CN114279779A - Method for preparing cement clinker test sample in laboratory - Google Patents
Method for preparing cement clinker test sample in laboratory Download PDFInfo
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- CN114279779A CN114279779A CN202111475276.1A CN202111475276A CN114279779A CN 114279779 A CN114279779 A CN 114279779A CN 202111475276 A CN202111475276 A CN 202111475276A CN 114279779 A CN114279779 A CN 114279779A
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000004568 cement Substances 0.000 title claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 29
- 239000010883 coal ash Substances 0.000 claims abstract description 23
- 238000001354 calcination Methods 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000013329 compounding Methods 0.000 claims abstract description 3
- 238000002360 preparation method Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 10
- 235000012054 meals Nutrition 0.000 claims description 5
- 238000001073 sample cooling Methods 0.000 claims description 5
- 238000010583 slow cooling Methods 0.000 claims description 4
- 238000010791 quenching Methods 0.000 claims description 3
- 230000000171 quenching effect Effects 0.000 claims description 2
- 238000000265 homogenisation Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 75
- 235000012431 wafers Nutrition 0.000 description 33
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 238000003825 pressing Methods 0.000 description 7
- 238000007664 blowing Methods 0.000 description 5
- 239000000292 calcium oxide Substances 0.000 description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 239000012856 weighed raw material Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 235000019738 Limestone Nutrition 0.000 description 3
- 239000010881 fly ash Substances 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 239000006028 limestone Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000011005 laboratory method Methods 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid group Chemical group C(C1=CC=CC=C1)(=O)O WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- JTRONPPAUSSTQI-UHFFFAOYSA-N ethane-1,2-diol;ethanol Chemical compound CCO.OCCO JTRONPPAUSSTQI-UHFFFAOYSA-N 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000006101 laboratory sample Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
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Abstract
The invention provides a method for preparing a cement clinker test sample in a laboratory. The method comprises the following steps: the method comprises the following steps of proportioning raw materials and coal ash, and then sequentially grinding, mixing, preparing a sample sheet, drying and calcining the sample sheet, and cooling the sample sheet to obtain a finished sample product; wherein, the compounding includes: adding water into the raw materials and the coal ash, uniformly stirring, and sequentially passing the uniformly stirred wet materials through the first screen 1 time and the second screen 2-3 times. The method can greatly improve the homogenization degree of the laboratory prepared sample and keep the consistency of the test sample in the test process.
Description
Technical Field
The invention relates to the technical field of cement clinker, in particular to a method for preparing a cement clinker test sample in a laboratory.
Background
When the physical and chemical properties of the cement clinker are studied in a laboratory, a cement clinker test sample is firstly prepared in the laboratory. The existing preparation methods of cement clinker test samples in a laboratory are mostly as follows: mixing raw materials and coal ash, scattering particles during mixing, generally stirring while pressing, adding water into the materials, applying a certain pressure to pressurize, and keeping constant for a certain time to ensure that the density of the material section is uniform. The sample amount obtained by the traditional laboratory sample preparation method is small, and the method is not enough for physicochemical inspection of cement clinker; and may not be reproducible for preparing larger sample volumes.
Therefore, there is a need to study the existing laboratory methods for preparing cement clinker test samples.
Disclosure of Invention
To this end, the present invention provides a method for laboratory preparation of cement clinker test samples.
Specifically, the method for preparing the cement clinker test sample in the laboratory provided by the invention comprises the steps of using raw materials and coal ash as raw materials to prepare materials, and sequentially carrying out grinding, mixing, sample sheet preparation, sample sheet drying and calcining, and sample sheet cooling to obtain a sample finished product; wherein, the compounding includes: adding water into the raw materials and the coal ash, uniformly stirring, and sequentially passing the uniformly stirred wet materials through the first screen 1 time and the second screen 2-3 times.
The invention discovers that the fineness of the raw materials for preparing the cement clinker is small, when the raw materials are mixed by adding water, the adhesion is increased, the materials are more easily adhered into a mass, and the homogenization degree of a test sample is further reduced. The uniformly mixed wet material is mixed by adopting the mixing mode, particularly under the condition of the screening and mixing times, the aggregation and adhesion among particles are favorably eliminated or weakened, and the segregation phenomenon is avoided, so that the uniformity of the obtained wet material is greatly improved, and the consistency of a cement clinker test sample is further maintained.
Preferably, the aperture of the first screen is 0-5mm larger than the maximum specification of ground raw materials and coal ash; the aperture of the second screen is 5-10mm larger than that of the first screen. Under the conditions, the consistency of cement clinker test samples is kept, and meanwhile, the screening efficiency is favorably improved. It can be understood that when the materials on the screen cannot be smoothly screened due to the fact that the materials are agglomerated and adhered and then the sizes of the materials are larger than the aperture of the screen holes, the materials can be broken up in modes of beating and the like to ensure that all the materials on the screen can be smoothly screened.
Preferably, the method for preparing the sample wafer comprises the following steps: and (3) placing the mixed wet material into a test mold according to 220g of the wet material after mixing, and maintaining the pressure for 40-80s under the condition of 50-70 tons of pressurization to obtain a sample wafer.
Preferably, the addition amount of the coal ash is 2-3% of the mass of the raw meal.
Preferably, the amount of water added is 8-10% of the total mass of the raw meal and the coal ash.
Preferably, the drying temperature is 100-120 ℃, and the drying time is 10-15 hours.
Preferably, the calcining comprises: and heating the dried sample wafer to 900-800 ℃, cooling to 600-800 ℃, and calcining according to a preset heating program.
Preferably, the sample cooling includes a rapid cooling method or a slow cooling method.
In particular, the amount of the solvent to be used,
the quenching mode is as follows: taking the calcined sample wafer together with the saggar out of the high-temperature furnace, pouring the sample wafer into a cage-type rotary cooling machine, quickly turning over to crush the sample wafer, and simultaneously reducing the temperature of the sample wafer to be below 80 ℃ by adopting blast cooling to obtain a sample finished product;
the slow cooling mode is as follows: and (3) the calcined sample wafer and the saggar are cooled to 800-.
Based on the technical scheme, the invention has the following beneficial effects:
the method can greatly improve the homogenization degree of the laboratory prepared sample and keep the consistency of the test sample in the test process.
Drawings
FIG. 1 is a lithofacies diagram of a test sample prepared in example 1 of the present invention;
FIG. 2 is a phase diagram of a test sample prepared in comparative example 1 of the present invention.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. The reagents or instruments used are conventional products available from regular distributors, not indicated by the manufacturer.
Example 1
The method for preparing the cement clinker test sample in the laboratory provided by the embodiment comprises the following steps:
(1) ingredients
Raw materials (particle size is less than or equal to 3 mm): the total weight is 1200g, wherein 1051.2g of limestone, 21.6g of iron ore dressing, 87.6g of fly ash and 39.6g of iron ore;
coal ash (particle size less than or equal to 0.2 mm): 26.8 g;
water: 110.4 g.
(2) Mixing material
Grinding accurately weighed raw materials and coal ash, sieving with a 0.355mm square-hole sieve, putting into a mortar stirring pot, adding water, and rotating at 140 + -5 r/min; stirring for 2 minutes under the revolution of 62 +/-5 r/min, and then, passing the stirred wet material through a 0.5mm square-hole sieve and then mixing for 2 times through a 0.9mm square-hole sieve.
(3) Preparation of coupons
Accurately weighing 200 +/-1 g of the stirred wet material, and pressing one sample wafer, namely six sample wafers; and pressing the sample by using a manual and electric integrated sample press, putting the sample into a test mold, and pressurizing for 60 tons and maintaining the pressure for 60 s.
(4) Sample drying and calcining
Putting the pressed sample wafer into an electrothermal blowing drying oven at 105 ℃ for continuous drying for 12 hours; placing the dried gasket at the bottom of the sagger, and vertically placing the sample piece for calcination on the gasket; and (3) heating the high-temperature furnace to 950 ℃, then cooling to 700 ℃, then putting the sample wafer and the sagger into the high-temperature furnace together, and heating according to a preset heating program: reach 950 ℃ over 45 minutes; preserving the heat for 30 minutes at 950 ℃; reaching 1450 ℃ after 35 minutes of heat preservation; and keeping the temperature for 15 minutes according to the test requirement, and calcining the sample wafer.
(5) Sample cooling
And (3) rapidly taking the calcined sample wafer together with the saggar out of the high-temperature furnace, pouring the sample wafer into a cage-type rotary cooling machine by using a turnover device, rapidly turning over to crush the sample wafer, and simultaneously carrying out forced air cooling for 5 minutes by using a fan to reduce the temperature of the sample wafer to be below 80 ℃.
Example 2
The method for preparing the cement clinker test sample in the laboratory provided by the embodiment comprises the following steps:
(1) ingredients
Raw materials (particle size is less than or equal to 5 mm): the total weight is 1200g, wherein 1016.7g of limestone, 91.4g of clay, 52.2g of fly ash and 16.6g of iron ore are contained;
coal ash (particle size less than or equal to 0.3 mm): 23.1 g;
water: 92.1 g.
(2) Mixing material
Grinding accurately weighed raw materials and coal ash samples, putting the ground raw materials and coal ash samples into a mortar stirring pot, adding water, and rotating at 140 +/-5 r/min; stirring for 2 minutes under the revolution of 62 +/-5 r/min, and then, passing the stirred wet material through a 0.6mm square-hole sieve and then through a 1.0mm square-hole sieve for mixing for 2 times.
(3) Preparation of coupons
Accurately weighing 200 +/-1 g of the stirred wet material, and pressing one sample wafer, namely six sample wafers; and pressing the sample by using a manual and electric integrated sample press, putting the sample into a test mold, and pressurizing for 60 tons and maintaining the pressure for 60 s.
(4) Sample drying and calcining
Putting the pressed sample wafer into an electrothermal blowing drying oven at 105 ℃ for continuous drying for 12 hours; placing the dried gasket at the bottom of the sagger, and vertically placing the sample piece for calcination on the gasket; and (3) heating the high-temperature furnace to 950 ℃, then cooling to 700 ℃, then putting the sample wafer and the sagger into the high-temperature furnace together, and heating according to a preset heating program: reach 950 ℃ over 45 minutes; preserving the heat for 30 minutes at 950 ℃; reaching 1450 ℃ after 35 minutes of heat preservation; and keeping the temperature for 15 minutes according to the test requirement, and calcining the sample wafer.
(5) Sample cooling
After the calcination is finished, the high-temperature furnace is automatically powered off according to a set program, the sample and the saggar are continuously placed in the high-temperature furnace for calcination, when the temperature naturally drops to 900 ℃, the calcined sample and the saggar are rapidly taken out of the high-temperature furnace, the sample wafer is poured into a cage type rotary cooling machine by using a turning device and is rapidly turned over to be crushed, and meanwhile, the sample wafer is cooled for 5 minutes by using air blowing of an electric fan, so that the temperature of the sample wafer is reduced to be below 80 ℃.
Example 3
The method for preparing the cement clinker test sample in the laboratory provided by the embodiment comprises the following steps:
the method for preparing the cement clinker test sample in the laboratory provided by the embodiment comprises the following steps:
(1) ingredients
Raw materials (particle size is less than or equal to 5 mm): the total weight is 1200g, wherein 1019.3g of limestone, 67.1g of sludge, 86.8g of fly ash and 16.6g of iron ore are contained;
coal ash (particle size less than or equal to 0.1 mm): 23.2 g;
water: 92.1 g.
(2) Mixing material
Grinding accurately weighed raw materials and coal ash samples, putting the ground raw materials and coal ash samples into a mortar stirring pot, adding water, and rotating at 140 +/-5 r/min; stirring for 2 minutes under the revolution of 62 +/-5 r/min, and then, passing the stirred wet material through a 0.7mm square-hole sieve and then through a 1.1mm square-hole sieve for mixing for 2 times.
(3) Preparation of coupons
Accurately weighing 200 +/-1 g of the stirred wet material, and pressing one sample wafer, namely six sample wafers; and pressing the sample by using a manual and electric integrated sample press, putting the sample into a test mold, and pressurizing for 60 tons and maintaining the pressure for 60 s.
(4) Sample drying and calcining
Putting the pressed sample wafer into an electrothermal blowing drying oven at 105 ℃ for continuous drying for 12 hours; placing the dried gasket at the bottom of the sagger, and vertically placing the sample piece for calcination on the gasket; and (3) heating the high-temperature furnace to 950 ℃, then cooling to 700 ℃, then putting the sample wafer and the sagger into the high-temperature furnace together, and heating according to a preset heating program: reach 950 ℃ over 45 minutes; preserving the heat for 30 minutes at 950 ℃; reaching 1450 ℃ after 35 minutes of heat preservation; and keeping the temperature for 15 minutes according to the test requirement, and calcining the sample wafer.
(5) Sample cooling
After the calcination is finished, the high-temperature furnace is automatically powered off according to a set program, the sample and the saggar are continuously placed in the high-temperature furnace for calcination, when the temperature naturally drops to 900 ℃, the calcined sample and the saggar are rapidly taken out of the high-temperature furnace, the sample wafer is poured into a cage type rotary cooling machine by using a turning device and is rapidly turned over to be crushed, and meanwhile, the sample wafer is cooled for 5 minutes by using air blowing of an electric fan, so that the temperature of the sample wafer is reduced to be below 80 ℃.
Comparative example 1
The laboratory method for preparing cement clinker test samples provided in this comparative example 1 differs from example 1 only in that:
step (2) mixing materials: grinding accurately weighed raw materials and coal ash samples, putting the ground raw materials and coal ash samples into a mortar stirring pot, adding water, and rotating at 140 +/-5 r/min; and (3) revolving at the rotating speed of 62 +/-5 r/min, stirring for 2 minutes, passing the stirred wet material through a 0.5mm square-hole sieve, and then mixing for 4 times through a 0.9mm square-hole sieve.
Test example
The test samples prepared in examples 1 to 3 and comparative example 1 were examined for the f-CaO content.
The method for detecting the content of f-CaO comprises the following steps: weighing about 0.5g of test sample, accurately measuring to 0.000l g, placing into a 250mL dry conical flask, adding 30mL of ethylene glycol-ethanol solution, placing a dry stirrer, installing a condenser tube, placing on a free calcium oxide tester, stirring the solution at a proper speed, simultaneously heating and boiling, when the condensed ethanol begins to continuously drip down, continuously heating and slightly boiling for 5min under stirring, taking off the conical flask, and immediately titrating with benzoic acid-anhydrous ethanol standard titration solution until reddish disappears.
The results are shown in Table 1.
TABLE 1
| Test sample | f-CaO content |
| Example 1 | 0.32％ |
| Example 2 | 0.30％ |
| Example 3 | 0.38％ |
| Comparative example 1 | 0.77％ |
The results show that the f-CaO content values of examples 1-3 are significantly lower than comparative example 1, indicating a higher homogeneity of the test samples prepared by the method of the invention.
FIGS. 1 and 2 are lithofacies diagrams of test samples of example 1 and comparative example 1, respectively, from which it can be seen that the various minerals in the test samples prepared in example 1 are uniformly distributed; the test samples prepared in comparative example 1 had a heterogeneous mineral distribution.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for preparing cement clinker test samples in a laboratory is characterized in that raw materials and coal ash are used as raw materials for proportioning, and then grinding, mixing, sample preparation, sample drying and calcining and sample cooling are sequentially carried out to obtain a finished sample; wherein, the compounding includes: adding water into the raw materials and the coal ash, uniformly stirring, and sequentially passing the uniformly stirred wet materials through the first screen 1 time and the second screen 2-3 times.
2. The method of laboratory preparation of cement clinker test samples as claimed in claim 1, wherein the first screen has a mesh size 0-5mm larger than the maximum size of ground raw meal and coal ash; the aperture of the second screen is 5-10mm larger than that of the first screen.
3. The method for laboratory preparation of cement clinker test samples according to claim 1 or 2, wherein the method for sample preparation comprises: and (3) placing the mixed wet material into a test mold according to 220g of the wet material after mixing, and maintaining the pressure for 40-80s under the condition of 50-70 tons of pressurization to obtain a sample wafer.
4. A method for laboratory preparation of test samples of cement clinker according to any of claims 1 to 3, characterized in that the coal ash is added in an amount of 2 to 3% of the mass of the raw meal.
5. A method for laboratory preparation of test samples of cement clinker according to any of claims 1 to 4, characterized in that the water is added in an amount of 8 to 10% of the total mass of raw meal and coal ash.
6. The method for laboratory preparation of cement clinker test samples as claimed in any one of claims 1 to 5, wherein the drying temperature is 100 ℃ and 120 ℃ for 10 to 15 hours.
7. The method for laboratory preparation of cement clinker test samples according to any of claims 1 to 6, wherein the calcination comprises: and heating the dried sample wafer to 900-800 ℃, cooling to 600-800 ℃, and calcining according to a preset heating program.
8. The method for laboratory preparation of cement clinker test specimens as defined in any one of claims 1 to 7, wherein said specimen cooling comprises a quench cooling mode or a slow cooling mode.
9. The method for laboratory preparation of cement clinker test samples as claimed in claim 8, wherein said quenching means is: and (3) rapidly taking the calcined sample wafer and the saggar out of the high-temperature furnace, pouring the sample wafer into a cage type rotary cooling machine, rapidly turning over to crush the sample wafer, and simultaneously reducing the temperature of the sample wafer to be below 80 ℃ by adopting blast cooling to obtain a sample finished product.
10. The method of laboratory preparing cement clinker test samples of claim 8, wherein the slow cooling mode is: and (3) the calcined sample wafer and the saggar are cooled to 800-.
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