CN114058346B - Calcium silicate hydrate suspension and preparation method and application thereof - Google Patents
Calcium silicate hydrate suspension and preparation method and application thereof Download PDFInfo
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- CN114058346B CN114058346B CN202010759805.XA CN202010759805A CN114058346B CN 114058346 B CN114058346 B CN 114058346B CN 202010759805 A CN202010759805 A CN 202010759805A CN 114058346 B CN114058346 B CN 114058346B
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/24—Alkaline-earth metal silicates
Abstract
The invention provides a calcium silicate hydrate suspension, a preparation method and application thereof. The calcium silicate hydrate suspension comprises a product of a reaction of a calcium compound, an alkoxysilane and water under the presence of a catalyst selected from amantadine hydrochloride and/or urotropin. The invention starts from a microscopic nano structure, synthesizes and screens a target CSH product with more single component and more regular structure. A granular CSH is obtained, which can obviously enhance the early strength of cement and does not accelerate the setting.
Description
Technical Field
The invention belongs to the technical field of well cementation, and particularly relates to a calcium silicate hydrate suspension, and a preparation method and application thereof.
Background
The main raw materials for cementing oil and gas wells are oil well cement, cement additives and admixtures. Over the years, along with the continuous development of the petroleum industry, the development difficulty of petroleum and natural gas is higher and higher, as the exploration and drilling areas of oil and gas wells are wider and deeper, and the development of deep-sea oil and gas exploration, the development of unconventional oil and gas and the like are added, the well cementation environment is worse and worse (high-temperature, high-pressure, ultra-low pressure loss, deep water, high corrosion environment and the like), the well cementation process is more and more complex, and the requirement on the well cementation technology is higher and higher. Advances in well cementing technology have also raised new requirements for the performance of the oil well cement, cement admixtures, and admixtures used. Therefore, oil well cement, cement admixtures and admixture are continuously developed and perfected, and the performance thereof is continuously improved along with the requirements of well cementation technology and technology.
The oil well cement belongs to silicate cement, which is cement taking silicate cement clinker as a basic material and is specially used for cementing oil and gas wells. It is produced according to certain physical and chemical performance standards as dictated by the conditions of use. The main mineral component of oil well cement is calcium silicate, the content of calcium silicate in cement can be up to 75%, and the calcium silicate reacts with water to form hydrated calcium silicate, which plays an important role in the performance of cement paste and set cement.
Disclosure of Invention
In order to solve the technical problems, the invention screens out an optimal structure with induced assembly characteristics on cement hydration products by synthesizing hydrated calcium silicate with a specific structure, and improves the comprehensive performance of cement paste and set cement.
The invention provides a calcium silicate hydrate suspension, which comprises calcium silicate hydrate and a catalyst, wherein the catalyst is amantadine hydrochloride and/or urotropine.
According to some embodiments of the invention, the catalyst is amantadine hydrochloride and urotropin.
According to some embodiments of the invention, the mass ratio of amantadine hydrochloride and urotropin is 0.1 to 10, such as 0.3.
According to some embodiments of the invention, the mass ratio of amantadine hydrochloride and urotropin is 0.1 to 1.
According to some embodiments of the invention, the mass ratio of amantadine hydrochloride and urotropin is 0.5.
According to some embodiments of the invention, the calcium silicate hydrate has an average particle size of 100 to 300nm.
According to some embodiments of the invention, the calcium silicate hydrate is present in the suspension in an amount of 8 to 20% by mass.
According to some embodiments of the invention, the suspension of calcium silicate hydrate comprises the reaction product of a calcium compound, an alkoxysilane and water in the presence of a catalyst selected from amantadine hydrochloride and/or urotropin.
According to some embodiments of the invention, the calcium compound is selected from one or more of calcium nitrate, calcium chloride and calcium oxide.
According to some embodiments of the invention, the alkoxysilane is selected from C1-C6 alkoxysilanes.
According to some embodiments of the invention, the alkoxysilane is selected from one or more of tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, and tetra-n-butoxysilane.
According to some embodiments of the invention, the molar ratio of the calcium compound to the alkoxysilane, based on the molar ratio of calcium to silicon, is from 0.8 to 1.2.
According to some embodiments of the invention, the molar ratio of the calcium compound to the alkoxysilane, based on the molar ratio of calcium to silicon, is 1.
According to some embodiments of the invention, the ratio of the calcium compound to water is 1.
According to some embodiments of the invention, the catalyst is added in an amount of 0.005 to 0.05wt%, such as 0.01wt%, 0.015wt%, 0.025wt%, 0.030wt%, 0.035wt%, 0.045wt%, and any value therebetween, based on the total amount of the calcium compound, alkoxysilane, and water.
According to some embodiments of the invention, the catalyst is added in an amount of 0.02 to 0.04wt% based on the total amount of the calcium compound, alkoxysilane and water.
According to some embodiments of the invention, the temperature of the reaction is between 30 and 70 ℃, preferably between 40 and 60 ℃.
According to some embodiments of the invention, the reaction time is 2 to 10h, preferably 4 to 8h.
In a second aspect of the present invention, there is provided a process for producing a calcium silicate hydrate suspension comprising reacting a calcium compound, an alkoxysilane and water in the presence of a catalyst selected from amantadine hydrochloride and/or urotropin.
According to some embodiments of the invention, the catalyst is amantadine hydrochloride and urotropin.
According to some embodiments of the present invention, the mass ratio of amantadine hydrochloride and urotropine is from 0.1 to 10, such as from 0.3.
According to some embodiments of the invention, the mass ratio of amantadine hydrochloride and urotropin is 0.1 to 1.
According to some embodiments of the invention, the mass ratio of amantadine hydrochloride and urotropin is 0.5.
According to some embodiments of the invention, the calcium compound is selected from one or more of calcium nitrate, calcium chloride and calcium oxide.
According to some embodiments of the invention, the alkoxysilane is selected from C1-C6 alkoxysilanes.
According to some embodiments of the invention, the alkoxysilane is selected from one or more of tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, and tetra-n-butoxysilane.
According to some embodiments of the invention, the molar ratio of the calcium compound to the alkoxysilane, expressed as a molar ratio of calcium to silicon, is from 0.8 to 1.2, for example 0.9.
According to some embodiments of the invention, the molar ratio of the calcium compound to the alkoxysilane, based on the molar ratio of calcium to silicon, is 1.
According to some embodiments of the invention, the mass ratio of the calcium compound to water is 1.
According to some embodiments of the invention, the mass ratio of the calcium compound to water is 1.
In the invention, the calcium compound and the water are in the above-defined proportion range, and the final product concentration of the calcium silicate hydrate suspension is between 20 and 8 percent. When the product concentration is more than 20%, the fluidity is poor, the use is not facilitated, in addition, the crystal form control of the product is not facilitated due to the higher concentration, and the good crystal form is very important for the product performance. On the other hand, the concentration of 8% or less is too low, and the significance in the practical process is not great.
According to some embodiments of the invention, the catalyst is added in an amount of 0.005 to 0.05wt%, such as 0.01wt%, 0.015wt%, 0.025wt%, 0.030wt%, 0.035wt%, 0.045wt%, and any value therebetween, based on the total amount of the calcium compound, alkoxysilane, and water.
According to some embodiments of the invention, the catalyst is added in an amount of 0.02 to 0.04wt% of the total amount of the calcium compound, alkoxysilane and water.
According to some embodiments of the invention, the temperature of the reaction is between 30 and 70 ℃.
According to some embodiments of the invention, the temperature of the reaction is between 40 and 60 ℃.
According to some embodiments of the invention, the reaction time is between 2 and 10h.
According to some embodiments of the invention, the reaction time is 4-8h.
In some advantageous embodiments of the invention, the Calcium Silicate Hydrate (CSH) material is prepared using a sedimentation process:
calcium nitrate tetrahydrate and tetraethoxysilane are used as raw materials. The method comprises the following specific steps: respectively weighing raw materials according to the stoichiometric ratio of 1-1 molar ratio of calcium to silicon, putting the raw materials into a reaction kettle, adding distilled water according to the mass ratio of water to solid being 10. The catalyst is from amantadine hydrochloride and/or urotropin.
The third aspect of the invention provides application of the calcium silicate hydrate suspension of the first aspect or the calcium silicate hydrate suspension prepared by the method of the second aspect in well cementation.
In a fourth aspect, the invention provides a well cementation cement slurry, which comprises the calcium silicate hydrate suspension of the first aspect or the calcium silicate hydrate suspension prepared by the method of the second aspect and cement.
According to some embodiments of the invention, the suspension of calcium silicate hydrate is present in an amount of 0.1 to 5% by mass, for example 1%, 1.5% or 3% by mass of the cement.
According to some embodiments of the invention, the suspension of calcium silicate hydrate is present in an amount of 0.5 to 2% by mass of the cement.
The invention starts from a microscopic nano structure, synthesizes and screens a target CSH product with more single component and more regular structure. The calcium silicate hydrate in the calcium silicate hydrate suspension is in a regular granular shape, has good suspension property, and is easy to disperse and carry in the using process. Compared with the prior art, the early strength of the cement is obviously enhanced, and the setting is not accelerated (the CSH crystal seed is used as the setting accelerator generally).
Drawings
FIG. 1 is an electron micrograph of a suspension of Synthesis example 3 of the present invention.
FIG. 2 is a graph showing the cement hydration heat release rate after adding sample JHG and sample Q \ R \ P in the example of the invention.
FIG. 3 is a graph showing the exotherm of cement hydration after adding samples JHG and Q \ R \ P in the example of the present invention.
FIG. 4 shows the addition of sample R \ P in the example according to the present invention 5 \Q 5 The subsequent cement hydration heat release rate curve chart.
FIG. 5 shows the addition of sample R \ P 5 \Q 5 Graph of the subsequent cement hydration exotherm.
FIG. 6 is a graph of the cement slurry hydration heat release rate after the addition of C-S-H seed crystals in the prior art.
FIG. 7 is a graph of the cement slurry hydration exotherm after the addition of C-S-H seeds in the prior art.
Detailed Description
For easy understanding of the present invention, the present invention will be described in detail with reference to examples, which are provided for illustrative purposes only and are not intended to limit the scope of the present invention.
The starting materials or components used in the present invention may be commercially or conventionally prepared unless otherwise specified.
Synthesis example 1
Respectively weighing raw materials of calcium nitrate tetrahydrate and tetraethoxysilane which are used as raw materials according to the stoichiometric ratio of calcium-silicon molar ratio of 1.
Synthesis example 2
The preparation method was the same as in synthesis example 1, except that three-ten-thousandth of urotropine catalyst was added to obtain a liquid CSH product R.
Synthesis example 3
The preparation method is the same as that of synthesis example 1, except that three-ten-thousandth of a catalyst mixed by amantadine hydrochloride and urotropin is added, wherein the mass ratio of the amantadine hydrochloride to the urotropin is 1.
Synthesis example 4
The preparation method is the same as that of synthesis example 3, except that the raw materials are respectively weighed according to the stoichiometric ratio of 1.5 calcium-silicon molar ratio.
Synthesis example 5
The preparation method is the same as that of synthesis example 3, except that the raw materials are respectively weighed according to the stoichiometric ratio of 0.5 calcium-silicon molar ratio.
Synthesis example 6
The preparation method was the same as in synthesis example 1, except that the catalyst added was triethanolamine to give a liquid CSH product DP.
Test example:
washing the products of synthesis examples 1-6 with distilled water, petroleum ether and absolute ethyl alcohol for 2-3 times, drying at 80 ℃ under vacuum condition to obtain calcium silicate hydrate, and testing the sample by adopting an electron microscope.
Comparative example 1 preparation of blank Cement grout (neat paste) and set Cement
100 parts by weight of oil well cement and 44 parts by weight of water were weighed. Placing water in a mixing container, rotating the stirrer at low speed (4000 + -200 rpm), adding the weighed cement within 15 seconds, covering the stirrer, and stirring at high speed (12000 + -500 rpm) for 35 seconds to obtain blank cement paste with density of 1.88g/cm 3 。
Pouring the blank cement paste into a curing module with the thickness of 4cm multiplied by 16cm, putting the curing module into a water bath with the temperature of 90 ℃ for curing for 24/72 hours, and taking out the solidified cement to obtain a blank cement stone module.
Comparative example 2: silica fume-added cement paste (silica fume paste) and set cement preparation
100 parts by weight of oil well cement, 35 parts by weight of silica powder (180 meshes) accounting for 35% of the weight of the cement, and 59.4 parts by weight of water are weighed. Placing water in a mixing container, rotating a stirrer at low speed (4000 +/-200 rpm), adding the weighed mixture of cement and silicon powder within 15 seconds, covering a cover of the stirrer, and continuously stirring at high speed (12000 +/-500 rpm) for 35 seconds to obtain cement paste with the density of 1.89g/cm 3 。
Pouring the cement paste into a curing module with the thickness of 4cm multiplied by 16cm, putting the curing module into a water bath with the temperature of 120 ℃ and the pressure of 20MPa for curing for 72 hours, and taking out the cured cement to obtain the silica-alumina cement module.
Examples 1 to 6: adding CSH (Q, R, P1, P2, DP) cement slurry and set cement to prepare (i.e. 2% Q, 2% R, 2% P, 2% P1, 2% P2, 2%
100 parts by weight of oil well cement, 42 parts by weight of water and 2 parts by weight of CSH liquid product are weighed out. Water and CSH liquid product were placed in a mixing vessel and the mixer was rotated at low speed (4000. + -. 200 rpm) and the weighed cement was added over 15 seconds, the mixer lid was closed and mixing continued at high speed (12000. + -. 500 rpm) for 35 seconds to produce the grout of examples 1-10 having a density of 1.88g/cm 3 。
And pouring the blank cement paste into a curing module with the length of 4cm multiplied by 16cm, putting the curing module into a water bath with the temperature of 90 ℃ for curing for 24/72 hours, and taking out the solidified cement to obtain a blank set cement module.
Example 7: preparation of Cement mortar and set with CSH (P) added (i.e. 0.5% P)
The procedure is as in comparative example 2, except that the amounts added are varied: 100 parts by weight of oil well cement, 43.5 parts by weight of water and 0.5 part by weight of CSH liquid product were weighed out.
Example 8: cement paste and set preparation with addition of CSH (P) (i.e. 1% P)
The procedure is as in comparative example 2, except that the amounts added are varied: 100 parts by weight of oil well cement, 43 parts by weight of water and 1 part by weight of CSH liquid product were weighed out.
Testing of compression strength of set cement
The compression strength of the cement block is tested by a German Toni compression and bending tester at room temperature of 25 ℃. The test results are shown in tables 1 and 2.
TABLE 1 Effect of 2% C-S-H addition on the compression Strength of set cement at 90 ℃
TABLE 2 Effect of P on Cement compressive Strength at 120 ℃
As can be seen from the results in table 1: the spherical C-S-H crystals Q, R and P obviously increase the strength of the set cement. And (4) investigating the influence of adding silica powder and changing the adding amount of the sample on the strength of the set cement at high temperature by using the sample P. The results are shown in table 2, the sample P still significantly increases the strength of the set cement under the high-temperature silica powder system, and the strength is significantly increased as P increases.
Cement hydration heat test
The cement hydration heat was tested at room temperature 25 ℃ using a German Toni hydration heat tester. The test results are shown in FIGS. 2-5.
Sample JHG (fig. 2, 3): weigh 2 grams of Jiahua G-grade cement and weigh 5mL of distilled water.
Sample Q \ P \ R (FIGS. 2-5): weighing 2G of Jiahua G-grade cement, weighing 5mL of distilled water, and respectively weighing 0.02G of Q, P or R
Sample P 5 \Q 5 (FIG. 4, FIG. 5): weighing 2G of Jiahua G-grade cement, weighing 5mL of distilled water, and respectively weighing 0.05G of P or Q.
In the prior art, reference is made to the law of the influence of C-S-H seeds on cement hydration heat and hydration rate (figures 6, 7) (jongying, military release, zhao amber. Study of nano-sized hydrated calcium silicate seeds as well cement set accelerator [ J ]. Drilling and completion fluids, 2015,5, 68-71.). As can be seen from FIG. 6, with the increase of the addition amount of the C-S-H seed crystal, the induction period of cement hydration is obviously shortened, the curve of the acceleration period is steep, and the arrival time of the peak point of the heat flow curve is shortened. The heat flow curve characteristics described above demonstrate the effect of the C-S-H seeds in helping to accelerate cement hydration. As can be seen from FIG. 7, the hydration heat release of the cement shows an increasing trend along with the increase of the addition amount of the C-S-H seed crystals within 96H, which shows that the C-S-H seed crystals accelerate the early hydration degree of the cement, that is, the seed crystals accelerate the early hydration reaction of the cement, and have obvious coagulation promoting effect.
And (3) observing the influence rule of the three samples of Q, R and P on the hydration heat and the hydration rate of the cement (figures 2 and 3). The amount of cement added in the test was 2g, the amount of water added was 5mL, the amount of sample added was 1% (0.02 g) of the cement, and the measurement was carried out at 25 ℃.
As can be seen from FIG. 2, with the increase of the addition amount of C-S-H, the heat release at the early induction period and the acceleration period of cement hydration is obviously increased; the induction period and the acceleration period show obvious delay trends, and the arrival time of the peak point of the heat flow curve tends to delay. The above heat flow profile characteristics illustrate a completely different effect of helping to accelerate cement hydration from conventional C-S-H seeds (fig. 6).
It can be seen from figure 3 that the cement hydration exotherm increased by more than 1 fold with the addition of synthetic C-S-H and was significantly delayed. The C-S-H has obvious enhancement effect on early hydration of cement, and is different from the C-S-H delayed hydration effect of new and formed C-S-H crystal seeds of the common C-S-H crystal seeds.
The sample addition is increased from 1% (0.02 g) to 5% (0.05 g) of the cement, and the influence rule of the sample on the hydration heat and hydration rate of the cement is examined (figures 4 and 5). As can be seen from the figure, the effect on the cement hydration law is not changed after the addition amount is increased. Only the hydration exotherm is reduced.
From the above results, it can be seen that the spherical CSH for reinforcing well cementation set cement provided by the present invention can reinforce set cement without accelerating the setting (without accelerating the hydration process), unlike the conventional CSH seed crystal.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described in relation to an exemplary embodiment, and it is understood that the words which have been used herein are words of description and illustration, rather than words of limitation. Modifications may be made to the invention as defined within the scope of the claims and modifications may be made without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
Claims (21)
1. A calcium silicate hydrate suspension comprises calcium silicate hydrate and a catalyst, wherein the catalyst is amantadine hydrochloride and/or urotropine; the calcium silicate hydrate suspension is prepared by reacting calcium compound, alkoxy silane and water in the presence of a catalyst;
the calcium compound is selected from one or more of calcium nitrate, calcium chloride and calcium oxide; and/or the alkoxysilane is selected from C1-C6 alkoxysilanes;
the molar ratio of the calcium compound to the alkoxysilane, in terms of calcium to silicon molar ratio, is from 0.8 to 1.2; and/or the mass ratio of the calcium compound to water is 1; and/or the catalyst is added in an amount of 0.005 to 0.05wt% based on the total amount of the calcium compound, alkoxysilane and water.
2. The calcium silicate hydrate suspension according to claim 1, wherein the alkoxysilane is one or more selected from tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, and tetra-n-butoxysilane.
3. The calcium silicate hydrate suspension according to claim 1, wherein the molar ratio of the calcium compound to the alkoxysilane is 1; and/or the mass ratio of the calcium compound to water is 1; and/or the catalyst is added in an amount of 0.02 to 0.04wt% based on the total amount of the calcium compound, alkoxysilane and water.
4. The calcium silicate hydrate suspension of claim 1, wherein the catalyst is amantadine hydrochloride and urotropin, and the mass ratio of the amantadine hydrochloride to the urotropin is 0.1-10.
5. The calcium silicate hydrate suspension according to claim 4, wherein the mass ratio of amantadine hydrochloride to urotropin is from 0.1 to 1.
6. The calcium silicate hydrate suspension according to claim 5, wherein the mass ratio of amantadine hydrochloride to urotropin is 0.5.
7. The calcium silicate hydrate suspension according to any one of claims 1 to 6, wherein the calcium silicate hydrate has an average particle diameter of 100 to 300nm; the mass content of the calcium silicate hydrate in the suspension is 8-20%.
8. A method for preparing a calcium silicate hydrate suspension, which comprises reacting a calcium compound, an alkoxysilane and water in the presence of a catalyst selected from amantadine hydrochloride and/or urotropin.
9. The method of claim 8, wherein the catalyst is amantadine hydrochloride and urotropin, and the mass ratio of the amantadine hydrochloride to the urotropin is 0.1.
10. The method of claim 9, wherein the mass ratio of amantadine hydrochloride to urotropin is 0.1.
11. The method according to claim 10, wherein the mass ratio of amantadine hydrochloride to urotropin is 0.5 to 1.
12. A method according to any one of claims 8 to 11, wherein the calcium compound is selected from one or more of calcium nitrate, calcium chloride and calcium oxide;
and/or the alkoxysilane is selected from a C1-C6 alkoxysilane.
13. The method of claim 12, wherein the alkoxysilane is selected from one or more of tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, and tetra-n-butoxysilane.
14. The process according to any one of claims 8 to 11, characterized in that the molar ratio of calcium compound to alkoxysilane, expressed as calcium to silicon, is from 0.8 to 1.2;
and/or the mass ratio of the calcium compound to water is 1;
and/or the catalyst is added in an amount of 0.005 to 0.05wt% based on the total amount of the calcium compound, alkoxysilane and water.
15. The method according to claim 14, wherein the molar ratio of the calcium compound to the alkoxysilane is 1;
and/or the mass ratio of the calcium compound to water is 1;
and/or the catalyst is added in an amount of 0.02 to 0.04wt% based on the total amount of the calcium compound, alkoxysilane and water.
16. The process according to any one of claims 8 to 11, wherein the temperature of the reaction is 30 to 70 ℃;
and/or the reaction time is 2-10h.
17. The method of claim 16, wherein the temperature of the reaction is 40-60 ℃; and/or the reaction time is 4-8h.
18. Use of a calcium silicate hydrate suspension according to any one of claims 1 to 7 or prepared by a method according to any one of claims 8 to 17 for cementing wells.
19. A well cementing cement slurry comprising a calcium silicate hydrate suspension as defined in any one of claims 1 to 7 or a calcium silicate hydrate suspension prepared by the method as defined in any one of claims 8 to 17 and a cement.
20. A cementing slurry according to claim 19, wherein the suspension of hydrated calcium silicate is present in an amount of 0.1-5% by mass of the cement.
21. A cementing slurry according to claim 20, wherein the suspension of hydrated calcium silicate is present in an amount of 0.5-2% by mass of the cement.
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| CN105670582A (en) * | 2016-03-09 | 2016-06-15 | 中石化石油工程技术服务有限公司 | Preparation method of high-temperature-resistant great-temperature-difference cement paste for oilfield well cementing |
| CN106542757A (en) * | 2016-10-25 | 2017-03-29 | 中国石油集团川庆钻探工程有限公司长庆固井公司 | A kind of alcamines reinforcing agent and preparation method and applications |
| CN106746834A (en) * | 2016-11-28 | 2017-05-31 | 中铁十二局集团有限公司 | A kind of graphene-based nanocrystal class early strength agent and preparation method thereof |
| CN109679600A (en) * | 2019-01-23 | 2019-04-26 | 中国石油大学(华东) | Mixed and modified superelevation temperature high-performance well cementing mortar architecture of nano material and preparation method thereof |
| CN109824822A (en) * | 2019-01-28 | 2019-05-31 | 中国石油大学(华东) | Temperature response type high temperature retarder suitable for oil gas well cementing operation and preparation method thereof and cementing slurry |
| CN109650398A (en) * | 2019-02-19 | 2019-04-19 | 科之杰新材料集团有限公司 | A kind of hydrated calcium silicate early strength agent and preparation method thereof |
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