CN107954680A - A kind of high-temperature chlorine oxygen magnesium thermosetting resin gelling system and firming body and its preparation method - Google Patents

A kind of high-temperature chlorine oxygen magnesium thermosetting resin gelling system and firming body and its preparation method Download PDF

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Publication number
CN107954680A
CN107954680A CN201610902252.2A CN201610902252A CN107954680A CN 107954680 A CN107954680 A CN 107954680A CN 201610902252 A CN201610902252 A CN 201610902252A CN 107954680 A CN107954680 A CN 107954680A
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China
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parts
thermosetting resin
chlorine oxygen
oxygen magnesium
gelling system
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Inventor
谭春勤
周仕明
陈雷
高元
初永涛
赵艳
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China Petroleum and Chemical Corp
Sinopec Research Institute of Petroleum Engineering
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China Petroleum and Chemical Corp
Sinopec Research Institute of Petroleum Engineering
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Priority to CN201610902252.2A priority Critical patent/CN107954680A/en
Publication of CN107954680A publication Critical patent/CN107954680A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/30Compositions 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 magnesium cements or similar cements
    • C04B28/32Magnesium oxychloride cements, e.g. Sorel cement
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B22/00Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
    • C04B22/08Acids or salts thereof
    • C04B22/16Acids or salts thereof containing phosphorus in the anion, e.g. phosphates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/12Nitrogen containing compounds organic derivatives of hydrazine
    • C04B24/123Amino-carboxylic acids
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/42Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/46Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
    • C09K8/467Compositions 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
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/42Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/46Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
    • C09K8/467Compositions 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
    • C09K8/473Density reducing additives, e.g. for obtaining foamed cement compositions
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/20Mortars, concrete or artificial stone characterised by specific physical values for the density
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength

Abstract

The present invention relates to a kind of the high-temperature chlorine oxygen magnesium thermosetting resin gelling system and firming body and its preparation method in oil gas well cementing operation field.The high-temperature chlorine oxygen magnesium thermosetting resin gelling system, includes epoxy resin latex, epoxy curing agent, chlorine oxygen magnesium framework material and high temperature adjustable solidification agent;The epoxy resin latex is selected from least one of diglycidyl ether type, glycidyl ester type, alicyclic type, glycidic amine type, linear aliphatic race type epoxy resin;The epoxy curing agent is selected from least one of acid anhydrides, carboxylic acid, amine compounds, phenolic compound, polyalcohol;The high-temperature chlorine oxygen magnesium thermosetting resin gelling system can heating, pressurization etc. under the conditions of can crosslinking curing formed tridimensional network high-molecular organic material, by excellent heat resistance, the advantages that good compression strength and toughness, excellent adhesive force, realize 90~120 DEG C of hot environment cementing concrete annular space long term seals.

Description

A kind of high-temperature chlorine oxygen magnesium thermosetting resin gelling system and firming body and its preparation method
Technical field
The present invention relates to oil gas well cementing operation field, furtherly, is related to a kind of high-temperature chlorine oxygen magnesium thermosetting resin gel System and firming body and its preparation method.
Background technology
Oil-well cement is the portland cement of calcium oxide type, belongs to the cementitious material of the hydraulicity.It can be with water by certain Ratio be mixed into cement mortar, and harden into underground with certain compression strength, the impervious Behavior of Hardened Cement Paste with durability, and Can also there are wide adaptability and compatibility with various additives, extra material, density, intensity and hardening time are in a certain range It is interior to realize design and control, can easily meet the needs of conventional cementing engineering, the general sealing as casing and cementing is situated between Matter, is widely used for over more than 100 years in all kinds of operations such as oil drilling, completion, well workover, has ensured the smooth exploitation of oil gas field.
However, as various countries in recent years constantly increase the demand of clean energy resource, the especially unconventionaloil pool such as shale gas Field constantly puts into exploitation, and conventional oil-well cement also exposes it and ensureing oil/gas well casing programme integrality, adapting to small Deficiency in terms of gap environment and extensive perforation and acidfracturing treatment.Conventional hardened oilwell cement is a kind of brittleness material easily shunk Material, its intrinsic hydration characteristics, use environment (high temperature, high pressure) and construction technology (high water-cement ratio, high fluidity) determine it With several critical defects:High volume contraction, high filter loss and high brittleness.The volume contraction of cement mortar slurry causes cement sheath It is cementing etc to cannot be guaranteed, it is also possible to form microgap, trigger formation fluid channelling.Foreign literature shows, ordinary cement slurry Volume can be shunk more than 5% after 120h is conserved, while analog study shows, microgap of the cement sheath interface there are 0.01mm Has channeling can occur.Under intense loading lotus percussion, cement sheath can rupture and form macroscopic cracking and interface high brittleness Behavior of Hardened Cement Paste Destroy.And high leak-off make it that dehydration bridge blinding occurs for cement mortar in the construction process and dehydration shrinkage, cement mortar filtrate enter oil gas After layer, payzone can be also polluted.Therefore, portland cement easily makes since the external force such as material deformation or underground high temperature, high pressure acts on Behavior of Hardened Cement Paste crystal inside is undergone phase transition, and triggers microannulus, microcrack, influences the integrality of Behavior of Hardened Cement Paste.Downhole fluid also can at the same time Behavior of Hardened Cement Paste is caused to corrode, each discontinuous running such as drilling well, completion, volume increase and production may all cause cement sheath and annular space sealing Damage, causes annular space seal failure.Some preventions and remedial measure are all passivitys, and success rate is not high, and expense compares It is expensive.For Tail Pipe For Complicated Deep Wells, ultra-deep oil/gas well, annular channeling often occurs, it is poor mainly due to cementing concrete ring bonding quality, Stratum high pressure gas or water is caused to be altered along annular space microgap to well head or casing, and " weightlessness " of cement mortar during curing Phenomenon also results in has channeling, and being continuously increased with the production time, and annular space situation with pressure is also continuously increased.Sinopec is in recent years Also there is annular space situation with pressure the general light gone into operation successively, the gas field such as burnt masonry dam.The reason for causing annular space with pressure, has very much, but Itself deficiency as oil well cement material is one of most important one factor.
Therefore, oil gas water breakthrough has become the difficulty that a urgent need of oil-gas field development solves after how preventing well cementation Topic.Wherein, consider from material angle, seek to develop the developing direction that new gelling system is casing and cementing.
Chinese patent CN105367036A discloses a kind of low temperature magnesia oxychloride cement and preparation method thereof, disclosed in it Magnesia oxychloride cement and thermosetting resin are only applicable to building trade, coating industry etc., and are all single use, and are not carried out both Combination, it is even more impossible to realize that the two combines later performance control technique.
The content of the invention
In order to solve the above-mentioned problems in the prior art, the present invention proposes a kind of high-temperature chlorine oxygen magnesium thermosetting resin gelling System.Relate in particular to a kind of high-temperature chlorine oxygen magnesium thermosetting resin gelling system and firming body and its preparation method.The present invention's High-temperature chlorine oxygen magnesium thermosetting resin gelling system, is mainly used for 90~120 DEG C of hot environment oil gas well cementing operation fields, makes up special In the case of cement slurry property deficiency, solve part well cementation problem, under special hole condition realize part substitute cement mortar application, carry The leakproofness of high annular space, ensures the efficient production of oil/gas well.The characteristics of high-temperature chlorine oxygen magnesium thermosetting resin gelling system of the present invention It is:Can under the conditions of heating, pressurization etc. can crosslinking curing form the high-molecular organic material of tridimensional network, dependence is excellent Heat resistance, the advantages that good compression strength and toughness, excellent adhesive force, realize 90~120 DEG C of hot environments well cementation Cement annular space long term seal.
A kind of high-temperature chlorine oxygen magnesium thermosetting resin gelling system of one of the object of the invention, includes epoxy resin latex, epoxy Component including resin curing agent, chlorine oxygen magnesium framework material and high temperature adjustable solidification agent;The chlorine oxygen magnesium framework material is selected from light-burned Magnesia and magnesium chloride;The high temperature adjustable solidification agent includes the mixing of polyphosphoric acids salt medium temperature adjustable solidification agent and edta salt quasi-chelate compound Thing;The edta salt quasi-chelate compound is preferably at least one of EDETATE SODIUM salt, EDTA calcium salts, more preferably EDTA calcium salts;
Each component dosage is counted by 100 parts by weight of light calcined magnesia dosage, 100 parts of light calcined magnesia, 100 parts of magnesium chloride, 4~25 parts of epoxy resin latex, preferably 5~20 parts, 2.5~10 parts of epoxy curing agent, 0.5~2 part of fluid loss agent, poly 3~18 parts of phosphoric acid salt medium temperature adjustable solidification agent, preferably 5~15 parts, edta salt quasi-chelate compound are 3~5 parts, defoamer 0.05~0.5 Part, 0~40 part of density palliative, 0~40 part of density heavy weight additive, 35~120 parts of water.
The epoxy resin latex be selected from diglycidyl ether type, glycidyl ester type, alicyclic type, glycidic amine type, At least one of curable epoxies such as linear aliphatic race type epoxy resin, preferably glycidic amine type, curable epoxy Resin may include at least one epoxy resin, and epoxy resin is those compounds for including at least one vicinal epoxy group.Ring Oxygen tree fat can be saturation or unsaturation, aliphatic series, alicyclic, aromatics or heterocycle and can be substitution.Epoxy resin Can be monomer or polymer.
The epoxy curing agent is selected from acid anhydrides, carboxylic acid, amine compounds, phenolic compound, and at least one in polyalcohol Kind, preferably amine compounds;
The fluid loss agent may be selected from fluid loss agent of polyvinyl alcohol fluid loss agent, terpolymer etc., preferably polyethylene Alcohol fluid loss agent.
The density palliative can be high antibody glass microballoon density palliative.Water can be fresh water.Defoamer can be silicone oil Defoamer.
The firming body of a kind of high-temperature chlorine oxygen magnesium thermosetting resin gelling system of the two of the object of the invention, by the high-temperature chlorine oxygen Magnesium thermosetting resin gelling system cures and obtains.
A kind of preparation method of high-temperature chlorine oxygen magnesium thermosetting resin gelling system of the three of the object of the invention, including following step Suddenly:First each component is weighed according to the above ratio;Then by magnesium chloride, epoxy resin latex, epoxy curing agent, defoamer, more Quadrafos medium temperature adjustable solidification agent is uniformly mixed to obtain mixing liquid with edta salt quasi-chelate compound, fluid loss agent, water, under agitation finally Other components including light calcined magnesia are added, is uniformly mixed, obtains the high-temperature chlorine oxygen magnesium thermosetting resin gelling system.
The slurry rheology of the high-temperature chlorine oxygen magnesium thermosetting resin gelling system configuration of the present invention is good, is easy to cementing operation.This Thermosetting resin cementitious material in the high-temperature chlorine oxygen magnesium thermosetting resin gelling system of invention can be handed under conditions of heating, pressurization Connection is formed by curing netted three-dimensional-structure, and heat resistance is high, and compression is unlikely to deform, and has excellent adhesive force, shock resistance, corrosion-resistant etc. Advantage.The high-temperature chlorine oxygen magnesium thermosetting resin gelling system effectively increases cures body elasticity under high temperature, reduces Young's modulus, So that firming body has higher impact resistance and higher shearing glue-joint strength, realize that medium temperature condition lower hardening time is controllable, Meet cementing operation condition.It can be controlled by the mixture high temperature adjustable solidification agent for adding polyphosphate and edta salt quasi-chelate compound Chlorine oxygen magnesium thermosetting resin gelling system is adjustable in 90~120 DEG C of thickening times.Can be into one with the use of chlorine oxygen magnesium framework material Step improves or regulates and controls the performances such as the density of aathermoset resin system, intensity, rheology, hardening time, moreover it is possible to because magnesia is swollen Swollen characteristic improves the cementing strength of an interface and second interface, while casing and cementing basic demand is met, additionally it is possible to solves oil The problems such as easily damaged existing for well cement, cementing difference, overcome the correlation deficiency of oil-well cement, realize and substitute cement applications in well cementation Engineering, improves annular space leakproofness, ensures the efficient production of oil/gas well.The present invention high-temperature chlorine oxygen magnesium thermosetting resin gelling system be This area high temperature well cementation provides a kind of new selection, has broad application prospects.
Embodiment
With reference to embodiment, the present invention is further illustrated.But the present invention is not restricted by the embodiments.
Embodiment 1
(1) 300g light calcined magnesias (MgO, Mei Shen Chemical Co., Ltd.s of Xingtai city), magnesium chloride 300g are weighed (MgCl2, Shandong Zibo Hua Yan Chemical Co., Ltd.s), polyvinyl alcohol fluid loss agent 6g (FSAM, Shandong Dezhou continental shelf auxiliary agent Factory), polyphosphoric acids salt medium temperature adjustable solidification agent 30g (NP2, Shandong Dezhou continental shelf auxiliary reagent factory), edta salt quasi-chelate compound 15g (NP3, Shandong Dezhou continental shelf auxiliary reagent factory, EDTA calcium salts), silicon oil foam killer 1.5g (DZX, Shandong Dezhou continental shelf auxiliary reagent factory), Glycidyl amine type epoxy resin lotion 60g (RS, Shandong Dezhou continental shelf auxiliary reagent factory), Polyamines Curing Agents of Epoxy Resins 30g (RSC, Shandong Dezhou continental shelf auxiliary reagent factory), fresh water 135g.
(2) by magnesium chloride, glycidyl amine type epoxy resin lotion, Polyamines Curing Agents of Epoxy Resins, silicon oil foam killer, more The mixture of polyphosphoric acid salt medium temperature adjustable solidification agent and edta salt quasi-chelate compound, polyvinyl alcohol fluid loss agent, mixing of fresh water are uniform to be obtained Mixing liquid;
(3) in the mixing container, mixing liquid is added, blender is rotated for (4000 ± 200 revs/min) with low speed, and 15 Light calcined magnesia powder is added in second, covers the lid of blender, and continue stirring 35 under (12000 ± 500 revs/min) at a high speed Second, stir evenly and obtain high-temperature chlorine oxygen magnesium thermosetting resin gelling system, density 1.65g/cm3
High-temperature chlorine oxygen magnesium thermosetting resin gelling is detected according to GB/T19139-2012 cement mortar main performance test methods The basic performance of system, the result is shown in such as table 1 below.
1 density 1.65g/cm of table3High-temperature chlorine oxygen magnesium thermosetting resin gelling system basic performance
Good by the high-temperature chlorine oxygen magnesium thermosetting resin gelling system rheological characteristic of 1 visible the application of table, the thickening time is adjustable.
According to (1)~(3) operating method, added in mixed powder high antibody glass microballoon density palliative 0~ 120g or density 0~120g of heavy weight additive, changes fresh water amount between 105~360g, can obtain density in 1.28~1.78g/cm3 High-temperature chlorine oxygen magnesium thermosetting resin gelling system.According to GB/T 19139-2012 cement mortar main performance test methods to high temperature Chlorine oxygen magnesium thermosetting resin gelling system firming body carries out Evaluating Mechanical Properties, and interior has been investigated under different densities, high-temperature chlorine oxygen magnesium 120 DEG C of maintenance 24h compression strength of thermosetting resin gelling system firming body, as a result such as table 2.
2 different densities high-temperature chlorine oxygen magnesium thermosetting resin gelling system compressive strength of solidified body of table
Density, g/cm3 1.78 1.74 1.70 1.68 1.60 1.52 1.45 1.28
Compression strength, MPa 18.4 24.2 19.6 17.5 14.0 9.3 7.5 4.8
As shown in Table 2, when high-temperature chlorine oxygen magnesium thermosetting resin gelling system density is less than 1.74g/cm3When, high-temperature chlorine oxygen magnesium The compression strength of thermosetting resin gelling system dramatically increases, maximum up to 24.2MPa.
Embodiment 2~5
The dosage of polyphosphoric acids salt medium temperature adjustable solidification agent is changed to 15g, 24g, 30g, 45g respectively, while by edta salt class The dosage of chelating agent changes 9g, 9g, 9g, 15g into respectively, the dosage and step of other components with (1) the step of embodiment 1~ (3) it is identical, high-temperature chlorine oxygen magnesium thermosetting resin gelling system is made.
The high-temperature chlorine oxygen magnesium thermosetting resin gelling system that embodiment 2~5 is obtained is according to GB/T19139-2012 cement mortars Main performance test method carries out thickening time test, the results are shown in Table 3.
The high-temperature chlorine oxygen magnesium thermosetting resin gelling system thickening time of the different adjustable solidification agent dosages of table 3
Formula Thickening time, min
15gNP2+9gNP3 (embodiment 2) 189
24gNP2+9gNP3 (embodiment 3) 220
30gNP2+9gNP3 (embodiment 4) 242
45gNP2+15gNP3 (embodiment 5) 270
As seen from Table 3, as the increase of adjustable solidification agent dosage, high-temperature chlorine oxygen magnesium thermosetting resin gelling system thickening time are linear Increase, illustrates that the adjustable solidification agent can realize curing time control, meets different well's conditions demand.
Embodiment 6~8
The dosage of glycidyl amine type epoxy resin lotion is changed to 15g, 30g, 45g respectively, the dosage of other components and Step is identical with (1) the step of embodiment 1~(3), and high-temperature chlorine oxygen magnesium thermosetting resin gelling system is made.
The height of embodiment 1 and embodiment 6~8 is detected according to Q/SH 0275.1-2009 cement mortar main performances test method The elasticity modulus of warm chlorine oxygen magnesium thermosetting resin gelling system, the result is shown in such as table 4 below.
The high-temperature chlorine oxygen magnesium thermosetting resin gelling system of the different epoxy resin dosages of table 4 cures bulk modulus
Formula Elasticity modulus, GPa
15gRS (embodiment 6) 3.9
30gRS (embodiment 7) 3.7
45gRS (embodiment 8) 3.6
60gRS (embodiment 1) 3.2
As can be seen from Table 4, laboratory test shows, high-temperature chlorine oxygen magnesium thermosetting resin gelling system firming body has relatively low Elasticity modulus, with the increase of epoxy resin dosage, elasticity modulus energy linear reduction, meets the needs of different well's conditions.
Embodiment 9
(1) 300g light calcined magnesias (MgO, Mei Shen Chemical Co., Ltd.s of Xingtai city), magnesium chloride 300g are weighed (MgCl2, Shandong Zibo Hua Yan Chemical Co., Ltd.s), polyvinyl alcohol fluid loss agent 6g (FSAM, Shandong Dezhou continental shelf auxiliary agent Factory), polyphosphoric acids salt medium temperature adjustable solidification agent 30g (NP2, Shandong Dezhou continental shelf auxiliary reagent factory), edta salt quasi-chelate compound 15g (NP3, Shandong Dezhou continental shelf auxiliary reagent factory), silicon oil foam killer 1.5g (DZX, Shandong Dezhou continental shelf auxiliary reagent factory), glycidol Ether type epoxy lotion 15g (RSN, Shandong Dezhou continental shelf auxiliary reagent factory), Polyamines Curing Agents of Epoxy Resins 7.5g (RSC, Shandong Dezhou continental shelf auxiliary reagent factory), fresh water 202.5g.
(2) by magnesium chloride, diglycidyl ether type epoxy resin emulsion, Polyamines Curing Agents of Epoxy Resins, silicon oil foam killer, more The mixture of polyphosphoric acid salt medium temperature adjustable solidification agent and edta salt quasi-chelate compound, polyvinyl alcohol fluid loss agent, mixing of fresh water are uniform to be obtained Mixing liquid;
(3) in the mixing container, mixing liquid is added, blender is rotated for (4000 ± 200 revs/min) with low speed, and 15 Light calcined magnesia powder is added in second, covers the lid of blender, and continue stirring 35 under (12000 ± 500 revs/min) at a high speed Second, stir evenly and obtain high-temperature chlorine oxygen magnesium thermosetting resin gelling system, density 1.65g/cm3
High-temperature chlorine oxygen magnesium thermosetting resin gelling is detected according to GB/T19139-2012 cement mortar main performance test methods The basic performance of system, the result is shown in table 5 below.
5 density 1.65g/cm of table3High-temperature chlorine oxygen magnesium thermosetting resin gelling system basic performance
It can be seen that high-temperature chlorine oxygen magnesium thermosetting resin gelling system rheological characteristic prepared by the embodiment of the present application 9 is good, the thickening time can Adjust.

Claims (7)

1. a kind of high-temperature chlorine oxygen magnesium thermosetting resin gelling system, it is characterised in that include epoxy resin latex, epoxy resin cure Agent, chlorine oxygen magnesium framework material and high temperature adjustable solidification agent;
The chlorine oxygen magnesium framework material is selected from light calcined magnesia and magnesium chloride;The high temperature adjustable solidification agent is included in polyphosphoric acids salt Warm adjustable solidification agent and edta salt quasi-chelate compound;
Each component dosage is counted as 100 parts by weight using light calcined magnesia dosage and includes following component:100 parts of light calcined magnesia, chlorination 100 parts of magnesium, 4~25 parts of epoxy resin latex, 2.5~10 parts of epoxy curing agent, 0.5~2 part of fluid loss agent, polyphosphoric acids 3~18 parts of salt medium temperature adjustable solidification agent, edta salt quasi-chelate compound are 3~5 parts, 0.05~0.5 part of defoamer, density palliative 0~ 40 parts, 0~40 part of density heavy weight additive, 35~120 parts of water.
A kind of 2. high-temperature chlorine oxygen magnesium thermosetting resin gelling system according to claim 1, it is characterised in that:
Each component dosage is counted as 100 parts by weight using light calcined magnesia dosage and includes following component:100 parts of light calcined magnesia, chlorination 100 parts of magnesium, 5~20 parts of epoxy resin latex, 2.5~10 parts of epoxy curing agent, 0.5~2 part of fluid loss agent, polyphosphoric acids 5~15 parts of salt medium temperature adjustable solidification agent, edta salt quasi-chelate compound are 3~5 parts, 0.05~0.5 part of defoamer, density palliative 0~ 40 parts, 0~40 part of density heavy weight additive, 35~120 parts of water.
A kind of 3. high-temperature chlorine oxygen magnesium thermosetting resin gelling system according to claim 1 or 2, it is characterised in that the epoxy Resin emulsion is selected from diglycidyl ether type, glycidyl ester type, alicyclic type, glycidic amine type, linear aliphatic race type ring oxygen At least one of resin.
A kind of 4. high-temperature chlorine oxygen magnesium thermosetting resin gelling system according to claim 1 or 2, it is characterised in that the epoxy Resin curing agent is selected from least one of acid anhydrides, carboxylic acid, amine compounds, phenolic compound, polyalcohol.
A kind of 5. high-temperature chlorine oxygen magnesium thermosetting resin gelling system according to claim 1 or 2, it is characterised in that the EDTA Salt quasi-chelate compound is at least one of EDETATE SODIUM salt, EDTA calcium salts.
6. according to a kind of firming body of high-temperature chlorine oxygen magnesium thermosetting resin gelling system of any one of them of Claims 1 to 5, its It is characterized in that:The firming body of the high-temperature chlorine oxygen magnesium thermosetting resin gelling system is by the high-temperature chlorine oxygen magnesium thermosetting resin gel System cures and obtains.
7. according to a kind of preparation method of high-temperature chlorine oxygen magnesium thermosetting resin gelling system of any one of them of Claims 1 to 5, It is characterized by comprising following steps:By magnesium chloride, epoxy resin latex, epoxy curing agent, defoamer, polyphosphate Class medium temperature adjustable solidification agent is uniformly mixed to obtain mixing liquid with edta salt quasi-chelate compound, fluid loss agent, water, adds including light-burned oxidation Other components including magnesium, are uniformly mixed, obtain the high-temperature chlorine oxygen magnesium thermosetting resin gelling system.
CN201610902252.2A 2016-10-18 2016-10-18 A kind of high-temperature chlorine oxygen magnesium thermosetting resin gelling system and firming body and its preparation method Pending CN107954680A (en)

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CN108948658A (en) * 2018-05-16 2018-12-07 河南理工大学 A kind of preparation method of chlorine oxygen magnesium whisker/epoxy resin composite material
CN109504356A (en) * 2018-11-21 2019-03-22 西南石油大学 A kind of high strength, low elasticity water-soluble resin mortar architecture and its application
CN109534774A (en) * 2017-09-21 2019-03-29 中国石油化工股份有限公司 A kind of medium temperature magnesium oxysulfide thermosetting resin gelling system and preparation method thereof
CN112574729A (en) * 2019-09-27 2021-03-30 中国石油化工股份有限公司 Coagulation regulating composition, coagulation regulating agent and application thereof
CN114196387A (en) * 2021-07-16 2022-03-18 中国石油天然气集团有限公司 Shear-dilution type acid-soluble inorganic curing plugging agent, and preparation method and application thereof

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CN109534774A (en) * 2017-09-21 2019-03-29 中国石油化工股份有限公司 A kind of medium temperature magnesium oxysulfide thermosetting resin gelling system and preparation method thereof
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CN112574729A (en) * 2019-09-27 2021-03-30 中国石油化工股份有限公司 Coagulation regulating composition, coagulation regulating agent and application thereof
CN112574729B (en) * 2019-09-27 2022-07-15 中国石油化工股份有限公司 Coagulation regulating composition, coagulation regulating agent and application thereof
CN114196387A (en) * 2021-07-16 2022-03-18 中国石油天然气集团有限公司 Shear-dilution type acid-soluble inorganic curing plugging agent, and preparation method and application thereof

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Application publication date: 20180424