Magnetic composite fluid polishing solution and preparation method thereof

By pretreating and melting oxidizing the nickel slag, modified nickel slag was prepared for the preparation of magnetic composite fluid polishing liquid, which solved the problems of low utilization rate of nickel slag and environmental pollution, and achieved high added value utilization and excellent polishing effect of nickel slag.

CN120059604APending Publication Date: 2025-05-30LANZHOU UNIVERSITY OF TECHNOLOGY
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Patent Information

Application Number
CN202411296777.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-18
Publication Date
2025-05-30

AI Technical Summary

Technical Problem

In the prior art, the comprehensive utilization rate of nickel slag is relatively low, and the treatment methods are mostly open-pit storage or landfill, which leads to waste of resources and environmental pollution. The high value-added elements Fe, Ni, Co, and Cu are ignored and cannot be effectively utilized in the magnetic composite fluid polishing liquid.

Method used

Modified nickel slag is obtained by mixing the nickel slag with alkaline oxide, pretreatment, and subsequent melt oxidation. Modified nickel slag partially replaces carbonyl iron powder and is used to prepare magnetic composite fluid polishing liquid.

Benefits of technology

It has achieved the improvement of the added value of nickel slag on the basis of ensuring the polishing effect, significantly reducing the impact of nickel slag treatment on the environment, and solving the problem that magnetic field assisted polishing cannot be used in industry.

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Abstract

The invention provides a magnetic composite fluid polishing solution and a preparation method thereof, and belongs to the technical field of recovery and treatment of industrial waste residues. The magnetic composite fluid polishing solution provided by the invention comprises the following components in percentage by mass: 20-50% of carbonyl iron powder, 5-15% of modified nickel slag, 7-20% of abrasive particles, 1-5% of cellulose and 30-50% of magnetic fluid, the preparation method of the modified nickel slag comprises the following steps: mixing nickel slag with alkaline oxide to obtain pretreated nickel slag; and the pretreated nickel slag is subjected to melting oxidation, and the modified nickel slag is obtained. According to the method, the nickel slag is mixed with the alkaline oxide, the alkalinity of the nickel slag is adjusted, and subsequent melting oxidation of the nickel slag is facilitated; and then melting oxidation is carried out, ferromagnetic particles in the nickel slag are reduced, the modified nickel slag is obtained, carbonyl iron powder is partially replaced with the modified nickel slag, and the additional value of the nickel slag can be increased on the basis that the polishing effect of the magnetic composite fluid polishing solution is guaranteed.
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Description

Technical Field

[0001] The present invention belongs to the technical field of the recycling and treatment of industrial waste residues, and particularly relates to a magnetic composite fluid polishing liquid and a preparation method thereof. Background Art

[0002] A large amount of high-temperature slag is discharged during the smelting process of nickel ore. After water quenching, nickel slag is obtained, and the slag production accounts for almost 80-90% of the raw material amount. Nickel slag has become the fourth largest smelting industrial waste residue after slag, steel slag, and red mud. At present, the comprehensive utilization rate of nickel slag is relatively low, and its treatment methods are mostly open-air stacking or landfill, which not only wastes resources and occupies a large amount of land, but also damages the surrounding ecological environment, seriously restricting the sustainable development of the nickel-iron industry. At the same time, high-value elements such as Fe, Ni, Co, and Cu in it are ignored. At present, there is no relevant research on using nickel slag for magnetic composite fluid polishing liquid. Therefore, how to use nickel slag for magnetic composite fluid polishing liquid on the basis of ensuring the polishing effect of the magnetic composite fluid polishing liquid and improving the added value of nickel slag has become a technical problem to be solved urgently in this field. Summary of the Invention

[0003] The purpose of the present invention is to provide a magnetic composite fluid polishing liquid and a preparation method thereof. The magnetic composite fluid polishing liquid provided by the present invention can not only improve the added value of nickel slag, but also ensure the polishing effect.

[0004] In order to achieve the above-mentioned invention purpose, the present invention provides the following technical solutions:

[0005] The present invention provides a magnetic composite fluid polishing liquid, which comprises the following components in mass percentage: 20-50% of carbonyl iron powder, 5-15% of modified nickel slag, 7-20% of abrasive grains, 1-5% of cellulose, and 30-50% of magnetic fluid;

[0006] The preparation method of the modified nickel slag comprises the following steps:

[0007] (1) Mix nickel slag with basic oxides to obtain pretreated nickel slag;

[0008] (2) Carry out melting oxidation on the pretreated nickel slag obtained in the step (1) to obtain modified nickel slag.

[0009] Preferably, it comprises the following components in mass percentage: 30-45% of carbonyl iron powder, 5-10% of modified nickel slag, 12-15% of abrasive grains, 3-5% of cellulose, and 40-45% of magnetic fluid.

[0010] Preferably, it comprises the following components in mass percentage: 35-40% of carbonyl iron powder, 5-10% of modified nickel slag, 12-13% of abrasive grains, 3-4% of cellulose, and 40-42% of magnetic fluid.

[0011] Preferably, the particle size of the carbonyl iron powder is 1-10 μm.

[0012] Preferably, the particle size of the modified nickel slag is 7-100 μm.

[0013] Preferably, the particle size of the abrasive grains is 1-10 μm.

[0014] Preferably, the nickel slag in the step (1) is blast furnace nickel iron slag.

[0015] Preferably, the ternary basicity of the nickel slag pretreated in the step (1) is 0.2-1.0.

[0016] Preferably, the temperature of the melting oxidation in the step (2) is 1300-1750 °C, and the time of the melting oxidation is 40-90 min.

[0017] The present invention also provides a preparation method of the magnetic composite fluid polishing liquid described in the above technical solution, including:

[0018] Mixing carbonyl iron powder, modified nickel slag, abrasive grains, cellulose and magnetic fluid to obtain a magnetic composite fluid polishing liquid.

[0019] The present invention provides a magnetic composite fluid polishing liquid, which includes the following components in mass percentage: 20-50% of carbonyl iron powder, 5-15% of modified nickel slag, 7-20% of abrasive grains, 1-5% of cellulose and 30-50% of magnetic fluid; the preparation method of the modified nickel slag includes the following steps: mixing nickel slag with basic oxides to obtain pretreated nickel slag; performing melting oxidation on the pretreated nickel slag to obtain modified nickel slag. The present invention first mixes nickel slag with basic oxides to adjust the basicity of nickel slag, which can displace FeO in nickel slag and is beneficial to the subsequent melting oxidation of nickel slag; then performs melting oxidation to reduce ferromagnetic particles in nickel slag to obtain modified nickel slag. Using modified nickel slag to partially replace carbonyl iron powder can improve the added value of nickel slag while ensuring the polishing effect of the magnetic composite fluid polishing liquid. Experimental results show that after polishing a workpiece with the magnetic composite fluid polishing liquid provided by the present invention, the roughness reduction rate R a is 92.635-96.296%. Specific Embodiments

[0020] The present invention provides a magnetic composite fluid polishing liquid, which includes the following components in mass percentage: 20-50% of carbonyl iron powder, 5-15% of modified nickel slag, 7-20% of abrasive grains, 1-5% of cellulose and 30-50% of magnetic fluid;

[0021] The preparation method of the modified nickel slag includes the following steps:

[0022] (1) Mixing nickel slag with basic oxides to obtain pretreated nickel slag;

[0023] (2) subject the pretreated nickel slag obtained in step (1) to melting oxidation to obtain modified nickel slag.

[0024] The present invention does not have special limitations on the sources of the raw materials, and commercially available products well-known to those skilled in the art can be used.

[0025] By mass percentage, the magnetic composite fluid polishing liquid provided by the present invention comprises 20-50% of carbonyl iron powder. In the present invention, the carbonyl iron powder is a magnetic particle, providing magnetism for the magnetic composite fluid polishing liquid.

[0026] As an embodiment, the mass percentage content of the carbonyl iron powder can be 30-45%, or can be 35-40%.

[0027] In the present invention, the particle size of the carbonyl iron powder is preferably 1-10 μm. As an embodiment, the particle size of the carbonyl iron powder can be 3 μm, 5 μm, 7 μm, and 9 μm.

[0028] By mass percentage, the magnetic composite fluid polishing liquid provided by the present invention further comprises 5-15% of modified nickel slag; the particle size of the modified nickel slag is preferably 7-100 μm. In the present invention, the modified nickel slag is a magnetic particle, providing magnetism for the magnetic composite fluid polishing liquid.

[0029] As an embodiment, the mass percentage content of the modified nickel slag can be 5-10%.

[0030] In the present invention, the preparation method of the modified nickel slag comprises the following steps:

[0031] (1) Mix nickel slag with basic oxides to obtain pretreated nickel slag;

[0032] (2) subject the pretreated nickel slag obtained in step (1) to melting oxidation to obtain modified nickel slag.

[0033] The present invention mixes nickel slag with basic oxides to obtain pretreated nickel slag. The present invention uses basic oxides to adjust the basicity of nickel slag, which is beneficial to the subsequent melting oxidation of nickel slag.

[0034] In the present invention, the nickel slag is preferably blast furnace nickel iron slag; the particle size of the nickel slag is preferably 4.75-65 μm. As an embodiment, the particle size of the nickel slag can be 40 μm.

[0035] As an embodiment, the main mineral phase of the blast furnace nickel iron slag can be fayalite.

[0036] As an implementation manner, the chemical composition of the nickel slag may be, by mass percentage: Fe 36.74%, Si 16.23%, Mg 5.96%, Ca 0.84%, K 0.53%, Na 0.44%, Ni 0.38%, Cu 0.28%, Cr 0.13%, Mn 0.13%, Co 0.10%, P 0.04%, Zn 0.04%, Pb 0.004%, S 0.76% and others 37.396%.

[0037] As an implementation manner, the mass content of Fe in the nickel slag 2+ may be 33.42%.

[0038] In the present invention, the basic oxide is preferably CaO. The present invention has no special limitation on the particle size of the basic oxide, and the particle size well-known to those skilled in the art can be adopted. In the present invention, during the process of melting and oxidation, CaO has a stronger binding effect with SiO in the nickel slag 2 to displace FeO from fayalite and inhibit the formation of fayalite.

[0039] The present invention has no special limitation on the operation of mixing the nickel slag and the basic oxide, and the technical solution for preparing the mixed material well-known to those skilled in the art can be adopted.

[0040] In the present invention, the ternary basicity of the pretreated nickel slag is preferably 0.2 - 1.0. Limiting the ternary basicity of the pretreated nickel slag within the above range in the present invention is beneficial to the subsequent melting and oxidation.

[0041] As an implementation manner, the ternary basicity of the pretreated nickel slag may be 0.3 - 0.6, and may also be 0.4 - 0.6.

[0042] After obtaining the pretreated nickel slag, the present invention performs melting and oxidation on the pretreated nickel slag to obtain a modified nickel slag. In the present invention, performing melting and oxidation on the pretreated nickel slag can convert the nickel slag into magnetic particles that can be used for magnetic composite fluid polishing.

[0043] In the present invention, the reaction equation of the melting and oxidation is as follows:[[]]END]]

[0044] Fe 2 SiO 4 +2CaO = 2FeO + Ca 2 SiO 4

[0045] 6FeO + O 2 = 2Fe 3 O 4

[0046] 3Fe 2 SiO 4 +6CaO+O 2 =2Fe 3 O 4 +3Ca 2 SiO 4 。

[0047] The main mineral phase of nickel slag is fayalite, and its chemical composition is mainly FeO, MgO, SiO 2 , and ferromagnetic particles can be reduced after melting oxidation and applied in magnetic field assisted polishing as a magnetic composite fluid polishing liquid.

[0048] In the present invention, the temperature of the melting oxidation is preferably 1300 - 1750 °C; the time of the melting oxidation is preferably 40 - 90 min. Limiting the temperature and time of the melting oxidation within the above ranges in the present invention can improve the degree of melting oxidation, thereby improving the polishing effect.

[0049] As an implementation manner, the temperature of the melting oxidation can be 1400 - 1700 °C, and can also be 1550 - 1600 °C; the time of the melting oxidation can be 50 - 80 min, and can also be 60 - 70 min.

[0050] In the present invention, the mechanism for heating to the melting oxidation temperature is preferably to first heat to 1200 °C at a rate of 250 - 350 °C / min, and then heat to the melting oxidation temperature at a rate of 1 - 10 °C / min. Adopting the above heating mechanism in the present invention is beneficial to the subsequent melting oxidation.

[0051] As an implementation manner, the mechanism for heating to the melting oxidation temperature can be to first heat to 1200 °C at a rate of 300 °C / min, and then heat to the melting oxidation temperature at a rate of 5 °C / min.

[0052] After the melting oxidation is completed, the present invention preferably cools and crushes the product obtained by the melting oxidation in sequence to obtain modified nickel slag.

[0053] In the present invention, the cooling rate is preferably 5 - 15 °C / min. As an implementation manner, the cooling rate can be 10 °C / min.

[0054] The present invention has no special limitation on the crushing operation, and the particle size of the modified nickel slag can be crushed to the range of 50 - 100 μm by using the operations well-known to those skilled in the art.

[0055] By mass percentage, the magnetic composite fluid polishing liquid provided by the present invention further includes 7 - 20% abrasive grains; the particle size of the abrasive grains is preferably 1 - 10 μm; the material of the abrasive grains is preferably Al2 O 3 , diamond, silicon dioxide or silicon carbide. In the present invention, the abrasive grains can improve the polishing effect, and limiting the mass content of the abrasive grains within the above range can improve the polishing effect.

[0056] As an embodiment, the mass percentage content of the abrasive grains can be 12-15%, and can also be 12-13%; the particle size of the abrasive grains can be 1 μm; the material of the abrasive grains can be Al 2 O 3 .

[0057] By mass percentage, the magnetic composite fluid polishing liquid provided by the present invention further includes 1-5% of cellulose; the cellulose is preferably α-cellulose. In the present invention, the cellulose can increase the viscosity.

[0058] As an embodiment, the mass percentage content of the cellulose can be 3-5%, and can also be 3-4%.

[0059] By mass percentage, the magnetic composite fluid polishing liquid provided by the present invention further includes 30-50% of magnetic fluid; the magnetic fluid is preferably an aqueous magnetic fluid containing Fe 3 O 4 ; the particle size of the Fe 3 O 4 is preferably 10-30 nm; the mass content of Fe 3 O 4 in the magnetic fluid is preferably 2%. In the present invention, the magnetic fluid can improve the polishing effect.

[0060] As an embodiment, the mass percentage content of the magnetic fluid can be 40-45%, and can also be 40-42%.

[0061] The present invention uses the material obtained by melting and oxidizing nickel slag to replace the use of relatively expensive carbonyl iron powder, which can not only significantly solve the environmental impact caused by the stacking of nickel slag, but also greatly alleviate the problem that magnetic field-assisted polishing cannot be used industrially, and solve the problem of subsurface damage caused by hard polishing.

[0062] The present invention realizes the recycling of solid waste and the high-value functional reuse of materials. Through the light treatment of nickel slag, the magnetic fluid ultra-precision machining technology based on nickel slag is directly realized, which has the advantage of low cost, provides a new solution for the recycling of nickel slag, and conforms to the concept of zero emission and pollution-free.

[0063] The present invention uses nickel slag as a raw material, and through a molten oxidation reaction under alkaline conditions, it is transformed into magnetic particles that can be used for magnetic composite fluid polishing. This not only realizes the full resource utilization, increases economic benefits, but also promotes the application of composite fluid polishing in industry and reduces costs.

[0064] The present invention also provides a method for preparing the magnetic composite fluid polishing liquid described in the above technical solution, including:

[0065] Mix carbonyl iron powder, modified nickel slag, abrasive grains, cellulose and magnetic fluid to obtain a magnetic composite fluid polishing liquid.

[0066] In the present invention, the mixing of the carbonyl iron powder, modified nickel slag, abrasive grains, cellulose and magnetic fluid is preferably carried out under stirring conditions. The present invention has no special limitation on the operation of the stirring, as long as the components are mixed evenly.

[0067] The preparation method provided by the present invention has a simple process.

[0068] Next, the technical solutions in the present invention will be clearly and completely described in conjunction with the embodiments in the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments in the present invention without creative efforts belong to the scope of protection of the present invention.

[0069] The nickel slag used in the embodiment is blast furnace nickel iron slag; the main mineral phase of the blast furnace nickel iron slag is fayalite;

[0070] The chemical composition of the nickel slag is as follows in mass percentage: Fe 36.74%, Si 16.23%, Mg 5.96%, Ca 0.84%, K 0.53%, Na 0.44%, Ni 0.38%, Cu 0.28%, Cr 0.13%, Mn 0.13%, Co 0.10%, P 0.04%, Zn 0.04%, Pb 0.004%, S 0.76% and others 37.396%; the mass content of Fe in the nickel slag 2+ is 33.42%.

[0071] Example 1

[0072] The magnetic composite fluid polishing liquid is composed of the following components in mass percentage: 40% carbonyl iron powder, 5% modified nickel slag, Al 2 O 3 12%, 3% α-cellulose and 40% water-based magnetic fluid containing 2 wt% Fe 3 O 4 ;

[0073] Among them, the particle size of the carbonyl iron powder is 7 μm, the particle size of the modified nickel slag is 7 μm, and the particle size of Al 2 O 3 is 1 μm, and the particle size of Fe 3 O 4 is 10 nm;

[0074] The preparation method of the modified nickel slag is as follows:

[0075] (1) Mix the nickel slag with CaO to obtain the pre-treated nickel slag with a ternary basicity of 0.6; among them, the particle size of the nickel slag is 40 μm;

[0076] (2) Heat the pre-treated nickel slag obtained in step (1) to 1200 °C at a rate of 300 °C / min, then heat it to 1550 °C at a rate of 5 °C / min for 60 min of melting oxidation, and then cool it to room temperature at a rate of 10 °C / min, and crush it to obtain the modified nickel slag;

[0077] The preparation method of the magnetic composite fluid polishing liquid is:

[0078] Mix the carbonyl iron powder, the modified nickel slag, Al 2 O 3 , α-cellulose and the water-based magnetic fluid containing Fe 3 O 4 by mechanical stirring to obtain the magnetic composite fluid polishing liquid.

[0079] Example 2

[0080] On the basis of Example 1, change the composition of the magnetic composite fluid polishing liquid. The magnetic composite fluid polishing liquid is composed of the following components by mass percentage: 35% of carbonyl iron powder, 10% of modified nickel slag, Al 2 O 3 12%, 3% of α-cellulose and 40% of the water-based magnetic fluid containing Fe 3 O 4 , and other conditions remain unchanged.

[0081] Example 3

[0082] On the basis of Example 1, change the composition of the magnetic composite fluid polishing liquid. The magnetic composite fluid polishing liquid is composed of the following components by mass percentage: 30% of carbonyl iron powder, 15% of modified nickel slag, Al 2 O 3 12%, 3% of α-cellulose and 40% of the water-based magnetic fluid containing 2 wt% Fe 3 O 4 , and other conditions remain unchanged.

[0083] Comparative Example 1

[0084] The magnetic composite fluid polishing liquid consists of the following components by mass percentage: 45% carbonyl iron powder, 12% Al 2 O 3 12, 3% α-cellulose, and 40% water-based magnetic fluid containing 2 wt% Fe 3 O 4 ;

[0085] The particle size of the carbonyl iron powder is 7 μm; the particle size of Al 2 O 3 is 1 μm; the particle size of Fe 3 O 4 is 10 nm;

[0086] The preparation method of the magnetic composite fluid polishing liquid is as follows:

[0087] Mechanically stir the carbonyl iron powder, Al 2 O 3 , α-cellulose, and the water-based magnetic fluid containing Fe 3 O 4 to obtain the magnetic composite fluid polishing liquid.

[0088] The polishing effect of the magnetic composite fluid polishing liquid prepared by using Examples 1 to 3 and Comparative Example 1 was tested. The test method was to measure the surface roughness of the workpiece before and after polishing by a white light interferometer. The results are shown in Table 1.

[0089] Table 1 Polishing effects of the magnetic composite fluid polishing liquid prepared by Examples 1 to 3 and Comparative Example 1

[0090] Project <![CDATA[R ai / μm]]> <![CDATA[R ap / μm]]> <![CDATA[R a %]]> Comparative Example 1 0.496 0.009 98.185 Example 1 0.513 0.019 96.296 Example 2 0.487 0.022 95.482 Example 3 0.516 0.038 92.635

[0091] Note: R ai and R ap in the table respectively represent the surface roughness of the workpiece before and after polishing; due to the different initial surface roughnesses of the workpieces, the surface roughness reduction rate R a % is defined to represent the polishing effect of the magnetic composite fluid polishing liquid:

[0092] R a % = (1 - R ap / R ai ) × 100%.

[0093] As can be seen from Table 1, although the magnetic composite fluid polishing liquid provided by the present invention uses nickel slag, it also has excellent polishing effects.

[0094] As can be seen from the above examples and comparative examples, the magnetic composite fluid polishing liquid provided by the present invention can not only increase the added value of nickel slag, but also ensure the polishing effect.

[0095] The above are only the preferred embodiments of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.

Claims

1. A magnetic composite fluid polishing liquid, comprising the following components in percentage by mass: 20-50% carbonyl iron powder, 5-15% modified nickel slag, 7-20% abrasive particles, 1-5% cellulose and 30-50% magnetic fluid; The preparation method of the modified nickel slag comprises the following steps: (1) mixing nickel slag with basic oxide to obtain pre-treated nickel slag; (2) subjecting the pre-treated nickel slag obtained in step (1) to melt oxidation to obtain modified nickel slag.

2. The magnetic composite fluid polishing liquid according to claim 1, characterized in that: The invention comprises the following components in percentage by mass: 30-45% of carbonyl iron powder, 5-10% of modified nickel slag, 12-15% of abrasive grains, 3-5% of cellulose and 40-45% of magnetic fluid.

3. The magnetic composite fluid polishing liquid according to claim 2, characterized in that: The invention comprises the following components in percentage by mass: 35-40% of carbonyl iron powder, 5-10% of modified nickel slag, 12-13% of abrasive grains, 3-4% of cellulose and 40-42% of magnetic fluid.

4. The magnetic composite fluid polishing liquid according to any one of claims 1 to 3, characterized in that: The particle size of the carbon-based iron powder is 1 to 10 μm.

5. The magnetic composite fluid polishing liquid according to any one of claims 1 to 3, characterized in that: The particle size of the modified nickel slag is 7 to 100 μm.

6. The magnetic composite fluid polishing liquid according to any one of claims 1 to 3, characterized in that: The particle size of the abrasive particles is 1 to 10 μm.

7. The magnetic composite fluid polishing liquid according to claim 1, characterized in that: The nickel slag in the step (1) is blast furnace ferronickel slag.

8. The magnetic composite fluid polishing liquid according to claim 1, characterized in that: The ternary basicity of the nickel slag pre-treated in step (1) is 0.2-1.

0.

9. The magnetic composite fluid polishing liquid according to claim 1, characterized in that: The temperature of the melt oxidation in the step (2) is 1300-1750° C., and the time of the melt oxidation is 40-90 minutes.

10. The method for preparing the magnetic composite fluid polishing liquid according to any one of claims 1 to 9, comprising: Carbonyl iron powder, modified nickel slag, abrasive grains, cellulose and magnetic fluid are mixed to obtain a magnetic composite fluid polishing liquid.