CN115838254A - Molybdenum tailing micro powder admixture for mortar or concrete and preparation method thereof - Google Patents
Molybdenum tailing micro powder admixture for mortar or concrete and preparation method thereof Download PDFInfo
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- CN115838254A CN115838254A CN202211421138.XA CN202211421138A CN115838254A CN 115838254 A CN115838254 A CN 115838254A CN 202211421138 A CN202211421138 A CN 202211421138A CN 115838254 A CN115838254 A CN 115838254A
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 90
- 239000011733 molybdenum Substances 0.000 title claims abstract description 90
- 239000004567 concrete Substances 0.000 title claims abstract description 21
- 239000004570 mortar (masonry) Substances 0.000 title claims abstract description 21
- 239000000843 powder Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000498 ball milling Methods 0.000 claims abstract description 41
- 239000002245 particle Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 20
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims abstract description 12
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 12
- 239000000176 sodium gluconate Substances 0.000 claims abstract description 12
- 229940005574 sodium gluconate Drugs 0.000 claims abstract description 12
- 235000012207 sodium gluconate Nutrition 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 10
- 229920005646 polycarboxylate Polymers 0.000 claims description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 239000008030 superplasticizer Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 17
- 238000000227 grinding Methods 0.000 abstract description 14
- 239000000126 substance Substances 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000012752 auxiliary agent Substances 0.000 abstract 1
- 230000000717 retained effect Effects 0.000 abstract 1
- 238000001238 wet grinding Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 22
- 238000005054 agglomeration Methods 0.000 description 9
- 230000002776 aggregation Effects 0.000 description 9
- 230000008569 process Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 235000010755 mineral Nutrition 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000004566 building material Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000009837 dry grinding Methods 0.000 description 2
- 238000005065 mining Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241000282994 Cervidae Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000010883 coal ash Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009440 infrastructure construction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a molybdenum tailing micro powder admixture used in mortar or concrete and a preparation method thereof, comprising molybdenum tailings, triethanolamine accounting for 0.04-0.08% of the mass of the molybdenum tailings, sodium gluconate accounting for 0.1-0.2% of the mass of the molybdenum tailings and a polycarboxylic acid water reducing agent accounting for 0.05-0.15% of the mass of the molybdenum tailings; the molybdenum tailings and water are fully mixed, then triethanolamine, sodium gluconate and a polycarboxylic acid water reducing agent are added, mixed and ball-milled for 20-30min, and the admixture of the molybdenum tailings micropowder is obtained after drying. According to the invention, by adopting a technical method of physical wet grinding and chemical grinding aid for the molybdenum tailings, the fineness and the dispersity of particles are improved while the ball milling time and the energy consumption are greatly reduced, and the activity of the molybdenum tailings micropowder serving as an admixture in mortar or concrete is improved by the retained chemical auxiliary agent.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to a molybdenum tailing micro powder admixture used in mortar or concrete and a preparation method thereof.
Background
Mineral resources are gradually being depleted as an irreproducible resource, and tailings as a secondary resource are highly regarded by countries in the world. Practice proves that comprehensive utilization of tailing resources can change waste into valuable, can convert harm into profit, and is needed for economic construction and environmental protection.
China is a large molybdenum resource country, and with the increase of the exploitation amount of molybdenum ores, a large amount of molybdenum tailings are generated. The ore deposits discovered at present are mostly low-grade ore deposits, so the tailing production rate is high in the ore dressing process, the tailing amount is large, the occupied area is wide, and the environmental pollution and the potential hazard are large. Meanwhile, a large amount of molybdenum tailings are not recycled, so that resource waste is caused, and the sustainable development of the mine is severely restricted. The molybdenum tailings are a secondary resource, and have the characteristics of large stockpiling amount, complex components, low utilization rate and the like, and the problem of recycling the tailings is urgent.
The admixture is an important component of modern concrete materials, accounts for about 15-55% of gelled materials in single-component concrete, and the price of raw materials such as the admixture is greatly increased due to the large demand of infrastructure construction in China on the concrete materials.
At present, research on preparation of molybdenum tailings into micro powder for use in concrete admixture is carried out, and the preparation process is carried out by directly ball-milling the molybdenum tailings, but the method has low efficiency, the ball-milling time does not significantly reduce the particle size, the particle size of the particles is not significantly reduced after the ball-milling time is more than 60min, as shown in figure 1, the micro powder is easy to agglomerate, and for the agglomeration of the particles, a good dispersion method is not available at present, as shown in figure 2 [1,2].
Therefore, the method has the advantages of improving the ball milling efficiency of the molybdenum tailings, avoiding particle agglomeration and improving the activity of the prepared molybdenum tailing micro powder, and is an urgent problem to be solved in preparing admixtures in the molybdenum tailing building material utilization.
[1] Treimor, diriping, fractal study of milled molybdenum tailings size distribution [ J ] mining research and development, 2016,36 (11): 32-35.
[2] Experimental study on preparing mineral admixtures by using molybdenum tailings [ J ] mineral product protection and utilization, 2017, (4) 90-95.
Disclosure of Invention
The invention aims to solve the problems of low ball milling efficiency, insignificant ball milling effect, easy particle agglomeration and low particle activity in the ball milling process in the prior art, and the invention aims to provide a molybdenum tailing micropowder admixture for mortar or concrete and a preparation method thereof.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a molybdenum tailing micro powder admixture used in mortar or concrete comprises molybdenum tailings, triethanolamine accounting for 0.04-0.08% of the mass of the molybdenum tailings, sodium gluconate accounting for 0.1-0.2% of the mass of the molybdenum tailings and a polycarboxylic acid water reducing agent accounting for 0.05-0.15% of the mass of the molybdenum tailings.
Further, the molybdenum tailings mainly contain SiO 2 、Al 2 O 3 And Fe 2 O 3 The sum of the content of the molybdenum tailings, the molybdenum tailings and the molybdenum tailings is not less than 80wt%, and the particle size of the molybdenum tailings is 0.1-0.3mm.
Furthermore, the polycarboxylate superplasticizer is synthesized by adopting a methyl allyl polyoxyethylene ether macromonomer, has a solid content of more than or equal to 40 percent, and is light yellow viscous liquid.
The invention also provides a preparation method of the molybdenum tailing micro powder admixture, which comprises the steps of fully mixing molybdenum tailings and water, adding triethanolamine, sodium gluconate and a polycarboxylic acid water reducing agent, mixing and ball-milling for 20-30min, and drying to obtain the molybdenum tailing micro powder admixture.
Further, the mass ratio of the molybdenum tailings to the water is 1:1.0-1.2.
Further, the ball milling rotating speed is 100-200r/min, the ball-material ratio is 1-3:1
According to the invention, triethanolamine, sodium gluconate and a polycarboxylate water reducer are compounded to serve as a chemical grinding aid, and firstly, the triethanolamine, the sodium gluconate and the polycarboxylate water reducer are all surfactants, so that the surface energy of molybdenum tailing particles can be reduced, and the molybdenum tailing particles are more easily crushed in the friction and collision process; secondly, triethanolamine is used as an early strength agent, sodium gluconate is used as a retarder, and a polycarboxylic acid water reducing agent is used as a water reducing agent, so that the working performance and the early strength of mortar or concrete are improved; and the three are always kept in the admixture of the molybdenum tailing micropowder in the preparation process, which is beneficial to improving the activity of the molybdenum tailing micropowder serving as the admixture in mortar or concrete. In a word, the molybdenum tailings, the three components and the molybdenum tailings are mixed and ball-milled, so that the ball-milling efficiency is improved, the particle agglomeration is avoided, when the molybdenum tailings, the early strength of mortar or concrete can be improved, the working performance of the mortar or concrete is improved, the activity is improved, and the doping amount of an additive in the preparation of the mortar or concrete is reduced.
Compared with the prior direct ball milling mode, the invention has the advantages that:
(1) The ball milling time is shortened by more than 50%, the efficiency is improved by more than 50%, and the energy consumption of ball milling is greatly reduced;
(2) The amount of the 45 mu m sieve residue of the ball-milled particles is reduced by 500 percent, so that the fineness of the particles is greatly improved;
(3) The molybdenum tailing micro powder particles have good dispersibility, and particle agglomeration caused by the increase of the specific surface area of the particles in the direct ball milling process is avoided;
(4) The chemical grinding aid is combined, so that the grinding efficiency and the particle dispersion are improved, and the chemical grinding aid is always kept in the micro powder admixture, so that the activity of the prepared molybdenum tailing admixture is improved, and the molybdenum tailing admixture is more suitable for being used in mortar or concrete.
Drawings
Fig. 1 shows the effect of direct physical ball milling time on the particle size distribution of molybdenum tailings.
As shown in fig. 1, the direct physical ball milling method has low efficiency, the ball milling time does not significantly reduce the particle size, and the particle size is not significantly reduced any more after the ball milling time is longer than 60 min.
FIG. 2 is a diagram of a molybdenum micropowder admixture directly subjected to physical ball milling for 60 min.
As shown in figure 2, the molybdenum tailing micro powder is easy to agglomerate.
FIG. 3 is a graph showing the effect of ball milling time on the particle size distribution of molybdenum tailings in the method of the present invention.
As shown in fig. 3, compared with direct physical ball milling, when the method of the present invention is used for ball milling molybdenum tailings, the particle size of the molybdenum tailings particles is significantly reduced with the increase of the ball milling time.
Fig. 4 is a diagram of a substance of the molybdenum tailing micropowder prepared in example 1.
As shown in figure 4, the molybdenum tailings are ball-milled by the method of the invention, the particle dispersibility is good, and no agglomeration is seen.
FIGS. 5 (a) - (e) show the water demand ratio (a), the fluidity ratio (b), the change of fluidity over time (c) for 1h, the 7d activity index (d) and the 28d activity index (e) of the mortar prepared by using the molybdenum tailing micro powder prepared in example 1 and comparative examples 1-7 as admixtures, respectively.
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited to the examples.
It should be noted that the molybdenum tailings adopted in this embodiment are derived from molybdenum tailings produced by mining group of illinoen deer borygmus of black dragon river after molybdenum metal is refined, and mainly contain SiO 2 、Al 2 O 3 And Fe 2 O 3 。
Example 1
Mixing molybdenum tailings and water according to a mass ratio of 1:1, putting the mixture into a ball mill, adding triethanolamine accounting for 0.04 percent of the mass of the molybdenum tailings, 0.2 percent of sodium gluconate and 0.1 percent of polycarboxylic acid water reducing agent, and stirring the mixture at the rotating speed of the ball mill of 150r/min in a ball-to-material ratio of 2:1, ball milling for 20min, and finally drying at 50 ℃ to obtain the molybdenum tailing micropowder admixture with the water content of less than or equal to 1%.
Comparative example 1
The method adopts a direct dry grinding mode, the rotating speed of the ball mill is 150r/min, and the ball-material ratio is 2:1, ball milling for 40min.
Comparative example 2
The method adopts a direct dry grinding mode, the rotating speed of the ball mill is 150r/min, and the ball-material ratio is 2:1, ball milling for 80min.
Comparative example 3
The difference is that only triethanolamine accounting for 0.04 percent of the mass of the molybdenum tailings is added and the ball milling time is 40min as in example 1.
Comparative example 4
The difference is that only sodium gluconate accounting for 0.2 percent of the mass of the molybdenum tailings is added, and the ball milling time is 40min as in example 1.
Comparative example 5
The difference is only that a polycarboxylate superplasticizer accounting for 0.1 percent of the mass of the molybdenum tailings is added, and the ball milling time is 40min as in example 1.
Comparative example 6
The only difference was that only commercial grinding aid I (produced by Shandong Mao chemical Co., ltd., PET-V200 grinding aid) was added and the ball milling time was 40min as in example 1.
Comparative example 7
The only difference from example 1 was that only commercial grinding aid II (Henan scientific chemical product Co., ltd., AMP-95 grinding aid) was added, and the ball milling time was 40min.
TABLE 1 results of molybdenum micropowder obtained in example 1 and comparative examples 1 to 7
As shown in table 1, the results of the tests on the particle size D (50), the specific surface area, and the 45um sieve residue in the molybdenum tailings micropowder particles obtained in example 1 and comparative examples 1 to 7 are shown.
As can be seen from comparative example 1, when the molybdenum tailing micro powder is prepared by directly adopting a ball milling method, the ball milling is carried out for 40min, particles are not obviously agglomerated, the medium particle size is 18.1um, and the comparative area is 340m 2 And the 45um screen residue is 26.5, the specific surface area of the particles is small, and the activity requirement is not met.
As can be seen from comparative example 2, when the molybdenum tailing micropowder is prepared by directly adopting the ball milling method, obvious agglomeration occurs when the ball milling is carried out for 80min, the medium particle size is 15.9um, and the comparative area is 337m 2 The grain size is 48.1 percent in a 45-micron sieve margin/km, the sieve margin is obviously increased compared with that of the comparative example 1, the specific surface area of the grains is small, serious agglomeration occurs, the activity is reduced, the grains cannot be used as admixture, and the comparative example 2 also shows that the grains cannot be effectively thinned due to the fact that the ball milling time is prolonged.
The results in table 1 show that the problem of particle agglomeration can be solved when the three materials are independently adopted as the grinding aid, the ball milling time is also reduced to a certain extent, but the particle size is not obviously reduced, and the 45um screen residue is not obviously reduced.
Comparative examples 6 and 7 are both grinding aid test results purchased in the market, and as can be seen from table 1, the grinding aid purchased in the market has a certain improvement in effect compared with comparative examples 1 to 5, but is not obvious, that is, the comparative area is not significantly increased, and the screen allowance of 45um is reduced.
According to the invention, triethanolamine, sodium gluconate and a polycarboxylate water reducer are compounded for ball milling, and the results in Table 1 show that after the three materials are compounded and used as a grinding aid, the median particle size of particles is basically consistent with the ratio of 1-7 by ball milling for 20min, and the specific surface area of the particles is remarkably increased, so that the grinding aid achieves the aim that 452m 2 The/kg, 45um screen allowance is reduced to 5.1%, the particle milling effect is obvious, and the method has better technical advantages.
Table 2 shows the performance results of the mortar prepared by using the molybdenum tailing micro powder prepared in example 1 and comparative examples 1-7 as an admixture. The test method is carried out according to the standard coal ash (GB/T1596-2017) used in cement and concrete and the recycled micropowder (JG/T573-2020) used in concrete and mortar. FIGS. 5 (a) - (e) show the water demand ratio, fluidity ratio, change of fluidity over 1h, activity index at 7d and activity index at 28d of the mortar prepared by using the molybdenum tailing micro powder prepared in example 1 and comparative examples 1-7 as admixtures, respectively. As can be seen from FIG. 5, the mortar prepared by using the molybdenum tailing micropowder (example 1) prepared by the method of the invention as the admixture has the best main performance index parameters, and meets the performance requirements of the admixture for mortar and concrete.
TABLE 2 mortar Performance results for the preparation of molybdenum tailings micropowder obtained in example 1 and comparative examples 1-7 as an admixture
Claims (6)
1. A molybdenum tailing micro powder admixture used in mortar or concrete is characterized in that: comprises molybdenum tailings, triethanolamine accounting for 0.04-0.08% of the mass of the molybdenum tailings, sodium gluconate accounting for 0.1-0.2% of the mass of the molybdenum tailings and a polycarboxylic acid water reducing agent accounting for 0.05-0.15% of the mass of the molybdenum tailings.
2. The admixture of molybdenum tailings micropowder of claim 1, wherein: the molybdenum tailings mainly contain SiO 2 、Al 2 O 3 And Fe 2 O 3 The sum of the content of the molybdenum tailings, the molybdenum tailings and the molybdenum tailings is not less than 80wt%, and the particle size of the molybdenum tailings is 0.1-0.3mm.
3. The admixture of molybdenum tailings micropowder of claim 1, wherein: the polycarboxylate superplasticizer is synthesized by adopting a methyl allyl polyoxyethylene ether macromonomer, has the solid content of more than or equal to 40 percent, and is light yellow viscous liquid.
4. The preparation method of the molybdenum tailings micropowder admixture as claimed in any one of claims 1 to 3, which is characterized in that: the molybdenum tailings and water are fully mixed, then triethanolamine, sodium gluconate and a polycarboxylic acid water reducing agent are added, mixed and ball-milled for 20-30min, and the admixture of the molybdenum tailings micropowder is obtained after drying.
5. The method of claim 4, wherein: the mass ratio of the molybdenum tailings to the water is 1:1.0-1.2.
6. The method of claim 4, wherein: the ball milling speed is 100-200r/min, the ball-material ratio is 1-3:1.
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