CN108484978B - Steel slag-micro silicon powder composite rubber filler with reinforcing-flame-retardant synergistic performance - Google Patents
Steel slag-micro silicon powder composite rubber filler with reinforcing-flame-retardant synergistic performance Download PDFInfo
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- C08L9/06—Copolymers with styrene
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Abstract
The invention discloses a steel slag-micro silicon powder composite rubber filler with reinforcement-flame retardant synergistic performance and a preparation method thereof, belonging to the field of recycling of solid waste resources. The filler comprises water, a silane coupling agent, steel slag and micro silicon powder. The preparation method of the filler comprises the following steps: firstly, mixing and dispersing water and a silane coupling agent to obtain a silane coupling agent solution; then mixing the steel slag and the micro silicon powder, and stirring the mixture to obtain a steel slag-micro silicon powder mixture; and finally, mixing and stirring the steel slag-micro silicon powder mixture and the silane coupling agent solution to obtain the steel slag-micro silicon powder composite rubber filler. The invention not only solves the problems of higher price and single function of main fillers of carbon black and white carbon black in the rubber industry, but also improves the mechanical property and the flame retardant property of rubber; and the recycling of industrial waste is realized, the efficiency of metallurgical enterprises is promoted, the cost of the rubber product industry is reduced, and the current industrial development requirements of energy conservation, environmental protection and recycling economy are met.
Description
Technical Field
The invention belongs to the field of recycling of solid waste resources, and particularly relates to a steel slag-micro silicon powder composite rubber filler with reinforcement-flame retardant synergistic performance and a preparation method thereof.
Background
The steel slag is solid waste generated in the steel-making process and accounts for about 15 to 20 percent of the steel-making yield. The steel slag mainly comprises calcium, iron, silicon, magnesium and a small amount of oxides of aluminum, manganese, phosphorus and the like, namely SiO2、Fe2O3、Al2O3、ZnO、CaO、MgO、P2O5、MnO、SO3And the like, and also contains free calcium oxide, metallic iron, and the like. The micro silicon powder is a large amount of SiO with strong volatility produced in an ore-smelting electric furnace when ferroalloy is used for smelting ferrosilicon and industrial silicon (metallic silicon)2And Si gas, which is quickly oxidized, condensed and precipitated with air after being discharged. At present, the steel slag and the silica fume are largeThe materials are piled up, not only the precious land is occupied, but also the surrounding environment and the underground water are polluted. Therefore, how to utilize the steel slag and the micro silicon powder in a large scale and high efficiency to realize the reduction of the environment and the synergy of enterprises is a problem which needs to be solved urgently.
Rubber is used as a polymer material with wide application, and a large amount of filler is required in the preparation and processing process of the rubber so as to improve the mechanical property, the processing property and the filling capacity. At present, the commonly used rubber fillers mainly comprise carbon black, white carbon black and the like, but the production of the carbon black and the white carbon black is complex in process, and a large amount of energy and resources are consumed, so that the cost is high. In the face of the problems, the steel slag with high alkalinity and the micro silicon powder belong to porous substances and are potential reinforcing fillers; meanwhile, the alkalinity of the steel slag has a synergistic reaction effect on the silica fume, so that the silica fume is favorable for forming a compact flame-retardant amorphous siliceous layer, and the steel slag is a potential flame-retardant filler.
Disclosure of Invention
The invention provides a steel slag-micro silicon powder composite rubber filler with reinforcement-flame retardant synergistic performance, aiming at solving the problems that the main fillers of carbon black and white carbon black in the existing rubber industry are high in price and single in function, steel slag and micro silicon powder are directly added into rubber and are very easy to agglomerate, and the compatibility between an inorganic interface of the steel slag-micro silicon powder and an organic interface of the rubber is poor.
The invention is realized by the following technical scheme.
The invention provides a steel slag-micro silicon powder composite rubber filler with reinforcement-flame retardant synergistic performance, which comprises the following components in percentage by weight:
the water is deionized water; the silane coupling agent is industrially pure; the steel slag is molten iron desulphurization tailings, casting residues, converter hot splashing slag, converter roller slag, electric furnace hot splashing slag, electric furnace roller slag and a mixture thereof, and the particle size of the steel slag is 2.0-120.0 mu m; the particle size of the micro silicon powder is 6.5-43.8 μm.
The invention also provides a preparation method of the steel slag-micro silicon powder composite rubber filler, which comprises the following steps:
firstly, mixing water and a silane coupling agent, and dispersing the mixture for 15-35 min by using an ultrasonic disperser to obtain a silane coupling agent solution; then mixing the steel slag and the micro silicon powder, and stirring the mixture for 7 to 10 hours at normal temperature under sealing by using a constant-temperature magnetic stirrer to obtain a steel slag-micro silicon powder mixture; and finally, mixing the steel slag-micro silicon powder mixture with a silane coupling agent solution, and stirring for 2-4 hours at the stirring temperature of 60-80 ℃ by using a constant-temperature magnetic stirrer to obtain the steel slag-micro silicon powder composite rubber filler.
The scientific principle of the invention is as follows:
on one hand, the steel slag and the micro silicon powder both have porous structures, so that the contact area with rubber can be increased, and the reinforcing effect is achieved. The alkalinity of the steel slag has a synergistic reaction effect on the silica fume, and is beneficial to the silica fume to form a compact amorphous siliceous layer, so that the flame retardant effect is achieved.
On the other hand, the silane coupling agent solution is used for modifying the surface of the steel slag-micro silicon powder mixture to form the steel slag-micro silicon powder composite rubber filler, so that the defect of poor compatibility of the steel slag-micro silicon powder inorganic interface and the rubber organic interface is overcome, and the reinforcing effect is further improved.
In addition, as the steel slag is used as a high-alkalinity substance, the steel slag-micro silicon powder is filled in the rubber, so that the vulcanization speed of the rubber can be accelerated.
Compared with the prior art, the invention has the following technical effects:
1. the invention solves the problems that the main fillers of carbon black and white carbon black in the existing rubber industry have higher price and single function, steel slag and micro silicon powder are directly added into rubber and are easy to agglomerate, and the compatibility between an inorganic interface of the steel slag-micro silicon powder and an organic interface of the rubber is poor.
2. The steel slag and the silica fume are compounded to be used as the rubber filler, so that the problem that the price of carbon black and white carbon black which are main fillers in the rubber industry is high is solved, and the mechanical property and the flame retardant property of the rubber are improved; and the recycling of industrial waste is realized, the efficiency of metallurgical enterprises is promoted, the cost of the rubber product industry is reduced, and the current industrial development requirements of energy conservation, environmental protection and recycling economy are met.
Detailed Description
The present invention will be described in detail with reference to specific examples, but the present invention is not limited to the examples.
Firstly, the invention relates to a preparation method of steel slag-micro silicon powder composite rubber filler with reinforcement-flame retardant synergistic performance
Example 1
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the water is deionized water; the silane coupling agent is industrially pure; the steel slag is molten iron desulphurization tailings, and the particle size of the steel slag is 5.6-110.4 mu m; the particle size of the micro silicon powder is 6.8-35.2 μm.
Firstly, mixing water and a silane coupling agent, and dispersing the mixture for 20min by using an ultrasonic disperser to obtain a silane coupling agent solution; then mixing the steel slag and the micro silicon powder, and stirring the mixture for 9 hours at normal temperature under sealing by using a constant-temperature magnetic stirrer to obtain a steel slag-micro silicon powder mixture; and finally, mixing the steel slag-micro silicon powder mixture with a silane coupling agent solution, and stirring for 4 hours at the stirring temperature of 65 ℃ by using a constant-temperature magnetic stirrer to obtain the steel slag-micro silicon powder composite rubber filler.
Example 2
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the water is deionized water; the silane coupling agent is industrially pure; the steel slag is casting residue, and the particle size of the steel slag is 4.5-104.2 mu m; the particle size of the micro silicon powder is 7.8-42.1 μm.
Firstly, mixing water and a silane coupling agent, and dispersing the mixture for 30min by using an ultrasonic disperser to obtain a silane coupling agent solution; then mixing the steel slag and the micro silicon powder, and stirring the mixture for 7 hours at normal temperature under sealing by using a constant-temperature magnetic stirrer to obtain a steel slag-micro silicon powder mixture; and finally, mixing the steel slag-micro silicon powder mixture with a silane coupling agent solution, and stirring for 3 hours at the stirring temperature of 75 ℃ by using a constant-temperature magnetic stirrer to obtain the steel slag-micro silicon powder composite rubber filler.
Example 3
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the water is deionized water; the silane coupling agent is industrially pure; the steel slag is hot splashing slag of a converter, and the particle size of the steel slag is 2.6-92.1 mu m; the particle size of the micro silicon powder is 8.3-43.1 μm.
Firstly, mixing water and a silane coupling agent, and dispersing the mixture for 25min by using an ultrasonic disperser to obtain a silane coupling agent solution; then mixing the steel slag and the micro silicon powder, and stirring the mixture for 10 hours at normal temperature under sealing by using a constant-temperature magnetic stirrer to obtain a steel slag-micro silicon powder mixture; and finally, mixing the steel slag-micro silicon powder mixture with a silane coupling agent solution, and stirring for 3 hours at the stirring temperature of 60 ℃ by using a constant-temperature magnetic stirrer to obtain the steel slag-micro silicon powder composite rubber filler.
Example 4
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the water is deionized water; the silane coupling agent is industrially pure; the steel slag is converter roller slag and electric furnace hot splashing slag, and the mass fraction ratio of the converter roller slag to the electric furnace hot splashing slag is 50: 50 with the grain diameter of 3.9-115.2 μm; the particle size of the micro silicon powder is 8.2-36.5 μm.
Firstly, mixing water and a silane coupling agent, and dispersing the mixture for 35min by using an ultrasonic disperser to obtain a silane coupling agent solution; then mixing the steel slag and the micro silicon powder, and stirring the mixture for 8 hours at normal temperature under sealing by using a constant-temperature magnetic stirrer to obtain a steel slag-micro silicon powder mixture; and finally, mixing the steel slag-micro silicon powder mixture with a silane coupling agent solution, and stirring for 2 hours at the stirring temperature of 80 ℃ by using a constant-temperature magnetic stirrer to obtain the steel slag-micro silicon powder composite rubber filler.
Example 5
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the water is deionized water; the silane coupling agent is industrially pure; the steel slag is electric furnace hot splashing slag and electric furnace roller slag, the mass fraction ratio of the electric furnace hot splashing slag to the electric furnace roller slag is 50: 50, and the particle size is 4.5-116.6 μm; the particle size of the micro silicon powder is 8.9-42.9 μm.
Firstly, mixing water and a silane coupling agent, and dispersing for 15min by using an ultrasonic disperser to obtain a silane coupling agent solution; then mixing the steel slag and the micro silicon powder, and stirring the mixture for 9 hours at normal temperature under sealing by using a constant-temperature magnetic stirrer to obtain a steel slag-micro silicon powder mixture; and finally, mixing the steel slag-micro silicon powder mixture with a silane coupling agent solution, and stirring for 4 hours at the stirring temperature of 70 ℃ by using a constant-temperature magnetic stirrer to obtain the steel slag-micro silicon powder composite rubber filler.
Example 6
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the water is deionized water; the silane coupling agent is industrially pure; the steel slag is molten iron desulphurization tailings, casting residues and converter hot splashing slag, the mass fraction ratio of the molten iron desulphurization tailings, the casting residues and the converter hot splashing slag is 30: 40: 30, and the particle size of the steel slag is 3.1-113.6 microns; the particle size of the micro silicon powder is 7.4-43.2 μm.
Firstly, mixing water and a silane coupling agent, and dispersing the mixture for 30min by using an ultrasonic disperser to obtain a silane coupling agent solution; then mixing the steel slag and the micro silicon powder, and stirring the mixture for 8 hours at normal temperature under sealing by using a constant-temperature magnetic stirrer to obtain a steel slag-micro silicon powder mixture; and finally, mixing the steel slag-micro silicon powder mixture with a silane coupling agent solution, and stirring for 3 hours at the stirring temperature of 75 ℃ by using a constant-temperature magnetic stirrer to obtain the steel slag-micro silicon powder composite rubber filler.
Comparative example 1
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the steel slag is molten iron desulphurization tailings, casting residues and converter hot splashing slag, the mass fraction ratio of the molten iron desulphurization tailings, the casting residues and the converter hot splashing slag is 30: 40: 30, and the particle size of the steel slag is 3.1-113.6 microns; the particle size of the micro silicon powder is 7.4-43.2 μm.
Mixing the steel slag and the micro silicon powder, and stirring the mixture for 8 hours at normal temperature under sealing by using a constant-temperature magnetic stirrer to obtain the steel slag-micro silicon powder composite rubber filler.
Comparative example 2
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the water is deionized water; the steel slag is molten iron desulphurization tailings, casting residues and converter hot splashing slag, the mass fraction ratio of the molten iron desulphurization tailings, the casting residues and the converter hot splashing slag is 30: 40: 30, and the particle size of the steel slag is 3.1-113.6 microns; the particle size of the micro silicon powder is 7.4-43.2 μm.
Firstly, mixing steel slag and micro silicon powder, and stirring the mixture for 8 hours at normal temperature under sealing by using a constant-temperature magnetic stirrer to obtain a steel slag-micro silicon powder mixture; and finally, mixing the steel slag-micro silicon powder mixture with water, and stirring for 3 hours at the stirring temperature of 75 ℃ by using a constant-temperature magnetic stirrer to obtain the steel slag-micro silicon powder composite rubber filler.
Comparative example 3
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the water is deionized water; the silane coupling agent is industrially pure; the steel slag is molten iron desulphurization tailings, casting residues and converter hot splashing slag, the mass fraction ratio of the molten iron desulphurization tailings, the casting residues and the converter hot splashing slag is 30: 40: 30, and the particle size of the steel slag is 3.1-113.6 microns.
Firstly, mixing water and a silane coupling agent, and dispersing the mixture for 30min by using an ultrasonic disperser to obtain a silane coupling agent solution; then mixing the steel slag with the silane coupling agent solution, and stirring for 3 hours at the stirring temperature of 75 ℃ by using a constant-temperature magnetic stirrer to obtain the steel slag rubber filler.
Comparative example 4
The components used for preparing 100g of the product of the invention and the mass ratio thereof are as follows:
the water is deionized water; the silane coupling agent is of industrial purity.
Mixing water and a silane coupling agent, and dispersing the mixture for 30min by using an ultrasonic disperser to obtain a silane coupling agent solution.
Secondly, the mechanical property test and the flame retardant property test of the steel slag-micro silicon powder composite rubber filler added with rubber
The performance detection processes of the preparation examples 1 to 6 and the comparative examples 1 to 4 are as follows:
placing 100 parts of styrene butadiene rubber into an open mill for thin passing for 3-5 times, adding the styrene butadiene rubber into an internal mixer (the internal mixing temperature is 70 ℃) for mixing for 3min, sequentially adding 2.5 parts of zinc oxide mixed sample for mixing for 1min, adding 25 parts of carbon black and 25 parts of steel slag-micro silicon powder composite rubber filler (25 parts) mixed sample for mixing for 1min, adding 1.0 part of accelerator and 1.5 parts of sulfur, mixing for 1min, and taking out for later use, namely internal mixing rubber; putting the banburying rubber into an open mill for thin passing 6-8 times, wrapping for 5 times by a triangular bag, standing for 12 hours, weighing 60g of the banburying rubber, vulcanizing by a four-column type flat vulcanizing machine at the vulcanizing temperature of 145 ℃, and standing for 24 hours after vulcanizing for a certain time to obtain the steel slag-micro silicon powder composite styrene-butadiene rubber.
The tensile property of the steel slag-micro silicon powder composite styrene-butadiene rubber is tested by the determination of the tensile stress strain property of vulcanized rubber or thermoplastic rubber (GB/T528-2009); determination of tear Strength of vulcanized rubber or thermoplastic rubber (pants-type, right-angled, crescent-shaped test specimens) (GB/T529-2008) the tear Strength of the steel slag-silicon micropowder composite styrene-butadiene rubber was tested; method for press-in hardness test of vulcanized rubber or thermoplastic rubber part 1: the hardness of the steel slag-micro silicon powder composite styrene butadiene rubber is tested by a Shore durometer method (Shore hardness); testing the Limiting Oxygen Index (LOI) of the steel slag-micro silicon powder composite styrene-butadiene rubber by an oxygen index method (GB/T2406-1993) of a plastic combustion performance test method; a test method UL94 (ISBN 0-7629 and 0082-2) for testing the combustion performance of equipment and device plastic materials tests the vertical combustion level of the steel slag-micro silicon powder composite styrene-butadiene rubber.
TABLE 1 mechanical and flame-retardant properties of steel slag-silica fume compounded styrene-butadiene rubber
Placing 100 parts of natural rubber into an open mill, thinly passing the natural rubber for 1-3 times, adding the natural rubber into an internal mixer (at an internal mixing temperature of 70 ℃) for mixing for 3min, sequentially adding a zinc oxide (6.0 parts) mixed sample for mixing for 1min, adding a carbon black (25 parts) and a steel slag-silica fume composite rubber filler (25 parts) mixed sample for mixing for 1min, adding an accelerator (0.5 part) and sulfur (2.5 parts) for mixing for 1min, and taking out the mixture for later use, namely internal mixing rubber; placing the banburying rubber into an open mill for thin passing for 2-4 times, wrapping for 3 times by a triangular bag, standing for 12 hours, weighing 60g of the banburying rubber, vulcanizing by a four-column type flat vulcanizing machine at the vulcanizing temperature of 145 ℃, standing for 24 hours after vulcanizing for a certain time to obtain the steel slag-micro silicon powder composite natural rubber
The tensile property of the steel slag-micro silicon powder composite natural rubber is tested in the determination of the tensile stress strain property of vulcanized rubber or thermoplastic rubber (GB/T528-2009); determination of tear Strength of vulcanized rubber or thermoplastic rubber (pants-type, right-angled, crescent-shaped test specimens) (GB/T529-2008) the tear Strength of the steel slag-micro silicon powder compounded natural rubber was tested; method for press-in hardness test of vulcanized rubber or thermoplastic rubber part 1: the hardness of the steel slag-micro silicon powder composite natural rubber is tested by a Shore durometer method (Shore hardness); testing the Limiting Oxygen Index (LOI) of the steel slag-micro silicon powder composite natural rubber by an oxygen index method (GB/T2406-1993) of a plastic combustion performance test method; a test method UL94 (ISBN 0-7629 and 0082-2) for the combustion performance of equipment and device plastic materials tests the vertical combustion level of the steel slag-micro silicon powder composite natural rubber.
Table 2. mechanical properties and flame retardant property of steel slag-micro silicon powder composite natural rubber
Claims (1)
1. The steel slag-micro silicon powder composite rubber filler with the reinforcement-flame retardant synergistic performance is characterized by comprising the following components in percentage by weight:
the water is deionized water; the silane coupling agent is industrially pure; the steel slag is one or more of molten iron desulphurization tailings, casting residues, converter hot splashing slag, converter roller slag, electric furnace hot splashing slag and electric furnace roller slag, and the particle size of the steel slag is 2.0-120.0 mu m; the particle size of the micro silicon powder is 6.5-43.8 μm;
the preparation of the steel slag-micro silicon powder composite rubber filler with reinforcement-flame retardant synergistic performance comprises the following steps:
firstly, mixing water and a silane coupling agent, and dispersing the mixture for 15-35 min by using an ultrasonic disperser to obtain a silane coupling agent solution; then mixing the steel slag and the micro silicon powder, and stirring the mixture for 7 to 10 hours at normal temperature under sealing by using a constant-temperature magnetic stirrer to obtain a steel slag-micro silicon powder mixture; and finally, mixing the steel slag-micro silicon powder mixture with a silane coupling agent solution, and stirring for 2-4 hours at the stirring temperature of 60-80 ℃ by using a constant-temperature magnetic stirrer to obtain the steel slag-micro silicon powder composite rubber filler.
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| WO2022233032A1 (en) * | 2021-05-07 | 2022-11-10 | 德州学院 | Method for preparing composite pigment and filler for coating by using silica fume |
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| CN106543487A (en) * | 2015-09-16 | 2017-03-29 | 上海中冶环境工程科技有限公司 | A kind of rubber using slag micro powder as rubber filler |
| CN106893139A (en) * | 2017-03-30 | 2017-06-27 | 安徽工业大学 | A kind of modified porous slag for gum filler and preparation method thereof |
| JP6183256B2 (en) * | 2014-03-19 | 2017-08-23 | 三菱マテリアル株式会社 | Rubber composition and rubber molded body |
| CN107501611A (en) * | 2017-09-19 | 2017-12-22 | 安徽工业大学 | A kind of slag red mud compounded rubber filler with the fire-retardant synergisticing performance of reinforcement |
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| JP6183256B2 (en) * | 2014-03-19 | 2017-08-23 | 三菱マテリアル株式会社 | Rubber composition and rubber molded body |
| CN106543487A (en) * | 2015-09-16 | 2017-03-29 | 上海中冶环境工程科技有限公司 | A kind of rubber using slag micro powder as rubber filler |
| CN106893139A (en) * | 2017-03-30 | 2017-06-27 | 安徽工业大学 | A kind of modified porous slag for gum filler and preparation method thereof |
| CN107501611A (en) * | 2017-09-19 | 2017-12-22 | 安徽工业大学 | A kind of slag red mud compounded rubber filler with the fire-retardant synergisticing performance of reinforcement |
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