Adjusting agent for solving abnormal gelation and thickening time inversion of high temperature cement slurry and preparation method thereof

Abstract

The present application provides a kind of cementing agent for solving the abnormal gelation and thickening time inversion of high temperature cement slurry and its preparation method.The raw material composition of the cementing agent includes 1-4 parts of aluminum salt,1-2 parts of sodium salt,1-2 parts of calcium salt,1-2 parts of magnesium salt and 1-6 parts of other materials by weight;Wherein, the other materials include one or a combination of several of zinc oxide, olivine, spodumene and lan crystal stone.The preparation method of the cementing agent is: according to weight, mix aluminum salt, sodium salt, calcium salt, magnesium salt and other materials uniformly to obtain the cementing agent.The cementing agent of the present application can solve the problems such as "bulge" of thickening curve, poor linear relationship between thickening time and dosage and temperature interval "inversion" caused by "core" of cement slurry at high temperature, at the same time, the cementing agent has no adverse effect on the rheological property, stability and fluid loss performance of cement slurry, and can improve the cementing quality.

Description

TECHNICAL FIELD

[0001] The present application relates to a setting regulator for solving abnormal gelation and reverse thickening time of high-temperature cement slurry and a preparation method thereof, and belongs to the field of drilling and cementing in oil and gas field development. BACKGROUND

[0002] In recent years, with the deepening of exploration and development, the number of deep and ultra-deep wells is increasing, and the well depth is increasing. The bottom hole temperature during cementing is also increasing. Under high temperature conditions, the hydration speed of cement is further accelerated, and a retarder is needed to adjust the hydration speed of cement and control the thickening time to ensure the safety of cementing operation. There are many types of high-temperature retarders, mainly including organic phosphoric acid (salt), borax (acid) compound, hydroxy phosphoric acid (salt) compound, etc., and AMPS polymer, among which polymer retarders are widely used. At present, under high temperature conditions, polymer retarders generally have some problems: ① In the temperature sensitive interval of 110-150℃, abnormal fluctuation phenomena such as "bulge" and "step" in the thickening line type mutation may occur, which threatens the safety of cementing operation and has a certain impact on the rheological properties of cement slurry; ② Under ultra-high temperature conditions, the linear relationship between the amount of retarder and the thickening time is poor, and even the amount of retarder and the thickening time show an exponential relationship, which leads to a sharp increase in the amount of additive to meet the safety conditions of cementing operation; ③ The thickening time appears "reversed" with the temperature interval, that is, under the same amount of retarder, with the increase of temperature, the thickening time cannot be shortened, but is prolonged.

[0003] At present, when the cement slurry shows abnormal thickening line type such as "bulge", early strength agent is often introduced, the dispersing agent is adjusted, and the types and amount of ultra-fine materials in the cement slurry system are adjusted to solve the problem, but the actual operation process often has a large amount of test work and the effect is not obvious. Some institutions have also developed corresponding retarders to prevent abnormal thickening line type and fluid loss additives. CN110204236A discloses a cementing regulator for oil well cement, which is prepared by compounding silicon powder, sodium silicate, sodium sulfate and borax in a certain proportion, which can ensure that the AMPS polymer fluid loss additive has a normal thickening curve in the temperature interval of 120-150℃, and has no adverse effect on the other comprehensive performance of the cement slurry system. CN106008844A discloses a strong inhibitory medium-high temperature oil well retarder and a preparation method thereof, which uses a graft copolymerization method to prepare a polymer medium-high temperature oil well cement retarder containing branched structure and strong inhibition, which can effectively inhibit the "core" and other abnormal gelation phenomena. The above-mentioned patents can solve the problem of abnormal thickening line type to some extent, but the applicable temperature range is insufficient, and the problem of "reversal" of thickening time, amount and temperature under ultra-high temperature conditions cannot be solved.

[0004] Therefore, it is necessary to develop a setting regulator to solve the problems of "bulge" of thickening curve, poor linear relationship between thickening time and dosage and "inverted" temperature range caused by "core" of cement slurry at high temperature. SUMMARY

[0005] To solve the above technical problems, the present application aims to provide a setting regulator for solving abnormal cementing and inverted thickening time of cement slurry at high temperature and a preparation method thereof. The setting regulator provided by the present application can solve the problems of "bulge" of thickening curve, poor linear relationship between thickening time and dosage and "inverted" temperature range caused by "core" of cement slurry at high temperature.

[0006] To achieve the above-mentioned purpose, the present application provides a setting regulator for solving abnormal cementing and inverted thickening time of cement slurry at high temperature, which comprises, in parts by weight, 1-4 parts of aluminum salt, 1-2 parts of sodium salt, 1-2 parts of calcium salt, 1-2 parts of magnesium salt and 1-6 parts of other materials; wherein the other materials include one or a combination of several of zinc oxide, olivine, spodumene and lanxinite.

[0007] In the above setting regulator, preferably, the weight ratio of the aluminum salt, the sodium salt, the calcium salt, the magnesium salt and the other materials is (2-3):(1-2):(1-2):(1-2):(1-2).

[0008] In the above setting regulator, preferably, the aluminum salt includes two of aluminum nitrate, aluminum chloride, aluminum sulfide, aluminum silicate and basic aluminum silicate sulfate; the first aluminum salt is one of aluminum nitrate, aluminum chloride and aluminum sulfide, and the second aluminum salt is one of aluminum silicate and basic aluminum silicate sulfate. More preferably, the weight ratio of the first aluminum salt to the second aluminum salt is (1-1.5):1.

[0009] In the above setting regulator, preferably, the sodium salt includes two of sodium chloride, sodium fluoride, sodium oxalate, sodium formate, sodium nitrate, sodium metasilicate, sodium fluosilicate, sodium chlorate and sodium bisulfite; the first sodium salt is one of sodium chloride, sodium fluoride, sodium oxalate and sodium formate, and the second sodium salt is one of sodium nitrate, sodium metasilicate, sodium fluosilicate, sodium chlorate and sodium bisulfite. More preferably, the weight ratio of the first sodium salt to the second sodium salt is (2-4):1. Even more preferably, the weight ratio of the first sodium salt to the second sodium salt is (2-3):1.

[0010] In the above setting regulator, preferably, the calcium salt includes one or a combination of several of calcium sulfate, calcium formate, calcium hydrogen phosphate and calcium propionate.

[0011] In the above-mentioned coagulation controller, preferably, the magnesium salt comprises two of basic magnesium sulfate, magnesium carbonate, magnesium oxide hexahydrate, magnesium chloride and magnesium oxide, etc.; the first magnesium salt is one of basic magnesium sulfate, magnesium carbonate and magnesium oxide hexahydrate, and the second magnesium salt is one of magnesium chloride and magnesium oxide. More preferably, the weight ratio of the first magnesium salt to the second magnesium salt is (2-4):1. Particularly preferably, the weight ratio of the first magnesium salt to the second magnesium salt is (2-3):1.

[0012] In the above-mentioned coagulation controller, preferably, the other material comprises two of zinc oxide, olivine, spodumene and lanthanite, etc.; the first other material is one of zinc oxide and olivine, and the second other material is one of spodumene and lanthanite. More preferably, the weight ratio of the first other material to the second other material is (2-3):1. Particularly preferably, the weight ratio of the first other material to the second other material is 2:1.

[0013] The second aspect of the present application provides a preparation method of the above-mentioned coagulation controller for solving abnormal gelation and reverse thickening time of high-temperature cement slurry, which comprises the following steps: uniformly mixing the aluminum salt, the sodium salt, the calcium salt, the magnesium salt and the other material according to the weight parts to obtain the coagulation controller for solving abnormal gelation and reverse thickening time of high-temperature cement slurry.

[0014] In the above-mentioned preparation method, the mixing can be carried out in a conventional mixing device in the field.

[0015] The third aspect of the present application provides a cement slurry system containing the above-mentioned coagulation controller for solving abnormal gelation and reverse thickening time of high-temperature cement slurry.

[0016] According to the specific embodiment of the present application, preferentially, the raw material composition of the cement slurry system comprises, in weight parts: 100 parts of cement, 0.5-4 parts of the coagulation controller, 25-50 parts of reinforcing material, 0.5-4 parts of retarder, 1-6 parts of fluid loss additive, 0.3-1.5 parts of dispersant, 0.5-3 parts of suspension stabilizer, 0.1-1 part of defoaming agent, and 44-100 parts of water.

[0017] In the above-mentioned cement slurry system, the cement can comprise one of G-grade oil well cement, such as Ji Hua G-grade, Hua You G-grade, Sheng Wei G-grade and Meng Cheng G-grade, etc.

[0018] In the above-mentioned cement slurry system, the reinforcing material can be a reinforcing material commonly used in the field of cement slurry system, such as but not limited to reinforcing material DRB-1S, high-temperature reinforcing material DRB-2S, etc.

[0019] In the cement slurry system, the retarder can be a retarder commonly used in the cement slurry system in the art, including an acrylamide polymer type retarder and / or a 2-acrylamide-2-methylpropane sulfonic acid polymer type retarder, etc.

[0020] In the cement slurry system, the fluid loss additive can be a fluid loss additive commonly used in the cement slurry system in the art, including an acrylamide polymer type fluid loss additive, etc.

[0021] In the cement slurry system, the dispersant can be a dispersant commonly used in the cement slurry system in the art. The dispersant can include one or a combination of several of an aldehyde ketone polycondensate type dispersant, a polystyrene sulfonate type dispersant, and a polycarboxylic acid type dispersant, etc.

[0022] In the cement slurry system, the suspension stabilizer can be a suspension stabilizer commonly used in the cement slurry system in the art, such as but not limited to suspension stabilizer DRK-3S, etc.

[0023] In the cement slurry system, the defoaming agent can be a defoaming agent commonly used in the cement slurry system in the art. The defoaming agent can include one of an organic ester, a polyoxypropylene glycerol ether, and a polydimethylsiloxane, etc.

[0024] According to the specific embodiments of the present application, the preparation method of the cement slurry system can be a conventional preparation method in the art, for example, the raw materials are respectively dry mixed, wet mixed, and then the dry mixed material and the wet mixed material are uniformly mixed, so that the cement slurry system is prepared.

[0025] The present application provides a setting regulator for solving abnormal gelation and thickening time inversion of high-temperature cement slurry, a preparation method thereof, and a cement slurry system containing the setting regulator. The setting regulator has an applicable temperature of 90-220℃; it can synergistically act with a polymer type retarder at high temperature, and can solve the problems of "bulging" of thickening curve, poor linear relationship between thickening time and dosage, and temperature interval "inversion", etc. caused by "core" of cement slurry at high temperature; at the same time, the setting regulator has no adverse effect on the conventional performances of cement slurry, such as rheological property, stability, and fluid loss performance, etc.; the setting regulator can ensure the safety of high-temperature deep well cementing construction, improve the cementing quality, and further ensure the efficient development of deep oil and gas resources. DETAILED DESCRIPTION

[0026] In order to have a clearer understanding of the technical features, objectives and beneficial effects of the present application, the technical solutions of the present application are described in detail as follows, but it should not be understood as a limitation on the implementable scope of the present application.

[0027] The experiment was carried out according to the standard GB / T 19139-2012 "Oil well cement test method", and the thickening performance, fluidity, API fluid loss, and sedimentation stability of the cement slurry system were evaluated. The main experimental instruments include: 30-60 type V-shaped edge stirrer, 8240 type high temperature and high pressure thickening instrument, and products of CHANDLER company.

[0028] In the following comparative examples and examples, the raw materials used include:

[0029] The oil well cement is high sulfate-resistant type (HSR) G-grade oil well cement produced by Jiuhua Special Cement Co., Ltd.;

[0030] The strength stabilizer is high-purity quartz sand with a mesh size of 1500;

[0031] The reinforcing material DRB-1S is produced by China Petroleum Engineering Technology Research Institute Co., Ltd.;

[0032] The suspension stabilizer DRK-3S is produced by China Petroleum Engineering Technology Research Institute Co., Ltd.;

[0033] The retarder is acrylamide polymer type retarder DRH-2L produced by China Petroleum Engineering Technology Research Institute Co., Ltd.;

[0034] The fluid loss reducer DRF-1S is produced by China Petroleum Engineering Technology Research Institute Co., Ltd.;

[0035] The dispersant is aldehyde ketone polycondensate type dispersant DRS-1S produced by China Petroleum Engineering Technology Research Institute Co., Ltd.;

[0036] The defoaming agent is phosphoric acid tributyl ester commonly used in the art;

[0037] The experimental water is distilled water.

[0038] Comparative Example 1

[0039] This comparative example provides a cement slurry system, the raw material composition of which includes, by weight: 100 parts of G-grade oil well cement, 35 parts of strength stabilizer, 2 parts of retarder, 3 parts of fluid loss reducer, 1 part of dispersant, 1 part of suspension stabilizer, 0.2 parts of defoaming agent, and 50 parts of water.

[0040] The preparation method of the cement slurry system is a conventional preparation method in the art, for example, the raw materials are dry mixed and wet mixed respectively, then the dry mixed material and the wet mixed material are mixed uniformly, and the cement slurry system is prepared.

[0041] The density of the cement slurry system is 1.90 g / cm 3 , the experimental cycle temperature is 140℃, and the experimental results are shown in Table 1.

[0042] Comparative Example 2

[0043] The cement slurry system of this comparative example is prepared by the same method as Comparative Example 1, and its raw material composition includes, by weight parts: 100 parts of G-grade oil well cement, 35 parts of reinforcing material, 2.2 parts of retarder, 3 parts of fluid loss additive, 1 part of dispersant, 1 part of suspension stabilizer, 0.2 part of defoaming agent, and 50 parts of water.

[0044] The density of the cement slurry system is 1.90 g / cm 3 The experimental cycle temperature is 140℃, and the experimental results are shown in Table 1.

[0045] Comparative Example 3

[0046] The cement slurry system of this comparative example is prepared by the same method as Comparative Example 1, and its raw material composition includes, by weight parts: 100 parts of G-grade oil well cement, 35 parts of reinforcing material, 2.4 parts of retarder, 3 parts of fluid loss additive, 1 part of dispersant, 1 part of suspension stabilizer, 0.2 part of defoaming agent, and 49.5 parts of water.

[0047] The density of the cement slurry system is 1.90 g / cm 3 The experimental cycle temperature is 140℃, and the experimental results are shown in Table 1.

[0048] Comparative Example 4

[0049] The cement slurry system of this comparative example is prepared by the same method as Comparative Example 1, and its raw material composition includes, by weight parts: 100 parts of G-grade oil well cement, 35 parts of reinforcing material, 2.4 parts of retarder, 3 parts of fluid loss additive, 1 part of dispersant, 1 part of suspension stabilizer, 0.2 part of defoaming agent, and 49.5 parts of water.

[0050] The density of the cement slurry system is 1.90 g / cm 3 The experimental cycle temperature is 140℃, and the experimental results are shown in Table 1.

[0051] Comparative Example 5

[0052] The cement slurry system of this comparative example is prepared by the same method as Comparative Example 1, and its raw material composition includes, by weight parts: 100 parts of G-grade oil well cement, 35 parts of reinforcing material, 2.4 parts of retarder, 3 parts of fluid loss additive, 1 part of dispersant, 1 part of suspension stabilizer, 0.2 part of defoaming agent, and 49.5 parts of water.

[0053] The density of the cement slurry system is 1.90 g / cm 3 The experimental cycle temperature is 140℃, and the experimental results are shown in Table 1.

[0054] Comparative Example 6

[0055] The cement slurry system provided by the present comparative example comprises, in parts by weight, 100 parts of G-grade oil well cement, 40 parts of reinforcing material, 3 parts of retarder, 2 parts of setting time regulator, 4 parts of fluid loss additive, 1 part of dispersing agent, 1.5 parts of suspension stabilizer, 0.2 parts of defoaming agent, and 52 parts of water.

[0056] The setting time regulator comprises, in parts by weight, 2 parts of aluminum salt (aluminum nitrate: aluminum chlorate = 1:1), 2 parts of sodium salt (sodium fluoride: sodium formate = 2:1), 1 part of calcium salt (calcium sulfate), and 2 parts of magnesium salt (magnesium sulfate: magnesium oxide = 2:1). The aluminum salt, the sodium salt, and the magnesium salt are all compounded in a weight ratio. The setting time regulator is prepared by the following steps: mixing the aluminum salt, the sodium salt, the calcium salt, and the magnesium salt in a mixing device according to the weight parts to obtain the setting time regulator.

[0057] The cement slurry system is prepared by the same method as in Comparative Example 1.

[0058] The density of the cement slurry system is 1.90 g / cm 3 The experimental cycle temperature is 180°C, and the experimental results are shown in Table 1.

[0059] Comparative Example 7

[0060] The cement slurry system provided by the present comparative example comprises, in parts by weight, 100 parts of G-grade oil well cement, 40 parts of reinforcing material, 3 parts of retarder, 2 parts of setting time regulator, 4 parts of fluid loss additive, 1 part of dispersing agent, 1.5 parts of suspension stabilizer, 0.2 parts of defoaming agent, and 52 parts of water.

[0061] The setting time regulator comprises, in parts by weight, 2 parts of aluminum salt (aluminum nitrate), 2 parts of sodium salt (sodium fluoride), 1 part of calcium salt (calcium sulfate), 2 parts of magnesium salt (magnesium sulfate), and 1 part of other material (olivine). The setting time regulator is prepared by the following steps: mixing the aluminum salt, the sodium salt, the calcium salt, and the magnesium salt in a mixing device according to the weight parts to obtain the setting time regulator.

[0062] The cement slurry system is prepared by the same method as in Comparative Example 1.

[0063] The density of the cement slurry system is 1.90 g / cm 3 The experimental cycle temperature is 180°C, and the experimental results are shown in Table 1.

[0064] Comparative Example 8

[0065] The comparative example 1 provides a cement slurry system, whose raw material composition includes, in parts by weight: 100 parts of G-grade oil well cement, 40 parts of reinforcing material, 3 parts of retarder, 2 parts of setting time controller, 4 parts of fluid loss additive, 1 part of dispersing agent, 1.5 parts of suspension stabilizer, 0.2 parts of defoaming agent, and 52 parts of water.

[0066] The setting time controller is prepared by the following steps: the aluminum salt, the sodium salt, the calcium salt, the magnesium salt and the other material are mixed uniformly in a mixing device according to the weight parts to obtain the setting time controller.

[0067] The cement slurry system is prepared by the same method as the comparative example 1.

[0068] The density of the cement slurry system is 1.90 g / cm 3 The experimental cycle temperature is 180℃, and the experimental results are shown in Table 1.

[0069] Example 1

[0070] The setting time controller is prepared by the following steps: the aluminum salt, the sodium salt, the calcium salt, the magnesium salt and the other material are mixed uniformly in a mixing device according to the weight parts to obtain the setting time controller.

[0071] The setting time controller is prepared by the following steps: the aluminum salt, the sodium salt, the calcium salt, the magnesium salt and the other material are mixed uniformly in a mixing device according to the weight parts to obtain the setting time controller.

[0072] The cement slurry system is prepared by the same method as the comparative example 1.

[0073] The density of the cement slurry system is 1.90 g / cm 3 The experimental cycle temperature is 140℃, and the experimental results are shown in Table 2.

[0074] Example 2

[0075] The cement slurry system of the present example comprises, by weight parts, 100 parts of G-grade oil well cement, 35 parts of reinforcing material, 2.2 parts of retarder, 2 parts of the setting time adjusting agent of Example 1, 3 parts of fluid loss additive, 1 part of dispersing agent, 1 part of suspension stabilizer, 0.2 part of defoaming agent, and 50.5 parts of water. The cement slurry system is prepared in the same manner as Comparative Example 1.

[0076] The density of the cement slurry system is 1.90 g / cm 3 The experimental cycle temperature is 140°C, and the experimental results are shown in Table 2.

[0077] Example 3

[0078] The cement slurry system of the present example comprises, by weight parts, 100 parts of G-grade oil well cement, 35 parts of reinforcing material, 2.4 parts of retarder, 2 parts of the setting time adjusting agent of Example 1, 3 parts of fluid loss additive, 1 part of dispersing agent, 1 part of suspension stabilizer, 0.2 part of defoaming agent, and 50.5 parts of water. The cement slurry system is prepared in the same manner as Comparative Example 1.

[0079] The density of the cement slurry system is 1.90 g / cm 3 The experimental cycle temperature is 140°C, and the experimental results are shown in Table 2.

[0080] Example 4

[0081] The cement slurry system of the present example comprises, by weight parts, 100 parts of G-grade oil well cement, 35 parts of reinforcing material, 2.6 parts of retarder, 2 parts of the setting time adjusting agent of Example 1, 3 parts of fluid loss additive, 1 part of dispersing agent, 1 part of suspension stabilizer, 0.2 part of defoaming agent, and 50 parts of water. The cement slurry system is prepared in the same manner as Comparative Example 1.

[0082] The density of the cement slurry system is 1.90 g / cm 3 The experimental cycle temperature is 140°C, and the experimental results are shown in Table 2.

[0083] Example 5

[0084] The setting time adjusting agent of the present example comprises, by weight parts, 2 parts of aluminum salt (aluminum chloride: aluminum silicate = 1.5:1), 2 parts of sodium salt (sodium chloride: sodium nitrate = 2.5:1), 1 part of calcium salt (calcium sulfate), 2 parts of magnesium salt (basic magnesium sulfate: magnesium oxide = 3:1), and 1 part of other materials (zinc oxide: spodumene = 2:1). The aluminum salt, sodium salt, magnesium salt, and other materials are each compounded with two kinds of materials in a weight ratio of 1:1. The setting time adjusting agent is prepared in the same manner as Example 1.

[0085] The cement slurry system of the present example is prepared by using 100 parts of G-grade oil well cement, 35 parts of reinforcing material, 2.6 parts of retarder, 2 parts of the setting time adjusting agent of the present example, 3 parts of fluid loss additive, 1 part of dispersing agent, 1 part of suspension stabilizer, 0.2 part of defoaming agent, and 50 parts of water.

[0086] The density of the cement slurry system is 1.90 g / cm 3 The experimental cycle temperature is 150℃, and the experimental results are shown in Table 2.

[0087] Example 6

[0088] The setting time adjusting agent of the present example is prepared by using 2 parts of aluminum salt (aluminum nitrate: aluminum silicate = 1.5:1), 2 parts of sodium salt (sodium fluoride: sodium nitrate = 2.5:1), 1 part of calcium salt (calcium formate), 2 parts of magnesium salt (magnesium carbonate: magnesium oxide = 3:1), and 1 part of other materials (zinc oxide: spodumene = 2:1). The aluminum salt, sodium salt, magnesium salt, and other materials are all compounded by two kinds, and the compounding ratio is weight ratio. The preparation steps of the setting time adjusting agent are the same as those of Example 1.

[0089] The cement slurry system of the present example is prepared by using 100 parts of G-grade oil well cement, 35 parts of reinforcing material, 2.6 parts of retarder, 2 parts of the setting time adjusting agent of the present example, 3 parts of fluid loss additive, 1 part of dispersing agent, 1 part of suspension stabilizer, 0.2 part of defoaming agent, and 50 parts of water.

[0090] The density of the cement slurry system is 1.90 g / cm 3 The experimental cycle temperature is 160℃, and the experimental results are shown in Table 2.

[0091] Example 7

[0092] The setting time adjusting agent of the present example is prepared by using 3 parts of aluminum salt (aluminum sulfide: aluminum silicate = 1:1), 1 part of sodium salt (sodium fluoride: sodium nitrate = 3:1), 2 parts of calcium salt (calcium propionate), 2 parts of magnesium salt (magnesium oxide hexahydrate: magnesium chloride = 3:1), and 2 parts of other materials (zinc oxide: spodumene = 2:1). The aluminum salt, sodium salt, magnesium salt, and other materials are all compounded by two kinds, and the compounding ratio is weight ratio. The preparation steps of the setting time adjusting agent are the same as those of Example 1.

[0093] The cement slurry system of the present example is prepared by using 100 parts of G-grade oil well cement, 40 parts of reinforcing material, 3 parts of retarder, 2 parts of the setting time adjusting agent of the present example, 4 parts of fluid loss additive, 1 part of dispersing agent, 1.5 parts of suspension stabilizer, 0.2 parts of defoaming agent, and 52 parts of water.

[0094] The density of the cement slurry system is 1.90 g / cm 3 The experimental cycle temperature is 180℃, and the experimental results are shown in Table 2.

[0095] Example 8

[0096] The setting time adjusting agent of the present example is prepared by using 3 parts of aluminum salt (aluminum sulfide: aluminum silicate = 1:1), 1 part of sodium salt (sodium fluoride: sodium nitrate = 3:1), 2 parts of calcium salt (calcium sulfate), 2 parts of magnesium salt (magnesium oxide hexahydrate: magnesium chloride = 3:1), and 2 parts of other materials (zinc oxide: spodumene = 2:1). The aluminum salt, sodium salt, magnesium salt, and other materials are all compounded in two ways, and the compounding ratio is weight ratio. The preparation steps of the setting time adjusting agent are the same as those of Example 1.

[0097] The cement slurry system of the present example is prepared by using 100 parts of G-grade oil well cement, 40 parts of reinforcing material, 3 parts of retarder, 2 parts of the setting time adjusting agent of the present example, 4 parts of fluid loss additive, 1 part of dispersing agent, 1.5 parts of suspension stabilizer, 0.2 parts of defoaming agent, and 52 parts of water.

[0098] The density of the cement slurry system is 1.90 g / cm 3 The experimental cycle temperature is 200℃, and the experimental results are shown in Table 2.

[0099] Table 1 Experimental results of comparative examples

[0100]

[0101] Table 2 Experimental results of examples

[0102]

[0103]

[0104] As shown in Table 2, the flow degree of all examples is greater than 22 cm, the API fluid loss is less than 50 mL, and the free water content is 0, which meets the requirements of well cementing construction. The thickening performance test shows that the thickening time of all examples is adjustable, and the thickening curve is normal without abnormal gelation phenomenon such as "bulging".

[0105] From the data of Comparative Example 1, Comparative Example 2 and Comparative Example 3, under the same experimental conditions, when the amount of the retarder is increased from 2 parts to 2.2 parts (Comparative Example 1 and Comparative Example 2), the fluidity of the cement slurry, the API fluid loss and the settlement stability do not change obviously, the thickening time is increased from 209 min to 216 min, the increase is not obvious, and the thickening curve appears the "bulging" phenomenon. When the amount of the retarder is increased from 2.2 parts to 2.4 parts (Comparative Example 2 and Comparative Example 3), the thickening time is increased from 216 min to 263 min, the increase is 47 min. From Comparative Example 1, Comparative Example 2 and Comparative Example 3, under the condition that the amount of the retarder is increased uniformly, the increase of the thickening time is obviously disproportionate, the linear relationship is poor, and the "bulging" phenomenon appears.

[0106] From the data of Comparative Example 1 and Comparative Example 4, under the same amount of the retarder, when the experimental temperature is increased from 140℃ to 150℃, the fluidity of the cement slurry, the API fluid loss and the settlement stability do not change obviously, but the thickening time is increased from 209 min to 241 min, that is, with the increase of the temperature, the thickening time is not shortened, but is prolonged, and the "inverted" phenomenon of the thickening time and the temperature appears.

[0107] From the data of Comparative Example 5, when the circulating temperature reaches 180℃, the "bulging" phenomenon of the thickening curve appears. From the data of Comparative Example 6, 2 parts of the setting regulator are introduced into the cement slurry formula, but the formula composition of the setting regulator is not completely consistent with the present application, the setting regulator does not contain other materials in the present application, and the "bulging" phenomenon of the thickening curve cannot be eliminated. From the data of Comparative Example 7 and Comparative Example 8, 2 parts of the setting regulator are introduced into the cement slurry formula, but the formula composition of the setting regulator is not completely consistent with the present application, the aluminum salt, the sodium salt, the magnesium salt and other materials are not compounded with two kinds, or the two kinds of compounding are different from the present application, the "bulging" phenomenon of the thickening curve cannot be eliminated, and the "stepped" phenomenon appears.

[0108] In Comparative Example 1, 2 parts of the setting regulator are introduced to obtain Example 1, under the same experimental conditions, the fluidity of the cement slurry, the API fluid loss and the settlement stability of Example 1 do not change obviously, the thickening curve of Example 1 is normal, and the "bulging" phenomenon does not appear.

[0109] In the comparative example 2, 2 parts of the coagulation controller are introduced to obtain the example 2, under the same experimental conditions, the thickening time is prolonged from 213 min to 242 min, increased by 29 min. On the basis of the example 2, the amount of the retarder is increased from 2.2 parts to 2.4 parts to obtain the example 3, and the thickening time of the example 3 is 274 min, increased by 32 min. On the basis of the example 3, the amount of the retarder is increased from 2.4 parts to 2.6 parts to obtain the example 4, and the thickening time is 301 min, increased by 27 min. From the comparative example 2, the example 2, the example 3 and the example 4, it can be known that after introducing 2 parts of the coagulation controller, with the increase of the retarder, the thickening time is gradually prolonged, and the amount and the thickening time have a good linear relationship.

[0110] The thickening time of the example 4 is 301 min, the thickening time of the example 5 is 264 min, and the thickening time of the example 6 is 177 min. From the example 4, the example 5 and the example 6, it can be known that under the same amount of the retarder, with the increase of the temperature, the thickening time of the cement slurry is gradually shortened, and the phenomenon of the "inverted hanging" of the thickening time and the temperature does not appear, and the thickening curve is normal.

[0111] From the example 7 and the example 8, it can be known that after introducing 2 parts of the coagulation controller, the thickening curve of the cement slurry is normal, and the "bulging" phenomenon does not appear.

[0112] Therefore, the application provides a coagulation controller for solving the abnormal gelation of the high-temperature cement slurry and the inverted hanging of the thickening time and a preparation method thereof. The application has the following advantages. The application provides a coagulation controller for solving the abnormal gelation of the high-temperature cement slurry and the inverted hanging of the thickening time and a preparation method thereof. The application has the following advantages.

Claims

1. A setting regulator for resolving abnormal setting and inverted thickening time in high-temperature cement slurry, comprising, by weight, the following raw materials: 1-4 parts aluminum salt, 1-2 parts sodium salt, 1-2 parts calcium salt, 1-2 parts magnesium salt and 1-6 parts other materials; The aluminum salt includes two of aluminum nitrate, aluminum chloride, aluminum sulfide, aluminum silicate, and basic aluminum silicate sulfate; the first aluminum salt is one of aluminum nitrate, aluminum chloride, and aluminum sulfide, and the second aluminum salt is one of aluminum silicate and basic aluminum silicate sulfate, and the weight ratio of the first aluminum salt to the second aluminum salt is (1~1.5):

1. The sodium salt includes two of the following: sodium chloride, sodium fluoride, sodium oxalate, sodium formate, sodium nitrate, sodium metasilicate, sodium fluorosilicate, sodium chlorate, and sodium bisulfite; the first sodium salt is one of sodium chloride, sodium fluoride, sodium oxalate, and sodium formate, and the second sodium salt is one of sodium nitrate, sodium metasilicate, sodium fluorosilicate, sodium chlorate, and sodium bisulfite, wherein the weight ratio of the first sodium salt to the second sodium salt is (2~4):1; The calcium salt includes one or a combination of calcium sulfate, calcium formate, calcium hydrogen phosphate, and calcium propionate; The magnesium salt includes two of the following: basic magnesium sulfate, magnesium carbonate, magnesium oxide hexahydrate, magnesium chloride, and magnesium oxide; the first magnesium salt is one of basic magnesium sulfate, magnesium carbonate, and magnesium oxide hexahydrate, and the second magnesium salt is one of magnesium chloride and magnesium oxide; the weight ratio of the first magnesium salt to the second magnesium salt is (2~4):

1. The other materials include two of zinc oxide, olivine, spodumene, and kyanite; the first other material is one of zinc oxide and olivine, and the second other material is one of spodumene and kyanite, with a weight ratio of (2~3):1 between the first other material and the second other material.

2. A method for preparing the setting regulator according to claim 1, which solves the problem of abnormal setting and inverted thickening time in high-temperature cement slurry, comprising the following steps: The aluminum salt, sodium salt, calcium salt, magnesium salt, and other materials are mixed evenly according to the stated weight proportions to obtain the setting regulator that solves the problem of abnormal gelation and inverted thickening time in high-temperature cement slurry.

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