A polyvinyl chloride composite material based on graphite tailings and a method for manufacturing the same

Abstract

A polyvinyl chloride composite material based on graphite tailings and a manufacturing method thereof belong to the technical field of polyvinyl chloride composite material preparation. In order to improve the use performance of polyvinyl chloride composite materials, the present invention comprises weighing isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine and hydroxyl-terminated polycaprolactone respectively according to weight parts, mixing them evenly and adding them to toluene to carry out a replacement reaction under the protection of a nitrogen atmosphere, adding ether after the reaction is completed to carry out multiple precipitation washings, and vacuum drying the obtained solid to obtain 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone; weighing graphite tailings powder, polyvinyl chloride powder, calcium zinc stabilizer, plasticizer and 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone respectively according to weight parts, mixing them evenly in a mixer, obtaining a mixture for hot pressing, and maintaining the pressure after the hot pressing is completed to cool and shape naturally to obtain a polyvinyl chloride composite material based on graphite tailings.

Description

Technical Field

[0001] The invention belongs to the technical field of preparation of polyvinyl chloride composite materials, and in particular relates to a polyvinyl chloride composite material based on graphite tailings and a manufacturing method thereof. Background Art

[0002] At present, mineral resources have become an important means of production for people's social life and scientific and technological progress because of their non-renewable nature, difficulty in replacing in a short period of time and special applicability. With the continuous development and utilization of mineral resources to meet social development, the tailings problem has become increasingly serious. A large amount of tailings can directly cause serious pollution to the surrounding environment. The residual beneficiation agents, excessive heavy metals and arsenic compounds in the tailings can penetrate into the soil and cause pollution after rain erosion and weathering. In addition, the accumulated tailings resources have high potential energy, and mudslides are more likely to occur in extreme weather. Under the background of the goals of carbon peak and carbon neutrality, the rational reuse of tailings resources can not only improve the comprehensive utilization rate of mineral resources, but also indirectly reduce energy consumption and carbon dioxide emissions in the process of mineral resource mining. At present, the main ways to utilize tailings in China are filling underground mining areas, reselection of valuable elements and land reclamation. Among them, the recovery rate of tailings reselection is low and the consumption of tailings is small. Filling the goaf requires a large amount of cement, resulting in high costs. Therefore, it is necessary to seek a tailings treatment method with high utilization rate, strong feasibility and low cost.

[0003] As one of the world's top five general-purpose plastics, polyvinyl chloride is currently widely used in packaging materials, wires and cables, pipes, and building materials. However, polyvinyl chloride has poor creep resistance and is prone to creep deformation when used outdoors for a long time. It also has low heat resistance and is extremely flammable. It is prone to dripping when burned, which hinders the development and application of polyvinyl chloride in high-demand scenarios. Graphite tailings are inorganic rigid materials with high strength and heat resistance. They can be used as modified materials for polyvinyl chloride to enrich its performance. However, graphite tailings are composed of inorganic oxides such as SiO2 and Al2O3, which have large polarity differences with polyvinyl chloride. Simple filling and blending are difficult to achieve the ideal interface layer strength, which will directly affect the performance of the composite material. Summary of the invention

[0004] The problem to be solved by the present invention is to improve the use performance of a polyvinyl chloride composite material, and to provide a polyvinyl chloride composite material based on graphite tailings and a manufacturing method thereof.

[0005] To achieve the above object, the present invention is implemented through the following technical solutions:

[0006] A method for manufacturing a polyvinyl chloride composite material based on graphite tailings comprises the following steps:

[0007] S1. Weigh 2-amino-4-hydroxy-6-methylpyrimidine, hexamethylene diisocyanate and N-methylpyrrolidone according to their weight, mix them evenly and add them to a reactor, react under nitrogen protection, add dichloromethane after the reaction, slowly add n-heptane solution after mixing, perform precipitation and filtration several times, and vacuum dry the obtained solid to obtain isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine for standby use;

[0008] S2. Weigh caprolactone, 1,3-propylene glycol and stannous octoate in parts by weight, mix well and perform polymerization under nitrogen protection, add dichloromethane after the polymerization reaction is completed, add anhydrous ethanol after mixing and perform precipitation and filtration several times, and the obtained solid is vacuum dried to obtain hydroxyl-terminated polycaprolactone for standby use;

[0009] S3. Weigh the isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine obtained in step S1 and the hydroxy-terminated polycaprolactone obtained in step S2 respectively according to their weight parts, mix them evenly and add them to toluene to carry out a replacement reaction under the protection of a nitrogen atmosphere, add ether after the reaction to precipitate and wash several times, and vacuum dry the obtained solid to obtain 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone for standby use;

[0010] S4. Graphite tailings powder, polyvinyl chloride powder, calcium zinc stabilizer, plasticizer and 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone obtained in step S3 were weighed in parts by weight, and mixed evenly in a mixer to obtain a mixture for standby use;

[0011] S5. The mixed material obtained in step S4 is paved into a slab, and then pre-pressed. After the pre-pressing is completed, hot pressing is performed. After the hot pressing is completed, the pressure is maintained and naturally cooled to form a shape, so as to obtain a polyvinyl chloride composite material based on graphite tailings.

[0012] Furthermore, the added amounts of materials in step S1 are weighed according to the following weight proportions: 4 to 80 parts of 2-amino-4-hydroxy-6-methylpyrimidine, 10 to 200 parts of hexamethylene diisocyanate, 1 to 20 parts of N-methylpyrrolidone, 20 to 400 parts of dichloromethane, and 200 to 5000 parts of n-heptane; the reaction temperature for the reaction under nitrogen protection is 90 to 110° C., and the reaction time is 8 to 12 h.

[0013] Furthermore, the added amounts of materials in step S2 are weighed according to the following weight proportions: 5 to 120 parts of caprolactone, 1 to 5 parts of 1,3-propylene glycol, 1 to 6 parts of stannous octoate, 20 to 300 parts of dichloromethane, and 300 to 5000 parts of anhydrous ethanol; the reaction temperature of the polymerization reaction is 120 to 140° C., and the reaction time is 4 to 10 hours.

[0014] Furthermore, the added amounts of materials in step S3 are weighed according to the following weight proportions: 10 to 200 parts of isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine, 5 to 50 parts of hydroxyl-terminated polycaprolactone, 30 to 500 parts of toluene, and 200 to 5000 parts of ether; the reaction temperature of the replacement reaction is 100 to 120° C., and the reaction time is 10 to 16 hours.

[0015] Furthermore, the added amounts of materials in step S4 are weighed according to the following weight proportions: 50 to 500 parts of graphite tailings powder, 20 to 200 parts of polyvinyl chloride powder, 2 to 40 parts of calcium zinc stabilizer, 2 to 60 parts of plasticizer, and 2 to 30 parts of 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone; the mixing time in the mixer is 1 to 2 hours.

[0016] Furthermore, the plasticizer in step S4 is one of dioctyl phthalate, dibutyl phthalate, dioctyl terephthalate and dinonyl phthalate.

[0017] Furthermore, in step S4, the particle size of the polyvinyl chloride powder is 60-200 meshes, and the particle size of the graphite tailings powder is 100-400 meshes.

[0018] Furthermore, in step S5, the thickness of the slab laid is 1 to 10 mm, the pre-pressing pressure at room temperature is 1 to 2 MPa, and the pre-pressing time is 10 to 20 min; the hot pressing temperature is set to 140 to 180°C, the hot pressing pressure is 5 to 10 MPa, and the hot pressing time is 10 to 30 min.

[0019] Furthermore, the vacuum drying temperature is 50 to 80° C., and the vacuum drying time is 8 to 12 hours.

[0020] A method for manufacturing a polyvinyl chloride composite material based on graphite tailings. The polyvinyl chloride composite material based on graphite tailings is manufactured, and the thickness of the polyvinyl chloride composite material based on graphite tailings is 4 mm.

[0021] Beneficial effects of the present invention:

[0022] The present invention discloses a method for manufacturing a polyvinyl chloride composite material based on graphite tailings, and uses a 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone to modify the polyvinyl chloride composite material based on graphite tailings. On the one hand, the 2-amino-4-hydroxy-6-methylpyrimidine at the end of the polycaprolactone belongs to a polar hydrogen bonding site, and can form multiple hydrogen bonds with the polar surface of the graphite tailings; on the other hand, the polyester lactone molecular chain itself has a weak polarity and is similar to the polarity of polyvinyl chloride, and the two have good compatibility, and the long-chain polycaprolactone can form a physical cross-linking point with polyvinyl chloride, which is not available in small molecule interface compatibilizers. In summary, this 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone can be used as an interface compatibilizer to improve the interface compatibility problem between graphite tailings and polyvinyl chloride.

[0023] The present invention discloses a method for manufacturing a polyvinyl chloride composite material based on graphite tailings. The polycaprolactone terminated with 2-amino-4-hydroxy-6-methylpyrimidine improves the interface compatibility of the composite material and can significantly improve the mechanical properties of the composite material.

[0024] The manufacturing method of the polyvinyl chloride composite material based on graphite tailings described in the present invention can further increase the content of solid graphite tailings by using a hot pressing molding process, and the hot pressing process causes less wear on the machine, and can produce plates with larger specifications and sizes. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is a real photo of a polyvinyl chloride composite material based on graphite tailings prepared by the present invention. DETAILED DESCRIPTION

[0026] In order to make the purpose, technical solution and advantages of the present invention more clear, the present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention, that is, the specific embodiments described are only part of the embodiments of the present invention, rather than all of the specific embodiments. The components of the specific embodiments of the present invention described and shown in the drawings herein can be arranged and designed in various different configurations, and the present invention can also have other embodiments.

[0027] Therefore, the following detailed description of the specific embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the invention claimed for protection, but merely represents the selected specific embodiments of the present invention. Based on the specific embodiments of the present invention, all other specific embodiments obtained by those skilled in the art without making creative work are within the scope of protection of the present invention.

[0028] In order to further understand the content, features and effects of the present invention, the following specific implementation methods are given as examples, and the attached Figure 1 The detailed instructions are as follows:

[0029] Embodiment 1:

[0030] A method for manufacturing a polyvinyl chloride composite material based on graphite tailings comprises the following steps:

[0031] S1. Weigh 2-amino-4-hydroxy-6-methylpyrimidine, hexamethylene diisocyanate and N-methylpyrrolidone according to their weight, mix them evenly and add them to a reactor, react under nitrogen protection, add dichloromethane after the reaction, slowly add n-heptane solution after mixing, perform precipitation and filtration several times, and vacuum dry the obtained solid to obtain isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine for standby use;

[0032] Further, the added amount of the materials in step S1 is weighed according to the following weight parts: 10 parts of 2-amino-4-hydroxy-6-methylpyrimidine, 20 parts of hexamethylene diisocyanate, 4 parts of N-methylpyrrolidone, 100 parts of dichloromethane, and 1000 parts of n-heptane; the reaction temperature for the reaction under nitrogen protection is 90° C., and the reaction time is 12 h;

[0033] S2. Weigh caprolactone, 1,3-propylene glycol and stannous octoate in parts by weight, mix well and perform polymerization under nitrogen protection, add dichloromethane after the polymerization reaction is completed, add anhydrous ethanol after mixing and perform precipitation and filtration several times, and the obtained solid is vacuum dried to obtain hydroxyl-terminated polycaprolactone for standby use;

[0034] Furthermore, the added amount of the materials in step S2 is weighed according to the following weight parts: 20 parts of caprolactone, 3 parts of 1,3-propylene glycol, 1 part of stannous octoate, 80 parts of dichloromethane, and 1000 parts of anhydrous ethanol; the reaction temperature of the polymerization reaction is 120° C., and the reaction time is 8 hours;

[0035] S3. Weigh the isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine obtained in step S1 and the hydroxy-terminated polycaprolactone obtained in step S2 respectively according to their weight parts, mix them evenly and add them to toluene to carry out a replacement reaction under the protection of a nitrogen atmosphere, add ether after the reaction to precipitate and wash several times, and vacuum dry the obtained solid to obtain 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone for standby use;

[0036] Furthermore, the added amounts of materials in step S3 are weighed according to the following weight parts: 50 parts of isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine, 20 parts of hydroxyl-terminated polycaprolactone, 200 parts of toluene, and 1500 parts of ether; the reaction temperature of the replacement reaction is 110° C., and the reaction time is 12 h;

[0037] S4. Graphite tailings powder, polyvinyl chloride powder, calcium zinc stabilizer, plasticizer and 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone obtained in step S3 were weighed in parts by weight, and mixed evenly in a mixer to obtain a mixture for standby use;

[0038] Furthermore, the plasticizer in step S4 is dioctyl terephthalate;

[0039] Furthermore, in step S4, the particle size of the polyvinyl chloride powder is 100 mesh, and the particle size of the graphite tailings powder is 200 mesh;

[0040] Further, the added amount of materials in step S4 is weighed according to the following weight parts: 200 parts of graphite tailings powder, 100 parts of polyvinyl chloride powder, 10 parts of calcium zinc stabilizer, 15 parts of plasticizer, and 10 parts of 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone; the mixing time in the mixer is 1 hour;

[0041] S5. The mixture obtained in step S4 is paved into a slab, and then pre-pressed, hot pressed after the pre-pressing is completed, and the pressure is maintained after the hot pressing is completed and naturally cooled to obtain a polyvinyl chloride composite material based on graphite tailings;

[0042] Furthermore, in step S5, the thickness of the slab laid is 4 mm, the pre-pressing pressure at room temperature is 2 MPa, and the pre-pressing time is 10 min; the hot pressing temperature is set to 160°C, the hot pressing pressure is 8 MPa, and the hot pressing time is 20 min.

[0043] Furthermore, in this embodiment, the vacuum drying temperature is 80° C., and the vacuum drying time is 8 hours.

[0044] The polyvinyl chloride composite material based on graphite tailings manufactured by the manufacturing method of the polyvinyl chloride composite material based on graphite tailings described in this embodiment has a tensile strength of up to 19.33 MPa, a tensile fracture stress of up to 19.24 MPa, a flexural strength of up to 38.97 MPa, and a flexural modulus of up to 7101 MPa.

[0045] Embodiment 2:

[0046] A method for manufacturing a polyvinyl chloride composite material based on graphite tailings comprises the following steps:

[0047] S1. Weigh 2-amino-4-hydroxy-6-methylpyrimidine, hexamethylene diisocyanate and N-methylpyrrolidone according to their weight, mix them evenly and add them to a reactor, react under nitrogen protection, add dichloromethane after the reaction, slowly add n-heptane solution after mixing, perform precipitation and filtration several times, and vacuum dry the obtained solid to obtain isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine for standby use;

[0048] Further, the added amount of the materials in step S1 is weighed according to the following weight parts: 2-amino-4-hydroxy-6-methylpyrimidine is 25 parts, hexamethylene diisocyanate is 80 parts, N-methylpyrrolidone is 12 parts, dichloromethane is 180 parts, and n-heptane is 2000 parts; the reaction temperature for the reaction under nitrogen protection is 100° C., and the reaction time is 12 hours;

[0049] S2. Weigh caprolactone, 1,3-propylene glycol and stannous octoate in parts by weight, mix well and perform polymerization under nitrogen protection, add dichloromethane after the polymerization reaction is completed, add anhydrous ethanol after mixing and perform precipitation and filtration several times, and the obtained solid is vacuum dried to obtain hydroxyl-terminated polycaprolactone for standby use;

[0050] Furthermore, the added amount of the materials in step S2 is weighed according to the following weight parts: 60 parts of caprolactone, 3 parts of 1,3-propylene glycol, 1 part of stannous octoate, 150 parts of dichloromethane, and 2500 parts of anhydrous ethanol; the reaction temperature of the polymerization reaction is 140° C., and the reaction time is 6 hours;

[0051] S3. Weigh the isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine obtained in step S1 and the hydroxy-terminated polycaprolactone obtained in step S2 respectively according to their weight parts, mix them evenly and add them to toluene to carry out a replacement reaction under the protection of a nitrogen atmosphere, add ether after the reaction to precipitate and wash several times, and vacuum dry the obtained solid to obtain 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone for standby use;

[0052] Furthermore, the added amounts of materials in step S3 are weighed according to the following weight parts: 120 parts of isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine, 30 parts of hydroxyl-terminated polycaprolactone, 300 parts of toluene, and 3000 parts of ether; the reaction temperature of the replacement reaction is 100° C., and the reaction time is 16 hours;

[0053] S4. Graphite tailings powder, polyvinyl chloride powder, calcium zinc stabilizer, plasticizer and 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone obtained in step S3 were weighed in parts by weight, and mixed evenly in a mixer to obtain a mixture for standby use;

[0054] Furthermore, the plasticizer in step S4 is dioctyl phthalate;

[0055] Furthermore, in step S4, the particle size of the polyvinyl chloride powder is 100 mesh, and the particle size of the graphite tailings powder is 200 mesh;

[0056] Further, the added amount of materials in step S4 is weighed according to the following weight parts: 300 parts of graphite tailings powder, 150 parts of polyvinyl chloride powder, 12 parts of calcium zinc stabilizer, 15 parts of plasticizer, and 15 parts of 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone; the mixing time in the mixer is 1 hour;

[0057] S5. The mixture obtained in step S4 is paved into a slab, and then pre-pressed, hot pressed after the pre-pressing is completed, and the pressure is maintained after the hot pressing is completed and naturally cooled to obtain a polyvinyl chloride composite material based on graphite tailings;

[0058] Furthermore, in step S5, the thickness of the slab laid is 4 mm, the pre-pressing pressure at room temperature is 2 MPa, and the pre-pressing time is 15 min; the hot pressing temperature is set to 150°C, the hot pressing pressure is 8 MPa, and the hot pressing time is 30 min.

[0059] Furthermore, in this embodiment, the vacuum drying temperature is 70° C., and the vacuum drying time is 10 h.

[0060] The polyvinyl chloride composite material based on graphite tailings manufactured by the manufacturing method of the polyvinyl chloride composite material based on graphite tailings described in this embodiment has a tensile strength of up to 19.93 MPa, a tensile fracture stress of up to 19.81 MPa, a flexural strength of up to 39.99 MPa, and a flexural modulus of up to 7552 MPa.

[0061] Embodiment 3:

[0062] A method for manufacturing a polyvinyl chloride composite material based on graphite tailings comprises the following steps:

[0063] S1. Weigh 2-amino-4-hydroxy-6-methylpyrimidine, hexamethylene diisocyanate and N-methylpyrrolidone according to their weight, mix them evenly and add them to a reactor, react under nitrogen protection, add dichloromethane after the reaction, slowly add n-heptane solution after mixing, perform precipitation and filtration several times, and vacuum dry the obtained solid to obtain isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine for standby use;

[0064] Furthermore, the added amounts of materials in step S1 are weighed according to the following weight parts: 4 parts of 2-amino-4-hydroxy-6-methylpyrimidine, 10 parts of hexamethylene diisocyanate, 1 part of N-methylpyrrolidone, 20 parts of dichloromethane, and 200 parts of n-heptane; the reaction temperature for the reaction under nitrogen protection is 90° C., and the reaction time is 8 hours;

[0065] S2. Weigh caprolactone, 1,3-propylene glycol and stannous octoate in parts by weight, mix well and perform polymerization under nitrogen protection, add dichloromethane after the polymerization reaction is completed, add anhydrous ethanol after mixing and perform precipitation and filtration several times, and the obtained solid is vacuum dried to obtain hydroxyl-terminated polycaprolactone for standby use;

[0066] Furthermore, the added amount of the materials in step S2 is weighed according to the following weight parts: 5 parts of caprolactone, 1 part of 1,3-propylene glycol, 1 part of stannous octoate, 20 parts of dichloromethane, and 300 parts of anhydrous ethanol; the reaction temperature of the polymerization reaction is 120° C., and the reaction time is 4 hours;

[0067] S3. Weigh the isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine obtained in step S1 and the hydroxy-terminated polycaprolactone obtained in step S2 respectively according to their weight parts, mix them evenly and add them to toluene to carry out a replacement reaction under the protection of a nitrogen atmosphere, add ether after the reaction to precipitate and wash several times, and vacuum dry the obtained solid to obtain 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone for standby use;

[0068] Furthermore, the added amount of the materials in step S3 is weighed according to the following weight parts: 10 parts of isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine, 5 parts of hydroxyl-terminated polycaprolactone, 30 parts of toluene, and 200 parts of ether; the reaction temperature of the replacement reaction is 100° C., and the reaction time is 10 h;

[0069] S4. Graphite tailings powder, polyvinyl chloride powder, calcium zinc stabilizer, plasticizer and 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone obtained in step S3 were weighed in parts by weight, and mixed evenly in a mixer to obtain a mixture for standby use;

[0070] Furthermore, the plasticizer in step S4 is dioctyl phthalate;

[0071] Furthermore, in step S4, the particle size of the polyvinyl chloride powder is 100 mesh, and the particle size of the graphite tailings powder is 200 mesh;

[0072] Further, the added amount of materials in step S4 is weighed according to the following weight parts: 50 parts of graphite tailings powder, 20 parts of polyvinyl chloride powder, 2 parts of calcium zinc stabilizer, 2 parts of plasticizer, and 2 parts of 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone; the mixing time in the mixer is 1 hour;

[0073] S5. The mixture obtained in step S4 is paved into a slab, and then pre-pressed, hot pressed after the pre-pressing is completed, and the pressure is maintained after the hot pressing is completed and naturally cooled to obtain a polyvinyl chloride composite material based on graphite tailings;

[0074] Furthermore, in step S5, the thickness of the slab laid is 4 mm, the pre-pressing pressure at room temperature is 1 MPa, and the pre-pressing time is 10 min; the hot pressing temperature is set to 140°C, the hot pressing pressure is 5 MPa, and the hot pressing time is 10 min.

[0075] Furthermore, in this embodiment, the vacuum drying temperature is 50° C., and the vacuum drying time is 12 hours.

[0076] The polyvinyl chloride composite material based on graphite tailings manufactured by the method for manufacturing the polyvinyl chloride composite material based on graphite tailings described in this embodiment has a larger specification and size of the produced plate.

[0077] Embodiment 4:

[0078] A method for manufacturing a polyvinyl chloride composite material based on graphite tailings comprises the following steps:

[0079] S1. Weigh 2-amino-4-hydroxy-6-methylpyrimidine, hexamethylene diisocyanate and N-methylpyrrolidone according to their weight, mix them evenly and add them to a reactor, react under nitrogen protection, add dichloromethane after the reaction, slowly add n-heptane solution after mixing, perform precipitation and filtration several times, and vacuum dry the obtained solid to obtain isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine for standby use;

[0080] Further, the added amount of the materials in step S1 is weighed according to the following weight parts: 80 parts of 2-amino-4-hydroxy-6-methylpyrimidine, 200 parts of hexamethylene diisocyanate, 20 parts of N-methylpyrrolidone, 400 parts of dichloromethane, and 5000 parts of n-heptane; the reaction temperature for the reaction under nitrogen protection is 110° C., and the reaction time is 12 h;

[0081] S2. Weigh caprolactone, 1,3-propylene glycol and stannous octoate in parts by weight, mix well and perform polymerization under nitrogen protection, add dichloromethane after the polymerization reaction is completed, add anhydrous ethanol after mixing and perform precipitation and filtration several times, and the obtained solid is vacuum dried to obtain hydroxyl-terminated polycaprolactone for standby use;

[0082] Furthermore, the added amount of the materials in step S2 is weighed according to the following weight parts: 120 parts of caprolactone, 5 parts of 1,3-propylene glycol, 6 parts of stannous octoate, 300 parts of dichloromethane, and 5000 parts of anhydrous ethanol; the reaction temperature of the polymerization reaction is 140° C., and the reaction time is 10 hours;

[0083] S3. Weigh the isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine obtained in step S1 and the hydroxy-terminated polycaprolactone obtained in step S2 respectively according to their weight parts, mix them evenly and add them to toluene to carry out a replacement reaction under the protection of a nitrogen atmosphere, add ether after the reaction to precipitate and wash several times, and vacuum dry the obtained solid to obtain 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone for standby use;

[0084] Furthermore, the added amounts of materials in step S3 are weighed according to the following weight parts: 200 parts of isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine, 50 parts of hydroxyl-terminated polycaprolactone, 500 parts of toluene, and 5000 parts of ether; the reaction temperature of the replacement reaction is 120° C., and the reaction time is 16 h;

[0085] S4. Graphite tailings powder, polyvinyl chloride powder, calcium zinc stabilizer, plasticizer and 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone obtained in step S3 were weighed in parts by weight, and mixed evenly in a mixer to obtain a mixture for standby use;

[0086] Furthermore, the plasticizer in step S4 is dibutyl phthalate;

[0087] Furthermore, in step S4, the particle size of the polyvinyl chloride powder is 100 mesh, and the particle size of the graphite tailings powder is 200 mesh;

[0088] Further, the added amount of materials in step S4 is weighed according to the following weight parts: 50 to 500 parts of graphite tailings powder, 200 parts of polyvinyl chloride powder, 40 parts of calcium zinc stabilizer, 60 parts of plasticizer, and 30 parts of 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone; the mixing time in the mixer is 2 hours;

[0089] S5. The mixture obtained in step S4 is paved into a slab, and then pre-pressed, hot pressed after the pre-pressing is completed, and the pressure is maintained after the hot pressing is completed and naturally cooled to obtain a polyvinyl chloride composite material based on graphite tailings;

[0090] Furthermore, in step S5, the thickness of the slab laid is 4 mm, the pre-pressing pressure at room temperature is 2 MPa, and the pre-pressing time is 20 min; the hot pressing temperature is set to 180°C, the hot pressing pressure is 10 MPa, and the hot pressing time is 30 min.

[0091] Furthermore, in this embodiment, the vacuum drying temperature is 80° C., and the vacuum drying time is 8 hours.

[0092] The method for manufacturing a polyvinyl chloride composite material based on graphite tailings described in this embodiment manufactures a polyvinyl chloride composite material based on graphite tailings, and the polyvinyl chloride composite material based on graphite tailings significantly improves mechanical properties.

[0093] Embodiment 5:

[0094] A method for manufacturing a polyvinyl chloride composite material based on graphite tailings comprises the following steps:

[0095] S1. Weigh 2-amino-4-hydroxy-6-methylpyrimidine, hexamethylene diisocyanate and N-methylpyrrolidone according to their weight, mix them evenly and add them to a reactor, react under nitrogen protection, add dichloromethane after the reaction, slowly add n-heptane solution after mixing, perform precipitation and filtration several times, and vacuum dry the obtained solid to obtain isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine for standby use;

[0096] Further, the added amount of the materials in step S1 is weighed according to the following weight parts: 30 parts of 2-amino-4-hydroxy-6-methylpyrimidine, 50 parts of hexamethylene diisocyanate, 5 parts of N-methylpyrrolidone, 200 parts of dichloromethane, and 1000 parts of n-heptane; the reaction temperature for the reaction under nitrogen protection is 100° C., and the reaction time is 10 h;

[0097] S2. Weigh caprolactone, 1,3-propylene glycol and stannous octoate in parts by weight, mix well and perform polymerization under nitrogen protection, add dichloromethane after the polymerization reaction is completed, add anhydrous ethanol after mixing and perform precipitation and filtration several times, and the obtained solid is vacuum dried to obtain hydroxyl-terminated polycaprolactone for standby use;

[0098] Furthermore, the added amount of the materials in step S2 is weighed according to the following weight parts: 20 parts of caprolactone, 2 parts of 1,3-propylene glycol, 2 parts of stannous octoate, 100 parts of dichloromethane, and 2000 parts of anhydrous ethanol; the reaction temperature of the polymerization reaction is 130° C., and the reaction time is 6 hours;

[0099] S3. Weigh the isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine obtained in step S1 and the hydroxy-terminated polycaprolactone obtained in step S2 respectively according to their weight parts, mix them evenly and add them to toluene to carry out a replacement reaction under the protection of a nitrogen atmosphere, add ether after the reaction to precipitate and wash several times, and vacuum dry the obtained solid to obtain 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone for standby use;

[0100] Furthermore, the added amounts of materials in step S3 are weighed according to the following weight parts: 50 parts of isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine, 20 parts of hydroxyl-terminated polycaprolactone, 100 parts of toluene, and 2000 parts of ether; the reaction temperature of the replacement reaction is 110° C., and the reaction time is 14 h;

[0101] S4. Graphite tailings powder, polyvinyl chloride powder, calcium zinc stabilizer, plasticizer and 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone obtained in step S3 were weighed in parts by weight, and mixed evenly in a mixer to obtain a mixture for standby use;

[0102] Furthermore, the plasticizer in step S4 is dinonyl phthalate;

[0103] Furthermore, in step S4, the particle size of the polyvinyl chloride powder is 100 mesh, and the particle size of the graphite tailings powder is 200 mesh;

[0104] Further, the added amount of materials in step S4 is weighed according to the following weight parts: 100 parts of graphite tailings powder, 100 parts of polyvinyl chloride powder, 10 parts of calcium zinc stabilizer, 10 parts of plasticizer, and 10 parts of 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone; the mixing time in the mixer is 2 hours;

[0105] S5. The mixture obtained in step S4 is paved into a slab, and then pre-pressed, hot pressed after the pre-pressing is completed, and the pressure is maintained after the hot pressing is completed and naturally cooled to obtain a polyvinyl chloride composite material based on graphite tailings;

[0106] Furthermore, in step S5, the thickness of the slab laid is 4 mm, the pre-pressing pressure at room temperature is 1.5 MPa, and the pre-pressing time is 15 min; the hot pressing temperature is set to 150°C, the hot pressing pressure is 6 MPa, and the hot pressing time is 20 min.

[0107] Furthermore, in this embodiment, the vacuum drying temperature is 60° C., and the vacuum drying time is 10 h.

[0108] The polyvinyl chloride composite material based on graphite tailings manufactured by the method for manufacturing the polyvinyl chloride composite material based on graphite tailings described in this embodiment has greatly improved interface compatibility of the polyvinyl chloride composite material based on graphite tailings.

[0109] It should be noted that relational terms such as "first" and "second" are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the existence of other identical elements in the process, method, article or device including the elements.

[0110] Although the present application has been described above with reference to specific embodiments, various modifications may be made thereto and parts thereof may be replaced with equivalents without departing from the scope of the present application. In particular, as long as there is no structural conflict, the various features in the specific embodiments disclosed in the present application may be used in combination with each other in any manner, and the fact that these combinations are not exhaustively described in this specification is only for the sake of omitting space and saving resources. Therefore, the present application is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.

Claims

1. A method for producing a polyvinyl chloride composite material based on graphite tailings, characterized in that: The steps include: S1. Weigh 2-amino-4-hydroxy-6-methylpyrimidine, hexamethylene diisocyanate and N-methylpyrrolidone according to their weight, mix them evenly and add them to a reactor, react under nitrogen protection, add dichloromethane after the reaction, slowly add n-heptane solution after mixing, perform precipitation and filtration several times, and vacuum dry the obtained solid to obtain isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine for standby use; S2. Weigh caprolactone, 1,3-propylene glycol and stannous octoate in parts by weight, mix well and perform polymerization under nitrogen protection, add dichloromethane after the polymerization reaction is completed, add anhydrous ethanol after mixing and perform precipitation and filtration several times, and the obtained solid is vacuum dried to obtain hydroxyl-terminated polycaprolactone for standby use; S3. Weigh the isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine obtained in step S1 and the hydroxy-terminated polycaprolactone obtained in step S2 respectively according to their weight parts, mix them evenly and add them to toluene to react under the protection of nitrogen atmosphere, add ether after the reaction to precipitate and wash several times, and vacuum dry the obtained solid to obtain 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone for standby use; S4. Graphite tailings powder, polyvinyl chloride powder, calcium zinc stabilizer, plasticizer and 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone obtained in step S3 were weighed in parts by weight, and mixed evenly in a mixer to obtain a mixture for standby use; S5. The mixed material obtained in step S4 is paved into a slab, and then pre-pressed. After the pre-pressing is completed, hot pressing is performed. After the hot pressing is completed, the pressure is maintained and naturally cooled to form a shape, so as to obtain a polyvinyl chloride composite material based on graphite tailings.

2. The method for producing a polyvinyl chloride composite material based on graphite tailings according to claim 1, characterized in that: The added amounts of materials in step S1 are weighed according to the following weight proportions: 4 to 80 parts of 2-amino-4-hydroxy-6-methylpyrimidine, 10 to 200 parts of hexamethylene diisocyanate, 1 to 20 parts of N-methylpyrrolidone, 20 to 400 parts of dichloromethane, and 200 to 5000 parts of n-heptane; the reaction temperature for the reaction under nitrogen protection is 90 to 110° C., and the reaction time is 8 to 12 h.

3. The method for producing a polyvinyl chloride composite material based on graphite tailings according to claim 2, characterized in that: The added amounts of materials in step S2 are weighed according to the following weight parts: 5 to 120 parts of caprolactone, 1 to 5 parts of 1,3-propylene glycol, 1 to 6 parts of stannous octoate, 20 to 300 parts of dichloromethane, and 300 to 5000 parts of anhydrous ethanol; the reaction temperature of the polymerization reaction is 120 to 140° C., and the reaction time is 4 to 10 hours.

4. The method for producing a polyvinyl chloride composite material based on graphite tailings according to claim 3, characterized in that: The added amounts of materials in step S3 are weighed according to the following weight proportions: 10 to 200 parts of isocyanate-terminated 2-amino-4-hydroxy-6-methylpyrimidine, 5 to 50 parts of hydroxyl-terminated polycaprolactone, 30 to 500 parts of toluene, and 200 to 5000 parts of ether; the reaction temperature of the reaction is 100 to 120° C., and the reaction time is 10 to 16 hours.

5. The method for producing a polyvinyl chloride composite material based on graphite tailings according to claim 4, characterized in that: The added amounts of materials in step S4 are weighed according to the following weight proportions: 50 to 500 parts of graphite tailings powder, 20 to 200 parts of polyvinyl chloride powder, 2 to 40 parts of calcium zinc stabilizer, 2 to 60 parts of plasticizer, and 2 to 30 parts of 2-amino-4-hydroxy-6-methylpyrimidine-terminated polycaprolactone; the mixing time in the mixer is 1 to 2 hours.

6. The method for producing a polyvinyl chloride composite material based on graphite tailings according to claim 5, characterized in that: The plasticizer in step S4 is one of dioctyl phthalate, dibutyl phthalate, dioctyl terephthalate and dinonyl phthalate.

7. The method for producing a polyvinyl chloride composite material based on graphite tailings according to claim 6, characterized in that: In step S4, the particle size of the polyvinyl chloride powder is 60-200 meshes, and the particle size of the graphite tailings powder is 100-400 meshes.

8. The method for producing a polyvinyl chloride composite material based on graphite tailings according to claim 7, characterized in that: The thickness of the slab laid in step S5 is 1 to 10 mm, the pre-pressing pressure at room temperature is 1 to 2 MPa, and the pre-pressing time is 10 to 20 min; the hot pressing temperature is set to 140 to 180°C, the hot pressing pressure is 5 to 10 MPa, and the hot pressing time is 10 to 30 min.

9. The method for producing a polyvinyl chloride composite material based on graphite tailings according to claim 1, characterized in that: The vacuum drying temperature is 50-80° C., and the vacuum drying time is 8-12 hours.

10. A polyvinyl chloride composite material based on graphite tailings manufactured by the method for manufacturing a polyvinyl chloride composite material based on graphite tailings according to any one of claims 1 to 9, characterized in that: The thickness of the polyvinyl chloride composite material based on graphite tailings is 4 mm.

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