;
(3) solution obtained in step (2) is added drop-wise in the mixed solution that step (1) obtains, and after dripping, reaction 2h, obtains the toughness reinforcing latex admixture having weak slow setting and control dehydration effect concurrently.
Comparative example 1
(1) get that 96g particle diameter is 100nm, solid content is 37.5% polybutadiene latex, 12g vinylbenzene, 3.6g sodium lauryl sulphate, 0.18g hydrogen phosphide cumene, 0.4g ethylenediamine tetraacetic acid (EDTA), join in reaction vessel, 70 DEG C, under rotating speed is the condition of 200r/min, stir, obtain mixed solution, continue to stir;
(2) get 12g2-acrylamide-2-methylpro panesulfonic acid and 75g water puts into a container, be stirred to dissolve; Add 0.3g glucose, 0.3g iron vitriol, is stirred to dissolve;
(3) solution obtained in step (2) is added drop-wise in the mixed solution that step (1) obtains, and after dripping, reaction 3h, obtains contrast latex admixture.
Comparative example 2
(1) get that 96g particle diameter is 100nm, solid content is 37.5% polybutadiene latex, 12g vinylbenzene, 3.6g sodium lauryl sulphate, 0.18g hydrogen phosphide cumene, 0.4g ethylenediamine tetraacetic acid (EDTA), join in reaction vessel, 70 DEG C, under rotating speed is the condition of 200r/min, stir, obtain mixed solution, continue to stir;
(2) get 12gN, N-DMAA and 75g water put into a container, are stirred to dissolve; Add 0.3g glucose, 0.3g iron vitriol, is stirred to dissolve;
(3) solution obtained in step (2) is added drop-wise in the mixed solution that step (1) obtains, and after dripping, reaction 3h, obtains contrast latex admixture.
The toughness reinforcing grout having the latex admixture (being called for short latex admixture) of weak slow setting and control dehydration effect concurrently that table 2 obtains for containing embodiment 1-4 respectively, and the contrast latex admixture cement slurry property test containing comparative example 1-2 is as shown in table 2.
Table 2
Note: the cement that the present invention uses is for praising magnificent cement in Sichuan.Water In The Experiment mud prescription is: 600g cement, and the add-on of latex admixture or contrast latex admixture is equivalent to 8% of cement quality, water cement ratio 0.44.
Embodiment 1-4 compares with comparative example 1 respectively, can find, introduces latex admixture, not only has good toughening effect, and had obvious improvement to the fluid loss of grout, can control in 100mL.
Embodiment 1-4 compares with comparative example 2 respectively, can find, introduces latex admixture, has better delayed coagulation.In sum, embodiment 1-4 latex admixture has triple effects of toughness reinforcing, weak slow setting and control dehydration.
Do scanning electron microscope at 80 DEG C of maintenances grout of 2 days, see Fig. 5;
Do scanning electron microscope at 80 DEG C of maintenances grout containing 8% embodiment 1 latex admixture of 2 days, see Fig. 6;
Can find out that from Electronic Speculum figure ortho-water mudstone internal structure exists a large amount of hole, and for being mixed with the grout of latex admixture of the present invention, latex particle can evenly spread in slurry, along with the carrying out of hydrated reaction of cement, the micelle gathered on hydrated product surface forms continuous film and links together with hydrated product, define a kind of tridimensional network of compound, final formation gel-like film covers hydrated calcium silicate gel, illustrates that the toughening mechanism of latex admixture of the present invention is membrane formation mechanism.
Containing 8% embodiment 1 latex admixture grout 80 DEG C, multiviscosisty curve under 40MPa condition is shown in Fig. 7, as can be seen from multiviscosisty curve, 80 DEG C, under 40MPa condition, grout multiviscosisty curve containing latex admixture is normal, without bag heart phenomenon, multiviscosisty substantially at a right angle, performance is fine.
Containing the grout of 8% embodiment 1 latex admixture, adding Industrial Salt makes mass content be 10%, 80 DEG C, multiviscosisty curve under 40MPa condition is shown in Fig. 8, as can be seen from multiviscosisty curve, at 80 DEG C, 40MPa and under adding the condition of Industrial Salt in formula, system containing latex admixture is still very stable, multiviscosisty curve is normal, rectangular multiviscosisty, and transition time is very short, meet construction requirement, illustrate that the grout adding latex admixture has good anti-salt-stable.
Claims (5)
1. the toughness reinforcing preparation method having the latex admixture of weak slow setting and control dehydration effect concurrently, is characterized in that comprising the steps:
(1) get that 32-100 mass parts particle diameter is 100-300nm, solid content is 37.5% polybutadiene latex, 30-10 mass parts vinylbenzene, 1.2-5 mass parts sodium lauryl sulphate, Sodium dodecylbenzene sulfonate or sodium abietate, 0.1-0.54 mass parts hydrogen phosphide cumene, 0.2-1.2 mass parts ethylenediamine tetraacetic acid (EDTA) or trisodium phosphate, join in reaction vessel, 50-80 DEG C, under rotating speed is the condition of 150-350r/min, stir, obtain mixed solution, continue to stir;
(2) get 6-2 mass parts 2-acrylamide-2-methylpro panesulfonic acid or Sodium styrene sulfonate, 4-6 mass parts N,N-DMAA or acrylamide, 2-4 mass parts vinylformic acid and 126-75 mass parts water put into a container, be stirred to dissolve; Add 0.3-1.0 mass parts glucose, 0.3-0.9 mass parts iron vitriol, is stirred to dissolve;
(3) solution obtained in step (2) is added drop-wise in the mixed solution that step (1) obtains, and after dripping, reaction 2-4h, obtains the toughness reinforcing latex admixture having weak slow setting and control dehydration effect concurrently.
2. method according to claim 1, it is characterized in that step (1) is: get that 96 mass parts particle diameters are 100-300nm, solid content is 37.5% polybutadiene latex, the vinylbenzene of 12 mass parts, 3.6-4.8 part sodium lauryl sulphate or sodium abietate, 0.18-0.36 mass parts hydrogen phosphide cumene, 0.4-0.8 mass parts ethylenediamine tetraacetic acid (EDTA), join in reaction vessel, 60-70 DEG C, under rotating speed is the condition of 200-300r/min, stir, obtain mixed solution, continue to stir.
3. method according to claim 1, it is characterized in that step (2) is: get the 2-acrylamide-2-methylpro panesulfonic acid of 4 mass parts, the N of 5 mass parts, the vinylformic acid of N-DMAA, 3 mass parts and the water of 75 mass parts put into a container, are stirred to dissolve; Add the glucose of 0.3-1.0 mass parts, the iron vitriol of 0.3-0.6 mass parts, is stirred to dissolve.
4. method according to claim 1, is characterized in that step (3) reaction times is 3h.
5. the toughness reinforcing latex admixture having weak slow setting and control dehydration effect concurrently prepared of the method for one of claim 1-4.
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| CN114181352A (en) * | 2021-11-10 | 2022-03-15 | 中国石油天然气集团有限公司 | Polymer material, preparation method thereof and well cementation cement slurry system |
| CN114989361A (en) * | 2022-06-16 | 2022-09-02 | 中国石油天然气集团有限公司 | Preparation method of cement paste high-temperature-resistant fluid loss agent |
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