Functional agent using steel slag as rubber filler and preparation method of functional agent

By combining stearic acid, silane coupling agent, coconut oil fatty acid diethanolamide, acrylic resin and amino silicone oil for modification, the problems of dispersibility and high oil absorption value of steel slag as rubber filler were solved, and good dispersion and hydrophobicity of steel slag in rubber system were achieved, thus improving the stability of rubber filler.

CN121159944APending Publication Date: 2025-12-19ANHUI UNIVERSITY OF TECHNOLOGY
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Patent Information

Application Number
CN202511578430.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-10-31
Publication Date
2025-12-19

AI Technical Summary

Technical Problem

Steel slag, when used as a rubber filler, suffers from poor dispersibility and high oil absorption, leading to decreased stability in asphalt mixtures and making them prone to cracking and spalling.

Method used

Steel slag is modified by using a combination of stearic acid, silane coupling agent, coconut oil fatty acid diethanolamide, acrylic resin and amino silicone oil. Through chemical reaction and physical coating, the polarity of the steel slag surface is reduced, forming a hydrophobic aggregate film, which improves dispersibility and reduces oil absorption value.

Benefits of technology

It significantly improves the dispersibility and hydrophobicity of steel slag in rubber systems, reduces oil absorption value, improves the compatibility between steel slag and rubber, prevents agglomeration, and enhances the stability of rubber fillers.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a functional agent using steel slag as rubber filler and a preparation method thereof, and belongs to the technical field of functional materials, and the functional agent comprises the following components by mass: 10-15% of stearic acid, 10-15% of a silane coupling agent, 20-30% of coconut diethanolamide, 8-12% of acrylic resin, and 30-50% of amino silicon oil. The stearic acid and alkaline substances in the steel slag are subjected to chemical reaction, a formed long-chain structure can be attached to the surface of the steel slag, the polarity of the surface of the steel slag is reduced, the hydrophobicity of the steel slag is improved, the dispersity of the steel slag in a rubber system is improved, and the oil absorption value is reduced.
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Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of functional materials, and particularly relates to a functional agent for steel slag as rubber filler and a preparation method thereof. BACKGROUND

[0002] Steel slag is a solid waste, and at present, it is stored in large quantities in the open air, which not only occupies valuable land, but also pollutes the surrounding environment and groundwater. Therefore, how to utilize steel slag on a large scale to achieve environmental reduction and enterprise efficiency is an urgent problem to be solved.

[0003] Using steel slag as rubber filler not only improves the added value of steel slag utilization, but also greatly reduces the production cost of rubber. However, there are problems that steel slag as rubber filler requires good dispersibility, low oil absorption value and high activation index. The excessively high oil absorption value of steel slag will cause problems in its application in asphalt mixture. Steel slag contains part of calcium oxide and magnesium oxide in free state, which reacts to produce volume expansion after encountering water, and the duration is long, thereby causing steel slag to have certain expansion hazards in engineering application. Specifically, the excessively high oil absorption value of steel slag will affect its adhesion with asphalt, leading to the decrease of stability of the mixture, and prone to cracking, peeling and other problems in the use process.

[0004] In the prior art, the method for controlling the oil absorption value of steel slag mainly includes surface modification and control of particle size. The former usually covers a layer of modified material on the surface of steel slag to reduce the pores between particles, thereby reducing the oil absorption value of steel slag. The latter controls the difference in particle size distribution, so that small particles enter the voids of large particles, to realize relatively close packing and reduce the oil absorption. For example, Chinese patent CN 112210231 A discloses a modified steel slag color filler, an epoxy paint formed therefrom, a preparation method thereof and an application thereof. The steel slag is modified by mixing epoxy resin, curing agent, dispersant and solvent, to form an epoxy paint, so that it is more stable, has better adhesion and wear resistance. However, the epoxy resin used in the modification method has poor compatibility with steel slag, which cannot guarantee good compatibility while improving the hydrophobicity of steel slag, which is not conducive to the dispersion of steel slag. SUMMARY

[0005] The present application provides a functional agent for steel slag as rubber filler and a preparation method thereof, which solves the problems of poor dispersibility and high oil absorption value of steel slag as rubber filler, and expands a new idea for high added value application of steel slag.

[0006] In order to solve the above technical problems, the inventors have summarized and obtained the technical scheme of the present application through practice, and the present application discloses a functional agent for steel slag as rubber filler, and the mass ratio of each component is as follows: 10-15% of stearic acid, 10-15% of silane coupling agent, 20-30% of coconut oil fatty acid diethanolamide, 8-12% of acrylic resin, and 30-50% of amino silicone oil.

[0007] Further, the mass ratio of each component is as follows: 14% of stearic acid, 11% of silane coupling agent, 26% of coconut oil fatty acid diethanolamide, 9% of acrylic resin, and 40% of amino silicone oil.

[0008] Further, the stearic acid is selected from one of C14 stearic acid, C16 stearic acid and C18 stearic acid.

[0009] Further, the silane coupling agent is selected from one of KH550 silane coupling agent, KH560 silane coupling agent and KH580 silane coupling agent.

[0010] Further, the coconut oil fatty acid diethanolamide is an industrial grade.

[0011] Further, the acrylic resin is a thermoplastic acrylic resin.

[0012] Further, the amino silicone oil is an industrial grade.

[0013] Further, the preparation method of the functional agent for steel slag as rubber filler described in any of the above, the steps are as follows:

[0014] (1) The stearic acid, the silane coupling agent and the coconut oil fatty acid diethanolamide are mixed, and then a mixture A is obtained by stirring with a constant temperature magnetic stirrer;

[0015] (2) The acrylic resin and the amino silicone oil are mixed, and then a mixture B is obtained by stirring with a constant temperature magnetic stirrer;

[0016] (3) The mixture A and the mixture B are mixed, and then the functional agent for steel slag as rubber filler is obtained by stirring with a constant temperature magnetic stirrer.

[0017] Further, in step (1), the stirring temperature is 30-40°C, the stirring rate is 200-300 r / min, and the stirring time is 30-45 min; in step (2), the stirring temperature is 30-40°C, the stirring rate is 250-350 r / min, and the stirring time is 30-45 min.

[0018] Further, in step (3), the stirring temperature is 25-35℃, the stirring rate is 200-250 r / min, and the stirring time is 45-60 min.

[0019] Compared with the prior art, the application has the following advantages:

[0020] (1) The stearic acid in the application reacts with the alkaline substances in the steel slag, and the long-chain structure formed can adhere to the surface of the steel slag, reducing the polarity of the surface of the steel slag and improving the hydrophobicity thereof, so that the dispersibility of the steel slag in the rubber system is improved and the oil absorption value is reduced.

[0021] (2) The application uses stearic acid and silane coupling agent in cooperation to limit the hydrogen bonds and hydroxyl groups on the surface of the steel slag from dissolving in water, which can further improve the hydrophobicity of the steel slag while ensuring good compatibility, and is beneficial to the dispersion in the rubber system.

[0022] (3) The coconut oil fatty acid diethanolamide used in the application has a specific amphiphilic molecular structure, and can convert the surface of the steel slag from hydrophilic and oleophobic to lipophilic and hydrophobic in cooperation with stearic acid; at the same time, the coconut oil fatty acid diethanolamide has good stability, and the amide group thereof can form hydrogen bonds between the micelles of stearic acid, preventing the steel slag from forming agglomeration when used in the rubber system.

[0023] (4) The rubber filler functional agent prepared in the application reacts with the steel slag, and the thermoplastic acrylic resin and amino silicone oil contained therein have a synergistic effect, forming a macromolecular film on the surface of the steel slag and reducing the oil absorption value of the surface of the steel slag; the film formed by aggregation does not have crosslinking reaction, and is a non-reactive attachment, so it will not affect the performance of stearic acid, silane coupling agent and coconut oil fatty acid diethanolamide. BRIEF DESCRIPTION OF DRAWINGS

[0024] Figure 1 Figure is the oil absorption value test diagram of the steel slag modified by the functional agent in examples 1-6 and comparative examples 1-2 of the application;

[0025] Figure 2 Figure is the activation index test diagram of the steel slag modified by the functional agent in examples 1-6 and comparative examples 1-2 of the application. DETAILED DESCRIPTION

[0026] In order to make the above-mentioned purposes, features and advantages of the application more obvious and easy to understand, the specific embodiments of the application will be described in detail below.

[0027] The raw materials or reagents used in the following examples and comparative examples are commercially available products or products prepared by conventional technical means unless otherwise specified.

[0028] The detection method of the solid waste-based self-repairing functional filler in the following examples and comparative examples is as follows:

[0029] Oil absorption value: the oil absorption value is determined according to the method of the standard (GB / T 5211.15-2014);

[0030] Activation index: according to the standard test method for activation index of organic modified inorganic powder materials (T-CSTM 01202-2024);

[0031] Example 1

[0032] A functional agent for steel slag as rubber filler, the mass ratio of each component is as follows:

[0033] 10% stearic acid, 15% silane coupling agent, 20% coconut fatty acid diethanolamide, 12% acrylic resin, 43% amino silicone oil.

[0034] Among them, the stearic acid is C14 stearic acid; the silane coupling agent is KH580 silane coupling agent; the coconut fatty acid diethanolamide is industrial grade; the acrylic resin is thermoplastic acrylic resin; the amino silicone oil is industrial grade.

[0035] The preparation method of the above-mentioned functional agent for steel slag as rubber filler is as follows:

[0036] (1) First, mix stearic acid, silane coupling agent and coconut fatty acid diethanolamide, use a constant temperature magnetic stirrer to stir at a temperature of 30℃ and a speed of 300r / min for 30min, obtain mixture A;

[0037] (2) Mix acrylic resin and amino silicone oil, use a constant temperature magnetic stirrer to stir at a temperature of 40℃ and a speed of 250r / min for 30min, obtain mixture B;

[0038] (3) Mix mixture A and mixture B, use a constant temperature magnetic stirrer to stir at a temperature of 25℃ and a speed of 250r / min for 45min, obtain the functional agent for steel slag as rubber filler.

[0039] Example 2

[0040] A functional agent for steel slag as rubber filler, the mass ratio of each component is as follows:

[0041] 15% stearic acid, 10% silane coupling agent, 30% coconut fatty acid diethanolamide, 8% acrylic resin, 37% amino silicone oil.

[0042] Wherein, the stearic acid is C18 stearic acid; the silane coupling agent is KH550 silane coupling agent; the coconut oil fatty acid diethanolamide is industrial grade; the acrylic resin is thermoplastic acrylic resin; the amino silicone oil is industrial grade.

[0043] The preparation method of the functional agent for steel slag as rubber filler is as follows:

[0044] (1) first, the stearic acid, the silane coupling agent and the coconut oil fatty acid diethanolamide are mixed, and a constant temperature magnetic stirrer is used to stir at a temperature of 40 DEG C and a speed of 250 r / min for 35 min to obtain a mixture A;

[0045] (2) the acrylic resin and the amino silicone oil are mixed, and a constant temperature magnetic stirrer is used to stir at a temperature of 35 DEG C and a speed of 350 r / min for 40 min to obtain a mixture B;

[0046] (3) the mixture A and the mixture B are mixed, and a constant temperature magnetic stirrer is used to stir at a temperature of 35 DEG C and a speed of 200 r / min for 60 min to obtain the functional agent for steel slag as rubber filler.

[0047] Example 3

[0048] A functional agent for steel slag as rubber filler, the mass ratio of each component is as follows:

[0049] 11% stearic acid, 13% silane coupling agent, 28% coconut oil fatty acid diethanolamide, 10% acrylic resin, 38% amino silicone oil.

[0050] Wherein, the stearic acid is C16 stearic acid; the silane coupling agent is KH550 silane coupling agent; the coconut oil fatty acid diethanolamide is industrial grade; the acrylic resin is thermoplastic acrylic resin; the amino silicone oil is industrial grade.

[0051] The preparation method of the functional agent for steel slag as rubber filler is as follows:

[0052] (1) first, the stearic acid, the silane coupling agent and the coconut oil fatty acid diethanolamide are mixed, and a constant temperature magnetic stirrer is used to stir at a temperature of 35 DEG C and a speed of 200 r / min for 45 min to obtain a mixture A;

[0053] (2) the acrylic resin and the amino silicone oil are mixed, and a constant temperature magnetic stirrer is used to stir at a temperature of 30 DEG C and a speed of 300 r / min for 35 min to obtain a mixture B;

[0054] (3) the mixture A and the mixture B are mixed, and a constant temperature magnetic stirrer is used to stir at a temperature of 30 DEG C and a speed of 230 r / min for 50 min to obtain the functional agent for steel slag as rubber filler.

[0055] Embodiment 4

[0056] A functional agent for steel slag as rubber filler, the mass ratio of each component is as follows:

[0057] 14% stearic acid, 11% silane coupling agent, 26% coconut oil fatty acid diethanolamide, 9% acrylic resin, 40% amino silicone oil.

[0058] Among them, stearic acid is C18 stearic acid; silane coupling agent is KH560 silane coupling agent; coconut oil fatty acid diethylamide is industrial grade; acrylic resin is thermoplastic acrylic resin; amino silicone oil is industrial grade.

[0059] The preparation method of the above-mentioned functional agent for steel slag as rubber filler, the steps are as follows:

[0060] (1) first, stearic acid, silane coupling agent and coconut oil fatty acid diethanolamide are mixed, and a constant temperature magnetic stirrer is used to stir at a temperature of 30℃ and a speed of 200r / min for 40min to obtain mixture A;

[0061] (2) acrylic resin and amino silicone oil are mixed, and a constant temperature magnetic stirrer is used to stir at a temperature of 30℃ and a speed of 350r / min for 45min to obtain mixture B;

[0062] (3) mixture A and mixture B are mixed, and a constant temperature magnetic stirrer is used to stir at a temperature of 35℃ and a speed of 210r / min for 55min to obtain the functional agent for steel slag as rubber filler.

[0063] Embodiment 5

[0064] A functional agent for steel slag as rubber filler, the mass ratio of each component is as follows:

[0065] 13% stearic acid, 14% silane coupling agent, 22% coconut oil fatty acid diethanolamide, 11% acrylic resin, 40% amino silicone oil.

[0066] Among them, stearic acid is C14 stearic acid; silane coupling agent is KH580 silane coupling agent; coconut oil fatty acid diethylamide is industrial grade; acrylic resin is thermoplastic acrylic resin; amino silicone oil is industrial grade.

[0067] The preparation method of the above-mentioned functional agent for steel slag as rubber filler, the steps are as follows:

[0068] (1) first, stearic acid, silane coupling agent and coconut oil fatty acid diethanolamide are mixed, and a constant temperature magnetic stirrer is used to stir at a temperature of 40℃ and a speed of 300r / min for 35min to obtain mixture A;

[0069] (2) Mix acrylic resin with amino silicone oil, use constant temperature magnetic stirrer to stir at 40℃ with 250r / min for 45min, obtain mixture B;

[0070] (3) Mix mixture A with mixture B, use constant temperature magnetic stirrer to stir at 25℃ with 240r / min for 50min, obtain functional agent for steel slag as rubber filler.

[0071] Example 6

[0072] A kind of functional agent for steel slag as rubber filler, the mass ratio of each component is as follows by mass percentage:

[0073] 12% stearic acid, 12% silane coupling agent, 24% coconut oil fatty acid diethanolamide, 9% acrylic resin, 43% amino silicone oil.

[0074] Wherein, stearic acid is C16 stearic acid; silane coupling agent is KH560 silane coupling agent; coconut oil fatty acid diethanolamide is industrial grade; acrylic resin is thermoplastic acrylic resin; amino silicone oil is industrial grade.

[0075] The preparation method of the above-mentioned functional agent for steel slag as rubber filler is as follows:

[0076] (1) First, mix stearic acid, silane coupling agent and coconut oil fatty acid diethanolamide, use constant temperature magnetic stirrer to stir at 35℃ with 250r / min for 40min, obtain mixture A;

[0077] (2) Mix acrylic resin with amino silicone oil, use constant temperature magnetic stirrer to stir at 35℃ with 300r / min for 40min, obtain mixture B;

[0078] (3) Mix mixture A with mixture B, use constant temperature magnetic stirrer to stir at 30℃ with 220r / min for 55min, obtain functional agent for steel slag as rubber filler.

[0079] Comparative Example 1

[0080] A kind of functional agent for steel slag as rubber filler, the mass ratio of each component is as follows by mass percentage:

[0081] 12% stearic acid, 12% silane coupling agent, 24% coconut oil fatty acid diethanolamide, 52% amino silicone oil.

[0082] The stearic acid is C16 stearic acid; the silane coupling agent is KH560 silane coupling agent; the coconut oil fatty acid diethanolamide is an industrial grade; and the amino silicone oil is an industrial grade.

[0083] The preparation method of the functional agent for the steel slag as the rubber filler is as follows:

[0084] (1) The stearic acid, the silane coupling agent and the coconut oil fatty acid diethanolamide are mixed, a constant temperature magnetic stirrer is used for stirring at a temperature of 35℃ and a rotating speed of 250r / min for 40min to obtain a mixture A;

[0085] (2) The mixture A and the acrylic resin are mixed, a constant temperature magnetic stirrer is used for stirring at a temperature of 30℃ and a rotating speed of 220r / min for 55min to obtain the functional agent for the steel slag as the rubber filler.

[0086] Comparative Example 2

[0087] A functional agent for the steel slag as the rubber filler, the mass ratio of each component is as follows:

[0088] 24% stearic acid, 24% silane coupling agent, 9% acrylic resin, 43% amino silicone oil.

[0089] The stearic acid is C16 stearic acid; the silane coupling agent is KH560 silane coupling agent; the acrylic resin is a thermoplastic acrylic resin; and the amino silicone oil is an industrial grade.

[0090] The preparation method of the functional agent for the steel slag as the rubber filler is as follows:

[0091] (1) The stearic acid and the silane coupling agent are mixed, a constant temperature magnetic stirrer is used for stirring at a temperature of 35℃ and a rotating speed of 250r / min for 40min to obtain a mixture A;

[0092] (2) The acrylic resin and the amino silicone oil are mixed, a constant temperature magnetic stirrer is used for stirring at a temperature of 35℃ and a rotating speed of 300r / min for 40min to obtain a mixture B;

[0093] (3) The mixture A and the mixture B are mixed, a constant temperature magnetic stirrer is used for stirring at a temperature of 30℃ and a rotating speed of 220r / min for 55min to obtain the functional agent for the steel slag as the rubber filler.

[0094] The functional agents for the steel slag as the rubber filler in Examples 1-6 and Comparative Examples 1-2 are used to modify 3% of the steel slag by mass fraction, the steel slag is mixed with the functional agent, stirred for 10min under a high-speed mixer, and the performance of the modified steel slag is tested, and the test results are shown in Table 1.

[0095] Table 1. Performance structure of steel slag modified by the functional agents in Examples 1-6 and Comparative Examples 1-2

[0096]

[0097] Analysis of Table 1 shows that the stearic acid used in this invention undergoes a chemical neutralization reaction with the alkaline substances (calcium hydroxide and aluminum hydroxide) in the steel slag, respectively generating calcium stearate (Ca[CH3(CH2)). 16 COO]2) and aluminum stearate (Al[CH3(CH2)) 16 COO]3) These two different long-chain structures can be physically coated onto the surface of steel slag, thereby reducing the polarity of the steel slag surface, improving its hydrophobicity, and thus improving the dispersibility of steel slag in the rubber system and reducing its oil absorption value.

[0098] Modification with a single silane coupling agent cannot control the water solubility of hydrogen bonds and hydroxyl groups on the surface of steel slag, resulting in poor modification effect. In other words, the modified steel slag has poor compatibility with the rubber system. Therefore, the synergistic use of stearic acid and silane coupling agent can limit the water solubility of hydrogen bonds and hydroxyl groups on the surface of steel slag, and further improve the hydrophobicity of steel slag while ensuring good compatibility, which is beneficial for dispersion in the rubber system.

[0099] according to Figure 1 , Figure 2 Comparing the data in Table 1, it can be seen that the oil absorption value of the functional agents used as rubber fillers in Examples 1-6 of this invention for steel slag is significantly lower than that of the comparative example, while the activation index is significantly higher than that of the comparative example. This is because coconut oil fatty acid diethanolamide has a specific amphiphilic molecular structure, which, in synergy with stearic acid, can change the surface of steel slag from hydrophilic to oleophilic to hydrophobic. At the same time, coconut oil fatty acid diethanolamide has good stability, and its amide groups can form hydrogen bonds with the micelles of stearic acid, preventing the steel slag from agglomerating in the rubber system. Thermoplastic acrylic resin is a type of solvent-based acrylic resin. In synergy with amino silicone oil, it can form a macromolecular aggregate film on the surface of steel slag, reducing the oil absorption value of the steel slag surface. The aggregate film does not undergo cross-linking reaction and belongs to non-reactive adhesion, so it does not affect the performance of stearic acid, silane coupling agent and coconut oil fatty acid diethanolamide.

Claims

1. A functional agent for steel slag as a rubber filler, characterized by, The mass ratio of each component is as follows in percentage by mass: stearic acid 10-15%, silane coupling agent 10-15%, coconut fatty acid diethanolamide 20-30%, acrylic resin 8-12%, and amino silicone oil 30-50%.

2. The functional agent for steel slag as a rubber filler according to claim 1, characterized by, The mass ratio of each component is as follows in percentage by mass: stearic acid 14%, silane coupling agent 11%, coconut fatty acid diethanolamide 26%, acrylic resin 9%, and amino silicone oil 40%.

3. The functional agent for steel slag as a rubber filler according to claim 1, characterized by, The stearic acid is selected from one of C14 stearic acid, C16 stearic acid and C18 stearic acid.

4. The functional agent for steel slag as a rubber filler according to claim 1, characterized by, The silane coupling agent is selected from one of KH550 silane coupling agent, KH560 silane coupling agent and KH580 silane coupling agent.

5. The functional agent for steel slag as a rubber filler according to claim 1, characterized by, The coconut fatty acid diethanolamide is of industrial grade.

6. The functional agent for steel slag as a rubber filler according to claim 1, characterized by, The acrylic resin is a thermoplastic acrylic resin.

7. The functional agent for steel slag as a rubber filler according to claim 1, characterized by, The amino silicone oil is of industrial grade.

8. A method for preparing a functional agent for steel slag as a rubber filler according to any one of claims 1 to 7, characterized by, The steps are as follows: (1) mixing stearic acid, silane coupling agent and coconut fatty acid diethanolamide, and obtaining mixture A by stirring with a constant temperature magnetic stirrer; (2) mixing acrylic resin and amino silicone oil, and obtaining mixture B by stirring with a constant temperature magnetic stirrer; (3) mixing mixture A and mixture B, and obtaining the functional agent for steel slag as rubber filler by stirring with a constant temperature magnetic stirrer.

9. The production method according to claim 8, characterized by, In step (1), the stirring temperature is 30-40℃, the stirring rate is 200-300r / min, and the stirring time is 30-45min; in step (2), the stirring temperature is 30-40℃, the stirring rate is 250-350r / min, and the stirring time is 30-45min.

10. The method of claim 8, wherein, In step (3), the stirring temperature is 25-35℃, the stirring rate is 200-250r / min, and the stirring time is 45-60min.

Citation Information

Patent Citations

  • Modified steel slag pigment filler, epoxy paint formed by modified steel slag pigment filler, and preparation method and application of epoxy paint

    CN112210231A