CN108117374A - A kind of heat-storing material and preparation method thereof - Google Patents

A kind of heat-storing material and preparation method thereof Download PDF

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CN108117374A
CN108117374A CN201711210568.6A CN201711210568A CN108117374A CN 108117374 A CN108117374 A CN 108117374A CN 201711210568 A CN201711210568 A CN 201711210568A CN 108117374 A CN108117374 A CN 108117374A
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heat
storing material
mass percentage
tailings
mass
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CN108117374B (en
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郭玉香
李媛
姚焯
曲殿利
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University of Science and Technology Liaoning USTL
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Abstract

The present invention relates to multifunctional material technical fields more particularly to a kind of heat-storing material and preparation method thereof.A kind of heat-storing material, which is characterized in that include the raw material of following parts by weight：24~34 parts of boron mud；19~29 parts of high ferro sulfate slag；200~400 parts of iron tailings；30~100 parts of magnesite tailings；5~10 parts of spent pulping liquor；The preparation method of heat-storing material, specifically comprises the following steps：(1) raw material crush, sieve, fine grinding, (2) dispensing, (3) be kneaded, (4) primary drying, (5) compression molding, (6) redrying, (7) sintering.The present invention is using discarded boron mud, high ferro sulfate slag, iron tailings and magnesite tailings as the high heat-storing material of Material synthesis, develop boron mud, high ferro sulfate slag, iron tailings and magnesite tailings comprehensive utilization new way, improve recycling rate, rationally using resource, boron mud, high ferro sulfate slag, iron tailings and magnesite tailings pollution of ecological environment are solved the problems, such as；Heat-storing material is widely used in the civil fields such as electric heater, air-conditioning.

Description

A kind of heat-storing material and preparation method thereof
Technical field
The present invention relates to multifunctional material technical fields more particularly to a kind of heat-storing material and preparation method thereof.
Background technology
Boron mud is remaining waste residue after boron industry produces borax, boric acid using boromagnesite mineral as raw material.Sulfate slag is also known as Huang Iron ore dries slag or slag, is the waste residue discharged during manufacturing sulfuric acid or sulfurous acid with pyrite.Main chemical compositions Fe2O3： 20-50%, SiO2：15-65%, Al2O3：10%, CaO：5%, MgO<5%, S：1-2%, generally also containing Cu, Co etc..Iron Tailing is the discarded object after iron ore dressing, is the chief component of industrial solid castoff.Magnesite is one kind with carbonic acid Magnesium is the natural minerals of main chemical compositions, is the main source of magnesium.It is miscellaneous when containing small amounts iron or quartz etc. in magnesite During matter, refractory material is not just suitable for preparing, such resource as tailings discharging, is occupied cultivated land and pollutes environment.
As it can be seen that above-mentioned four kinds of mineral are industrial waste residue, above-mentioned waste residue is piled into disease, not only land occupation resource, Ecological environment is also seriously destroyed, it is extremely urgent that processing is renovated to it.Therefore new approach need to be developed to be recycled boron mud again It utilizes, prepares the product with high utility value, realize the benign development of economy and benefit.
China produces about 40~500,000 tons of the yield of borax every year, and the alkaline boron mud at the same time generated reaches 160~2,000,000 tons, substantial amounts of boron mud accumulation is caused in order to produce borax for many years.Chinese more than 300 ten thousand tons of sulfuric acid of discharge every year Slag only make use of more than 100 ten thousand tons, remaining is all discharged into environment.Farmland, contaminated land are then occupied in accumulation；It is discharged into rivers then contaminant water Body.According to incompletely statistics, the iron tailings and barren rock that the whole world is discharged every year are in 10,000,000,000 more than t.More than existing 8000, China is state-run Mine and 110,000 Duo Ge small towns collective mines, nearly 5,000,000,000 t of tailing amount of stockpiling, year discharge tailing amount are up to 500,000,000 more than t, wherein Ferrous metal mines year, tailing disposal amount was up to 1.5 hundred million t.
Above-mentioned mineral have the advantages such as raw material supply is sufficient, production cost is low, but the only recyclable recycling of existing method is few Part is measured, and most waste residue is all piled into mountain by concentration, this not only wastes substantial amounts of land resource, but also seriously destroys Ecological environment.
The content of the invention
To overcome above-mentioned the deficiencies in the prior art, the present invention provides a kind of heat-storing materials and preparation method thereof.Utilize boron Mud, high ferro sulfate slag, iron tailings and magnesite tailings synthesis low-temperature heat accumulating material, are conducive to economize the land resource, protecting ecology Environment.
In order to achieve the above object, the present invention is realized using following technical scheme：
A kind of heat-storing material, which is characterized in that include the raw material of following parts by weight：
The boron mud granularity be 150~300 mesh, B2O3Mass percentage contains for 1.5~5.0%, MgO mass percentages It is 1~10%, Fe to measure as 30~45%, CaO mass percentages2O3Mass percentage is 10~30%, AL2O3Quality hundred It is 1~5%, Na to divide content2O mass percentages are 0.1~0.5%, SiO2Mass percentage is 5~30%.
The high ferro sulfate slag granularity is 150~300 mesh, and MgO mass percentages contain for 3~5%, CaO mass percentages It measures as 4~6%, Fe2O3Mass percentage is 30~40%, AL2O3Mass percentage is 5~11%, SiO2Quality percentage Content is 40~50%.
The iron tailings granularity is 150~300 mesh, and MgO mass percentages are for 1~3%, CaO mass percentages 0.2~0.5%, Fe2O3Mass percentage is 10~20%, AL2O3Mass percentage is 0.2~0.6%, SiO2Quality hundred It is 80~90% to divide content.
The magnesite tailings granularity is 150~300 mesh, and MgO mass percentages are 40~50%, CaO mass percentages Content is 1~1.5%, SiO2Mass percentage is that 3~6%, Ig mass percentages are 45~55%,
A kind of preparation method of heat-storing material, specifically comprises the following steps：
(1) raw material crush, sieve, fine grinding：By boron mud, high ferro sulfate slag, iron tailings, magnesite tailings crush, sieve, carefully Mill, it is 150~300 mesh to make its granularity；
(2) dispensing：Formula weighs raw material as described in Claims 1 to 5；
(3) it is kneaded：Mixture is placed in dry-mixed 20~50min in planetary ball mill；
(4) primary drying：Mixture is put into drying machine dry 12h；
(5) compression molding：5~10 parts of spent pulping liquors are added in dried mixture to be uniformly mixed, are suppressed under 30MPa IntoSample；
(6) redrying：Sample is dried for 24 hours at 110 DEG C；
(7) it is sintered：Sample at 1400~1550 DEG C is sintered, keeps the temperature 4h；
(8) traditional performance to sample is passed through：Cold crushing strength, apparent porosity and bulk density, the phase composition of XRD objects, SEM microstructures are studied, and measure its heat storage performance：Coefficient of thermal expansion, specific heat capacity calculate the synthetic ratio of magnesium ferrite, determine Optimum material proportion, it is ensured that the material of synthesis can be used as heat-storing material；
(9) performance indicator of heat-storing material is：Bulk density is 4.2g/cm3, the porosity 13.42%, the resistance to pressure of room temperature It spends for 118MPa, coefficient of thermal expansion is 8.9 × 10-6℃-1(1300 DEG C), specific heat capacity are 0.88KJ/ (Kg DEG C) (300 DEG C), are led Hot coefficient is 3.81W/ (mK) (300 DEG C).
Compared with prior art, the beneficial effects of the invention are as follows：
(1) using discarded boron mud, high ferro sulfate slag, iron tailings and magnesite tailings as Material synthesis heat-storing material, boron is developed Mud, high ferro sulfate slag, iron tailings and magnesite tailings comprehensive utilization new way, improve recycling rate, rationally using resource, Solve the problems, such as boron mud, high ferro sulfate slag, iron tailings and magnesite tailings pollution of ecological environment；
(2) heat-storing material of the synthesis with high heat storage performance, is applied in civil fields such as electric heater, air-conditionings.
Description of the drawings
Fig. 1 is the process flow chart of the present invention.
Specific embodiment
It is exemplified below six embodiments to illustrate as to the specific embodiment of the invention is raw materials used, particular content As shown in table 1.
Table 1：Embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, a kind of dispensing of 6 heat-storing material of embodiment Table
1 raw material proportioning of table (parts by weight)
Group Boron mud Sulfate slag Iron tailings Magnesite tailings
A 34 29 16 21
B 32 27 18 23
C 30 25 20 25
D 28 23 22 27
E 26 21 23 29
F 24 19 25 31
To pay special attention to take the mode of magnesia addition surplus in blending process, this is conducive to that each of sample is made Item performance.This is because magnesia has the fusing point of superelevation, reach 2800 DEG C, and it also has quite high activity, this is all sharp In the generation of solid phase reaction, it is easy to be sintered, adds in the refractoriness that excessive magnesia is more advantageous to improving composite material.If oxygen It is very few to change content of magnesium, the amount of liquid phase in made sample can be caused to increase, reduce fusing point, influence the high-temperature behavior of material.
The chemical composition (mass percentage) of 2 boron mud of table
Component B2O3 MgO CaO Fe2O3 Al2O3 Na2O SiO2 Burn tinctuer
Scope 1.5~5.0 30~45 1~10 10~30 1~5 0.1~0.5 5~30 20~25
3 sulfate slag main component (mass percentage) of table
Component MgO CaO Fe2O3 Al2O3 SiO2
4.28 4.75 34.56 9.82 45.16
4 iron tailings main component (mass percentage) of table
Component MgO CaO Fe2O3 Al2O3 SiO2
1.21 0.45 15.46 0.56 81.96
5 magnesite tailings main component (mass percentage) of table
Component MgO CaO SiO2 Ig
45.06 1.21 4.36 48.95
Technical process flow figure is as shown in Figure 1, the equipment used in technical process is as shown in table 6.
6 testing equipment of table
Device name Specifications and models Purposes
Sealed type sample pulverizer 2MZ-100 Crushing
Frequency conversion planetary ball mill QM-1SP4 It is batch mixing, levigate
Constant temperature blast drying oven It is dry
Desk type powder tablet press machine FYD-30 Sample preparation
High-temperature oxidation resistant trial furnace KYH It burns till
Microcomputer controlled electro-hydraulic servo universal testing machine WAW-1000 Strength at normal temperature detects
Apparent porosity, bulk density analyzer XQK-04 Survey apparent porosity and bulk density
Thermal dilatometer RPZ-03 Measure high-temperature expansion coefficient
X-ray diffractometer X’Pert Powder Ore deposit mutually detects
Scanning electron microscope ZEISS Microstructure analysis
Energy disperse spectroscopy OXFORD Qualitative and quantitative analysis
Preparation process：(1) raw material is placed in crushing in 2MZ-100 sealed type sample pulverizers, makes its granularity be 200 mesh.(2) raw material is weighed with the formula of table 1.(3) mixture is placed in dry-mixed 35min in QM-1SP4 frequency conversion planetary ball mills (4) mixture is placed in constant temperature blast drying oven drying 12h.(5) powder after dry 12h is mixed by bonding agent of spent pulping liquor It closes uniformly, addition is 7 parts, is pressed into the sample of 50 × 50mm of Φ, (6) by FYD-30 desk type powder tablet press machines under 30MPa Sample is positioned in constant temperature blast drying oven, is dried for 24 hours at 110 DEG C.(7) it is put into KYH at a temperature of 1400~1550 DEG C High-temperature oxidation resistant trial furnace is sintered, soaking time 4h.
The principle of material accumulation of heat is：Heat is stored in a specified pattern, and releases be subject to profit when needed With achieving the purpose that energy-saving.Heat-storing material utilizes the mode of " peak load shifting ", by the energy storage that peak times of power consumption are extra Get up, released again in the low power consumption phase, to save the energy and the electricity charge.It is required that material is fast when energy is stored Speed, but it is slow in release, to achieve the effect that continue to use, it is therefore desirable to which this material has appropriate heat conduction system Number, to guarantee to achieve the purpose that the fast storage of energy, slowly discharge.The density of magnesium ferrite is higher, and thermal conductivity factor is compared with it His material is high, thus in heat-storing material magnesium ferrite content it is higher, accumulation of heat effect is better.
Preliminary observation is carried out to the appearance of sample after burning, it, will be without property such as the group sample for finding to have serious problems It can detection.Traditional performance detection, X-ray diffraction analysis, microstructure analysis etc. are carried out to the good sample of appearance, sentenced with this Determine optimization formula, that is, determine the optimal growing amount of principal component in institute's prepared material.Finally to synthesis with magnesium ferrite and forsterite Heat storage performance for the material of principal crystalline phase is detected and characterizes.
Low-temperature heat accumulating material provided in an embodiment of the present invention, the hot physical property and working performance of heat-storing material are to weigh its performance Good and bad standard, in order to synthesize the heat-storing material with performances such as high-compactness, suitable amount of stored heat, meets the item that low temperature uses Part need to detect the related heat storage performance of institute's prepared material, mainly include：Compressive resistance, specific heat capacity, thermal conductivity factor, coefficient of thermal expansion, Density etc..The performance parameter of heat-storing material is as shown in table 7 made from each embodiment.
The apparent porosity (%) of material is made in 7 each embodiment of table under different sintering temperatures
A B C D E F
1430℃ 15.42 15.46 14.05 14.83 14.96 14.21
1460℃ 14.93 14.97 13.82 14.71 14.54 14.16
1480℃ 14.57 14.69 13.42 14.92 14.27 13.87
1520℃ 15.04 14.85 14.03 15.12 14.75 13.96
Referring to table 7, according to the apparent porosity of material made from each embodiment, determine that apparent porosity is most in each embodiment Small corresponding temperature is optimal sintering temperature, is 1480 DEG C.
At 1480 DEG C, the heat storage performance of heat-storing material is as shown in table 8 made from each embodiment.
8 each embodiment of table is in the performance of heat-storing material made from 1480 DEG C
It was found from above-mentioned data, the mineral phase composition of heat-storing material is magnesium ferrite phase (MgOFe2O3), forsterite phase (2MgO·SiO2), it is mutually formed both as combining as the essential mineral of sample, also has a small amount of magnetic iron ore phase in sample (Fe3O4) and periclase phase (MgO) and micro monticellite phase (CaOMgOSiO2) exist.The content of each crystalline phase is Magnesium ferrite accounts for 55.8wt%, and forsterite accounts for 19.2wt%, and periclase accounts for 12.5wt%, and magnetic iron ore accounts for 11.6wt%, calcium and magnesium olive Olive stone accounts for 0.9wt%.
It should be noted that due to containing B in boron mud3+Even if content is seldom but the influence to sintering is also very big, spy It is not to the influence in terms of refractory material, but for being beneficial for the heat-storing material of principal crystalline phase using magnesium ferrite and forsterite , B during the reaction3+Glass phase can be formed, is conducive to the sintering of each phase, while can also reduce the temperature that forsterite mutually generates Degree, this is also the reason for can generating forsterite under 1480 DEG C of this lower temperatures.
Octahedral structure is presented in magnesium ferrite phase crystal morphology, and mutually a part in the form of block-like is embedded in ferrous acid to forsterite In the structure of magnesium phase, another part is mutually collectively resided in unreacted periclase in the alternate gap of magnesium ferrite, magnetic iron ore phase Periclase phase surface is attached in the form of grain is block-like.Analysis finds, the magnesia in boron mud take part in each solid phase reaction into Row, a silica part reacts with magnesia forms forsterite, and another part then generates impurity phase calcium and magnesium olive Olive stone, B3+Play the role of acceleration of sintering, while the temperature of forsterite formation can be reduced.
Finally, the heat storage performance of the heat-storing material to being synthesized by optimum formula detects, and understands according to testing result, and correlation stores Hot property index is satisfied by the requirement used as heat-storing material.
Summary technical solution understands that the present invention is to the synthesis of boron mud, high ferro sulfate slag, iron tailings and magnesite tailings Improvement proposes a new process routes, proposes to utilize boron mud, high ferro sulfate slag, iron tailings and magnesite tailings synthesis accumulation of heat Material, applied to civil fields such as electric heater, air-conditionings.According to performance test results, boron mud, high ferro sulfate slag, iron are utilized Tailing and magnesite tailings synthesis heat-storing material are feasible, and technical process is environmentally protective, and the material synthesized is economical and practical, object It is U.S. inexpensive, it can both solve the problems, such as boron mud, high ferro sulfate slag, iron tailings and magnesite tailings Polluted area ecological environment, also Resource can be made full use of, obtains good economic and social benefit, is a very promising new research direction.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto, Any one skilled in the art in the technical scope disclosed by the present invention, technique according to the invention scheme and its Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (6)

1. a kind of heat-storing material, which is characterized in that include the raw material of following parts by weight：
2. a kind of heat-storing material according to claim 1, which is characterized in that the boron mud granularity is 150~300 mesh, B2O3Mass percentage be 1.5~5.0%, MgO mass percentages be 30~45%, CaO mass percentages be 1~ 10%, Fe2O3Mass percentage is 10~30%, AL2O3Mass percentage is 1~5%, Na2O mass percentages are 0.1~0.5%, SiO2Mass percentage is 5~30%.
3. a kind of heat-storing material according to claim 1, which is characterized in that the high ferro sulfate slag granularity is 150~300 Mesh, MgO mass percentages are that 3~5%, CaO mass percentages are 4~6%, Fe2O3Mass percentage for 30~ 40%, AL2O3Mass percentage is 5~11%, SiO2Mass percentage is 40~50%.
4. a kind of heat-storing material according to claim 1, which is characterized in that the iron tailings granularity is 150~300 mesh, MgO mass percentages are that 1~3%, CaO mass percentages are 0.2~0.5%, Fe2O3Mass percentage for 10~ 20%, AL2O3Mass percentage is 0.2~0.6%, SiO2Mass percentage is 80~90%.
5. a kind of heat-storing material according to claim 1, which is characterized in that the magnesite tailings granularity is 150~300 Mesh, MgO mass percentages are that 40~50%, CaO mass percentages are 1~1.5%, SiO2Mass percentage for 3~ 6%, Ig mass percentage are 45~55%.
6. a kind of preparation method of heat-storing material according to claim 1, which is characterized in that specifically comprise the following steps：
(1) raw material crush, sieve, fine grinding：By boron mud, high ferro sulfate slag, iron tailings, magnesite tailings crush, sieve, fine grinding, It is 150~300 mesh to make its granularity；
(2) dispensing：Formula weighs raw material as described in Claims 1 to 5；
(3) it is kneaded：Mixture is placed in dry-mixed 20~50min in planetary ball mill；
(4) primary drying：Mixture is put into drying machine dry 12h；
(5) compression molding：5~10 parts of spent pulping liquors are added in dried mixture to be uniformly mixed, are pressed under 30MPaSample；
(6) redrying：Sample is dried for 24 hours at 110 DEG C；
(7) it is sintered：Sample at 1400~1550 DEG C is sintered, keeps the temperature 4h；
(8) traditional performance to sample is passed through：Cold crushing strength, apparent porosity and bulk density, the phase composition of XRD objects, SEM are micro- It sees structure to be studied, measures its heat storage performance：Coefficient of thermal expansion, specific heat capacity calculate the synthetic ratio of magnesium ferrite, determine optimal former Material proportioning, it is ensured that the material of synthesis can be used as heat-storing material；
(9) performance indicator of heat-storing material is：Bulk density is 4.2g/cm3, the porosity 13.42%, cold crushing strength is 118MPa, coefficient of thermal expansion are 8.9 × 10-6℃-1(1300 DEG C), specific heat capacity be 0.88KJ/ (Kg DEG C) (300 DEG C), heat conduction system Number is 3.81W/ (mK) (300 DEG C).
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110295029A (en) * 2019-06-27 2019-10-01 攀枝花学院 Heat-storing material and preparation method thereof
CN113999021A (en) * 2021-10-21 2022-02-01 辽宁科技大学 Method for modifying impurities of magnesium-based refractory material with controllable morphology
CN115321947A (en) * 2022-08-11 2022-11-11 北京华厚能源科技有限公司 Iron-based heat storage brick and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110295029A (en) * 2019-06-27 2019-10-01 攀枝花学院 Heat-storing material and preparation method thereof
CN113999021A (en) * 2021-10-21 2022-02-01 辽宁科技大学 Method for modifying impurities of magnesium-based refractory material with controllable morphology
CN115321947A (en) * 2022-08-11 2022-11-11 北京华厚能源科技有限公司 Iron-based heat storage brick and preparation method thereof

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