CN104774601A - Gypsum microspheres and low elasticity modulus expansion well cementation cement system - Google Patents

Gypsum microspheres and low elasticity modulus expansion well cementation cement system Download PDF

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CN104774601A
CN104774601A CN201510169604.3A CN201510169604A CN104774601A CN 104774601 A CN104774601 A CN 104774601A CN 201510169604 A CN201510169604 A CN 201510169604A CN 104774601 A CN104774601 A CN 104774601A
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gypsum
cement
parts
microballoon
oil
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CN104774601B (en
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步玉环
柳华杰
郭辛阳
郭胜来
王春雨
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China University of Petroleum East China
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Abstract

The invention discloses gypsum microspheres and a low elasticity modulus expansion cement system suitable for medium and low temperature well cementation. The gypsum microspheres are obtained through inverse setting and hardening of a certain proportion of anhydrite, alpha-type hemihydrate gypsum and water. The low elasticity modulus expansion cement system comprises 100 parts of oil well cement, 10-40 parts of gypsum microspheres, 5-10 parts of micro-silicon and 65-75 parts of water, and the volume expansion of set cement and the reduction of elasticity modulus of the set cement are simultaneously realized due to the addition of the gypsum microspheres. The low elasticity modulus expansion cement system meets the long-term requirements of cement sheath isolation completeness and has important engineering significance for ensuring well cementation quality and long-term safety production of oil-gas wells.

Description

Gypsum microballoon and low elastic modulus expansion cementing cement system
Technical field
The present invention relates to a kind of gypsum microballoon and comprise its low elastic modulus expansion cementing cement system that can ensure cementing quality for a long time, belong to oil gas well cementing operation Material Field.
Background technology
Cementing concrete ring has the effect on supporting sleeve and packing stratum, and wherein, one is Main Function.Cement mantle provides Inter-zonal packing, prevents layer cross flow, avoids interlayer contamination, ensures oil gas safety in production.In order to realize this function, cement mantle must continuously and impermeable.After hardening of cement, the contraction of annular space Behavior of Hardened Cement Paste volume is one of principal element affecting cement mantle sealing property.Behavior of Hardened Cement Paste volumetric shrinkage mainly comprises chemical shrinkage and drying shrinkage.Chemical shrinkage is the defect of cement self; Drying shrinkage and water cement ratio positive correlation, in casing and cementing, in order to ensure grout pumpability, water cement ratio is higher, so its drying shrinkage is more serious.The most effectual way solving Behavior of Hardened Cement Paste volumetric shrinkage adds swelling agent in cement.Lattice dilatation agent and swelling agent of getting angry are that expanding agent type commonly used by oil well cement.
For lattice dilatation agent (gypsum and magnesium oxide), research shows (walks Yuhuan, Liu Huajie, Song Wenyu. lattice dilatation agent is on impact experiment [J] of cement-ferrule interface bonding capacity. petroleum journal, 2011,32 (6): 1067-1071.), although lattice dilatation agent add the contraction that can make up Behavior of Hardened Cement Paste volume, but effectively can not improve cementing quality, the ability making cement mantle opposing temperature and pressure change the stress-strain caused declines, and causes the consolidation strength of cement mantle and sleeve pipe significantly to decline after temperature and pressure changes.This is adding due to gypsum and the lattice dilatation agent of magnesium oxide class, can generate a large amount of crystal in cement mantle.The existence of a large amount of crystal adds the Young's modulus of Behavior of Hardened Cement Paste, reduces the ability of Behavior of Hardened Cement Paste opposing temperature and pressure change.
For swelling agent of getting angry, (Liu Huajie is found by research, step Yuhuan, Wang Xueying, Guo Xinyang. pore is to expansion well-cementing cement intensity effect [J] of getting angry. China University Of Petroleum Beijing's journal (natural science edition) 2014, 38 (2): 75-81.), the pore that swelling agent of getting angry produces has compensation water mudstone volumetric shrinkage and reduces the dual function of Behavior of Hardened Cement Paste Young's modulus, but the more difficult control of expansion process of getting angry, the uneven strength property affecting Behavior of Hardened Cement Paste on the contrary of gas cell distribution, so special process or swelling agent utilisation technology of getting angry should be taked when swelling agent is got angry in application, make hole diameter distribution range more concentrated, and these measures to implement be very difficult.
Volumetric shrinkage is Behavior of Hardened Cement Paste self-defect, the various borehole operation of Oil/gas Well simultaneously must apply pressure and thermal stresses to cement mantle, therefore requires that cement mantle has certain expansion character, and has lower Young's modulus, can be subject to, in loading-unloading process, preventing brittle rupture.So develop a kind of low elastic modulus expansion cementing cement system, cement mantle long-term integrity can be ensured, guarantee cementing quality and Oil/gas Well long-term safety be produced there is important engineering significance.
Summary of the invention
The object of the invention is to one of have problems to solve in above-mentioned prior art, a kind of gypsum microballoon and low elastic modulus expansion cementing cement system are provided.
The technical solution adopted for the present invention to solve the technical problems is:
One aspect of the present invention provides a kind of preparation method of gypsum microballoon, and the stirring that is added to the water after dehydrated gyp-, semi-hydrated gypsum being mixed obtains gypsum suspension liquid, then gypsum suspension liquid is joined continuation stirring in oil phase dispersion medium, filters to obtain gypsum microballoon; The mass percent of wherein said dehydrated gyp-, semi-hydrated gypsum and water is (10 ~ 30%): (30 ~ 50%): (30 ~ 50%), and described gypsum suspension liquid accounts for 5% ~ 25% of described oil phase dispersion medium volume.
Gypsum microballoon of the present invention is the product that a certain proportion of dehydrated gyp-, alpha semi-hydrated gypsum and water are obtained by anti-phase setting and harden.
Preferably, described semi-hydrated gypsum is alpha semi-hydrated gypsum.
Preferably, described dehydrated gyp-order number is 500 ~ 1000 orders.
Preferably, described alpha semi-hydrated gypsum order number is 500 ~ 1000 orders.
Preferably, the churning time of described gypsum suspension liquid is for being no more than 5min.
Preferably, it is 200 ~ 700r/min that described gypsum suspension liquid joins stirring velocity in oil phase dispersion medium, and churning time is 1 ~ 2h.
Preferably, described oil phase dispersion medium is Viscotrol C or rapeseed oil or soya-bean oil or Semen Maydis oil or peanut oil.
Adopt gypsum microballoon prepared by the preparation method of above-mentioned gypsum microballoon.
Preferably, the particle size range of described gypsum microballoon is 50 ~ 200 μm.
The present invention on the other hand provides a kind of low elastic modulus expansion cementing cement system, comprises following component and its each ingredients weight parts ratio consists of: oil well cement 100 parts, gypsum microballoon 10 parts ~ 40 parts, micro-silicon 5 parts ~ 10 parts, 65 parts ~ 75 parts, water.
Preferably, the weight part ratio of described each component and each component thereof consists of: oil well cement 100 parts, gypsum microballoon 25-30 part, micro-silicon 8-10 part, water 65-70 part.
Preferably, the weight part ratio of described each component and each component thereof consists of: oil well cement 100 parts, gypsum microballoon 25 parts, micro-silicon 8 parts, 65 parts, water.
Preferably, the weight part ratio of described each component and each component thereof consists of: oil well cement 100 parts, gypsum microballoon 30 parts, micro-silicon 10 parts, 70 parts, water.
The preparation method of above-mentioned low elastic modulus expansion cementing cement system, first by oil well cement, gypsum microballoon and micro-silicon are dry mixed, and then carry out with slurry by the system after being dry mixed and water according to standard.
Low elastic modulus expansion cementing cement system of the present invention has microdilatancy performance under middle cold condition, and grout has low Young's modulus after setting and hardening, namely the ropy problem of sealing that cement mantle volumetric shrinkage causes can be solved, can effectively resist stress-strain effect again, ensure cement mantle long-term integrity, better meet casing and cementing needs.
The present invention adopts special component and process exploitation to go out to have the gypsum microballoon of some strength, then adds in cement by gypsum microballoon, introduces micro-silicon, to prevent gypsum microspheres settle in cement simultaneously.Gypsum is the lattice dilatation agent that oil well cement is conventional, and therefore gypsum microballoon can make Behavior of Hardened Cement Paste expand; Introduce more moisture in process simultaneously due to exploitation gypsum microballoon, microballoon has many holes gap structure, makes its Young's modulus lower, and therefore gypsum microballoon can reduce the Young's modulus of Behavior of Hardened Cement Paste entirety simultaneously.But gypsum is as the lattice dilatation agent of oil well cement, and use temperature is no more than 85 DEG C in theory, thus the present invention and be not suitable for hot hole well cementation.
Achieve the adding of gypsum microballoon of the present invention the function making Behavior of Hardened Cement Paste volumetric expansion and reduce Behavior of Hardened Cement Paste Young's modulus simultaneously.Low elastic modulus expansion cementing cement system of the present invention is conducive to the long-term needs of cement mantle packing integrity, produces have important engineering significance to guarantee cementing quality and Oil/gas Well long-term safety.
Additional aspect of the present invention and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage will become obvious and easy understand from accompanying drawing below combining to the description of embodiment, wherein:
Fig. 1 is the microgram of gypsum microballoon (G1) of the present invention;
Fig. 2 is the microgram of gypsum microballoon (G2) of the present invention;
Fig. 3 is Behavior of Hardened Cement Paste volume change figure.
Embodiment
Be exemplary below by the embodiment be described with reference to the drawings, be intended to for explaining the present invention, and can not limitation of the present invention be interpreted as.
Embodiment 1 gypsum microballoon and preparation method thereof
After 6g dehydrated gyp-(625 order) and 14g alpha semi-hydrated gypsum (625 order) being mixed, join in 16g water, stir, churning time is 1.5min.Then at ambient temperature, joined by gypsum suspension liquid in 200g Semen Maydis oil, limit edged stirs, and stir speed (S.S.) is 500r/min, and gypsum suspension liquid joins after in Semen Maydis oil, continues to stir 2h.After stirring terminates, filter out gypsum microballoon, clean, room temperature is dried, and obtains the gypsum microballoon that particle diameter is about 100 μm, is designated as G1, as shown in Figure 1.
Embodiment 2 gypsum microballoon and preparation method thereof
After 4g dehydrated gyp-(800 order) and 16g alpha semi-hydrated gypsum (800 order) being mixed, join in 14g water, stir, churning time is 2min.Then at ambient temperature, joined by gypsum suspension liquid in 300g soya-bean oil, limit edged stirs, and stir speed (S.S.) is 600r/min, and gypsum suspension liquid joins after in soya-bean oil, continues to stir 2h.After stirring terminates, filter out gypsum microballoon, clean, room temperature is dried, and obtains the gypsum microballoon that particle size range is about 50 ~ 80 μm, is designated as G2, as shown in Figure 2.
Embodiment 3 low elastic modulus expansion cementing cement system
Cement-slurry method: G level oil well cement 100 parts+gypsum microballoon (G1) 25 parts+65 parts, micro-silicon 8 parts+water.Gained Behavior of Hardened Cement Paste sample is designated as C1.
Preparation method: by oil well cement, gypsum microballoon and micro-silicon are dry mixed, and then the system after being dry mixed and water are prepared grout according to GB19139-2003 oil-well cement test method.
Embodiment 4 low elastic modulus expansion cementing cement system
Cement-slurry method: G level oil well cement 100 parts+gypsum microballoon (G1) 30 parts+70 parts, micro-silicon 10 parts+water.Gained Behavior of Hardened Cement Paste sample is designated as C2.
Preparation method: by oil well cement, gypsum microballoon and micro-silicon are dry mixed, and then the system after being dry mixed and water are prepared grout according to GB19139-2003 oil-well cement test method.
Embodiment 5 low elastic modulus expansion cementing cement system
Cement-slurry method: G level oil well cement 100 parts+gypsum microballoon (G2) 30 parts+70 parts, micro-silicon 10 parts+water.Gained Behavior of Hardened Cement Paste sample is designated as C3.
Preparation method: by oil well cement, gypsum microballoon and micro-silicon are dry mixed, and then the system after being dry mixed and water are prepared grout according to GB19139-2003 oil-well cement test method.
Embodiment 6 low elastic modulus expansion cementing cement system
Cement-slurry method: H level oil well cement 100 parts+gypsum microballoon (G1) 30 parts+70 parts, micro-silicon 10 parts+water.Gained Behavior of Hardened Cement Paste sample is designated as C4.
Preparation method: by oil well cement, gypsum microballoon and micro-silicon are dry mixed, and then the system after being dry mixed and water are prepared grout according to GB19139-2003 oil-well cement test method.
In order to contrast, have selected traditional cements slurry formula:
G level oil well cement 100 parts+55 parts, micro-silicon 10 parts+water.Gained Behavior of Hardened Cement Paste sample is designated as C5.
H level oil well cement 100 parts+55 parts, micro-silicon 10 parts+water.Gained Behavior of Hardened Cement Paste sample is designated as C6.
According to GB 19139-2003 oil-well cement test method preparation grout, and test water mud slurry density, Behavior of Hardened Cement Paste ultimate compression strength, cement paste rheological and sedimentation stability.According to ANSI/API Recommended Practice 10B-5 standard, Behavior of Hardened Cement Paste volume change is measured.Behavior of Hardened Cement Paste Young's modulus adopts dynamic elastic modulus testing method to measure.In formula, adding of micro-silicon mainly prevents gypsum microspheres settle.Select cement sample C2 first to carry out rheological test, rheological test result is as shown in table 1, and cement paste rheological meets casing and cementing requirement as can be seen from the table.Under cement paste rheological meets casing and cementing requirement prerequisite, test the sedimentation stability of cement sample C2, test result is as shown in table 2, and Behavior of Hardened Cement Paste difference of densities per-cent is 0.715%, meets casing and cementing requirement.
Table 1 cement paste rheological
Table 2 grout sedimentation stability measuring result
Measuring position 1 (lowermost end) 2 3 4 5 (tops)
Behavior of Hardened Cement Paste density (g/cm 3) 1.678 1.675 1.670 1.669 1.666
Cement slurry density, ultimate compression strength and dynamic elastic modulus test result as shown in table 3.Behavior of Hardened Cement Paste volume change as shown in Figure 3.
Table 3 cement slurry density, ultimate compression strength and dynamic elastic modulus
As can be seen from table 3 and Fig. 3, adding of gypsum microballoon, realize the dual function of Behavior of Hardened Cement Paste microdilatancy and reduction Behavior of Hardened Cement Paste Young's modulus simultaneously.
The density the adding of gypsum microballoon making Behavior of Hardened Cement Paste and ultimate compression strength reduce, this is mainly because gypsum microballoon has comparatively multi-pore structure, the density of itself is lower, reduce the density of Behavior of Hardened Cement Paste, simultaneously because gypsum microballoon does not have gelling ability, therefore reduce Behavior of Hardened Cement Paste ultimate compression strength, but as can be seen from Table 3, under identical dosage, add the gypsum microballoon that particle diameter is less, the ultimate compression strength of Behavior of Hardened Cement Paste is larger.In order to explain better, citing document (Wang Qun. China's light weight cement research and apply overview [J]. drilling technique .1991,14 (2): 1-8) in data, as shown in table 4 and table 5.
Table 4 wilkinite is on the impact of Behavior of Hardened Cement Paste ultimate compression strength
Note: "--" original text does not provide related data in offering
Table 5 flyash is on the impact of Behavior of Hardened Cement Paste ultimate compression strength
As can be seen from table 4 and table 5, wilkinite and flyash add the density that can reduce Behavior of Hardened Cement Paste, but wilkinite and flyash are not having activity under activator existent condition very low, and therefore the ultimate compression strength of Behavior of Hardened Cement Paste all reduces.
Rubber grain has the effect reducing Behavior of Hardened Cement Paste Young's modulus, in order to be analyzed, (Lee is unit early for citing document, Guo little Yang. rubber powder is on the impact [J] of hardened oilwell cement mechanical property. oil drilling technology, 2008,36 (6): 52-55.) data in, as shown in table 6.
Table 6 rubber grain affects Mechanical Behavior of Hardened Cement Paste
As can be seen from Table 6, rubber grain reduces the Young's modulus of Behavior of Hardened Cement Paste, also reduce the ultimate compression strength of Behavior of Hardened Cement Paste, but rubber grain does not have the effect of compensation water mudstone volumetric shrinkage simultaneously.
So the present invention realizes Behavior of Hardened Cement Paste volumetric expansion and reduces Behavior of Hardened Cement Paste Young's modulus aspect to have significant advantage at the same time.
Although illustrate and describe embodiments of the invention, those having ordinary skill in the art will appreciate that: can carry out multiple change, amendment, replacement and modification to these embodiments when not departing from principle of the present invention and aim, scope of the present invention is by claim and equivalents thereof.

Claims (10)

1. a preparation method for gypsum microballoon, is characterized in that, the stirring that is added to the water after dehydrated gyp-, semi-hydrated gypsum being mixed obtains gypsum suspension liquid, then gypsum suspension liquid is joined continuation stirring in oil phase dispersion medium, filters to obtain gypsum microballoon; The mass percent of wherein said dehydrated gyp-, semi-hydrated gypsum and water is (10 ~ 30%): (30 ~ 50%): (30 ~ 50%), and described gypsum suspension liquid accounts for 5% ~ 25% of described oil phase dispersion medium volume.
2. preparation method according to claim 1, is characterized in that, described semi-hydrated gypsum is alpha semi-hydrated gypsum.
3. preparation method according to claim 1, is characterized in that, described dehydrated gyp-order number is 500 ~ 1000 orders, and described alpha semi-hydrated gypsum order number is 500 ~ 1000 orders.
4. preparation method according to claim 1, is characterized in that, the churning time of described gypsum suspension liquid is no more than 5min, and it is 200 ~ 700r/min that described gypsum suspension liquid joins stirring velocity in oil phase dispersion medium, and churning time is 1 ~ 2h.
5. preparation method according to claim 1, is characterized in that, described oil phase dispersion medium is Viscotrol C or rapeseed oil or soya-bean oil or Semen Maydis oil or peanut oil.
6. gypsum microballoon prepared by the preparation method described in any one of claim 1-5.
7. gypsum microballoon according to claim 6, is characterized in that, its particle size range is 50 ~ 200 μm.
8. a low elastic modulus expansion cementing cement system, is characterized in that, comprises following component and its each ingredients weight parts ratio consists of: oil well cement 100 parts, gypsum microballoon 10 ~ 40 parts, micro-silicon 5 ~ 10 parts, 65 ~ 75 parts, water.
9. low elastic modulus expansion cementing cement system according to claim 8, it is characterized in that, the weight part ratio of described each component and each component thereof consists of: oil well cement 100 parts, gypsum microballoon 25-30 part, micro-silicon 8-10 part, water 65-70 part.
10. the preparation method of the low elastic modulus expansion cementing cement system described in claim 8 or 9, is characterized in that, first by oil well cement, gypsum microballoon and micro-silicon are dry mixed, and is then undertaken with slurry by the system after being dry mixed and water.
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Cited By (2)

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CN116217139A (en) * 2023-01-03 2023-06-06 中曼石油天然气集团股份有限公司 Composite expansion toughening cement paste system and preparation method thereof

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