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    • 专利摘要:
    The invention discloses a reinforced, flame-retardant, wear-resistant, all-industrial solid waste composite rubber filler and a manufacturing method thereof and belongs to the field of industrial recycling of solid waste resources. The filler contains stainless steel slag, fly ash, phosphorus slag, magnesium slag, manganese slag, composite grinding aid, surface modifier, and water. The stainless steel slag, fly ash, phosphorus slag, magnesium slag, and manganese slag are all solid industrial wastes. The compound grinding aid is a mixture of glycerine, absolute ethanol and triethanolamine. The surface modifier It is a mixture of stearic acid and silane coupling agent KH550. The invention uses stainless steel slag, fly ash, phosphorus slag, magnesium slag and manganese slag to produce a purely industrial solid waste reinforcement-flame retardant-wear-resistant composite rubber packing, which not only lowers the cost of rubber packing but also increases the cost of rubber packing, it is functional and realizes the recycling of solid Industrial waste, promotes business efficiency, performance improvement and cost reduction of the rubber product industry and meets the current requirements of industrial development in terms of energy saving, environmental protection and circular economy.
    公开号:BE1027693B1
    申请号:E20205609
    申请日:2020-09-03
    公开日:2021-06-25
    发明作者:Shenghua Wu；Xiaoyan Du；Haili Li；Hao Zhang；Hongming Long；Zhifang Zong
    申请人:Univ Anhui Technology；
    IPC主号:
    专利说明:

    Description Reinforced, flame-retardant, wear-resistant, fully industrial BE2020 / 5609 composite rubber filler for solid waste and its manufacturing process Technical Field The invention belongs to the field of industrial recycling of solid waste resources and, in particular, relates to a reinforced, flame-retardant, wear-resistant, fully industrial composite rubber filler from solid waste and a manufacturing method thereof . Background technology Stainless steel slag, fly ash, phosphorus slag, magnesium slag, and manganese slag are solid industrial wastes. Among these, stainless steel slag is alkaline and its main components are CaO, Fe203, S102 and a small amount of ZnO, CuO, Cr203, PbO, etc. Heavy metal oxides, fly ash is acidic and its main components are S102, A1203, phosphorus slag is alkaline and its main components are CaO, SiO2 , P205, magnesium slag is alkaline, and its main components are CaO, S102, MgO3; Manganese slag is alkaline, and its main components are CaO, S102 and MnO. At present, a large number of open air storage areas of stainless steel slag, fly ash, phosphorus slag, magnesium slag and manganese slag not only occupy valuable land but also cause environmental pollution and groundwater pollution. Therefore, the urgent use of stainless steel slag, fly ash, phosphorus slag, magnestum slag and manganese slag on a large scale and to efficiently reduce environmental pollution and increase business efficiency is an urgent problem to be solved.
    As a widely used polymer material, rubber must use a large amount of fillers in its manufacture and processing in order to improve its mechanical properties, processing properties, as well as filling and compatibility. Rubber fillers in use at present mainly include carbon black (8,000 yuan / ton), silica (6,000 yuan / ton), etc. However, production of carbon black and silica is not only complicated in processes, but also consumes a lot of energy and resources, resulting in cost. Higher.
    Summary of the Invention To solve the problem of high price and single function of the main filler carbon black and
    Solving white carbon in the existing rubber industry, i.e. the problem of just reinforcing BE2020 / 5609 performance, the use of an acid solution for alkaline solid waste (such as stainless steel slag, phosphorus slag, magnesium slag, modification with manganese slag), the problems of unsafe operation and the pollution exhibits; Stainless steel slag, fly ash, phosphorus slag, magnesium slag and manganese slag Recycling and low added value; Stainless steel slag, fly ash, phosphorus slag, magnesium slag and manganese slag have poor grindability and tend to agglomerate when added directly to rubber, and there is a problem of poor compatibility between inorganic and organic interfaces: stainless steel slag, fly ash, phosphorus slag, magnesium slag and manganese slag are all it has some flame retardancy, but there is a problem that it cannot be synergistically flame retardant. The present invention provides a reinforced, flame-retardant, wear-resistant, all-industrial solid waste type composite rubber filler to solve the above problems.
    The present invention is realized by the following technical solutions.
    The present invention provides a reinforced, flame retardant, wear resistant, all industrial composite rubber filler for solid waste. The fully industrial composite rubber filler for solid waste has the following formula according to weight percent: stainless steel slag 20% -40% fly ash 20% 30% phosphorus slag 10% 15% magnesium slag 10% 15% manganese slag 10% 15% composite grinding aid 1% -3% surface modifier 2 % -4% Water 3% -9% The stainless steel slag, fly ash, phosphorus slag, magnesium slag and manganese slag are solid industrial wastes. The composite grinding aid is a mixture of glycerine, absolute ethanol and triethanolamine, the glycerine. The mass ratio of absolute
    Ethanol and triethanolamine is 4: 2: 1 + 1: 1: 1, the surface modifier is a BE2020 / 5809 mixture of stearic acid and silane coupling agent KH550 and the stearic acid and silane coupling agent. The mass ratio of the agent KH550 is 5: 1 - 1: 1 Optimization, the particle diameters of the stainless steel slag, fly ash, phosphorus slag, magnesium slag and manganese slag are less than 5 mm.
    The present invention also provides a manufacturing method of the above-mentioned reinforced, flame-retardant, wear-resistant, all-industrial composite rubber filler for solid waste, and the manufacturing method comprises the following steps: (1) Mixing and mixing of stainless steel slag, fly ash, phosphorus slag, magnesium slag, manganese slag and composite grinding aids grind with a planetary ball mill at a speed of 600 rpm - 900 rpm and a time of 90 mm - 120 min to obtain rem industrial solid waste composite micropowder, then use planetary ball mill to perform mechanochemical treatment of the composite industrial waste micropowder, its speed is 200rpm - 300rpm, time is 72h - 96h to get all industrial solid waste composite micropowder micropowder.
    (2) Mix the surface modifier with water and disperse it with an ultrasonic disperser having a power of 600 W - 900 W and a time of 60 min - 90 min to obtain a surface modifier solution.
    (3) Mix the ultrafine industrial solid waste composite powder with the surface modification solution and stir it with a planetary ball mill at a speed of 300 rpm - 500 rpm and a time of 120 min - 150 min to make a modified whole industry To obtain Ultra-fine composite powder for solid waste, ie a reinforced, flame-retardant, abrasion-resistant, fully industrial rubber filler made from solid waste.
    The scientific principle of the present invention: (1) Use the surfactant molecules glycerin, absolute ethanol and triethanolamine in the composite grinding aid to be used on the surface of the stainless steel slag, fly ash, phosphorus slag, magnesium slag and manganese slag to be ground. A single molecule adsorption film is created.
    During the crushing process, BE2020 / 5609 stainless steel slag, fly ash, phosphorus slag, magnesium slag and manganese slag are broken and the free valence bond is created on the fracture surface and the ion or molecule provided by the composite grinding aid, neutralization is carried out to reduce the aggregation tendency of the composite powder from solid waste throughout Eliminate or weaken industry and prevent the fracture surface from reuniting. (2) The porous structure of stainless steel slag, fly ash, phosphorus slag, magnesium slag and manganese slag can improve the adsorbing effect of soot and enlarge the contact area with rubber to achieve a reinforcing effect.
    Stainless steel slag, phosphorus slag, magnesium slag and manganese slag are all alkaline in the SiO2-CaO system.
    Appropriate alkalinity can accelerate the rate of rubber vulcanization, but too high an alkalinity can increase the brittleness of the rubber, which is why the SiO2-Al203 system is used. Acid fly ash modifies alkaline solid waste (such as stainless steel slag, phosphorus slag, magnesium slag, and manganese slag) to remove the To reduce the alkalinity of stainless steel slag, fly ash, phosphorus slag and a mixture of magnesium slag and manganese slag.
    Enhance the reinforcement effect. (3) The long time stirring and grinding method is used to promote the mechanochemical treatment of stainless steel slag, fly ash, phosphorus slag, magnesium slag and manganese slag, that is, the crushing process can reduce the particle size of the material and increase the specific surface area, such as the number of mechanochemical changes, such as the distortion the crystal structure and the lowering of the temperature of the thermal effect, form a flame retardant silicon-phosphorus-iron system, a silicon-phosphorus-magnesium system and a silicon-phosphorus-aluminum system to improve the flame retardant effect.
    Using MnO-containing manganese slag, a catalytic reaction occurs during the rubber vulcanization process to improve the stability of the network structure of the rubber system and achieve the purpose of improving the wear resistance.
    (4) Using stearic acid and silane coupling agent KH570 in the surface modifier BE2020 / 5609 to form an organic coating layer on the surface of the industrial solid waste composite ultrafine powder, reduce agglomeration of the industrial solid waste composite ultrafine powder, and improve the modification of the whole 5 industrial solid matter The dispersing effect of superfine waste composite powder can achieve the purpose of good compatibility with rubber.
    (5) The main components of the stainless steel slag are CaO, Fe 2 O 3, S10 2 and a small amount of heavy metal oxides such as ZnO, CuO, Cr 2 O 3 and PbO. Among these, heavy metal oxides such as ZnO, CuO, Cr 2 O 3 and PbO have a promoting effect in the rubber system.
    Or synergistic promotion to improve the synergistic properties of the wear resistance of rubber reinforcing flame retardants.
    Compared to the prior art, the present invention has the following technical effects:
    1. The present invention solves the problem of the high price and the single function of the main filler carbon black and white carbon in the existing rubber industry, that is, the problem of reinforcing performance only; Slag, magnesium slag and manganese slag) are modified, which brings with it the problems of unsafe operation and pollution: stainless steel slag, fly ash, phosphorus slag, magnestum slag and manganese slag recycling and problems with low added value; Stainless steel slag, fly ash, phosphorus slag, magnesium slag and manganese slag have poor grindability and agglomerate easily when added directly to rubber, and there is a problem of poor compatibility between inorganic and organic interfaces, stainless steel slag, fly ash, phosphorus slag and magnesium slag Manganese slag also has a certain degree of flame retardancy, but there is the problem that they cannot be synergistically flame retardant.
    2. The present invention uses stainless steel slag, fly ash, phosphorus slag, magnesium slag and manganese slag to produce rem industrial solid wastes that reinforce flame-resistant, wear-resistant composite rubber fillers, which not only lowers the cost of rubber fillers, but also expands the functionality of the rubber Filler and the realization of the recycling of BE2020 / 5609 solid industrial waste have promoted the efficiency of businesses, as well as the performance and cost reduction of the rubber product industry, which meets the current demands of industrial development in terms of energy saving, environmental protection and circular economy.
    Detailed Description The present invention will be described in detail below with reference to specific embodiments, but the present invention is not limited to the following embodiments.
    1. Manufacturing method of reinforced, flame-retardant, wear-resistant, all-industrial composite rubber filler from solid waste of the present invention. Example 1 Taking 100 g of the product of the present invention as an example, the components and their mass ratios are: stainless steel slag 28% fly ash 24% phosphorus slag 14 % Magnesium slag 10% manganese slag 12% composite grinding aid 3% surface modifier 2% water 7% The main chemical composition of stainless steel slag: CaO is 52.35%, SIO 2 is 23.68%, A12 O 3 is 8.31%, MgO is 7, 56%, Fe 2 O3 is 1.96%, Cr 2 O3 is 1.12%, PbO is 0.83%, P20 5 is 0.41%, CuO The main chemical composition of fly ash: SiO 2 is 51.53% , A12 03 is 27.78%, Fe 2 03 is 4.73%, and CaO is 5.21%. MgO is 1.03%, K20 is 1.13%, Na20 is 0.62%, TiO2 is 2.24%, SO3 is 1.87%, others are 3.86%, and its particle size is less than 5mm, the main chemical composition of phosphorus slag: CaO is 45.70%, Al2 O 3 is 2.57%, SiO 2 is 40.80%, K 2 O is 1.01%, P2O 5 is 3.91%, MgO is 3 , 32%, TiO 2 is 0.22%, MnO is 0.02%, others are 2,459 72020/5609, and its particle size is less than 5mm, the magnesium slag The main chemical composition: Na 2 O is 0.06%, MgO is 7.31%, Al 2 O 3 is 1.78%, SiO 2 is 31.24%, CaO is 51.21%, TiO 2 is 0.09%, Fe 2 O 3 is 4.45%, others is 3.86% and its particle size is less than 5 mm. The main chemical composition of the manganese slag: SiO 2 is 20.05%, A12 03 is 16.42%, CaO is 37.62%, MgO is 6.52%, SO 3 is 0.48%, Fe 2 O 3 is 1.23%, MnO is 10.87%, T1O 2 is 0.42%, the other is 6.39%, and its particle size is wen less than 5 mm, the composite grinding aid is a mixture of glycerin, anhydrous ethanol and triethanolamine, and the mass ratio of glycerin, anhydrous ethanol and triethanolamine is 2: 1: 1; Among these, glycerin, absolute ethanol, and triethanolamine are all analytical, the surface modifier is a mixture of stearic acid and silane coupling agent KH550, and the mass ratio of stearic acid and silane coupling agent KH550 is 5: 1 When stearic acid and silane coupling agent KH550 are both industrial, the water is deionized water .
    (1) Mix stainless steel slag, fly ash, phosphorus slag, magnesium slag, manganese slag and composite grinding aids and grind them with a planetary ball mill at a speed of 900rpm and a time of 100min to get a full industrial composite powder of solid Waste. The planetary ball mill is then used to mechanochemically treat the composite industrial waste micropowder at a speed of 250 rpm and a time of 72 hours to obtain a full ultrafine industrial solid waste composite powder.
    (2) Mix the surface modifier with water and disperse it with an ultrasonic disperser having a power of 600 W and a time of 80 minutes to obtain a surface modifier solution.
    (3) Mix the ultrafine industrial solid waste composite powder with the surface modification solution and stir it with a planetary ball mill at a speed of 500 rpm and a time of 150 minutes to obtain a modified ultrafine industrial solid waste composite powder. That means em reinforced, flame retardant,
    wear resistant, fully industrial solid waste composite rubber filler.
    BE2020 / 5609 Example 2 Using the example of the production of 100 g of the product of the present invention, the components and their mass ratios are: stainless steel slag 22% fly ash 30% phosphorus slag 13% magnesium slag 11% manganese slag 10% composite grinding aid 1% surface modifier 4% water 9 % The main chemical composition of stainless steel slag: CaO is 52.35%, SIO 2 is 23.68%, A12 O 3 is 8.31%, MgO is 7.56%, Fe 2 O3 is 1.96%, Cr 2 O3 is 1.12%, PbO is 0.83%, P20 5 is 0.41%, CuO The main chemical composition of fly ash: SiO 2 is 51.53%, A12 O 3 is 27.78%, Fe 2 O 3 is 4.73%, CaO is 5.21%, and others are 3.09%. The particle size is less than 5 mm.
    MgO is 1.03%, K2O is 1.13%, Na20 is 0.62%, TiO2 is 2.24%, SO3 is 1.87%, others are 3.86%, and its particle size is less than 5mm, the main chemical composition of phosphorus slag: CaO is 45.70%, A1203 is 2.57%, SiO 2 is 40.80%, K 2 O is 1.01%, P2O 5 is 3.91%, MgO is 3.32 %, TIO 2 is 0.22%, MnO is 0.02%, others are 2.45%, and its particle size is less than 5mm, the magnesium slag.The main chemical composition: Na 2 O is 0.06%, MgO is 7 , 31%, A12 O 3 is 1.78%, S10 2 is 31.24%, CaO is 51.21%, TIO 2 is 0.09%, Fe 2 O 3 is 4.45%, others are 3, 86% and its particle size is less than 5 mm.The main chemical composition of manganese slag: SiO 2 is 20.05%, Al 2 O 3 is 16.42%, CaO is 37.62%, MgO is 6.52%, SO 3 is 0.48%, Fe 2 O 3 is 1.23%, MnO is 10.87%, TiO 2 is 0.42%, the other is 6.39% and its particle size is less than 5 mm, the compound grinding aid is a mixture of glycerine, absolute ethanol and triethanolamine and the mass ratio of glycerine, absolute ethanol and triethanolamine is 4: 2: 1. BE2020 / 5609 Glycerine, absolute ethanol and triethanolamine are all analytically pure, the surface modifier is one Mixture of stearic acid and silane coupling agent KH550 and the mass ratio of stearic acid and silane coupling agent KH550 is 2: 1. When stearic acid and silane coupling agent KH550 are both industrial remedies, the water is deionized water.
    (1) Mix stainless steel slag, fly ash, phosphorus slag, magnesium slag, manganese slag and composite grinding aids, and grind them with a planetary ball mill at a speed of 700 rpm and a time of 110 min to get the whole industry composite powder from solid waste. The planetary ball mill is then used for mechanochemical treatment of the composite industrial waste micropowder at a rotation speed of 300 rpm and a time of 90 hours to obtain full ultrafine industrial solid waste composite powder.
    (2) Mix the surface modifier with water and disperse it with an ultrasonic disperser having a power of 700 W and a time of 90 minutes to obtain a surface modifier solution.
    (3) Mix the ultrafine industrial solid waste composite powder with the surface modification solution and stir it with a planetary ball mill at a speed of 300 rpm and a time of 130 minutes to obtain a modified ultrafine industrial solid waste composite powder. That is, a reinforced, flame retardant, wear resistant, all industrial solid waste composite rubber filler.
    Example 3 Using the example of the production of 100 g of the product of the present invention, the components and their mass ratios are: Stainless steel slag 26% Fly ash 28% Phosphorus slag 12% Magnesium slag 15% Manganese slag 11%
    Composite grinding aid 2% BE2020 / 5609 surface modifier 3% water 3% The main chemical composition of stainless steel slag: CaO is 52.35%, S1O 2 is 23.68%, A12 O3 is 8.31%, MgO is 7.56%, Fe 2 O 3 is 1.96%, Cr 2 O3 is 1.12%, PbO is 0.83%, P20 5 is 0.41%, CuO The main chemical composition of fly ash: S10 2 is 51.53%, A1 2 O 3 is 27.78%, Fe 2 O 3 is 4.73%, CaO is 5.21%, and others are 3.09%. The particle size is less than 5 mm.
    MgO is 1.03%, K20 is 1.13%, Na20 is 0.62%, T102 is 2.24%, SO3 is 1.87%, others are 3.86%, and its particle size is less than 5mm, the main chemical composition of phosphorus slag: CaO is 45.70%, Al203 is 2.57%, S10 2 is 40.80%, K 2 O is 1.01%, P2O 5 is 3.91%, MgO is 3.32 %, TIO 2 is 0.22%, MnO is 0.02%, others are 2.45%, and its particle size is less than 5mm, the magnesium slag.The main chemical composition: Na 2 O is 0.06%, MgO is 7 , 31%, Al 2 O 3 is 1.78%, S10 2 is 31.24%, CaO is 51.21%, TiO 2 is 0.09%, Fe 2 O 3 is 4.45%, others are 3 .86% and its particle size is less than 5 mm. The main chemical composition of manganese slag: SiO 2 is 20.05%, Al 2 O 3 is 16.42%, CaO is 37.62%, MgO is 6.52%, SO 3 is 0.48%, Fe 2 O 3 is 1.23%, MnO is 10.87%, TiO 2 is 0.42%, the other is 6.39%, and its particle size is less than 5 mm, the - composite grinding aid is a mixture of glycerin, anhydrous ethanol and triethanolamine, and the mass ratio of glycerin, anhydrous ethanol and triethanolamine is 4: 1: 1; Glycerin, anhydrous ethanol and triethanolamm are all analytically pure, the surface modifier is a mixture of stearic acid and silane coupling agent KH550 and the mass ratio of stearic acid and silane coupling agent KH550 is 3: 1 If stearic acid and silane coupling agent KH550 are both industrially pure, the water is deionized water. (1) Mix stainless steel slag, fly ash, phosphorus slag, magnesium slag, manganese slag and composite grinding aids, and grind them with a planetary ball mill at a speed of 600 rpm and a time of 120 min to get the whole industry composite powder from solid waste. The planetary ball mill is then used to BE2020 / 5609 mechanochemical treatment of the composite industrial waste micropowder at a speed of 200 rpm and a time of 84 hours to obtain a fully braced ultrafine industrial waste composite powder.
    (2) Mix the surface modifier with water and disperse it with an ultrasonic disperser having a power of 900 W and a time of 60 minutes to obtain a surface modifier solution.
    (3) Mix the ultrafine industrial solid waste composite powder with the surface modification solution and stir it with a planetary ball mill at a speed of 400 rpm and a time of 120 minutes to obtain a modified ultrafine industrial solid waste composite powder. That is, a reinforced, flame retardant, wear resistant, all industrial solid waste composite rubber filler. Example 4 Using the example of the production of 100 g of the product of the present invention, the components and their mass ratios are: stainless steel slag 26% fly ash 20% phosphorus slag 15% magnesium slag 13% manganese slag 15% composite grinding aid 3% surface modifier 3% water 5% chemical Main composition of stainless steel slag: CaO is 52.35%, SIO 2 is 23.68%, A12 O3 is 8.31%, MgO is 7.56%, Fe 2 O 3 is 1.96%, Cr 2 03 is 1, 12%, PbO is 0.83%, P20 5 is 0.41%, CuO The main chemical composition of fly ash: SiIO 2 is 51.53%, A12 03 is 27.78%, Fe 2 03 is 4.73% and CaO is 5.21%. MgO is 1.03%, K20 is 1.13%, Na20 is 0.62%, TiO2 is 2.24%, SO3 is 1.87%, others are 3.86%, and its particle size is less than 5mm, the main chemical composition of phosphorus slag:
    CaO is 45.70%, Al2 O 3 is 2.57%, SiO 2 is 40.80%, K 2 O is 1.01%, P2O 5 BE2020 / 5609 is 3.91%, MgO is 3.32% , TiO 2 is 0.22%, MnO is 0.02%, others are 2.45%, and its particle size is less than 5mm, the magnestum slag The main chemical composition: Na 2 O is 0.06%, MgO is 7, 31%, Al 2 O 3 is 1.78%, S10 2 is 31.24%, CaO is 51.21%, TiO 2 is 0.09%, Fe 2 O 3 is 4.45%, others are 3, 86% and its particle size is less than 5mm.The main chemical composition of manganese slag: SiO 2 is 20.05%, A12 03 is 16.42%, CaO is 37.62%, MgO is 6.52%, SO 3 is 0 , 48%, Fe 2 O 3 is 1.23%, MnO is 10.87%, TiO 2 is 0.42%, the other is 6.39% and its particle size is less than 5mm, the composite grinding aid is a mixture of glycerin, anhydrous ethanol and triethanolamine, and the mass ratio of glycerin, anhydrous ethanol and triethanolamine is 1: 1: 1; Glycerm, absolute ethanol and triethanolamm are all analytically pure, the surface modifier is a mixture of stearic acid and silane coupling agent KH550 and the mass ratio of stearic acid and silane coupling agent KH550 is 1: 1 If stearic acid and silane coupling agent KH550 are both industrially pure, the water is deionized water.
    (1) Mix stainless steel slag, fly ash, phosphorus slag, magnesium slag, manganese slag and composite grinding aids, and grind them with a planetary ball mill at a speed of 800 rpm and a time of 90 minutes, for the whole industry to obtain composite powder from solid waste. The planetary ball mill is then used for mechanochemical treatment of the composite industrial solid waste micropowder at a rotation speed of 300 rpm and a time of 96 hours to obtain a full ultrafine industrial solid waste composite powder.
    (2) Mix the surface modifier with water and disperse it with an ultrasonic disperser having a power of 800 W and a time of 70 minutes to obtain a surface modifier solution.
    (3) Mix the ultrafine industrial solid waste composite powder with the surface modification solution and stir it with a planetary ball mill at a speed of 400 rpm and a time of 140 minutes to obtain a modified ultrafine industrial solid waste composite powder.
    That is, a reinforced, flame retardant, BE2020 / 5609 wear resistant, fully industrial solid waste composite rubber filler.
    Example 5 Using the example of the production of 100 g of the product of the present invention, the components and their mass ratios are: stainless steel slag 27% fly ash 22% phosphorus slag 11% magnestum slag 14% manganese slag 13% compound slag 2% surface modifier 2% water 7% the chemical Main composition of stainless steel slag: CaO is 52.35%, SIO 2 is 23.68%, A12 O3 is 8.31%, MgO is 7.56%, Fe 2 O 3 is 1.96%, Cr 2 O3 is 1, 12%, PbO is 0.83%, P20 5 is 0.41%, CuO The main chemical composition of fly ash: SiIO 2 is 51.53%, A12 O3 is 27.78%, Fe 2 O3 is 4.73% and CaO is 5.21%. MgO is 1.03%, K20 is 1.13%, Na20 is 0.62%, TiO2 is 2.24%, SO3 is 1.87%, others are 3.86%, and its particle size is less than 5mm, the main chemical composition of phosphorus slag: CaO is 45.70%, Al2 O 3 is 2.57%, SiO 2 is 40.80%, K 2 O is 1.01%, P20 5 is 3.91%, MgO is 3 , 32%, TiO 2 is 0.22%, MnO is 0.02%, others are 2.45%, and its particle size is less than 5mm, the magnestum slag, the main chemical composition: Na 2 O is 0.06%, MgO is 7.31%, Al 2 O 3 is 1.78%, S10 2 is 31.24%, CaO is 51.21%, TiO 2 is 0.09%, Fe 2 O 3 is 4.45%, others is 3.86% and its particle size is less than 5 mm.The main chemical composition of manganese slag: SiO 2 is 20.05%, A12 03 is 16.42%, CaO is 37.62%, MgO is 6.52%, SO 3 is 0.48%, Fe 2 O 3 is 1.23%, MnO is 10.87%, TIO 2 is 0.42%, the other is 6.39%, and the particle size is less than 5 mm, the compound grinding aid is a mixture of Glycerm, absolute ethanol and
    Triethanolamine, and the mass ratio of glycerin, absolute ethanol and triethanolamine BE2020 / 5609 is 2: 2: 1. Glycerin, absolute ethanol and triethanolamine are all analytically pure, the surface modifier is a mixture of stearic acid and silane coupling agent KH550 and the mass ratio of stearic acid and silane coupling agent KH550 is 4: 1 If stearic acid and KH550 silane coupling agent are both industrially pure, the water is deionized water.
    (1) Mix and grind stainless steel slag, fly ash, phosphorus slag, magnesium slag, manganese slag and composite grinding aids with a planetary ball mill at a speed of 600 rpm and a time of 110 minutes. Solid waste composite powder. The planetary ball mill is then used to mechanochemically treat the composite industrial waste micropowder at a speed of 250 rpm and a time of 78 hours to obtain a full ultrafine industrial solid waste composite powder.
    (2) Mix the surface modifier with water and disperse it with an ultrasonic disperser having a power of 900 W and a time of 90 minutes to obtain a surface modifier solution.
    (3) Mix the ultrafine industrial solid waste composite powder with the surface modification solution and stir it with a planetary ball mill at a speed of 300 rpm and a time of 130 minutes to obtain a modified ultrafine industrial solid waste composite powder. That is, a reinforced, flame retardant, wear resistant, all industrial solid waste composite rubber filler.
    Example 6 Using the example of the preparation of 100 g of the product of the present invention, the components and their mass ratios are: stainless steel slag 24% fly ash 26% phosphorus slag 10% magnesium slag 12% manganese slag 14%
    Composite grinding aid 1% BE2020 / 5609 surface modifier 4% water 9% The main chemical composition of stainless steel slag: CaO is 52.35%, SIO 2 is 23.68%, A12 O3 is 8.31%, MgO is 7.56%, Fe 2 O 3 is 1.96%, Cr 2 O3 is 1.12%, PbO is 0.83%, P20 5 is 0.41%, CuO The main chemical composition of fly ash: SiIO 2 is 51.53%, A1 2 O 3 is 27.78%, Fe 2 O 3 is 4.73%, CaO is 5.21%, and others are 3.09%. The particle size is less than 5 mm.
    MgO is 1.03%, K20 is 1.13%, Na20 is 0.62%, T102 is 2.24%, SO3 is 1.87%, others are 3.86%, and its particle size is less than 5mm, the main chemical composition of phosphorus slag: CaO is 45.70%, Al203 is 2.57%, S10 2 is 40.80%, K 2 O is 1.01%, P2O 5 is 3.91%, MgO is 3.32 %, TIO 2 is 0.22%, MnO is 0.02%, others are 2.45%, and its particle size is less than 5mm, the magnesium slag.The main chemical composition: Na 2 O is 0.06%, MgO is 7 , 31%, Al 2 O 3 is 1.78%, S10 2 is 31.24%, CaO is 51.21%, TIO 2 is 0.09%, Fe 2 O 3 is 4.45%, others are 3 .86% and its particle size is less than 5 mm. The main chemical composition of manganese slag: SiO 2 is 20.05%, Al 2 O 3 is 16.42%, CaO is 37.62%, MgO is 6.52%, SO 3 is 0.48%, Fe 2 O 3 is 1.23%, MnO is 10.87%, TiO 2 is 0.42%, the other is 6.39%, and its particle size is less than 5 mm, the - composite grinding aid is a mixture of glycerin, anhydrous ethanol and triethanolamine, and the mass ratio of glycerin, anhydrous ethanol and triethanolamine is 2: 1: 1; Glycerin, anhydrous ethanol and triethanolamm are all analytically pure, the surface modifier is a mixture of stearic acid and silane coupling agent KH550 and the mass ratio of stearic acid and silane coupling agent KH550 is 3: 1 If stearic acid and silane coupling agent KH550 are both industrially pure, the water is deionized water. (1) Mix stainless steel slag, fly ash, phosphorus slag, magnesium slag, manganese slag and composite grinding aids, and grind them with a planetary ball mill at a speed of 700 rpm and a time of 100 min for a complete industry of solid composite powder Waste. The BE2020 / 5609 planetary ball mill is then used to mechanochemically treat the composite industrial waste micropowder at a speed of 200 rpm and a time of 84 hours to obtain a superfine ultrafine industrial waste composite powder.
    (2) Mix the surface modifier with water and disperse it with an ultrasonic disperser having a power of 700 W and a time of 80 minutes to obtain a surface modifier solution.
    (3) Mix the ultrafine industrial solid waste composite powder with the surface modification solution and stir it with a planetary ball mill at a speed of 500 rpm and a time of 150 minutes to obtain a modified ultrafine industrial solid waste composite powder. That is, a reinforced, flame retardant, wear resistant, all industrial solid waste composite rubber filler. Comparative Example 1 Using the example of the production of 100 g of the product of the present invention, the components and their mass ratios are: stainless steel slag 50% fly ash 0% phosphorus slag 10% magnesium slag 12% manganese slag 14% composite grinding aid 1% surface modifier 4% water 9% chemical Main composition of stainless steel slag: CaO is 52.35%, SIO 2 is 23.68%, A12 O3 is 8.31%, MgO is 7.56%, Fe 2 O 3 is 1.96%, Cr 2 03 is 1, 12%, PbO is 0.83%, P20 5 is 0.41%, CuO it is 0.37%, MnO is 0.32%, others are 3.09%, its particle size is less than 5mm, the chemical Main composition of phosphorus slag: CaO is 45.70%, A12 03 is 2.57%, SiO 2 is 40.80%, K 2 O is 1.01%, P20 5 it is 3.91%, MgO is 3.32 %, TiO 2 is 0.22%, MnO is 0.02%, others are 2.45%, and its particle size is less than 5mm; the main chemical composition of magnesium slag: Na 2 O is 0.06%, MgO is 7.31%, Al BE2020 / 5809 203 It is 1.78%, SiO 2 is 31.24%, CaO is 51.21%, TiO 2 is 0.09%, Fe 2 O3 is 4.45%, others are 3.86% and its particle size is less than 5mm, the main chemical composition of manganese slag: SiO 2 is 20.05%, Al203 it is 16.42 %, CaO is 37.62%, MgO is 6.52%, SO &sub3; is 0.48%, Fe O is 1.23%, MnO is 10.87%, TIO is 0.42% and others are 6.39% and its particle size is less than 5 mm; The agent is a mixture of glycerine, anhydrous ethanol and triethanolamine. The mass ratio of glycerin, anhydrous ethanol and triethanolamine is 2: 1: 1, with glycerin, anhydrous ethanol and triethanolamine all being analytically pure; The surface modifier is a mixture of stearic acid and silane coupling agent KH550, the mass ratio of stearic acid and silane coupling agent KH550 is 3: 1, and both stearic acid and silane coupling agent KH550 are industrially pure; The water is deionized water.
    (1) Mix stainless steel slag, phosphorus slag, magnesium slag, manganese slag and composite grinding aids and grind them with a planetary ball mill at a speed of 700 rpm and a time of 100 minutes to obtain a complete industrial solid waste composite powder. The planetary ball mill is then used to mechanochemically treat the composite industrial waste micropowder at a speed of 200 rpm and a time of 84 hours to obtain a fully braced ultrafine industrial waste composite powder.
    (2) Mix the surface modifier with water and disperse it with an ultrasonic disperser having a power of 700 W and a time of 80 minutes to obtain a surface modifier solution.
    (3) Mix the ultrafine industrial solid waste composite powder with the surface modification solution and stir it with a planetary ball mill at a speed of 500 rpm and a time of 150 minutes to obtain a modified ultrafine industrial solid waste composite powder. That is, a reinforced, flame retardant, wear resistant, all industrial solid waste composite rubber filler.
    Comparative Example 2 Taking the example of the preparation of 100 g of the product of the present invention, the
    Components and their mass ratios: BE2020 / 5609 slag made of stainless steel 46% fly ash 26% phosphor slag 0% magnestum slag 0% manganese slag 14% compound slag 1% surface modifier 4% water 9% The main chemical composition of stainless steel slag: CaO is 52.35%, SIO 2 is 23.68%, A12 O 3 is 8.31%, MgO is 7.56%, Fe 2 O 3 is 1.96%, Cr 2 O3 is 1.12%, PbO is 0.83%, P20 5 is 0.41%, CuO The main chemical composition of fly ash: SiIO 2 is 51.53%, A12 O 3 is 27.78%, Fe 2 O 3 is 4.73%, and CaO is 5.21%. MgO is 1.03%, K20 is 1.13%, Na20 is 0.62%, T102 is 2.24%, SO3 is 1.87%, others are 3.86%, and its particle size is less than 5mm; the main chemical composition of manganese slag: S102 is 20.05%. Al 2 O 3 is 16.42%, CaO is 37.62%, MgO is 6.52%, SO 3 is 0.48%, Fe 2 O 3 is 1.23%, MnO is 10.87%, TiO 2 is 0.42% and others are 6.39% and its particle size is less than 5 mm; The grinding media is a mixture of glycerin, anhydrous ethanol and triethanolamine. The mass ratio of glycerin, anhydrous ethanol and triethanolamm is 2: 1: 1, whereby glycerm, anhydrous ethanol and triethanolamine are all analytically pure.The surface modifier is a mixture of stearic acid and silane coupling agent KH550, the mass ratio of stearic acid and silane coupling agent KH550 is 3: 1, where stearic acid and silane coupling agent KH550 are industrially pure; The water is deionized water.
    (1) Mix stainless steel slag, fly ash, manganese slag and composite grinding aids and grind them with a planetary ball mill at a speed of 700 rpm and a time of 100 minutes to obtain a complete industrial solid waste fine powder. The planetary ball mill then becomes a mechanochemical one
    Treatment of the composite industrial waste micropowder at a speed BE2020 / 5609 of 200 rpm and a time of 84 hours was used to obtain a superfine ultrafine industrial waste composite powder.
    (2) Mix the surface modifier with water and disperse it with an ultrasonic disperser having a power of 700 W and a time of 80 minutes to obtain a surface modifier solution.
    (3) Mix the ultrafine industrial solid waste composite powder with the surface modification solution and stir it with a planetary ball mill at a speed of 500 rpm and a time of 150 minutes to obtain a modified ultrafine industrial solid waste composite powder. That is, a reinforced, flame retardant, wear resistant, all industrial solid waste composite rubber filler. Comparative Example 3 Taking the example of the production of 100 g of the product of the present invention, the components and their mass ratios are: stainless steel slag 38% fly ash 26% phosphorus slag 10% magnesium slag 12% manganese slag 0% composite grinding aid 1% surface modifier 4% water 9% chemical Main composition of stainless steel slag: CaO is 52.35%, SIO 2 is 23.68%, A12 O 3 is 8.31%, MgO is 7.56%, Fe 2 O3 is 1.96%, Cr 2 O3 is 1, 12%, PbO is 0.83%, P20 5 is 0.41%, CuO The main chemical composition of fly ash: S10 2 is 51.53%, A12 O 3 is 27.78%, Fe 2 O 3 is 4.73 %, CaO is 5.21% and others are 3.09%. The particle size is less than 5 mm. MgO is 1.03%, K2O is 1.13%, Na20 is 0.62%, TiO2 is 2.24%, SO3 is 1.87%, others are 3.86%, and its particle size is less than 5mm, the main chemical composition of phosphorus slag: CaO is 45.70%, A1203 is 2.57%, S10 2 is 40.80%, K 2 O is 1.01%, P2O 5 is 3.91%, MgO is BE2020 / 5609 3.32%, TIO 2 is 0.22%, MnO is 0.02%, others are 2.45% and its particle size is less than 5mm, the magnesium slag The main chemical composition: Na 2 O is 0.06%, MgO is 7.31%, Al 2 O 3 is 1.78%, S10 2 is 31.24%, CaO is 51.21%, TiO 2 is 0.09%, Fe 2 O 3 is 4.45%, others are 3.86% and its particle size is less than 5mm.The composite grinding aid is a mixture of glycerin, anhydrous ethanol and triethanolamine, and the mass ratio of glycerin, anhydrous ethanol and triethanolamine is 2: 1: 1, where glycerin, anhydrous ethanol and three ethanolamine is analytically rem that Surface modifier is a mixture of stearic acid and silane coupling agent KH550, the mass ratio of stearic acid and silane coupling agent KH550 is 3: 1, of which stearic acid and silane coupling agent KH550 is industrially pure, the water is deionized water.
    (1) Mix stainless steel slag, fly ash, phosphorus slag, magnestum slag and composite grinding aids and grind them with a planetary ball mill at a speed of 700 rpm and a time of 100 minutes to obtain a complete industrial solid waste composite micropowder. The planetary ball mill is then used for mechanochemical treatment of the composite industrial waste micropowder at a speed of 200 rpm and a time of 84 hours to obtain a fully braced ultrafine industrial waste composite powder.
    (2) Mix the surface modifier with water and disperse it with an ultrasonic disperser having a power of 700 W and a time of 80 minutes to obtain a surface modifier solution.
    (3) Mix the ultrafine industrial solid waste composite powder with the surface modification solution and stir it with a planetary ball mill at a speed of 500 rpm and a time of 150 minutes to obtain a modified ultrafine industrial solid waste composite powder. That is, a reinforced, flame retardant, wear resistant, all industrial solid waste composite rubber filler.
    2. The test of the mechanical properties, the test of the flame retardant properties and the test of the abrasion resistance of the fully industrial according to the invention
    Composite rubber filler of the present invention after adding rubber BE2020 / 5609 Preparatory Examples 1 to 6 and Comparative Examples 1 to 3: The performance recognition process is as follows: Put the natural rubber (100 parts) 2 to 4 times in the open mixer, put the natural rubber in the Indoor mixer (mixing temperature 70 ° C) and mix for 2 minutes.
    Then add zinc oxide (2.5 parts) to the mixed sample to mix. Add carbon black (25 parts) and reinforced, flame retardant, wear-resistant, all-industrial composite rubber filler (25 parts) for 2 minutes, mix for 2 minutes, add accelerator (1.0 part) and sulfur (1.5 parts).
    After mixing for 2 minutes, take it out to use, which is Banbury.
    Put the banbury in the open mixer 5 to 7 times, slap the triangular bag 5 times, and then park for 12 hours, weigh 60 g of the banbury and use a flat plate with four pillars and the vulcanizer is used for vulcanization and the vulcanization temperature is 145 ° C.
    After vulcanization for a period of time, it is left to stand for 24 hours in order to obtain a completely industrial natural rubber made from solid waste. "Determination of the tensile stress and elongation properties of vulcanized rubber or thermoplastic rubber" (GB / T528-2009) tests the tensile strength of all industrial natural rubbers from solid waste; "Determination of the tear strength of vulcanized rubber or thermoplastic rubber (pants, right angle), Crescent Specimen)" (GB / T529-2008) test the tear strength of purely industrial natural rubber from solid waste; “Test method for the indentation hardness of vulcanized rubber or thermoplastic rubber Part 1: Shore Durometer Method (Shore Hardness) "Test the hardness of all natural rubbers from industrial waste;" Determination of the rubber burning performance "(GB / T 10707-2008) test the limit oxygen index of all natural rubbers from industrial waste;" - Vulcanized rubber or thermoplastic rubber Determination of abrasion resistance (rotary roller abrasion machine method) "(GB / T9867-2008) tests the abrasion of all industrial natural rubber-solid rubber-natural rubbers.
    Table 1. Mechanical properties, flame retardancy and abrasion resistance of all industrial natural rubbers from solid waste
    Limitation of the tensile strength Shore A friction resistance Order number Oxygen index carry / mm ° (MPa) Hardness (kN / m) (%) Example 1 15.3 47.3 33.6 31.1 171 Example 2 15.1 45.2 30.9 30.8 174 Example 3 15.0 43.6 31.8 31.0 175 Example 4 14.9 46.1 30.4 30.8 173 Example 5 15.5 44.5 31.6 31.1 177 Example 6 15.7 44.7 31.7 30.9 172 Comparative Example 1 10.3 35.4 24.3 30.9 194 Comparative Example 2 14.6 41.7 29.6 23.5 181 Comparative Example 3 12.5 38.9 26.4 29.2 208
    权利要求:
    Claims (3)
    [1]
    1. Em reinforced, flame retardant, wear-resistant, fully industrial BE2020 / 5609 composite rubber filler for solid waste, which is characterized in that the fully industrial solid waste composite rubber filler has the following composition in terms of percentage by weight: stainless steel slag 20% -40% fly ash 20% 30% phosphorus slag 10% 15% magnesium slag 10% 15% manganese slag 10% - 15% compound slag 1% -—- 3% surface modifier 2% -4% water 3% 9% The stainless steel slag, fly ash, phosphorus slag, magnesium slag and Manganese slag is solid industrial waste. The composite grinding aid is a mixture of glycerine, absolute ethanol and triethanolamine, the glycerine. The mass ratio of absolute ethanol and triethanolamm is 4: 2: 1 - 1: 1: 1, the surface modifier is a mixture of stearic acid and silane coupling agent KH550 and the stearic acid and silane coupling agent The mass ratio of the agent KH550 is 5: 1 - 1: 1.
    [2]
    2. Reinforced, flame-retardant, wear-resistant, fully industrial composite rubber filler according to claim 1, characterized in that the stainless steel slag, fly ash, phosphorus slag, magnesium slag and manganese slag The particle size is less than 5 mm.
    [3]
    3. A method for producing the reinforced, flame-retardant, wear-resistant, fully industrial waste composite rubber filler according to claim 1, characterized by the following steps: (1) stainless steel slag, fly ash, phosphorus slag, magnesium slag, manganese slag and composite grinding aids and mix with a planetary ball mill at a Grinding speed of 600 rpm - 900 rpm and a time of 90 mm - 120 min to obtain a purely industrial composite micropowder for solid waste, then one
    Use planetary ball mill to perform mechanochemical treatment of the BE2020 / 5609 composite industrial waste micropowder at a speed of 200rpm - 300rpm and a time of 72h - 96h to obtain a full industrial solid waste composite super micropowder;
    (2) Mix the surface modifier with water and disperse it with an ultrasonic disperser with a power of 600 W - 900 W and a time of 60 min - 90 min to obtain the surface modifier solution;
    (3) Mix the ultrafine industrial solid waste composite powder with the
    Surface modification solution and stir it with a planetary ball mill with a
    Speed of 300 rpm - 500 rpm and a time of 120 min - 150 min to obtain a modified whole industry Ultrafine powder of composite materials for solid
    Waste, that is, a reinforced, flame retardant, abrasion resistant, fully industrial rubber filler made from solid waste.
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    法律状态:
    2021-06-28| FG| Patent granted|Effective date: 20210625 |
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    CN201911067845.1A|CN110643074A|2019-11-04|2019-11-04|Reinforcing, flame-retardant and wear-resistant all-industrial solid waste type composite rubber filler and preparation method thereof|
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