CN109655399B - Rapid detection method for sulfate erosion of cement-based material - Google Patents
Rapid detection method for sulfate erosion of cement-based material Download PDFInfo
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Abstract
The invention relates to the technical field of cement corrosion, and provides a method for rapidly detecting sulfate erosion of a cement-based material, which comprises the following steps: (1) arranging epoxy resin layers on the surfaces of the periphery of a cement-based material sample, and then soaking the cement-based material sample in a saturated calcium hydroxide solution for maintenance; (2) placing the sample obtained by maintenance in an electrochemical device for electrochemical acceleration, and carrying out X-ray mu CT detection after acceleration; after the test, placing the sample in an electrochemical device again for electrochemical acceleration and detection, and circulating until the detection is finished; the catholyte of the electrochemical device is a sulfate solution, and the anolyte is a strong alkali solution. In the electrochemical acceleration process, sulfate ions move from the cathode to the test piece under the action of an electric field, enter the interior of the test piece and then react with a cement hydration product to generate gypsum and ettringite. Compared with the corrosion only under the action of concentration difference, the corrosion speed of sulfate ions is obviously accelerated.
Description
Technical Field
The invention relates to the technical field of cement corrosion, in particular to a rapid detection method for sulfate erosion of a cement-based material.
Background
At present, cement concrete has become a main material of civil engineering and architectural engineering by virtue of the advantages thereof, and the application is wide. The durability of the cement concrete structure is closely related to the performance of concrete structure materials, and the cement concrete materials are easily corroded by harmful components in air, underground water and soil to cause strength reduction and volume deformation, so that the service life is reduced, and the original structural function of the concrete structure is lost when the concrete structure does not reach the preset service life.
The cement-based material is a porous medium material, and the erosion process of sulfate is accompanied by the change of the internal porosity and pore structure of the material. The porosity and the pore structure are main factors directly influencing the transmission process of ions in the cement-based material. Therefore, the loss due to sulfate attack is of great concern. The sulfate corrosion concrete is a long-term process accompanied by a complex physical and chemical process, the law of researching the damage of the sulfate corrosion concrete by adopting a field test is not easy to realize, and the existing domestic and foreign accelerated test method for the sulfate corrosion mainly comprises the steps of increasing the reaction area of a test piece, increasing the mass fraction of a corrosion solution, adopting a dry-wet circulation method, increasing the temperature of the solution, increasing the water-cement ratio and the like. The above-mentioned methods all have certain disadvantages, such as large dispersion of test results of small test pieces, changing composition by increasing temperature, and the like.
Disclosure of Invention
The invention aims to provide a method for rapidly detecting the corrosion of sulfate on a cement-based material so as to improve the detection speed.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for rapidly detecting sulfate erosion of a cement-based material, which is characterized by comprising the following steps of:
(1) arranging epoxy resin layers on the surfaces of the periphery of a cement-based material sample, and then soaking the cement-based material sample in a saturated calcium hydroxide solution for maintenance;
(2) placing the sample obtained by maintenance in an electrochemical device for electrochemical acceleration, and carrying out X-ray mu CT detection after acceleration;
after the test, placing the sample in an electrochemical device again for electrochemical acceleration and detection, and circulating until the detection is finished;
the catholyte of the electrochemical device is a sulfate solution, and the anolyte is a strong alkali solution.
Preferably, the cement-based material sample in the step (1) is cylindrical, and the periphery of the sample is the side surface of the cylinder.
Preferably, the height of the cylinder in the step (1) is 20-40 mm, and the diameter is 5-20 mm.
Preferably, the thickness of the epoxy resin layer in the step (1) is 0.3-1 mm.
Preferably, the sulfate solution in the step (2) is a sodium sulfate solution or a potassium sulfate solution;
the mass concentration of the sulfate solution is less than or equal to 42.5 percent.
Preferably, the strong alkali solution in the step (2) is a sodium hydroxide solution or a potassium hydroxide solution;
the mass concentration of the strong alkali solution is less than or equal to 42.5 percent.
Preferably, in the step (2), a pulse voltage is applied in the electrochemical acceleration process, the pulse voltage is 10-150V, and the pulse time is 10-60 s.
Preferably, the time of each electrochemical acceleration in the step (2) is independently 1-5 h.
The invention provides a method for rapidly detecting sulfate erosion of a cement-based material, which comprises the following steps: (1) arranging epoxy resin layers on the surfaces of the periphery of a cement-based material sample, and then soaking the cement-based material sample in a saturated calcium hydroxide solution for maintenance; (2) placing the sample obtained by maintenance in an electrochemical device for electrochemical acceleration, and carrying out X-ray mu CT detection after acceleration; after the test, placing the sample in an electrochemical device again for electrochemical acceleration and detection, and circulating until the detection is finished; the catholyte of the electrochemical device is a sulfate solution, and the anolyte is a strong alkali solution. In the electrochemical acceleration process, sulfate ions move from the cathode to the test piece under the action of an electric field, enter the interior of the test piece and then react with a cement hydration product to generate gypsum and ettringite. Compared with the corrosion only under the action of concentration difference, the corrosion speed of sulfate ions is obviously accelerated. The method has the advantages of short use time, no damage to the sample in the process, easy variable control, rapidness, no damage and accuracy.
Drawings
FIG. 1 is an electrochemical device used in the present invention;
FIG. 2 is a graph showing the change in the total pore volume of the sample of example 1.
Detailed Description
The invention provides a method for rapidly detecting sulfate erosion of a cement-based material, which comprises the following steps:
(1) arranging epoxy resin layers on the surfaces of the periphery of a cement-based material sample, and then soaking the cement-based material sample in a saturated calcium hydroxide solution for maintenance;
(2) placing the sample obtained by maintenance in an electrochemical device for electrochemical acceleration, and carrying out X-ray mu CT detection after acceleration;
after the test, placing the sample in an electrochemical device again for electrochemical acceleration and detection, and circulating until the detection is finished;
the catholyte of the electrochemical device is a sulfate solution, and the anolyte is a strong alkali solution.
And arranging epoxy resin layers on the peripheral surfaces of the cement-based material samples, and then soaking the cement-based material samples in a saturated calcium hydroxide solution for maintenance.
In the present invention, the cement-based material sample in step (1) is preferably in a cylindrical shape, and the periphery is specifically the side surface of the cylinder.
In the invention, the height of the cylinder in the step (1) is preferably 20-40 mm, more preferably 22-28 mm, and further preferably 25-26 mm; the diameter of the cylinder is preferably 5-20 mm, and more preferably 10-12 mm.
The method specifically comprises the steps of coating a layer of epoxy resin on the surface of the periphery of a cement-based material sample, and naturally drying the epoxy resin to obtain the epoxy resin layer. In the present invention, the thickness of the epoxy resin layer in the step (1) is preferably 0.3 to 1mm, and more preferably 0.5 to 0.7 mm. The epoxy resin layer can prevent erosion solution from permeating into a sample from the side surface, and further one-dimensional acceleration of an experiment is guaranteed.
According to the invention, the anode is preferably marked at one end of the sample, the cathode is preferably marked at the other end of the sample, and the anode and the cathode correspond to the anode and the cathode of the power supply when the sample is electrified, so that the sample is prevented from being taken out and disordered when being subjected to X-ray mu CT test, and the correct experiment is ensured.
After the epoxy resin layer is obtained, the sample is soaked in a saturated calcium hydroxide solution for curing. The method is carried out according to the method for maintaining the sample by adopting the non-flowing saturated calcium hydroxide solution in the standard GB/T50081-2002 of the test method for the mechanical property of the common concrete. In the invention, the curing time is preferably more than or equal to 28 days, the curing is to ensure that the sample is completely hydrated and has certain strength, and simultaneously the experimental conditions are consistent, and the interior of the sample is in a saturated state before electrification.
Placing the sample obtained by maintenance in an electrochemical device for electrochemical acceleration, and carrying out X-ray mu CT detection after the acceleration; and after the test, placing the sample in the electrochemical device again for electrochemical acceleration and detection, and cycling until the detection is finished.
In the embodiment of the invention, the electrochemical device is a self-contained device, and the device is specifically shown in fig. 1, wherein the sample part of the cylindrical sample marking anode is sleeved in the rubber tube, and nylon belts are used for binding the sample and the rubber tube at the upper part and the lower part which are overlapped, so as to prevent the anode solution from flowing into the cathode solution container; the funnel is added with anolyte, and an anolyte funnel is sleeved in the rubber tube; catholyte is added into the rectangular container.
In the invention, the catholyte of the electrochemical device is a sulfate solution, and the sulfate solution is preferably a sodium sulfate solution or a potassium sulfate solution; the mass concentration of the sulfate solution is preferably less than or equal to 42.5%, and more preferably 5-10%.
In the invention, the anolyte of the electrochemical device is a strong alkaline solution, and the strong alkaline solution is preferably a sodium hydroxide solution or a potassium hydroxide solution; the mass concentration of the strong alkali solution is preferably less than or equal to 42.5 percent, and more preferably 5-10 percent.
In the electrochemical acceleration process, catholyte is sulfate solution, sulfate ions move from a cathode to a test piece under the action of an electric field, enter the inside of the test piece and react with a cement hydration product to generate gypsum and ettringite. Compared with the corrosion only under the action of concentration difference, the corrosion speed of sulfate ions is obviously accelerated.
Because sulfate ions can be continuously consumed in the electrochemical acceleration process, the invention preferably supplements solutes in the catholyte and the anolyte at proper time in the acceleration process so as to maintain the concentration requirements of the catholyte and the anolyte; or replaced with new catholyte and anolyte each time electrochemical acceleration is performed.
In the invention, the electrochemical acceleration process in the step (2) is preferably applied by a pulse voltage, and the pulse voltage is preferably 10-150V, and more preferably 30-100V; the pulse time is preferably 10 to 60s, and more preferably 20 to 40 s. The invention takes the pulse voltage of 30V and the pulse time of 20s as an example, and the application of the pulse voltage specifically comprises the following steps: the first 20s is 30V constant voltage, the second 20s is 0V constant voltage, and the process is repeated.
In the invention, the time of each electrochemical acceleration in the step (2) is preferably 1-5 h independently, and more preferably 3 h; in the invention, when the calibration and acceleration are started, sulfate ions can rapidly enter the sample and then react with hydration products in the sample to generate ettringite or gypsum, so that pores in the sample are further blocked, the sulfate ions are difficult to enter the sample, the sulfate ion erosion speed is slowed, and the electrochemical acceleration time is sequentially prolonged.
In the scheme of the invention, after the first electrochemical acceleration is carried out for 3 days, the sample is approximately eroded by 2.1-3.0 mm. But then, as the sample is eroded deeper, the sulfate ions are more difficult to enter the inside of the sample, and the sample with the size of the invention is conservative, so that 8 times of cycle experiments can be carried out.
The X-ray micro-computed tomography (X-ray micro-CT) detection is carried out by adopting an X-ray micro-computed tomography (X-ray micro-CT) testing method well known by the technical personnel in the field, and the sample is not damaged. The X-ray mu CT detection can observe the change of the microstructure in the sample.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
In the embodiment, the cement paste is selected for an experiment, the upper surface and the lower surface of a cylindrical sample (the diameter is 10mm, and the height is 25mm) are firstly ground by sand paper, and epoxy sealing is not carried out; and (3) coating epoxy resin on the side surface of the cylindrical sample, and air-drying for 24 hours to obtain an epoxy resin layer with the thickness of 0.5 mm. And (3) making positive and negative pole marks and sample number marks on the upper and lower ends of the cylindrical sample by using a mark pen, and then putting the marked sample into a saturated calcium hydroxide solution for maintenance. A5 wt% calcium hydroxide solution and a 5 wt% sodium sulfate solution are prepared, and the solutions are fully dissolved after standing for one day.
The sample was mounted on the electrochemical device shown in FIG. 1, and the power was turned on (pulse voltage 30V, pulse time 20s), and after the 3 rd day of acceleration of the energization, the power was turned off, and the sample was taken out. And performing nondestructive X-ray mu CT test on the electrified and accelerated cylindrical sample by adopting X-ray mu CT test equipment, acquiring image information and processing data.
After the X-ray mu CT test is finished, the sample is taken out, is remounted in the electrochemical device (the catholyte and the anolyte are replaced by new prepared solution), is powered on (the pulse voltage is 30V, the pulse time is 20s), is powered off after the 3 rd day of acceleration of the electrification, and is taken out. And performing nondestructive X-ray mu CT test on the electrified and accelerated cylindrical sample by adopting X-ray mu CT test equipment, acquiring image information and processing data.
The cycle was continued for 6 more times and the experiment was ended.
The electric pulse accelerates sulfate ions to enter the sample, and the sulfate ions are combined with hydration products in the sample to generate gypsum and ettringite, the pores are gradually filled, and the pore volume is less and less. The total pore volume of the sample after the first electrochemical acceleration (3h) and the second electrochemical acceleration is finished is shown in fig. 2, and as can be seen from fig. 2, the total pore volume of the sample decreases with the prolonging of the electrochemical acceleration time, which indicates that the sample is corroded, and the feasibility of the method for accelerating the rapid corrosion of sulfate ions by electric pulses is proved.
Example 2
In the embodiment, cement mortar is selected for an experiment, the upper surface and the lower surface of a cylindrical sample (the diameter is 10mm, and the height is 25mm) are firstly ground by sand paper, and epoxy sealing is not carried out; and (3) coating epoxy resin on the side surface of the cylindrical sample, and air-drying for 24 hours to obtain an epoxy resin layer with the thickness of 0.5 mm. And (3) making positive and negative pole marks and sample number marks on the upper and lower ends of the cylindrical sample by using a mark pen, and then putting the marked sample into a saturated calcium hydroxide solution for maintenance. A40 wt% calcium hydroxide solution and a 40 wt% sodium sulfate solution are prepared, and the solution is fully dissolved after standing for one day.
The sample was mounted on an electrochemical device, and the power was turned on (pulse voltage 40V, pulse time 30s), and after the 3 rd day of acceleration of energization, the sample was taken out by turning off the power. And performing nondestructive X-ray mu CT test on the electrified and accelerated cylindrical sample by adopting X-ray mu CT test equipment, acquiring image information and processing data.
After the X-ray mu CT test is finished, the sample is taken out, is remounted in the electrochemical device (the catholyte and the anolyte are replaced by new prepared solution), is powered on (the pulse voltage is 40V, the pulse time is 30s), is powered off after the 3 rd day of acceleration of the electrification, and is taken out. And performing nondestructive X-ray mu CT test on the electrified and accelerated cylindrical sample by adopting X-ray mu CT test equipment, acquiring image information and processing data.
The cycle was continued for 6 more times and the experiment was ended.
The X-ray mu CT test result shows that the internal pores of the sample are gradually reduced, which indicates that the sample is gradually corroded.
Example 3
In the embodiment, cement concrete is selected for experiment, the upper surface and the lower surface of a cylindrical sample (the diameter is 10mm, the height is 25mm) are firstly ground by sand paper, and epoxy sealing is not carried out; and (3) coating epoxy resin on the side surface of the cylindrical sample, and air-drying for 24 hours to obtain an epoxy resin layer with the thickness of 0.5 mm. And (3) making positive and negative pole marks and sample number marks on the upper and lower ends of the cylindrical sample by using a mark pen, and then putting the marked sample into a saturated calcium hydroxide solution for maintenance. Preparing 15 wt% calcium hydroxide solution and 15 wt% sodium sulfate solution, and standing for one day to make the solutions fully dissolved.
The sample was mounted on an electrochemical device, and the power was turned on (pulse voltage was 100V, pulse time was 20s), and after the 3 rd day of acceleration of energization, the sample was taken out by turning off the power. And performing nondestructive X-ray mu CT test on the electrified and accelerated cylindrical sample by adopting X-ray mu CT test equipment, acquiring image information and processing data.
After the X-ray mu CT test is finished, the sample is taken out, is remounted in the electrochemical device (the catholyte and the anolyte are replaced by new prepared solution), is powered on (the pulse voltage is 100V, the pulse time is 20s), is powered off after the 3 rd day of acceleration of the electrification, and is taken out. And performing nondestructive X-ray mu CT test on the electrified and accelerated cylindrical sample by adopting X-ray mu CT test equipment, acquiring image information and processing data.
The cycle was continued for 6 more times and the experiment was ended.
The X-ray mu CT test result shows that the internal pores of the sample are gradually reduced, which indicates that the sample is gradually corroded.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A method for rapidly detecting sulfate erosion of a cement-based material is characterized by comprising the following steps:
(1) arranging epoxy resin layers on the surfaces of the periphery of a cement-based material sample, and then soaking the cement-based material sample in a saturated calcium hydroxide solution for maintenance;
(2) placing the sample obtained by maintenance in an electrochemical device for electrochemical acceleration, and carrying out X-ray mu CT detection after acceleration;
after the test, placing the sample in an electrochemical device again for electrochemical acceleration and detection, and circulating until the detection is finished;
the catholyte of the electrochemical device is a sulfate solution, and the anolyte is a strong alkali solution;
the cement-based material sample in the step (1) is cylindrical, and the periphery of the sample is the side surface of the cylinder;
the height of the cylinder in the step (1) is 20-40 mm, and the diameter is 5-20 mm;
the electrochemical device is a self-prepared device, the sample part of the cylindrical sample marking the anode is sleeved in the rubber tube, and a nylon belt is used for binding the sample and the rubber tube up and down in a superposition manner, so that the anode solution is prevented from flowing into the cathode solution container; the funnel is added with anolyte, and an anolyte funnel is sleeved in the rubber tube; catholyte is added into the rectangular container.
2. The detection method according to claim 1, wherein the thickness of the epoxy resin layer in the step (1) is 0.3 to 1 mm.
3. The detection method according to claim 1, wherein the sulfate solution in the step (2) is a sodium sulfate solution or a potassium sulfate solution;
the mass concentration of the sulfate solution is less than or equal to 42.5 percent.
4. The detection method according to claim 1, wherein the strong alkali solution in the step (2) is a sodium hydroxide solution or a potassium hydroxide solution;
the mass concentration of the strong alkali solution is less than or equal to 42.5 percent.
5. The detection method according to claim 1, wherein the electrochemical acceleration process in the step (2) is applied with a pulse voltage of 10-150V and a pulse time of 10-60 s.
6. The detection method according to claim 1, wherein the time of each electrochemical acceleration in the step (2) is independently 1-5 h.
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| CN110044811B (en) * | 2019-05-05 | 2021-11-30 | 重庆大学 | Device and method for testing low-temperature sulfate corrosion resistance of solid concrete |
| CN110208175B (en) * | 2019-07-09 | 2021-07-16 | 济南大学 | Method for testing sulfate erosion resistance of C3S hydration system by using dialysis bag |
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