CN105733519A - Hydrophilia paraffin microcapsule and early-strength low-hydration-heat-releasing cement system - Google Patents

Hydrophilia paraffin microcapsule and early-strength low-hydration-heat-releasing cement system Download PDF

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CN105733519A
CN105733519A CN201610242980.5A CN201610242980A CN105733519A CN 105733519 A CN105733519 A CN 105733519A CN 201610242980 A CN201610242980 A CN 201610242980A CN 105733519 A CN105733519 A CN 105733519A
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cement
parts
hydration
paraffin
low
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CN105733519B (en
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柳华杰
步玉环
郭权庆
赵乐天
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China University of Petroleum East China
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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
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/02—Materials undergoing a change of physical state when used
    • C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
    • C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage 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
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C04B28/06—Aluminous cements
    • 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
    • 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
    • C09K8/473—Density reducing additives, e.g. for obtaining foamed cement compositions
    • 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
    • C04B2103/0071—Phase-change materials, e.g. latent heat storage materials used in concrete compositions

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Structural Engineering (AREA)
  • Thermal Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Physics & Mathematics (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

The invention discloses a hydrophilia paraffin microcapsule and an early-strength low-hydration-heat-releasing cement system for low-temperature well cementation.The cement system comprised, by weight, 100 parts of silicate and aluminate composite cement with the mass ratio of 3:7-5:5, 5-10 parts of phase-change heat absorption materials, 10-25 parts of density reducing materials and 58.2-77.2 parts of water.The cement system has the advantages that the early strength is high, and the early-strength characteristic of the system at the low temperature is excellent compared with a conventional G-grade oil well cement system; the amount of heat released during hydration is small, the amount of the hydration released heat and system temperature rising generated by the hydration released heat of the system in a 24-h hydration test are low compared with the conventional G-grade oil well cement system, and the stability of deepwater stratum hydrate can be guaranteed accordingly; the compatibility of the system with early strength agents and retarders is good.

Description

The strongest low hydration heat cement system of hydrophilic paraffin microcapsule
Technical field
The present invention relates to a kind of hydrophilic paraffin microcapsule and strong low hydration heat cement system morning for low temperature well cementing, It is that one is particularly well-suited to deep-water low-temperature, hydrate layer cementing cement system, is also applied for freezing the well cementation of hydrate layer Operation.The invention belongs to oil gas well cementing operation Material Field.
Background technology
Along with the definition of scientific and technological progress deep water constantly changes, generally believe that the depth of water is more than the region of 500m and is at present Deepwater regions.The countries in the world demand sustainable growth to petroleum resources in recent years, deep water hydrocarbon resource becomes various countries and opens The focus adopted.
Deep water has abundant petroleum resources, and whole world deep water is contained more than 1000 × 108The petroleum resources of t, verifies oil Gas reserves are about 380 × 108T, accounts for the 34% of Global Oil and Gas Resources total amount.Deep water hydrocarbon finds that accounting for global Oil Gas finds Total amount constantly rises, and accounts for global Oil Gas deep water hydrocarbon discovery amount in 2002～2003 and finds that total amount is up to 65%.At present, Work at the exploration and development carrying out marine oil and gas more than 100 countries, the West Africa off coast of two sides, the current Atlantic Ocean, Basin, bank Persian and the Gulf of Mexico have become as the hot zones of 3 deep-water explorations.The Angola in West Africa and the Niger three Many new oil fields, continent, angle put into exploitation, and external oil company has explored out 46 deepwater successively in Angola, Niger area has explored out 10 × 10 especially8The deepwater of t, has 17 in West Africa in 2000～2005 according to statistics Go into operation in deep water hydrocarbon field；Brazil's oil daily output 17.8 × 10 of 20004T, the depth of water is oily at the deep water of 400～2000m Gas field contribute to the yield of 70%；Gulf of Mexico deep water hydrocarbon yield in 2000 has reached 0.37 × 108t.More than except Hot zones South Africa, Argentina, Britain, Norway, Canada, Australia, New Zealand waited all carrying out deep Aqueous hydrocarbon work of exploration and development.China's deepwater petroleum exploration development at the South Sea in recent years is also actively launching.
There is the challenge of many during deepwater development, wherein the well cementation of highly effective and safe is exactly to put huge in face of developer One of hang-up.Such as the low temperature environment of deep water, shallow seated groundwater-flow of air, low formation fracture pressure, gas hydrates Exist, the unfavorable factor such as high rental expenses becomes the huge challenge that deep water cementing faces: (1) conventional cementing water Mud system composition is typically based on dicalcium silicate and tricalcium silicate, but both compositions when ambient temperature is less than 5 DEG C Almost without hydration capability, and deepwater seabed temperature is typically at 4 DEG C, minimum can be to 0 DEG C, this can greatly extend shaft building Cycle and shaft building expense；(2) the non-cementation of deep water shallow-layer makes that the formation fracture pressure of shallow stratum is low, stratum Pressure is high, and the Density Window of cementing slurry is narrow, it is necessary to uses low-density cement mortar i.e. to add and can not participate in hydration reaction Density palliative, cause the problem that the gain in strength of relative Behavior of Hardened Cement Paste is slow and low；(3) process that hydrated cementitious condenses It is exothermic reaction, easily causes the decomposition of hydrate, cause borehole diameter to expand, produce has channeling, affect mud replacement The problems such as efficiency, finally impact cementing quality.Additionally, the decomposition of gas hydrates also can cause abnormal high Pressure, produces blowout even well kick accident.The especially sealing facing challenges of deep water shallow seated groundwater compound layer is the severeest Require that cement system has low-temperature high-early strength, low hydrated reaction heat.
At present, the deep water cementing cement system of research both at home and abroad has: (1) grain composition cement system；(2) foam water Mud system；(3) quick-hardening cement system；(4) the slag system of physics and chemi-excitation；(5) gypsum system is coagulated soon； (6) aluminium sulfate and G class g cement compound system etc..Grain composition cement system has certain aquation at low temperatures Ability, but its cost is of a relatively high；Needing the equipment of complexity in foamed cement system work progress, this is the narrowest to this It is a challenge for little drilling platforms, logistic work difficulty can be increased；Under quick-hardening cement system low temperature, strength development is relatively Hurry up, but system can discharge huge heat, this is extremely disadvantageous for the stability of gas hydrates；Slag system There is in 10 DEG C of environment of low temperature higher early strength, but the early strength in 0～4 DEG C of environment is the highest and slag body System does not accounts for the requirement of low hydration heat, and system can discharge the higher heat of hydration under physics and chemokinesis effect；Hurry up Solidifying gypsum system presents preferable low-temperature high-early strength performance when 15 DEG C, but coagulates Gypsum Fibrosum body in the environment of about 5 DEG C soon Epistasis energy morning of system is bad；Aluminium sulfate and the G class g cement compound system of Wang Chengwen et al. research have good low temperature Early powerful feature, but system hydration heat is higher, is unfavorable for stablizing of gas hydrates.Both at home and abroad to deep water cementing Research scarcely consider gas hydrates, but increasing research show the existence of gas hydrates for Deep water cementing is a huge potential safety hazard.Research shows, gas hydrates are stably deposited under the conditions of 10MPa Temperature not can exceed that 18 DEG C, and 1mol gas hydrate dissociation to produce 100L at the standard conditions left Right gas.The decomposition of gas hydrates may induce well kick even gas blowout accident.Research shows, G level oil well Cement hydration heat temperature in 20 DEG C of atmospheric environments can reach about 80 DEG C, adds outside the conventional reduction heat of hydration The material result such as spike flyash, slag are inconspicuous, also can only G class g cement petrochemical industry be put in the case of mixing 30% volume Heat drop as little as about 65 DEG C, and the comprcssive strength of system is adversely affected by extra material；Aluminate cement is at 20 DEG C In atmospheric environment, hydration heat temperature can reach about 110 DEG C.And the most conventional deep water cementing body of cement System is all based on the formula of the improvement such as G class g cement and aluminate cement, and these systems all do not account for hydration heat temperature The detrimental effect that hydrate stability is produced.Therefore, conventional deep water cementing cement system hydration heat temperature exceeds well over Gas hydrate dissociation temperature, is huge threat for gas hydrates stability.
Control hydrated cementitious heat release, be usually in cement mortar, add phase-change material.But, about how to reduce oil well Seldom, the phase-change material towards building building cement has some to grind in recent years in the phase-change material research of heat release in cement hydration process Study carefully achievement.Li Wei et al. uses suspension polymerization to be prepared for n-octadecane as core, styrene-neopentyl glycol two propylene Acid ester copolymer is the phase-change material micro-capsule of shell material, and prepared phase-change material micro-capsule pattern is complete, good dispersion (Li Wei,Zhang Xing xiang,You Ming.Fabrication of microencapsulated/nanoencapsulated phase change materials using suspension polymerization[J].Polym Mater Sci Eng,2010, 26 (2): 36～39)；Zhang Xue waits people quietly and is prepared for n-octadecane as PCM by miniemulsion interfacial polymerization, polyureas with And double-deck Na capsule (Zhang Xuejing, the Wang Jianping, Zhang that polystyrene is wall material Xingxiang.Preparation of double shell nanoencapsulated phase change materials by interfacial polymerization in an emulsion system[J].New Chem Mater,2011,39(1): 45-49)；Ren Xiaoliang et al. uses situ aggregation method with lauryl alcohol as core, and carbamide is shell material (Ren Xiaoliang,Wang Lixin,Ren Li,et al.Preparation of phase change materials microcapsules By in-situ polymerization [J] .J Funct Mater, 2005,36 (11): 1722-1727.) have studied core shell ratio, breast Change the rotating speed performance impact to phase-change thermal storage microcapsule, although prepared microcapsule heat storage performance is excellent, but because of core Material is expensive, causes the carrying cost of unit heat energy to rise, and with melamine formaldehyde resin, Lauxite is The harmful gass such as microcapsule prepared by shell material in use Diazolidinyl Urea are detrimental to health, and these are all to hinder The subject matter of its scale application.Paraffin is the more commonly used phase-change material, but owing to paraffin belongs to oil phase, Aqueous phase coalescence will separate, cement mortar can not be directly applied to.At present paraffin is applied to cement mortar, is usually First using porous material to be absorbed by paraffin, the most again by porous material and cement mixing, the porous material of employing is generally Kieselguhr and perlite, but this belongs to physical absorption, and part paraffin still there will be coalescence segregation phenomenon.So this Plant way can not be applied in casing and cementing exigent to cement slurry property.Other ways existing are to use to have Machine monomer mixes in paraffin, then carries out suspension polymerisation, synthesizes paraffin microcapsule, and paraffin is scattered in organic monomer polymerization After rack in, this kind of method preferably controls the coalescence of paraffin, but the paraffin microcapsule of synthesis in aqueous phase very Difficult dispersion.Zhang Qiuxiang et al. is with paraffin as core, and methyl methacrylate-acrylic acid copolymer is shell material, nano-silica SiClx is that modifying agent uses situ aggregation method to be prepared for paraffin microcapsule phase change energy storage material, but the method synthesis is micro- There is agglomeration in capsule, and synthesis technique is relative complex, and (Lu Hongbin, etc. nano-silica for Zhang Qiuxiang, Chen Jianhua The research [J] of SiClx modified paraffin microcapsule phase-change energy storage material. macromolecule journal, 2015 (6): 692-698.).
At present, the research of domestic deep water cementing cement system is primarily directed to the situation without hydrate existence.For deeply The research of the cementing cement system of water hydrate layer is the fewest.For solving low temperature and the natural gas of the well cementation of deep water hydrate layer Decomposition of hydrate problem, develops strong low hydration heat cement system a kind of novel morning for low temperature well cementing and has weight The meaning wanted.
Summary of the invention
It is an object of the invention to provide a kind of early strength height, the hydration heat amount deep water that is applicable to low, low density is hydrated The cementing cement system of nitride layer.
The present invention solves the concrete technical scheme of this technical barrier:
Present invention firstly provides a kind of phase-change material i.e. paraffin microcapsule (hereinafter referred PCM) with endothermic character, Preparation method: bright for methyl olefin(e) acid formicester, benzoyl peroxide, divinylbenzene, melt paraffin mix homogeneously are formed Oil phase, then nano silicon is stirred in 75 DEG C with deionized water the most bell become aqueous phase；By slow for above-mentioned oil phase Importing in aqueous phase, 85 DEG C of heating in water bath, the paraffin that 2000 revs/min of high-speed stirred can be prepared by the present invention for 2 hours is micro- Capsule；Wherein said methyl bright olefin(e) acid formicester, benzoyl peroxide, divinylbenzene, paraffin, nano silicon, The mass ratio of water is 100:3:0.5:100:16:1000.
Described paraffin melting point is 40 DEG C.
Hydrophilic paraffin microcapsule prepared by above-mentioned preparation method.
The application in controlling hydrated cementitious heat release of the above-mentioned hydrophilic paraffin microcapsule.
Present invention also offers strong low hydration heat cement system formula a kind of morning for low temperature well cementing, its feature exists The component of following weight portion is included in, this formula:
Silicate-aluminate complex cement, mass ratio is 3:7～5:5,100 parts；
Decalescence material 5～10 parts；
Density lightening material 10～25 parts；
Water 58.2～77.2 parts.
According to powerful feature morning under aluminate cement low temperature, even if also having stronger hydration capability at 0 DEG C, to G level oil Well cement adds aluminate cement, improves cement system hydration capability at low temperatures, obtain morning higher under low temperature Strong intensity, aluminate cement microdilatancy characteristic at low temperatures in addition so that will not shrink under cement system low temperature, Ensure well cementation bonding quality, it is to avoid the generation of microannulus.The cement system of the present invention be G level oil well cementing cement- The mixed system of aluminate cement, it is the slowest that the introducing of aluminate can make up G class g cement hydration reaction speed at low temperatures Shortcoming, improve early strength.The introducing of G class g cement can make whole system maintain on the basis of early strength, Hydration heat is less than fine aluminium acid salt cement system.In preferably, the mass ratio of silicate-aluminate complex cement is 5:5.
When the low hydration heat deep water cementing cement system of the present invention uses, mix the phase-change material i.e. paraffin of 5～10 parts Microcapsule, absorbs the heat release during the characteristic reduction system hydration reaction of heat when utilizing paraffin microcapsule to undergo phase transition Amount, it is ensured that the stability of gas hydrates utilizes the low-density characteristic of paraffin microcapsule to reduce the density of system simultaneously. The phase-change material dosage preferably gone out 5 parts～10 parts.
The density lightening material of the present invention is hollow glass floating bead.This hollow float bead originates from Ma'an Mountain of Sinosteel Corporation mine and grinds Study carefully institute, model Y-12000, real density 0.80g/cm3, comprcssive strength 82.75MPa, median diameter 35 μm.
When early-strength low hydration heat deep water cementing cement system uses, the glass of 0～25 weight portions can be mixed Floating bead, water-solid ratio 0.506～0.572 can make density 1.36～1.81g/cm3Low-density cement mortar.Obtain for Low temperature well cementing morning strong low hydration heat cement system the ratio of mud be 0.506～0.572.
The strong low hydration heat cement system a kind of morning for low temperature well cementing of the present invention has a following excellent properties:
(1) early strength is high, and compared with conventional G level oil-well cement system, under this system low temperature, early powerful feature is excellent.
(2) hydration heat amount is low, and this system hydration heat amount and hydration heat in 24h hydration heat is tested produce Raw system temperature rise more conventional G level oil-well cement system is the lowest, and this advantageously ensures that deep water stratum is hydrated The stability of thing.
(3) this system and early strength agent, retarder compatibility are good.
Accompanying drawing explanation
Fig. 1 is the microgram (× 30) of the phase-change material of the present invention；
Fig. 2 is the microgram (× 220) of the phase change paraffin microcapsule of the present invention；
Fig. 3 is the strong low hydration heat cement system 24h hydration reaction test morning temperature profile for low temperature well cementing；
Fig. 4 be for low temperature well cementing morning strong low hydration heat cement system viscous resistance performance test consistency curve.
Detailed description of the invention
Embodiment 1, the present invention a kind of morning for low temperature well cementing strong low hydration heat cement system hydration heat performance Evaluate
Hydrating heat measuring experiment cement is by formula:
G class g cement formula: 100 parts of good China+44 parts of water of G class g cement；
Quick-hardening cement formula :+44 parts of water of 100 parts of essence CA-50 aluminate cements；
Silicate-aluminate complex cement formula :+50 parts of essence CA-50 aluminate cements+44 of 50 parts of G class g cements Part water；
LTC cement system formula: 30 parts of G class g cements+10 parts of PCM+25 of+70 parts of essence CA-50 aluminate cements Part+77.2 parts of water of floating bead；
Wherein: the mineral composition of the 30 parts of victory Weihe River+70 parts of essence CA-50 aluminate cements of G class g cement and percent mass Ratio is: aluminium oxide 42.6%, calcium oxide 40.3%, silicon dioxide 9.5%, ferrum oxide 2.1%, titanium oxide 2%, three Sulfur oxide 1.3%, magnesium oxide 1.1%, surplus are trace element.
The wherein preparation method of PCM (hydrophilic paraffin microcapsule), comprises the following steps: by bright for methyl olefin(e) acid first Fat, benzoyl peroxide, divinylbenzene, melt paraffin mix homogeneously formed oil phase, then by nano silicon with Deionized water is stirring at low speed the most bell one-tenth aqueous phase in 75 DEG C；Above-mentioned oil phase is slowly imported in aqueous phase, 85 DEG C of water-baths Heating, 2000 revs/min of high-speed stirred can be prepared by the paraffin microsphere of the present invention for 2 hours；The bright alkene of wherein said methyl Acid formicester, benzoyl peroxide, divinylbenzene, paraffin, nano silicon, the mass ratio of water are 100:3:0.5:100:16:1000.Its microgram is as shown in Figure 1 and Figure 2.
Prove: prepared PCM does not has agglomeration, easily disperses in aqueous phase.
Can be seen that the paraffin microcapsule sphericity of preparation is good, epigranular, good dispersion are not reunited from Fig. 1, Fig. 2 Phenomenon, due to existence microcapsule favorable dispersibility in water of nano silicon during microcapsule uses, does not has Phenomenon incompatible with water occurs.
Prepare cement mortar according to API 10B-3-2004 standard, utilize direct method to measure cement system hydration heat in 24h And represent hydration heat process by exotherm form.The contrast present invention low hydration heat deep water cementing cement system and G Level oil-well cement system, quick-hardening cement system hydration heat curve, test result see Fig. 3 (test condition: normal pressure, 20 DEG C of isoperibols).Test result shows hydration heat in the present invention low hydration heat deep water cementing cement system 24h The temperature peak that amount, hydration heat produce is much smaller than G level oil-well cement system, hydrated blended cement system, quick-hardening cement body The thermal discharge of system and hydration heat temperature peak, present good low hydration heat characteristic, advantageously ensure that and cemented the well The stability of gas hydrates in journey, it is to avoid the well cementation accident that gas hydrate dissociation brings.
Embodiment 2, the present invention a kind of morning for low temperature well cementing strong low hydration heat cement system low temperature compressive property Evaluate
Water at low temperature mudstone comprcssive strength experiment cement-slurry method:
G class g cement formula: 100 parts of good China+44 parts of water of G class g cement；
Silicate-aluminate complex cement formula :+50 parts of essence CA-50 aluminate cements+44 of 50 parts of G class g cements Part water；
LTC cement system formula: 30 parts of G class g cements+10 parts of PCM+25 of+70 parts of essence CA-50 aluminate cements Part+77.2 parts of water of floating bead；
Prepare cement mortar according to API 10B-3-2004 standard, measure under cement slurry density, different temperatures curing condition anti- Compressive Strength, and compare with G level oil-well cement comprcssive strength, test result is shown in Table 1.Test result shows, this The low hydration heat deep water cementing cement system of invention comprcssive strength at low temperatures shows far above G level oil-well cement Go out the low-temperature high-early strength characteristic of excellence；System density is made to be reduced to 1.36g/cm mixing glass pearl3System is still afterwards Show epistasis energy morning of excellence.
Table 1
Embodiment 3, early strength agent strong low hydration heat cement system compressive property shadow morning for low temperature well cementing a kind of to the present invention Ring and evaluate
LTC# formula: 30 parts of G class g cements+10 parts of PCM+25 part glass of+70 parts of essence CA-50 aluminate cements Floating bead+77.2 parts water+early strength agent, density 1.36g/cm3
Preparing cement mortar according to API 10B-3-2004 standard, the cement system measuring the different early strength agent of addition is supported in difference Comprcssive strength at a temperature of protecting, test result is shown in Table 2.Test result shows triethanolamine, LiCl H2O is low to the present invention Hydration heat deep water cementing cement system has significantly early powerful feature good with system compatibility.
Table 2
Embodiment 4, the thickening performance of retarder strong low hydration heat cement system morning for low temperature well cementing a kind of to the present invention Impact is evaluated
Formula 1:30+10 parts of PCM+25 part glass pearls of+70 parts of essence CA-50 aluminate cements of part G class g cement + 77.2 parts of water (without retarder)
Formula 2:30+10 parts of PCM+25 part glass pearls of+70 parts of essence CA-50 aluminate cements of part G class g cement + 77.2 parts of water+retarder, density 1.36g/cm3
Prepare cement mortar according to API 10B-3-2004 standard and measure this cement slurry and tie up to the thickening in 15 DEG C of environment Time, research shows that the circulating temperature of cement mortar is about 15 DEG C during deep water cementing, and cement mortar is at 15 DEG C In environment, system thickening performance is extremely sensitive to temperature, therefore selects 15 DEG C to be thickened performance test temperature, formula for system 1 just loses fluid ability in 15 DEG C of environment within several minutes, formula 2 test result is shown in Table 3, Fig. 4.Test knot Fruit shows, boric acid is as system retarder, LiCl H2O is as system early strength agent, and boric acid dosage is thick when being 0.35 part Change time 189min, denseness 30～100Bc 15min transit time, less than 30min, present good short transient time Performance.
Table 3
Although an embodiment of the present invention has been shown and described and comparative example, those of ordinary skill in the art can manage Solve: these embodiments can be carried out in the case of without departing from the principle of the present invention and objective multiple change, amendment, Replacing and modification, the scope of the present invention is limited by claim and equivalent thereof.

Claims (7)

1. a paraffin microcapsule with endothermic character, it is characterized in that, its preparation method: by bright for methyl olefin(e) acid formicester, benzoyl peroxide, divinylbenzene, melt paraffin mix homogeneously formed oil phase, then nano silicon is stirred in 75 DEG C with deionized water the most bell become aqueous phase；Slowly being imported in aqueous phase by above-mentioned oil phase, 85 DEG C of heating in water bath, 2000 revs/min of high-speed stirred can be prepared by the paraffin microcapsule of the present invention for 2 hours；Wherein said methyl bright olefin(e) acid formicester, benzoyl peroxide, divinylbenzene, paraffin, nano silicon, the mass ratio of water are 100:3:0.5:100:16:1000.
2. the paraffin microcapsule that prepared by the preparation method described in claim 1.
3. the application in controlling hydrated cementitious heat release of the paraffin microcapsule described in claim 2.
4. strong low hydration heat cement system morning for low temperature well cementing, it is characterised in that this formula includes the component of following weight portion:
Silicate-aluminate complex cement, mass ratio is 3:7～5:5,100 parts；
Decalescence material 5 ~ 10 parts；
Density lightening material 10 ~ 25 parts；
58.2 ~ 77.2 parts of water.
Morning for low temperature well cementing the most according to claim 4 strong low hydration heat cement system, it is characterised in that the mass ratio of described silicate-aluminate complex cement is 3:7 ~ 5:5.
Morning for low temperature well cementing the most according to claim 4 strong low hydration heat cement system, it is characterised in that described decalescence material is the paraffin microcapsule described in claim 2.
Morning for low temperature well cementing the most according to claim 4 strong low hydration heat cement system, it is characterised in that described density lightening material is hollow glass floating bead.
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CN106947447B (en) * 2017-03-20 2019-05-10 西南石油大学 Thermo-sensitive expanding microcapsules agent for anti gassing-out and channeling control cement slurry system
CN106947447A (en) * 2017-03-20 2017-07-14 西南石油大学 Thermo-sensitive expanding microcapsules agent for anti gassing-out and channeling control cement slurry system
US11685683B2 (en) 2017-06-21 2023-06-27 China University Of Petroleum (East China) High-strength geopolymer hollow microsphere, preparation method thereof and phase change energy storage microsphere
CN108298905A (en) * 2018-02-10 2018-07-20 浙江泉峰建筑园林有限公司 A kind of strong concrete
CN111894520A (en) * 2019-05-06 2020-11-06 中石化石油工程技术服务有限公司 Method for regulating temperature of drilling fluid based on paraffin material
CN111154459A (en) * 2020-01-20 2020-05-15 河北工业大学 Organic-inorganic hybrid shell phase change capsule and preparation method thereof
CN111154459B (en) * 2020-01-20 2021-03-19 河北工业大学 Organic-inorganic hybrid shell phase change capsule and preparation method thereof
CN112521113A (en) * 2020-12-04 2021-03-19 交通运输部公路科学研究所 Low-temperature hydration hardening gel material and preparation method and application thereof
CN112898956A (en) * 2021-01-27 2021-06-04 西安工程大学 Temperature-responsive well cementation cement slurry and preparation method thereof
CN113201314A (en) * 2021-04-22 2021-08-03 东南大学 Preparation method and application of C-S-H/PEG1000 phase-change composite material
CN113201314B (en) * 2021-04-22 2022-02-11 东南大学 Preparation method and application of C-S-H/PEG1000 phase-change composite material
CN113266304A (en) * 2021-07-01 2021-08-17 中国石油大学(华东) Penetrating hydrate layer cementing method for prolonging long-acting production life of oil and gas well
CN113266304B (en) * 2021-07-01 2022-06-07 中国石油大学(华东) Penetrating hydrate layer cementing method for prolonging long-acting production life of oil and gas well

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