Nano titanium dioxide reinforced plastic compatilizer and preparation process thereof

By preparing nano-titanium dioxide-reinforced plastic compatibilizers and utilizing the chemical bonds between polyalkane polymers and grafted monomers, the problem of excessive components in polypropylene composites was solved, improving the mechanical properties and compatibility of the materials and achieving efficient resource utilization.

CN121378879APending Publication Date: 2026-01-23JIANGSU YUNJING NEW MATERIALS TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202511683017.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-11-17
Publication Date
2026-01-23

AI Technical Summary

Technical Problem

In existing technologies, polypropylene composite plastics contain too many compatibilizer components, which leads to resource waste and poor environmental performance, making it difficult to effectively improve the overall performance of polypropylene and inorganic material composites.

Method used

Nano-titanium dioxide-reinforced plastic compatibilizers were prepared by melt blending of polyalkane polymers and graft monomers. Polyalkane polymers were formed by reacting glucosamine laurylamide and dimethyl dichlorosilane, and graft monomers were formed by activating nano-silica through an EDC-NHS system, thereby achieving chemical bonding with polypropylene and brucite fibers.

Benefits of technology

It improves the tensile strength, elongation at break and impact resistance of polypropylene composites, while also improving compatibility with magnesia fiber, reducing resource waste and enhancing environmental friendliness.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a nano titanium dioxide reinforced plastic compatilizer and a preparation process thereof, and belongs to the technical field of high-molecular polymers. The invention is used for solving the technical problems in the prior art that in order to improve various properties between polypropylene and an inorganic material compound, the doped plastic compatilizer has excessive components, resources are wasted, and the environment is not protected. The preparation process of the nano titanium dioxide reinforced plastic compatibilizer comprises the following steps: melting, blending and extruding a multi-paraffin polymer and a grafting monomer to form the nano titanium dioxide reinforced plastic compatibilizer, the multi-paraffin polymer is obtained through reaction of glucosamine lauroyl and dimethyldichlorosilane in an alkaline environment, and the grafting monomer is obtained through reaction of a cyclization compound, nano silicon dioxide dispersion liquid and an EDC-NHS activation system.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of high molecular polymer, in particular to a nano-titanium dioxide reinforced plastic compatilizer and a preparation process thereof. BACKGROUND

[0002] As a thermoplastic material, polypropylene has a wide range of applications in packaging, construction, automotive, medical and electronic industries due to its excellent physical properties and chemical properties; however, in the actual application process, polypropylene has the disadvantages of low strength and rigidity, poor flame retardancy, etc., which limits its application range. In the past few decades, a large amount of research has been conducted on the compatibility and mixed phase of polypropylene blends in order to prepare polypropylene composite plastics with excellent comprehensive performance. If brucite fibers are doped in polypropylene, the flame retardancy of the brucite fibers can be improved; however, the brucite fibers cannot be uniformly dispersed in the polypropylene material. The compatilizer plays a bridging role in effectively connecting the polymers such as plastics and the fibers such as brucite.

[0003] Patent application CN105482268A discloses a propylene-based plastic compatilizer for automobile wire and a preparation method thereof. The propylene-based plastic compatilizer is prepared by mixing, extruding and granulating propylene-based elastomer, polypropylene, metallocene polyethylene, KN resin, grafted monomer maleic anhydride and related additives. The plastic compatilizer is prepared by physical entanglement of the components in the multi-component compatilizer in a molten state. The plastic compatilizer can achieve good compatibility between the resin base material and the inorganic flame retardant material, and can also improve the thermal decomposition performance of the polypropylene material, increase the elasticity and improve the processing performance. However, the plastic compatilizer introduces too many unnecessary functional components for functional integration. If a specific plastic compatilizer is designed, the performance requirements can be met while reducing resource waste.

[0004] In view of the above technical defects, a solution is provided. SUMMARY

[0005] The present application aims to provide a nano-titanium dioxide reinforced plastic compatilizer and a preparation process thereof, which can solve the technical problems of excessive components in the prepared plastic compatilizer, resource waste and environmental pollution in the prior art for comprehensively improving the performance of the polypropylene and inorganic material composite.

[0006] The object of the present application can be achieved by the following technical solutions: The multi-chain alkane polymer and the grafted monomer are melt blended and extruded to form a nano-titanium dioxide reinforced plastic compatilizer. The multi-chain alkane polymer is obtained by reacting glucosamine lauroyl and dimethyldichlorosilane in an alkaline environment; and the grafted monomer is obtained by reacting a cyclic compound, a nano-silica dispersion liquid and an EDC-NHS activation system.

[0007] Furthermore, the method for preparing the polyalkane polymer includes the following steps: A1. Acetone and water are mixed in a mass ratio of 1:1-2 to obtain a mixed solvent; glucosamine hydrochloride is mixed with the mixed solvent to obtain a reactant; sodium hydroxide solution is added dropwise to the reactant to adjust the pH to 8-9; lauroyl chloride is added dropwise to the reactant, and the reaction is continued at 55-65℃ for 2-3 hours to obtain the product; the product is then processed to prepare glucosamine lauroamide. Under alkaline conditions, glucosamine hydrochloride and lauroyl chloride undergo an acylation reaction. After impurity removal, glucosamine lauroamide is finally prepared. The reaction formula is as follows:

[0008] A2. Mix sodium hydroxide solution and glucosamine laurylamide, then add dimethyldichlorosilane dropwise to obtain the reaction system; reflux the reaction system at 60-70℃ for 2-4 hours, and the collected solid is the prepared polyalkane polymer.

[0009] Dimethyldichlorosilane is hydrolyzed to give silanol. Under alkaline conditions and high-temperature reflux, the amino group of glucosamine lauramide reacts with the silanol to prepare a polyalkane polymer.

[0010] Further, in step A1, the ratio of glucosamine hydrochloride, mixed solvent, and lauroyl chloride is 4.3-8.6 g: 100-120 mL: 4-10 mL; the post-processing steps include: adjusting the pH of the product to neutral, precipitating the precipitate, filtering, and obtaining a solid; washing the solid sequentially with deionized water and petroleum ether, then filtering, and vacuum drying at 70-80°C to constant weight, which is the prepared glucosamine lauroamide.

[0011] Further, in step A2, the concentration of the sodium hydroxide solution is 0.1-0.2 mol / L, and the ratio of sodium hydroxide solution, glucosamine lauroyl and dimethyldichlorosilane is 60-80 mL: 15-25 g: 6.5-13.5 mL.

[0012] Furthermore, the method for preparing the grafted monomer includes the following steps: B1. Mix ethanol solution and hydrochloric acid solution, then add resorcinol and stir to dissolve, then add hydroxyacetaldehyde to obtain a reaction solution; reflux the reaction solution at 75-80℃ for 4-6 hours, cool and filter to obtain a solid product; wash the solid product and vacuum dry to prepare a cyclized compound; Resorcinol reacts with hydroxyacetaldehyde to form cyclic compounds with calixarene-like structures.

[0013] B2. Nano-silica is added to water and ultrasonically dispersed to form a nano-silica dispersion; EDC and NHS are added to the nano-silica dispersion and ultrasonically dispersed to obtain a mixed solution; a cyclizer is added to the mixed solution, heated to react, and allowed to stand and cool to obtain the reactant; the reactant is filtered through a filter membrane and dried to constant weight to obtain the prepared graft unit.

[0014] Further, in step B1, the concentration of the ethanol solution is 90-95 wt%, and the concentration of the hydrochloric acid solution is 35-40 wt%; the ratio of the amount of ethanol solution, hydrochloric acid solution, resorcinol and hydroxyacetaldehyde is 30-40 mL: 10-15 mL: 10-11 g: 6.6-9 g.

[0015] Furthermore, in step B2, the ratio of nano-silica, water, EDC, NHS, and cyclizer is 5-15 mg: 15-20 mL: 60-80 mg: 80-100 mg: 15-20 g; the heating temperature is 80-90 °C, and the heating time is 10-12 h; the filter membrane has a pore size of 0.2-0.22 μm.

[0016] Furthermore, the weight ratio of the polyalkane polymer to the grafted monomer is 20-40:10-20, and the melt blending temperature is 250-260℃.

[0017] As another aspect of the present invention, a nano-titanium dioxide reinforced plastic compatibilizer is prepared by a preparation process of the nano-titanium dioxide reinforced plastic compatibilizer.

[0018] The present invention has the following beneficial effects: 1. Glucosamine lauramide consists of two parts: a long-chain alkyl group and a glucose backbone with amino substituents. Dimethyldichlorosilane reacts further with amino-containing glucosamine lauramide to prepare a polyalkane polymer. The long-chain alkyl group and multiple short chains in the polyalkane polymer can be wound around the polypropylene backbone, thereby improving the tensile strength and elongation at break, among other mechanical properties, of the compatibilizer-doped composite polyethylene. Furthermore, the polyalkane polymer contains polar atoms and functional groups, which can improve its compatibility with brucite fibers.

[0019] 2. Resorcinol and hydroxyacetaldehyde react to form cyclic compounds similar to calixaranes. 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide / N-hydroxysuccinimide achieves indirect coupling with hydroxyl groups through the activation of carboxyl groups. The cyclic compound is chemically bonded to nano-silica, i.e., nano-silica is embedded, thus preparing grafted units. The above grafted units and polyalkane polymers can be melt-blended to improve the impact resistance of the prepared compatibilizer. When the prepared nano-titanium dioxide reinforced plastic compatibilizer is melt-blended with polypropylene and brucite fibers, the compatibilizer contains groups that can react with polypropylene and brucite fibers. During the blending process, it can chemically react with the functional groups of each monomer in the blend components to form chemical bonds and hydrogen bonds, acting as a connecting bridge. Detailed Implementation

[0020] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention. Example 1

[0021] This embodiment provides a method for preparing a multi-chain alkane polymer for use as a nano-titanium dioxide reinforced plastic compatibilizer, comprising the following steps: A1, acetone, and water were mixed in a 1:1 mass ratio to obtain a mixed solvent. 4.3 g of glucosamine hydrochloride and 100 mL of the mixed solvent were added to a flask and stirred until homogeneous to obtain the reactant. The pH of the reactant was adjusted to 8 by adding 20 wt% sodium hydroxide solution dropwise. 4 mL of lauroyl chloride was added dropwise to the flask, and the reaction was continued at 55 °C for 2 h to obtain the product. The pH of the product was adjusted to neutral by adding 0.1 mol / L dilute sulfuric acid solution, causing a precipitate to form. The precipitate was filtered to obtain a solid. The solid was washed successively with deionized water and petroleum ether, then filtered under vacuum and dried at 70 °C to constant weight to finally obtain the product glucosamine lauroamide.

[0022] A2. Select a 250mL three-necked single-necked reaction flask. Insert a 100mL dropping funnel into one end of the flask, containing 6.5mL of dimethyldichlorosilane. Add 60mL of 0.1mol / L sodium hydroxide solution and 15g of glucosamine laurylamide to the flask. Then, add dimethyldichlorosilane dropwise to the flask at a rate of 1mL / min to obtain the reaction system. Connect the bottom of the flask to a packed column. The upper end of the column is a condenser, and the lower end is connected to a reflux bottle. The reactants and products entering the reflux bottle can be refluxed through the packed column. The reflux reaction temperature in the flask is 60℃, and the reflux reaction time is 2h. Collect the solid at the bottom of the flask; this is the prepared poly-chain alkane polymer. Example 2

[0023] This embodiment provides a method for preparing a multi-chain alkane polymer for use as a nano-titanium dioxide reinforced plastic compatibilizer, comprising the following steps: A1, acetone, and water were mixed in a 1:2 mass ratio to obtain a mixed solvent. 6.5 g of glucosamine hydrochloride and 115 mL of the mixed solvent were added to a flask and stirred until homogeneous to obtain the reactant. The pH of the reactant was adjusted to 8 by adding 25 wt% sodium hydroxide solution dropwise. 6 mL of lauroyl chloride was added dropwise to the flask, and the reaction was continued at 60 °C for 2.6 h to obtain the product. The pH of the product was adjusted to neutral by adding 0.12 mol / L dilute sulfuric acid solution, causing a precipitate to form. The precipitate was filtered to obtain a solid. The solid was washed successively with deionized water and petroleum ether, then filtered under vacuum and dried at 77 °C to constant weight to finally obtain the product glucosamine lauroamide.

[0024] A2. Select a 250mL three-necked single-necked reaction flask. Insert a 100mL dropping funnel into one end of the flask, containing 10mL of dimethyldichlorosilane. Add 75mL of 0.15mol / L sodium hydroxide solution and 20g of glucosamine laurylamide to the flask. Then, add dimethyldichlorosilane dropwise to the flask at a rate of 1mL / min to obtain the reaction system. Connect the bottom of the flask to a packed column. The upper end of the column is a condenser, and the lower end is connected to a reflux bottle. The reactants and products entering the reflux bottle can be refluxed through the packed column. The reflux reaction temperature in the flask is 66℃, and the reflux reaction time is 3h. Collect the solid at the bottom of the flask; this is the prepared poly-chain alkane polymer. Example 3

[0025] This embodiment provides a method for preparing a multi-chain alkane polymer for use as a nano-titanium dioxide reinforced plastic compatibilizer, comprising the following steps: A1, acetone, and water were mixed in a 1:2 mass ratio to obtain a mixed solvent. 8.6 g of glucosamine hydrochloride and 120 mL of the mixed solvent were added to a flask and stirred until homogeneous to obtain the reactant. The pH of the reactant was adjusted to 9 by adding 30 wt% sodium hydroxide solution dropwise. 10 mL of lauroyl chloride was added dropwise to the flask, and the reaction was continued at 65 °C for 3 h to obtain the product. The pH of the product was adjusted to neutral by adding 0.15 mol / L dilute sulfuric acid solution, causing a precipitate to form. The precipitate was filtered to obtain a solid. The solid was washed successively with deionized water and petroleum ether, then filtered under vacuum and dried at 80 °C to constant weight to finally obtain the product glucosamine lauroamide.

[0026] A2. Select a 250mL three-necked single-necked reaction flask. Insert a 100mL dropping funnel into one end of the flask, containing 13.5mL of dimethyldichlorosilane. Add 80mL of 0.2mol / L sodium hydroxide solution and 25g of glucosamine laurylamide to the flask. Then, add dimethyldichlorosilane dropwise to the flask at a rate of 1mL / min to obtain the reaction system. Connect the bottom of the flask to a packed column. The upper end of the column is a condenser, and the lower end is connected to a reflux bottle. The reactants and products entering the reflux bottle can be refluxed through the packed column. The reflux reaction temperature in the flask is 70℃, and the reflux reaction time is 4h. Collect the solid at the bottom of the flask; this is the prepared poly-chain alkane polymer. Example 4

[0027] This embodiment provides a method for preparing grafted monomers for compatibilizers of nano-titanium dioxide reinforced plastics, including the following steps: B1. Measure 30 mL of 90 wt% ethanol solution and 10 mL of 35 wt% hydrochloric acid solution into a 250 mL two-necked round-bottom flask, then add 10 g of solid resorcinol and stir until the resorcinol dissolves. Next, add 6.6 g of hydroxyacetaldehyde to the two-necked round-bottom flask to obtain the reaction solution. Reflux the reaction solution at 75 °C for 4 h, then cool to room temperature, and filter to remove the solvent, obtaining the solid product. Wash the solid product with an ice-cold methanol-water solution (ice-cold methanol and water mass ratio of 1:1), and dry under vacuum at 75 °C to constant weight, which is the prepared cyclic compound.

[0028] B2. Add 5g of nano-silica and 15mL of water to a 250mL beaker and sonicate at 2000Hz for 50min to obtain a nano-silica dispersion. Add 60mg of EDC and 80mg of NHS to the beaker, and continue sonicating at 2000Hz for 20min to obtain a mixture. Add 15g of the cyclizer to the beaker, and heat the beaker in a water bath to 80℃. Continue the reaction at this temperature for 10h, and then allow it to cool to room temperature to obtain the reactant. Filter the reactant through a 0.2μm filter membrane and collect the solid. Dry the solid at 70-80℃ to constant weight to obtain the prepared graft unit.

[0029] B3. By weight, 20 parts of the polyalkane polymer prepared in Example 1 and 10 parts of the grafting unit prepared in Example 4 are added to a twin-screw extruder and melt-blended and extruded at 250°C to obtain the nano-titanium dioxide reinforced plastic compatibilizer. Example 5

[0030] This embodiment provides a method for preparing grafted monomers for compatibilizers of nano-titanium dioxide reinforced plastics, including the following steps: B1. Measure 35 mL of 92 wt% ethanol solution and 12 mL of 37 wt% hydrochloric acid solution into a 250 mL two-necked round-bottom flask, then add 10.5 g of solid resorcinol and stir until the resorcinol dissolves. Next, add 7.8 g of hydroxyacetaldehyde to the two-necked round-bottom flask to obtain the reaction solution. Reflux the reaction solution at 78 °C for 5 h, then cool to room temperature, and filter to remove the solvent, obtaining the solid product. Wash the solid product with an ice-cold methanol-water solution (ice-cold methanol and water mass ratio of 1:1), and dry under vacuum at 78 °C to constant weight, which is the prepared cyclic compound.

[0031] B2. 10 mg of nano-silica and 18 mL of water were added to a 250 mL beaker and ultrasonically dispersed at 2300 Hz for 55 min to obtain a nano-silica dispersion. 70 mg of EDC and 90 mg of NHS were then added to the beaker, and ultrasonic dispersion was continued at 2600 Hz for 26 min to obtain a mixture. 18 g of the cyclizer was added to the beaker, and the beaker was heated in a water bath to 88 °C. The reaction was continued at this temperature for 11 h, and then allowed to cool to room temperature to obtain the reactant. The reactant was filtered through a 0.22 μm filter membrane, and the solid was collected. The solid was dried at 77 °C to constant weight, which is the prepared graft unit.

[0032] B3. According to the weight, 30 parts of the polyalkane polymer prepared in Example 2 and 15 parts of the grafting unit prepared in Example 5 are added to a twin-screw extruder and melt-blended and extruded at 255°C to obtain the nano-titanium dioxide reinforced plastic compatibilizer. Example 6

[0033] This embodiment provides a method for preparing grafted monomers for compatibilizers of nano-titanium dioxide reinforced plastics, including the following steps: B1. Measure 40 mL of 95 wt% ethanol solution and 15 mL of 40 wt% hydrochloric acid solution into a 250 mL two-necked round-bottom flask, then add 11 g of solid resorcinol and stir until the resorcinol dissolves. Next, add 9 g of hydroxyacetaldehyde to the two-necked round-bottom flask to obtain the reaction solution. Reflux the reaction solution at 80 °C for 6 h, then cool to room temperature, and filter to remove the solvent, obtaining the solid product. Wash the solid product with an ice-cold methanol-water solution (ice-cold methanol and water mass ratio of 1:1), and dry under vacuum at 80 °C to constant weight, which is the prepared cyclic compound.

[0034] B2. Add 15 mg of nano-silica and 20 mL of water to a 250 mL beaker and sonicate at 3000 Hz for 60 min to obtain a nano-silica dispersion. Add 80 mg of EDC and 100 mg of NHS to the beaker, and continue sonicating at 3000 Hz for 30 min to obtain a mixture. Add 20 g of the cyclizer to the beaker, and heat the beaker in a water bath to 90 °C. Continue the reaction at this temperature for 12 h, and allow it to cool to room temperature to obtain the reactant. Filter the reactant through a 0.2 μm filter membrane and collect the solid. Dry the solid at 80 °C to constant weight to obtain the prepared graft unit.

[0035] B3. By weight, 40 parts of the polyalkane polymer prepared in Example 3 and 20 parts of the grafting unit prepared in Example 6 were added to a twin-screw extruder and melt-blended and extruded at 260°C to obtain the nano-titanium dioxide reinforced plastic compatibilizer. Example 7

[0036] This embodiment provides a method for preparing composite polyethylene using nano-titanium dioxide-reinforced plastic compatibilizer, comprising the following steps: According to the weight percentage, 100 parts of polypropylene, 20 parts of magnesia fiber, and 10 parts of the nano-titanium dioxide reinforced plastic compatibilizer prepared in Example 4 were added to a twin-screw extruder for extrusion granulation. The speed of the twin-screw extruder was set to 200 r / min and the melt extrusion temperature was 200℃ to prepare composite polyethylene. Example 8

[0037] This embodiment provides a method for preparing composite polyethylene using nano-titanium dioxide-reinforced plastic compatibilizer, comprising the following steps: According to the weight percentage, 100 parts of polypropylene, 30 parts of magnesia fiber, and 16 parts of the nano-titanium dioxide reinforced plastic compatibilizer prepared in Example 5 were added to a twin-screw extruder for extrusion granulation. The speed of the twin-screw extruder was set to 250 r / min and the melt extrusion temperature was 205℃ to prepare composite polyethylene. Example 9

[0038] This embodiment provides a method for preparing composite polyethylene using nano-titanium dioxide-reinforced plastic compatibilizer, comprising the following steps: According to the weight percentage, 100 parts of polypropylene, 40 parts of magnesia fiber, and 20 parts of the nano-titanium dioxide reinforced plastic compatibilizer prepared in Example 6 were added to a twin-screw extruder for extrusion granulation. The speed of the twin-screw extruder was set to 300 r / min and the melt extrusion temperature was 220°C to prepare composite polyethylene.

[0039] Comparative Example 1 Compared to Example 9, step A2 was omitted, and the prepared polyalkane polymer was replaced with an equal mass of glucosamine lauramide.

[0040] Comparative Example 2 Compared to Example 9, the prepared polyalkane polymer was replaced with an equal mass of silane coupling agent KH550.

[0041] Comparative Example 3 Compared to Example 9, step B2 is omitted; in step B3, nano-silica and cyclized compound are compounded in a mass ratio of 3:4 to obtain a mixture; 20g of the mixture is used to replace the prepared grafting unit.

[0042] Performance testing: 1. According to GB / T1843-2008 "Standard for Determination of Impact Strength of Plastic Cantilever Beams", the composite polyethylene prepared in Examples 7-9 and Comparative Examples 1-3 were cut into standard cuboid strips with dimensions of 80 mm in length, 10 mm in width, and 4 mm in thickness, respectively. A notch of 1.5 mm was punched into each strip using a notching sample preparation machine. The impact performance of the strips was tested using a cantilever beam impact testing machine at 23°C.

[0043] 2. According to GB / T1040-2018 "Determination of Tensile Properties of Plastics", the composite polyethylene prepared in Examples 7-9 and Comparative Examples 1-3 were cut into dumbbell-shaped strips with a width of 4 mm, a length of 20 mm, and a thickness of 1 mm. The strips were tested on a tensile testing machine at a tensile rate of 5 mm / min.

[0044] 3. According to GB / T1043.2-2018 "Determination of Impact Properties of Simply Supported Beams of Plastics", the composite polyethylene prepared in Examples 7-9 and Comparative Examples 1-3 were cut into strips with a width of 10 mm, a length of 80 mm, and a thickness of 4 mm. The strips were subjected to bending performance testing using a testing machine at a testing rate of 2 mm / min.

[0045] 4. According to ISO 4589-2 "Test Standard for Burning Performance of Plastics", the composite polyethylene prepared in Examples 7-9 and Comparative Examples 1-3 was cut into standard strips of 100mm × 6.5mm × 3.2mm. The lowest oxygen index value of the standard strips when maintaining stable combustion was recorded using an oxygen index meter. Each standard strip was tested five times, and the average value was recorded as the LOI value of the corresponding strip. The specific test results are shown in Table 1.

[0046] Table 1. Sample Performance Test Data

[0047] Data Analysis: According to Table 1, the composite polyethylene prepared in Examples 7-9 of this invention exhibits high mechanical properties, specifically high notched impact strength, tensile strength, and elongation at break. However, in Comparative Example 1, the polyalkane polymer was prepared by replacing it with an equal mass of glucosamine lauramide. The polyalkane polymer contains more short branches and polar molecules, which helps improve the compatibility between the compatibilizer and polypropylene. Therefore, the notched impact strength, tensile strength, and elongation at break of the composite polyethylene prepared in Comparative Example 1 all decreased. In Comparative Example 2, the polyalkane polymer was replaced with the silane coupling agent KH550, resulting in a decrease in the notched impact strength, tensile strength, and elongation at break of the prepared composite polyethylene, indicating that the polyalkane polymer prepared in this invention has better compatibility than the coupling agent.

[0048] In Comparative Example 3, nano-silica encapsulated by a cyclizer was used instead of the blend of nano-silica and the cyclizer; the cyclizer has a calixarene-like structure, which can encapsulate nano-silica and synergistically enhance the flame retardant properties of nano-silica.

[0049] The above description is merely an example and illustration of the structure of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described, or use similar methods to replace them, as long as they do not deviate from the structure of the invention or exceed the scope defined in the claims, all of which should fall within the protection scope of the present invention.

[0050] In the description of this specification, references to terms such as "an embodiment," "example," and "specific example" indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0051] The preferred embodiments of the present invention disclosed above are merely illustrative of the invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the invention to specific implementations. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to better understand and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims

1. A preparation process for a nano-titanium dioxide reinforced plastic compatibilizer, characterized in that, It is prepared by the following steps: Poly-chain alkane polymers and grafted monomers are melt-blended and extruded to form nano-titanium dioxide-reinforced plastic compatibilizers; The polyalkane polymer is obtained by reacting glucosamine lauroyl and dimethyl dichlorosilane under an alkaline environment; the grafted monomer is obtained by reacting a cyclizer, a nano silica dispersion, and an EDC-NHS activation system.

2. The preparation process of the nano-titanium dioxide reinforced plastic compatibilizer according to claim 1, characterized in that, The method for preparing the polyalkane polymer includes the following steps: A1. Acetone and water are mixed in a mass ratio of 1:1-2 to obtain a mixed solvent; glucosamine hydrochloride is mixed with the mixed solvent to obtain a reactant; sodium hydroxide solution is added dropwise to the reactant to adjust the pH to 8-9, and lauroyl chloride is added dropwise. The reaction is continued at 55-65℃ for 2-3 hours to obtain the product; the product is then processed to prepare glucosamine lauroamide. A2. Mix sodium hydroxide solution and glucosamine lauramide, then add dimethyldichlorosilane dropwise to obtain the reaction system; reflux the reaction system at 60-70℃ for 2-4 hours, and the collected solid is the prepared polyalkane polymer.

3. The preparation process of the nano-titanium dioxide reinforced plastic compatibilizer according to claim 2, characterized in that, In step A1, the ratio of glucosamine hydrochloride, mixed solvent, and lauroyl chloride is 4.3-8.6 g: 100-120 mL: 4-10 mL. The post-processing steps include: adjusting the pH of the product to neutral, precipitating the precipitate, filtering, and obtaining a solid; washing the solid sequentially with deionized water and petroleum ether, filtering again, and vacuum drying at 70-80°C to constant weight, which is the prepared glucosamine lauroamide.

4. The preparation process of the nano-titanium dioxide reinforced plastic compatibilizer according to claim 2, characterized in that, In step A2, the concentration of sodium hydroxide solution is 0.1-0.2 mol / L, and the ratio of sodium hydroxide solution, glucosamine lauroyl and dimethyldichlorosilane is 60-80 mL: 15-25 g: 6.5-13.5 mL.

5. The preparation process of the nano-titanium dioxide reinforced plastic compatibilizer according to claim 1, characterized in that, The method for preparing the grafted monomer includes the following steps: B1. Mix ethanol solution and hydrochloric acid solution, then add resorcinol and stir to dissolve, then add hydroxyacetaldehyde to obtain a reaction solution; reflux the reaction solution at 75-80℃ for 4-6 hours, cool and filter to obtain a solid product; wash the solid product and vacuum dry to prepare a cyclized compound; B2. Nano-silica is added to water and ultrasonically dispersed to form a nano-silica dispersion; EDC and NHS are added to the nano-silica dispersion and ultrasonically dispersed to obtain a mixed solution; a cyclizer is added to the mixed solution, heated to react, and allowed to stand and cool to obtain the reactant; the reactant is filtered through a filter membrane and dried to constant weight to obtain the prepared graft unit.

6. The preparation process of the nano-titanium dioxide reinforced plastic compatibilizer according to claim 5, characterized in that, In step B1, the concentration of the ethanol solution is 90-95 wt%, and the concentration of the hydrochloric acid solution is 35-40 wt%; the ratio of the amount of ethanol solution, hydrochloric acid solution, resorcinol and hydroxyacetaldehyde is 30-40 mL: 10-15 mL: 10-11 g: 6.6-9 g.

7. The preparation process of the nano-titanium dioxide reinforced plastic compatibilizer according to claim 5, characterized in that, In step B2, the ratio of nano-silica, water, EDC, NHS and cyclizer is 5-15mg:15-20mL:60-80mg:80-100mg:15-20g; the heating temperature is 80-90℃ and the heating time is 10-12h; the filter membrane has a pore size of 0.2-0.22μm.

8. The preparation process of the nano-titanium dioxide reinforced plastic compatibilizer according to claim 1, characterized in that, The weight ratio of polyalkane polymer to grafted monomer is 20-40:10-20, and the melt blending temperature is 250-260℃.

9. A nano-titanium dioxide reinforced plastic compatibilizer prepared by a preparation process according to any one of claims 1-8.

Citation Information

Patent Citations

  • Car wire propenyl plastic compatilizer and preparation method thereof

    CN105482268A