CN112624712A - Temperature-resistant pressure-resistant cement-based plugging material and preparation method thereof - Google Patents
Temperature-resistant pressure-resistant cement-based plugging material and preparation method thereof Download PDFInfo
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- CN112624712A CN112624712A CN202011542015.2A CN202011542015A CN112624712A CN 112624712 A CN112624712 A CN 112624712A CN 202011542015 A CN202011542015 A CN 202011542015A CN 112624712 A CN112624712 A CN 112624712A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/06—Aluminous cements
- C04B28/065—Calcium aluminosulfate cements, e.g. cements hydrating into ettringite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
- C04B22/08—Acids or salts thereof
- C04B22/10—Acids or salts thereof containing carbon in the anion
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a temperature-resistant pressure-resistant cement-based plugging material and a preparation method thereof, wherein the material is prepared from the following raw materials in parts by weight: 40-60 parts of sulphoaluminate cement, 0.5-1 part of calcium nitrate, 0.5-1 part of sodium nitrite, 1-2 parts of lithium aluminum hydrotalcite, 0.5-1 part of zinc fluosilicate, 0.2-0.5 part of polycarboxylic acid water reducing agent, 30-34 parts of filling material and 0.1-0.3 part of tackifier. The plugging material has the advantages of cheap and easily-obtained raw materials, simple preparation process, excellent plugging efficiency of the obtained product, improved overall performance of the material due to higher stability of a hydration product, particularly heat resistance and pressure resistance, and ideal application prospect.
Description
Technical Field
The invention belongs to the technical field of plugging materials, and particularly relates to a temperature-resistant pressure-resistant cement-based plugging material and a preparation method thereof.
Background
The inorganic waterproof leaking stoppage material is a cement-based rapid leaking stoppage material commonly used in the existing waterproof leaking stoppage engineering, and the material takes a cement-based material as a main body, has the advantages of no toxicity, no odor, safety, environmental protection, water carrying operation, simple and convenient construction, rapid hardening, lower cost and the like compared with an organic waterproof leaking stoppage material, and has wide application in waterproof, seepage-proofing and emergency leaking stoppage engineering.
The cement-based material in the existing plugging material comprises sulphoaluminate cement, fluoroaluminate cement, phosphate cement and the like, wherein the sulphoaluminate Cement (CSA) is a third series of cement taking anhydrous calcium sulphoaluminate and beta dicalcium silicate as main clinker minerals, has the advantages of rapid strength development, good corrosion resistance and low carbon dioxide emission in the production process, is a material with wide application prospect, but has the defects of later strength retraction, incapability of reaching ideal standards of pressure resistance and heat resistance and the like, because the main hydration products of the sulphoaluminate cement are hydrated calcium aluminate (AFm) and ettringite, wherein the ettringite plays a skeleton role in a hardened structure, the stability of the ettringite in the plugging material system is poor, and when the gypsum amount in the system is exhausted, the ettringite can react with the calcium aluminate to generate hydrated calcium sulphoaluminate to cause the decomposition of the calcium sulphoaluminate to a certain degree, therefore, the performance of the sulphoaluminate cement can be improved by starting from the hydration product of the sulphoaluminate cement, and the overall performance of the plugging material is further improved.
Disclosure of Invention
The invention aims to make up the defects of the prior art and provides a temperature-resistant pressure-resistant cement-based plugging material and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
a temperature-resistant pressure-resistant cement-based plugging material is prepared from the following raw materials in parts by weight: 40-60 parts of sulphoaluminate cement, 0.5-1 part of calcium nitrate, 0.5-1 part of sodium nitrite, 1-2 parts of lithium aluminum hydrotalcite, 0.5-1 part of zinc fluosilicate, 0.2-0.5 part of polycarboxylic acid water reducing agent, 30-34 parts of filling material and 0.1-0.3 part of tackifier.
Preferably, the temperature-resistant pressure-resistant cement-based plugging material is prepared from the following raw materials in parts by weight: 50 parts of sulphoaluminate cement, 0.75 part of calcium nitrate, 0.75 part of sodium nitrite, 1.5 parts of lithium-aluminum hydrotalcite, 0.8 part of zinc fluosilicate, 0.3 part of polycarboxylic acid water reducing agent, 32 parts of filling material and 0.2 part of tackifier.
Further, the lithium aluminum hydrotalcite is prepared by the following steps:
(1) dissolving lithium nitrate and aluminum nitrate in water to form a mixed salt solution;
(2) dissolving sodium hydroxide and sodium carbonate in water to form a mixed alkali solution;
(3) and (3) feeding the mixed salt solution and the mixed alkali solution into a full back-mixing explosive nuclear reactor for mixing reaction, performing reflux crystallization on the obtained slurry at 100 ℃ for 4-6 hours, and finally washing the slurry to be neutral by using water to obtain the lithium-aluminum hydrotalcite.
Further, the concentration of lithium ions in the mixed salt solution in the step (1) is controlled to be 1.2-1.8mol/L, and the equivalent concentration ratio of the lithium ions to the aluminum ions is 4: 1.
Further, the concentration of hydroxide ions in the mixed alkali solution in the step (2) is controlled to be 1.2-1.8mol/L, and the equivalent concentration ratio of hydroxide ions to carbonate ions is 16: 1.
Further, the filling material is selected from one or more of fly ash, quartz sand and limestone particles.
Further, the tackifier is selected from any one of carboxymethyl cellulose, hydroxypropyl cellulose and resin gum powder.
The invention also provides a preparation method of the temperature-resistant pressure-resistant cement-based plugging material, which comprises the steps of weighing the raw materials in parts by weight, and uniformly stirring.
Further, when the plugging material is used, the plugging material is mixed with water with the mass of 0.5-1.5 times, the mixture is uniformly stirred to obtain slurry, and the slurry is filled into a leakage position.
The invention has the advantages that:
the leakage blocking material of the invention takes sulphoaluminate cement as a main material, by doping calcium nitrate and sodium nitrite into the sulphoaluminate cement, nitrate ions and nitrite ions generated after hydrolysis have stronger substitution sequence than carbonate ions and hydrated sulfate ions in the traditional additive gypsum, therefore, hydrated calcium aluminate nitrate and hydrated calcium nitrosaluminate are mainly generated in the competitive reaction after hydration, the stability of the hydrated calcium aluminate nitrate and the hydrated calcium nitrosaluminate is far higher than that of hydrated calcium sulphoaluminate, thus the stability of the sulphoaluminate cement hydration product ettringite is improved,
the invention simultaneously introduces lithium aluminum hydrotalcite components, is synthesized by nucleation, crystallization and isolation, has a typical layered structure, is used as a seed crystal material, and can reduce the nucleation energy when the hydrated product of the aluminosilicate cement is formed by the combined action of crystal nuclei and laminate metal ions, thereby improving the hydration reaction rate and increasing the material leakage stopping efficiency.
The plugging material has the advantages of cheap and easily-obtained raw materials, simple preparation process, excellent plugging efficiency of the obtained product, improved overall performance of the material due to higher stability of a hydration product, particularly heat resistance and pressure resistance, and ideal application prospect.
Detailed Description
The technical scheme of the invention is further explained by combining the specific examples as follows:
example 1
A temperature-resistant pressure-resistant cement-based plugging material is prepared from the following raw materials in parts by mass: 50kg of sulphoaluminate cement, 0.75kg of calcium nitrate, 0.75kg of sodium nitrite, 1.5kg of lithium-aluminum hydrotalcite, 0.8kg of zinc fluosilicate, 0.3kg of polycarboxylic acid water reducing agent, 32kg of fly ash and 0.2kg of carboxymethyl cellulose.
The lithium aluminum hydrotalcite is prepared by the following steps:
(1) dissolving lithium nitrate and aluminum nitrate in water to form a mixed salt solution, wherein the concentration of lithium ions is controlled to be 1.5mol/L, and the equivalent concentration ratio of the lithium ions to the aluminum ions is 4: 1;
(2) dissolving sodium hydroxide and sodium carbonate in water to form a mixed alkali solution, wherein the concentration of hydroxide ions is controlled to be 1.5mol/L, and the equivalent concentration ratio of the hydroxide ions to the carbonate ions is 16: 1;
(3) and (3) feeding the mixed salt solution and the mixed alkali solution into a full back-mixing explosive nuclear reactor for mixing reaction, refluxing and crystallizing the obtained slurry at 100 ℃ for 5 hours, and finally washing the slurry to be neutral by using water to obtain the lithium-aluminum hydrotalcite.
Weighing the raw materials according to the mass ratio, and uniformly stirring to obtain the plugging material.
Example 2
A temperature-resistant pressure-resistant cement-based plugging material is prepared from the following raw materials in parts by mass: 40kg of sulphoaluminate cement, 0.5kg of calcium nitrate, 0.5kg of sodium nitrite, 1kg of lithium-aluminum hydrotalcite, 0.5kg of zinc fluosilicate, 0.2kg of polycarboxylic acid water reducing agent, 30kg of quartz sand and 0.1kg of hydroxypropyl cellulose.
The lithium aluminum hydrotalcite is prepared by the following steps:
(1) dissolving lithium nitrate and aluminum nitrate in water to form a mixed salt solution, wherein the concentration of lithium ions is controlled to be 1.2mol/L, and the equivalent concentration ratio of the lithium ions to the aluminum ions is 4: 1;
(2) dissolving sodium hydroxide and sodium carbonate in water to form a mixed alkali solution, wherein the concentration of hydroxide ions is controlled to be 1.2mol/L, and the equivalent concentration ratio of the hydroxide ions to the carbonate ions is 16: 1;
(3) and (3) feeding the mixed salt solution and the mixed alkali solution into a full back-mixing explosive nuclear reactor for mixing reaction, refluxing and crystallizing the obtained slurry at 100 ℃ for 4 hours, and finally washing the slurry to be neutral by using water to obtain the lithium-aluminum hydrotalcite.
Weighing the raw materials according to the mass ratio, and uniformly stirring to obtain the plugging material.
Example 3
A temperature-resistant pressure-resistant cement-based plugging material is prepared from the following raw materials in parts by mass: 60kg of sulphoaluminate cement, 1kg of calcium nitrate, 1kg of sodium nitrite, 2kg of lithium-aluminum hydrotalcite, 1kg of zinc fluosilicate, 0.5kg of polycarboxylic acid water reducing agent, 34kg of limestone particles and 0.3kg of resin rubber powder.
The lithium aluminum hydrotalcite is prepared by the following steps:
(1) dissolving lithium nitrate and aluminum nitrate in water to form a mixed salt solution, wherein the concentration of lithium ions is controlled to be 1.8mol/L, and the equivalent concentration ratio of the lithium ions to the aluminum ions is 4: 1;
(2) dissolving sodium hydroxide and sodium carbonate in water to form a mixed alkali solution, wherein the concentration of hydroxide ions is controlled to be 1.8mol/L, and the equivalent concentration ratio of the hydroxide ions to the carbonate ions is 16: 1;
(3) and (3) feeding the mixed salt solution and the mixed alkali solution into a full back-mixing explosive nuclear reactor for mixing reaction, refluxing and crystallizing the obtained slurry at 100 ℃ for 6 hours, and finally washing the slurry to be neutral by using water to obtain the lithium-aluminum hydrotalcite.
Weighing the raw materials according to the mass ratio, and uniformly stirring to obtain the plugging material.
Comparative example 1
Compared with the example 1, the calcium nitrate and the sodium nitrite are replaced by the hemihydrate gypsum in the material, and the concrete steps are as follows:
a temperature-resistant pressure-resistant cement-based plugging material is prepared from the following raw materials in parts by mass: 50kg of sulphoaluminate cement, 1.5kg of semi-hydrated gypsum, 1.5kg of lithium-aluminum hydrotalcite, 0.8kg of zinc fluosilicate, 0.3kg of polycarboxylic acid water reducing agent, 32kg of fly ash and 0.2kg of carboxymethyl cellulose.
The lithium aluminum hydrotalcite is prepared by the following steps:
(1) dissolving lithium nitrate and aluminum nitrate in water to form a mixed salt solution, wherein the concentration of lithium ions is controlled to be 1.5mol/L, and the equivalent concentration ratio of the lithium ions to the aluminum ions is 4: 1;
(2) dissolving sodium hydroxide and sodium carbonate in water to form a mixed alkali solution, wherein the concentration of hydroxide ions is controlled to be 1.5mol/L, and the equivalent concentration ratio of the hydroxide ions to the carbonate ions is 16: 1;
(3) and (3) feeding the mixed salt solution and the mixed alkali solution into a full back-mixing explosive nuclear reactor for mixing reaction, refluxing and crystallizing the obtained slurry at 100 ℃ for 5 hours, and finally washing the slurry to be neutral by using water to obtain the lithium-aluminum hydrotalcite.
Weighing the raw materials according to the mass ratio, and uniformly stirring to obtain the plugging material.
Comparative example 2
Compared with the embodiment 1, no lithium aluminum hydrotalcite component is added in the material, and the concrete steps are as follows:
a temperature-resistant pressure-resistant cement-based plugging material is prepared from the following raw materials in parts by mass: 50kg of sulphoaluminate cement, 0.75kg of calcium nitrate, 0.75kg of sodium nitrite, 0.8kg of zinc fluosilicate, 0.3kg of polycarboxylic acid water reducing agent, 32kg of fly ash and 0.2kg of carboxymethyl cellulose.
Weighing the raw materials according to the mass ratio, and uniformly stirring to obtain the plugging material.
Comparative example 3
Compared with the embodiment 1, the material is prepared by using hemihydrate gypsum to replace calcium nitrate and sodium nitrite, and meanwhile, no lithium aluminum hydrotalcite component is added, and the concrete steps are as follows:
a temperature-resistant pressure-resistant cement-based plugging material is prepared from the following raw materials in parts by mass: 50kg of sulphoaluminate cement, 1.5kg of semi-hydrated gypsum, 0.8kg of zinc fluosilicate, 0.3kg of polycarboxylic acid water reducing agent, 32kg of fly ash and 0.2kg of carboxymethyl cellulose.
Weighing the raw materials according to the mass ratio, and uniformly stirring to obtain the plugging material.
And (3) performance testing:
the test is carried out according to indexes of GB23440-2009 inorganic waterproof plugging material, and the results are shown in tables 1 and 2:
TABLE 1
As can be seen from table 1, examples 1, 2 and 3 are superior to comparative examples in terms of the setting rate, which indicates that the plugging efficiency is higher, while comparative example 2 has a larger decrease in the setting rate than comparative example 1, and also reflects the effect of the lithium aluminum hydrotalcite component on increasing the hydration reaction rate.
TABLE 2
| Compressive strength MPa (3d) | Heat resistance (100 ℃, 5h) | |
| Example 1 | 17.6 | No cracking, peeling and falling off |
| Example 2 | 16.5 | No cracking, peeling and falling off |
| Example 3 | 17.1 | No cracking, peeling and falling off |
| Comparative example 1 | 13.8 | Small amount of cracking, peeling and falling off |
| Comparative example 2 | 15.2 | Small amount of cracking, peeling and falling off |
| Comparative example 3 | 11.7 | Partial cracking, peeling and falling off |
As can be seen from Table 2, examples 1, 2 and 3 are superior to comparative examples in compressive strength and heat resistance, and from comparative examples 1 and 2, the use of calcium nitrate and sodium nitrite has a better effect on the stability of the product ettringite after the material is hydrated, and the stability directly affects the compressive strength and heat resistance of the material, while the combination of calcium nitrate, sodium nitrite and lithium aluminum hydrotalcite has a better promotion effect on the performance of the product.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The temperature-resistant pressure-resistant cement-based plugging material is characterized by being prepared from the following raw materials in parts by weight: 40-60 parts of sulphoaluminate cement, 0.5-1 part of calcium nitrate, 0.5-1 part of sodium nitrite, 1-2 parts of lithium aluminum hydrotalcite, 0.5-1 part of zinc fluosilicate, 0.2-0.5 part of polycarboxylic acid water reducing agent, 30-34 parts of filling material and 0.1-0.3 part of tackifier.
2. The temperature-resistant pressure-resistant cement-based lost circulation material as claimed in claim 1, which is prepared from the following raw materials in parts by weight: 50 parts of sulphoaluminate cement, 0.75 part of calcium nitrate, 0.75 part of sodium nitrite, 1.5 parts of lithium-aluminum hydrotalcite, 0.8 part of zinc fluosilicate, 0.3 part of polycarboxylic acid water reducing agent, 32 parts of filling material and 0.2 part of tackifier.
3. The temperature-resistant pressure-resistant cement-based lost circulation material as claimed in claim 1, wherein the lithium aluminum hydrotalcite is prepared by the following steps:
(1) dissolving lithium nitrate and aluminum nitrate in water to form a mixed salt solution;
(2) dissolving sodium hydroxide and sodium carbonate in water to form a mixed alkali solution;
(3) and (3) feeding the mixed salt solution and the mixed alkali solution into a full back-mixing explosive nuclear reactor for mixing reaction, performing reflux crystallization on the obtained slurry at 100 ℃ for 4-6 hours, and finally washing the slurry to be neutral by using water to obtain the lithium-aluminum hydrotalcite.
4. The temperature and pressure resistant cement-based lost circulation material as claimed in claim 3, wherein the concentration of lithium ions in the mixed salt solution in step (1) is controlled to be 1.2-1.8mol/L, and the ratio of the equivalent concentration of lithium ions to the equivalent concentration of aluminum ions is 4: 1.
5. The temperature-resistant pressure-resistant cement-based plugging material as claimed in claim 3, wherein the concentration of hydroxide ions in the mixed alkali solution in the step (2) is controlled to be 1.2-1.8mol/L, and the equivalent concentration ratio of hydroxide ions to carbonate ions is 16: 1.
6. The temperature-resistant pressure-resistant cement-based lost circulation material as claimed in claim 1, wherein the filler is selected from any one or more of fly ash, quartz sand and limestone particles.
7. The temperature-resistant pressure-resistant cement-based lost circulation material as claimed in claim 1, wherein the tackifier is any one selected from carboxymethyl cellulose, hydroxypropyl cellulose and resin rubber powder.
8. A preparation method of the temperature-resistant pressure-resistant cement-based lost circulation material as claimed in any one of claims 1 to 7, characterized in that the material is prepared by weighing the raw materials according to the weight parts and uniformly mixing the raw materials.
9. The temperature-resistant pressure-resistant cement-based plugging material as claimed in claim 1, wherein the plugging material is mixed with water in an amount of 0.5-1.5 times the mass of the plugging material when in use, and the mixture is uniformly stirred to obtain slurry which is filled into a leakage position.
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Application publication date: 20210409 |