CN109655399A - A kind of rapid detection method of cement-based material by sulfate attack - Google Patents
A kind of rapid detection method of cement-based material by sulfate attack Download PDFInfo
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Abstract
The present invention relates to cement corrosion technology fields, a kind of cement-based material is provided by the rapid detection method of sulfate attack, is comprised the following steps: (1) being dipped in saturated calcium hydroxide solution and is conserved after epoxy resin layer is arranged in cement-based material sample surrounded surface；(2) the obtained sample that conserves is placed in progress electrochemistry acceleration in electrochemical appliance, X-ray μ CT detection is carried out after acceleration；Sample is placed in electrochemical appliance again after the test and carries out electrochemistry acceleration and detection, is recycled with this, until detection terminates；The catholyte of the electrochemical appliance is sulfate liquor, and anolyte is strong base solution.In electrochemistry accelerator of the present invention, sulfate ion is moved from cathode into test specimen under the action of electric field, into sample inside after reacted with hydrolysis product of cement, generate gypsum and entringite.Compared to the erosion only leaned under concentration difference effect, sulfate ion erosive velocity is obviously accelerated.
Description
Technical field
The present invention relates to cement corrosion technology field more particularly to a kind of cement-based materials by the quick inspection of sulfate attack
Survey method.
Background technique
Currently, cement concrete has become the main material of civil construction project by its advantage, it is widely used.Cement
The durability of concrete structure and concrete structure material performance are closely bound up, cement concrete material be easy by air,
Be lauched and soil in harmful components corrode, cause intensity decline, cubic deformation, and then service life caused to decline, so that mixed
Xtah Crude Clay structure is not up to scheduled Years Of Service and just loses original structure function.
Cement-based material is a kind of porous media material, and the erosion process of sulfate is along with material internal porosity and hole
The variation of gap structure.And porosity and pore structure are all the masters for directly affecting transmission process of the ion inside cement-based material
Want factor.Therefore, loss caused by sulfate attack will be paid much attention to.Sulfate attack concrete is a long-term process,
Complicated physical and chemical process is attended by simultaneously, and the regular comparison that its destruction is studied using field test is not easily accomplished, at present
It is mainly both at home and abroad the quality point for increasing test specimen response area, increasing attack solution to the accelerated test method of sulfate attack
Number, dry wet cycling method, promotion solution temperature, increase ratio of mud etc..Method mentioned above has the shortcomings that certain, such as lab scale
Part test result discrete type is big, increases temperature and changes constituent etc..
Summary of the invention
The purpose of the present invention is to provide a kind of cement-based materials by the rapid detection method of sulfate attack, to improve inspection
Degree of testing the speed.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of cement-based materials by the rapid detection method of sulfate attack, which is characterized in that includes
Following steps:
(1) cement-based material sample surrounded surface be arranged epoxy resin layer after be dipped in saturated calcium hydroxide solution into
Row maintenance；
(2) the obtained sample that conserves is placed in progress electrochemistry acceleration in electrochemical appliance, carries out X-ray after acceleration
μ CT detection；
Sample is placed in electrochemical appliance again after the test and carries out electrochemistry acceleration and detection, is recycled with this,
Until detection terminates；
The catholyte of the electrochemical appliance is sulfate liquor, and anolyte is strong base solution.
Preferably, cement-based material sample is in cylindrical shape in the step (1), and the surrounding is the side of cylindrical body.
Preferably, the height of cylindrical body is 20~40mm in the step (1), and diameter is 5~20mm.
Preferably, in the step (1) epoxy resin layer with a thickness of 0.3~1mm.
Preferably, sulfate liquor is metabisulfite solution or potassium sulfate solution in the step (2)；
Mass concentration≤42.5% of the sulfate liquor.
Preferably, strong base solution is sodium hydroxide solution or potassium hydroxide solution in the step (2)；
Mass concentration≤42.5% of the strong base solution.
Preferably, in the step (2) electrochemistry accelerator apply be pulse voltage, the pulse voltage be 10~
150V, burst length are 10~60s.
Preferably, the time that each electrochemistry accelerates in the step (2) independently is 1~5h.
The present invention provides a kind of cement-based materials by the rapid detection method of sulfate attack, comprises the following steps: (1)
It is dipped in saturated calcium hydroxide solution and is conserved after epoxy resin layer is arranged in cement-based material sample surrounded surface；(2)
The obtained sample that conserves is placed in progress electrochemistry acceleration in electrochemical appliance, X-ray μ CT detection is carried out after acceleration；Institute
It states test and sample is placed in progress electrochemistry acceleration and detection in electrochemical appliance again later, recycled with this, until detection knot
Beam；The catholyte of the electrochemical appliance is sulfate liquor, and anolyte is strong base solution.Cathode terminal solution of the present invention is sulfuric acid
Salting liquid, in the electrochemistry accelerator, sulfate ion is moved from cathode into test specimen under the action of electric field, into examination
Sample reacts behind inside with hydrolysis product of cement, generates gypsum and entringite.Compared to the erosion only leaned under concentration difference effect, sulfate radical
Ion erosion speed is obviously accelerated.The time that the method for the invention uses is shorter, lossless to sample in the process, easily controllable change
Amount, has the characteristics that quick, lossless, accurate.
Detailed description of the invention
Fig. 1 is electrochemical appliance used in the present invention；
Fig. 2 is 1 sample total pore volume variation diagram of embodiment.
Specific embodiment
The present invention provides a kind of cement-based materials by the rapid detection method of sulfate attack, comprises the following steps:
(1) cement-based material sample surrounded surface be arranged epoxy resin layer after be dipped in saturated calcium hydroxide solution into
Row maintenance；
(2) the obtained sample that conserves is placed in progress electrochemistry acceleration in electrochemical appliance, carries out X-ray after acceleration
μ CT detection；
Sample is placed in electrochemical appliance again after the test and carries out electrochemistry acceleration and detection, is recycled with this,
Until detection terminates；
The catholyte of the electrochemical appliance is sulfate liquor, and anolyte is strong base solution.
It is dipped in saturated calcium hydroxide solution and carries out after epoxy resin layer is arranged in cement-based material sample surrounded surface
Maintenance.
In the present invention, cement-based material sample is preferably in cylindrical shape in the step (1), and the surrounding is specially to justify
The side of cylinder.
In the present invention, the highly preferred of cylindrical body is 20~40mm in the step (1), more preferably 22~28mm,
Further preferably 25~26mm；The diameter of the cylindrical body is preferably 5~20mm, more preferably 10~12mm.
The present invention specifically coats one layer of epoxy resin in the cement-based material sample surrounded surface, is after natural air drying
For epoxy resin layer.In the present invention, the thickness of epoxy resin layer is preferably 0.3~1mm in the step (1), more preferably
0.5~0.7mm.Epoxy resin layer of the present invention can prevent attack solution from penetrating into sample from side, and then guarantee real
The one-dimensional acceleration tested.
The present invention preferably marks anode in one end of the sample, and the other end marks cathode, when energization and power positive cathode
It is corresponding, it avoids taking-up from doing X-ray μ CT test and causes confusion, guarantee the correct progress of experiment.
After obtaining epoxy resin layer, sample is dipped in saturated calcium hydroxide solution and conserves by the present invention.The present invention presses
According to molten using immobilising saturated calcium hydroxide in standard for test methods of mechanical properties of ordinary concrete " GB/T50081-2002 "
The method that liquid carries out sample maintenance carries out.In the present invention, the time of the maintenance preferably >=28 days, the maintenance is ensures to try
The complete aquation of sample has certain intensity, while guaranteeing that experiment condition is consistent, in a saturated state inside sample before being powered.
The obtained sample that conserves is placed in progress electrochemistry acceleration in electrochemical appliance by the present invention, carries out X- after acceleration
Ray μ CT detection；Sample is placed in electrochemical appliance again after the test and carries out electrochemistry acceleration and detection, is followed with this
Ring, until detection terminates.
In the specific embodiment of the invention, the electrochemical appliance is home-made contrivance, the device it is specific as shown in Figure 1, its
In, in the sample parts set entering glue pipe of cylindrical specimens label anode, and it is upper to use nylon tape to be overlapped in sample with sebific duct
Lower binding, prevents anodic dissolution from flowing into cathode solution container；Adding in funnel is anolyte, and anodic dissolution funnel organ is inserted in
In sebific duct；Add in cuboid container is catholyte.
In the present invention, the catholyte of the electrochemical appliance is sulfate liquor, and the sulfate liquor is preferably sulphur
Acid sodium solution or potassium sulfate solution；The mass concentration of the sulfate liquor preferably≤42.5%, more preferably 5~10%.
In the present invention, the anolyte of the electrochemical appliance is strong base solution, and the strong base solution is preferably hydroxide
Sodium solution or potassium hydroxide solution；The mass concentration of the strong base solution preferably≤42.5%, more preferably 5~10%.
In the electrochemistry accelerator, catholyte is sulfate liquor, under the action of electric field sulfate ion from
Cathode is moved into test specimen, into sample inside after reacted with hydrolysis product of cement, generate gypsum and entringite.Compared to only by dense
Erosion under degree difference effect, sulfate ion erosive velocity are obviously accelerated.
Due to can ceaselessly consume sulfate ion in electrochemistry accelerator, the present invention is in due course preferably in accelerator
The solute added in catholyte and anolyte, with maintain both concentration requirement；Or when carrying out electrochemistry acceleration every time,
It is substituted for new catholyte and anolyte.
In the present invention, what electrochemistry accelerator preferably applied in the step (2) is pulse voltage, the pulse electricity
Pressure is preferably 10~150V, more preferably 30~100V；Burst length is preferably 10~60s, more preferably 20~40s.This hair
Bright with the pulse voltage is 30V, for the burst length is 20s, the application of the pulse voltage specifically: preceding 20s is 30V perseverance
Voltage, rear 20s are 0V constant voltage, and circulation is gone down according to this.
In the present invention, the time that each electrochemistry accelerates in the step (2) is independently preferably 1~5h, more preferably
For 3h；In the present invention, just started into school accelerate when, sulfate ion can rapidly enter sample, afterwards with the aquation inside sample
Product reaction, generates entringite or gypsum, further blocks sample internal void, sulfate ion is caused to hardly enter in sample
Portion, sulfate ion erosive velocity are slowed by, and the electrochemistry acceleration time sequentially extends.
In the present invention program, after first time electrochemistry accelerates 3d, sample substantially corrodes 2.1~3.0mm.But later with
Sample erosion is deeper, and sulfate ion is difficult to enter inside sample, and the sample of size of the present invention is conservative can to carry out 8
Secondary circulation experiment.
X-ray μ CT detection of the present invention uses the microcosmic tomography (X- of X-ray well-known to those skilled in the art
Ray microcomputed tomography, X-ray μ CT) test method progress, it is lossless to sample.X-ray of the present invention
μ CT detection can observe the variation of sample internal microstructure.
Technical solution provided by the invention is described in detail below with reference to embodiment, but they cannot be understood
For limiting the scope of the present invention.
Embodiment 1
The present embodiment selection cement paste is tested, and (diameter 10mm is highly 25mm) two up and down to cylinder sample
Face is first polished with sand paper, not seal ring oxygen；Epoxy resin is smeared to cylinder sample side, air-dry 24 hours, obtained epoxy
Resin layer with a thickness of 0.5mm.Positive and negative polarities label is carried out in cylinder sample upper and lower side with marker to mark with specimen coding, then
The sample marked is put into saturated calcium hydroxide solution and is conserved.By preparing 5wt% concentration calcium hydroxide solution and 5wt%
Concentration metabisulfite solution stands one day and makes solution dissolution abundant.
Sample is mounted in electrochemical appliance shown in FIG. 1, powers on that (pulse voltage is 30V, and the burst length is
20s), it is powered after accelerating to the 3rd day, sample is taken out in power-off.Using X-ray μ CT test equipment to the cylinder for the acceleration that has been powered
Sample carries out lossless X-ray μ CT test, acquires image information, handles data.
After X-ray μ CT is tested, sample is taken out, is reinstalled in electrochemical appliance that (catholyte and anolyte have replaced
It is changed to newly with solution), power on (pulse voltage is 30V, and the burst length is 20s), after energization accelerates to the 3rd day, powers off, it will
Sample takes out.It carries out lossless X-ray μ CT using cylinder sample of the X-ray μ CT test equipment to the acceleration that has been powered to test, acquisition
Image information handles data.
It is further continued for circulation 6 times, experiment terminates.
Electric pulse accelerates sulfate ion to enter inside sample, in conjunction with hydrated product inside sample, generates gypsum and calcium
Aluminite, hole are gradually filled, and pore volume is fewer and fewer.First time electrochemistry accelerates (3h) and second of electrochemistry to accelerate knot
The total pore volume of sample is as shown in Fig. 2, as shown in Figure 2, with the extension of electrochemistry acceleration time, the hole of sample is total after beam
Volume decline, shows that sample is corroded, it was demonstrated that electric pulse accelerates the feasibility of sulfate ion rapid erosion method.
Embodiment 2
The present embodiment selection cement mortar is tested, and (diameter 10mm is highly 25mm) two up and down to cylinder sample
Face is first polished with sand paper, not seal ring oxygen；Epoxy resin is smeared to cylinder sample side, air-dry 24 hours, obtained epoxy
Resin layer with a thickness of 0.5mm.Positive and negative polarities label is carried out in cylinder sample upper and lower side with marker to mark with specimen coding, then
The sample marked is put into saturated calcium hydroxide solution and is conserved.By prepare 40wt% concentration calcium hydroxide solution with
40wt% concentration metabisulfite solution stands one day and makes solution dissolution abundant.
Sample is mounted in electrochemical appliance, is powered on (pulse voltage is 40V, and the burst length is 30s), is powered and adds
For speed to after the 3rd day, sample is taken out in power-off.Nothing is carried out using cylinder sample of the X-ray μ CT test equipment to the acceleration that has been powered
X-ray μ CT test is damaged, image information is acquired, handles data.
After X-ray μ CT is tested, sample is taken out, is reinstalled in electrochemical appliance that (catholyte and anolyte have replaced
It is changed to newly with solution), power on (pulse voltage is 40V, and the burst length is 30s), after energization accelerates to the 3rd day, powers off, it will
Sample takes out.It carries out lossless X-ray μ CT using cylinder sample of the X-ray μ CT test equipment to the acceleration that has been powered to test, acquisition
Image information handles data.
It is further continued for circulation 6 times, experiment terminates.
X-ray μ CT test result shows that sample internal void gradually decreases, and shows that sample is gradually corroded.
Embodiment 3
The present embodiment selection cement concrete is tested, and (diameter 10mm is highly 25mm) up and down two to cylinder sample
A face is first polished with sand paper, not seal ring oxygen；Epoxy resin is smeared to cylinder sample side, air-dry 24 hours, obtained ring
Oxygen resin layer with a thickness of 0.5mm.Positive and negative polarities label is carried out in cylinder sample upper and lower side with marker to mark with specimen coding,
The sample marked is put into saturated calcium hydroxide solution again and is conserved.By prepare 15wt% concentration calcium hydroxide solution with
15wt% concentration metabisulfite solution stands one day and makes solution dissolution abundant.
Sample is mounted in electrochemical appliance, is powered on (pulse voltage is 100V, and the burst length is 20s), is powered
After accelerating to the 3rd day, sample is taken out in power-off.It is carried out using cylinder sample of the X-ray μ CT test equipment to the acceleration that has been powered
Lossless X-ray μ CT test, acquires image information, handles data.
After X-ray μ CT is tested, sample is taken out, is reinstalled in electrochemical appliance that (catholyte and anolyte have replaced
It is changed to newly with solution), power on (pulse voltage is 100V, and the burst length is 20s), after energization accelerates to the 3rd day, power-off,
Sample is taken out.Lossless X-ray μ CT is carried out using cylinder sample of the X-ray μ CT test equipment to the acceleration that has been powered to test, and is adopted
Collect image information, handles data.
It is further continued for circulation 6 times, experiment terminates.
X-ray μ CT test result shows that sample internal void gradually decreases, and shows that sample is gradually corroded.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of cement-based material is by the rapid detection method of sulfate attack, which is characterized in that comprise the following steps:
(1) it is dipped in saturated calcium hydroxide solution and is supported after epoxy resin layer is arranged in cement-based material sample surrounded surface
Shield；
(2) the obtained sample that conserves is placed in progress electrochemistry acceleration in electrochemical appliance, X-ray μ CT is carried out after acceleration
Detection；
Sample is placed in electrochemical appliance again after the test and carries out electrochemistry acceleration and detection, is recycled with this, until
Detection terminates；
The catholyte of the electrochemical appliance is sulfate liquor, and anolyte is strong base solution.
2. detection method according to claim 1, which is characterized in that cement-based material sample is in circle in the step (1)
Bar shape, the surrounding are the side of cylindrical body.
3. detection method according to claim 2, which is characterized in that in the step (1) height of cylindrical body be 20~
40mm, diameter are 5~20mm.
4. detection method according to any one of claims 1 to 3, which is characterized in that epoxy resin in the step (1)
Layer with a thickness of 0.3~1mm.
5. detection method according to claim 1, which is characterized in that sulfate liquor is sodium sulphate in the step (2)
Solution or potassium sulfate solution；
Mass concentration≤42.5% of the sulfate liquor.
6. detection method according to claim 1, which is characterized in that strong base solution is sodium hydroxide in the step (2)
Solution or potassium hydroxide solution；
Mass concentration≤42.5% of the strong base solution.
7. detection method according to claim 1, which is characterized in that electrochemistry accelerator applies in the step (2)
Be pulse voltage, the pulse voltage be 10~150V, the burst length be 10~60s.
8. detection method according to claim 1, which is characterized in that in the step (2) each electrochemistry accelerate when
Between independently be 1~5h.
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| CN110208175A (en) * | 2019-07-09 | 2019-09-06 | 济南大学 | A method of it can using bag filter test C3S aquation system sulphate-corrosion resistance |
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