A nucleating agent composition, its preparation method and use

Abstract

The application relates to the technical field of nucleating agents, and particularly discloses a nucleating agent composition, a preparation method and application thereof, the nucleating agent composition comprising polytetrafluoroethylene and multilayer graphene, the polytetrafluoroethylene being intercalated in multilayer graphene layers, and the polytetrafluoroethylene being subjected to plasma surface treatment under a nitrogen-containing gas atmosphere. The polytetrafluoroethylene and the graphene are effectively combined, the multilayer graphene retains the excellent properties of the graphene, and compared with the inert graphene surface, the polytetrafluoroethylene can be intercalated into the multilayer graphene after being combined with the polytetrafluoroethylene subjected to surface treatment, the agglomeration of the graphene itself is inhibited, and the dispersibility of the graphene in a matrix is promoted; meanwhile, the advantages of the polymer nucleating agent and the inorganic nucleating agent are exerted, and the mechanical properties and the thermal properties of a product are improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of nucleating agents, more particularly, it relates to a nucleating agent composition, a preparation method and application thereof. BACKGROUND

[0002] Nucleating agents are new functional additives suitable for partially crystalline plastics such as polyethylene and polypropylene, which can accelerate the crystallization rate, increase the crystallization density and promote the grain size refinement by changing the crystallization behavior of the resin, so as to shorten the molding cycle, improve the transparency, surface gloss, tensile strength, rigidity, heat distortion temperature, impact resistance, creep resistance and other physical and mechanical properties of the product. Nucleating agents can be mainly divided into inorganic, organic and high molecular types according to their chemical structure. Inorganic nucleating agents mainly include talc, calcium oxide, graphene, calcium carbonate, etc. Organic nucleating agents mainly include carboxylic acid metal salts, phosphoric acid metal salts, sorbitol benzylidene derivatives, etc. High molecular nucleating agents mainly include alkali metal salts of polyester oligomers, fully aromatic polyester powder, polytetrafluoroethylene powder, etc.

[0003] In recent years, with the increasing demand for new high-efficiency nucleating agents, the development of high-efficiency nucleating agents has become more and more difficult, and the research and development speed has become slower and slower. Therefore, it is particularly important to modify different nucleating agents and prepare a more efficient nucleating agent composition than single nucleating agent through the synergistic effect of different nucleating agents. Therefore, it is of great significance to develop a new nucleating agent composition for the development of nucleating agents. SUMMARY

[0004] In order to develop a new nucleating agent composition to improve the crystallization effect on the resin, the present application provides a nucleating agent composition, a preparation method and application thereof.

[0005] In the first aspect, the present application provides a nucleating agent composition, which adopts the following technical scheme:

[0006] The nucleating agent composition comprises polytetrafluoroethylene and multi-layer graphene, the polytetrafluoroethylene is inserted into the multi-layer graphene sheet layer, and the polytetrafluoroethylene is obtained by plasma treatment under a nitrogen-containing gas atmosphere.

[0007] By adopting the technical scheme, polytetrafluoroethylene as a high polymer nucleating agent has a high specific surface area, which provides more crystallization nucleation interfaces, has excellent heterogeneous nucleation effect, and thus can significantly promote the crystallization kinetics of the resin; graphene as an inorganic nucleating agent has excellent mechanical properties, and the mechanical properties of the resin can be improved by adding a small amount of graphene. The polytetrafluoroethylene and the graphene are effectively combined in the application. Since the multilayer graphene not only retains the excellent properties of graphene, but also, compared with the inert graphene surface, the polytetrafluoroethylene can be inserted into the interlayer gap of the multilayer graphene after being combined with the surface-treated polytetrafluoroethylene, the aggregation of the graphene itself is inhibited, and thus the dispersibility of the graphene in the matrix is promoted; meanwhile, the advantages of the high polymer nucleating agent and the inorganic nucleating agent are exerted, and the mechanical properties and thermal properties of the product are improved.

[0008] In a specific implementable embodiment, the mass ratio of the polytetrafluoroethylene to the multilayer graphene is (6-8):(2-4).

[0009] By adopting the technical scheme, the mass ratio of the polytetrafluoroethylene to the graphene is optimized, and the nucleating agent composition obtained has a better crystallization effect on the resin.

[0010] In a specific implementable embodiment, the preparation method of the multilayer graphene is that the expanded graphite is placed in an ethanol solution, and ultrasonic treatment is performed to obtain the multilayer graphene.

[0011] By adopting the technical scheme, the expanded graphite has a worm-like appearance and is composed of many adhered and superimposed graphite scales, and there are many honeycomb-like micro-pores between the scales. The multilayer graphene is prepared from the expanded graphite in the application, so that the polytetrafluoroethylene can be inserted into the interlayer spacing of the multilayer graphene; meanwhile, the ultrasonic wave is generated by mechanical vibration, can propagate in the liquid, and can cause the rapid expansion of the micro-bubbles in the liquid. The shock wave generated by the ultrasonic expansion can exert an expansion force on the interlayer of the two-dimensional material. When the shock wave propagates to the pores of the two-dimensional material, a local high-pressure area is generated, which not only causes the expanded graphite to be peeled to form the multilayer graphene, but also expands the interlayer spacing of the multilayer graphene, so that the multilayer graphene is expanded.

[0012] In a specific implementable embodiment, the expanded graphite is obtained by oxidizing the graphite and then expanding the graphite at high temperature.

[0013] By adopting the technical scheme, the oxidizing agent reacts with the graphite to form an ionic compound which is preserved in the pores of the graphite, so as to expand the pores of the graphite, facilitate the insertion of the polytetrafluoroethylene into the layers of the multilayer graphene, and improve the combination of the two.

[0014] In a specific implementable embodiment, the polytetrafluoroethylene is obtained by plasma treatment in the presence of a nitrogen-containing gas atmosphere and polyethylene glycol.

[0015] By adopting the technical scheme, the inventors consider that polytetrafluoroethylene has excellent heterogeneous nucleation effect when searching for a suitable high molecular nucleating agent, but the compatibility of polytetrafluoroethylene is poor, and polytetrafluoroethylene is easy to agglomerate in the system, which is not conducive to better dispersion in graphene; introducing polyethylene glycol on the surface of polytetrafluoroethylene can effectively improve the surface activity of polytetrafluoroethylene, and through plasma treatment, on the one hand, the grafting of polytetrafluoroethylene and polyethylene glycol is realized, and on the other hand, the change of the surface structure of polytetrafluoroethylene and polyethylene glycol improves the adhesion, which is conducive to the adhesion of polytetrafluoroethylene on graphene, and further improves the combination of the two.

[0016] In one specific embodiment, the nucleating agent composition further comprises a sorbitol nucleating agent, which is one or more of bis-1,3:2,4-(4'-propylbenzylidene)-1-propyl sorbitol, 1,3:2,4-dibenzylidene sorbitol, 1,3:2,4-bis(p-methylbenzylidene) sorbitol, 1,3:2,4-bis(3,4-dimethylene benzylidene) sorbitol.

[0017] By adopting the technical scheme, the sorbitol nucleating agent first forms a dimer through intermolecular hydrogen bonds, and this dimer has a stable V-shaped structure that can well accommodate the spiral structure of the resin, so that the movement of the spiral structure of the resin is restricted, on the one hand, reducing the probability of returning to a random coil, and on the other hand, reducing the crystallization free energy, thereby promoting the nucleation of the resin. The present application adds the sorbitol nucleating agent as an organic nucleating agent, which interacts with the inorganic nucleating agent graphene and the polymer nucleating agent polytetrafluoroethylene through π-π bonds. The π-π bonds of the sorbitol nucleating agent interact with the hydrogen bonds of the multilayer graphene, promoting the mutual dispersion of the multilayer graphene and the sorbitol nucleating agent, improving the uniformity of the dispersion of the sorbitol nucleating agent in the matrix resin, multiplying the nucleation points of the matrix resin, accelerating the crystallization process of the matrix resin, and improving the crystallinity; at the same time, the sorbitol nucleating agent can modify the surface of the multilayer graphene through hydrogen bonding, adjust the compatibility between the resin and the multilayer graphene, and further improve the nucleation effect of the nucleating agent composition. Through the synergistic effect of the three, the mechanical and thermal properties of the product are improved.

[0018] In a second aspect, the present application provides a preparation method of the nucleating agent composition, which adopts the following technical scheme:

[0019] The preparation method of the nucleating agent composition is as follows: adding multilayer graphene into deionized water to obtain a suspension, and mixing with polytetrafluoroethylene, washing, drying, and adsorbing polytetrafluoroethylene in the multilayer graphene to obtain the nucleating agent composition.

[0020] By adopting the technical scheme, the preparation method is simple, and through the synergistic effect between the graphene and the polytetrafluoroethylene, the nucleating agent composition prepared has the advantage of being more efficient than a single nucleating agent.

[0021] In one specific implementation, the nucleating agent composition is prepared by the following steps.

[0022] The multilayer graphene is added into deionized water to obtain a suspension, and the polytetrafluoroethylene is mixed, washed, and dried to allow the polytetrafluoroethylene to be adsorbed in the graphene to obtain a nucleating agent composition A;

[0023] The nucleating agent composition A is modified by using a silane coupling agent and is dispersed in water to obtain a mixed solution A;

[0024] The sorbitol nucleating agent is added into an alcohol solvent to be dissolved to obtain a mixed solution B; the mass ratio of the sorbitol nucleating agent to the nucleating agent composition A is (35-75):(25-65);

[0025] The mixed solution B is added into the mixed solution A, is ultrasonically dispersed, and is spray dried to obtain the nucleating agent composition.

[0026] By adopting the technical scheme, the graphene is modified with the polytetrafluoroethylene nucleating agent composition A, and then is compounded with the sorbitol nucleating agent to obtain the nucleating agent composition. Compared with the sorbitol nucleating agent or the nucleating agent composition A alone, the nucleating agent after compounding has better mechanical properties and thermal properties under the same use amount. Meanwhile, the preparation process is simple, and the nucleating agent also has good dispersion and nucleation effects.

[0027] In one specific implementation, the silane coupling agent is an amino silane coupling agent.

[0028] By adopting the technical scheme, the nucleating agent after compounding of the graphene and the polytetrafluoroethylene is modified by using the amino silane coupling agent. The unique “two-end group” structure enables the silane coupling agent to build a “molecular bridge” between the nucleating agent composition A and the sorbitol nucleating agent, improves the performance and connectivity of the nucleating agent composition. The alkoxy group on one side of the amino silane coupling agent can react with the active groups such as the hydroxyl group or the carboxyl group on the surface of the graphene to form a stable chemical bond, thereby improving the dispersibility of the graphene. The amino group on the other side improves the binding force between the nucleating agent composition A and the sorbitol nucleating agent through the bonding effect, thereby significantly improving the nucleation effect of the nucleating agent composition.

[0029] In a third aspect, the present application provides an application of the nucleating agent composition, which adopts the following technical scheme.

[0030] Use of the nucleating agent composition in the preparation of semi-crystalline resins, the semi-crystalline resins being one or more of polypropylene, polyethylene, polylactic acid, polyurethane.

[0031] By adopting the technical scheme, the nucleating agent composition can be directly blended in the semi-crystalline resin processing process, and can give the semi-crystalline resin more excellent mechanical properties and processing properties.

[0032] In summary, the present application has the following beneficial effects:

[0033] 1. The present application inserts polytetrafluoroethylene into the multi-layer graphene sheet to form a nucleating agent composition, and through the synergistic effect between different nucleating agents, a more efficient nucleating agent composition than a single nucleating agent is prepared;

[0034] 2. The present application modifies polytetrafluoroethylene by polyethylene glycol, which is beneficial to the dispersion of polytetrafluoroethylene in graphene and the adhesion of polytetrafluoroethylene on graphene, improves the combination of the two, and thus improves the nucleation;

[0035] 3. The present application adds sorbitol nucleating agent in the nucleating agent composition, which interacts with inorganic nucleating agent graphene and polymer nucleating agent polytetrafluoroethylene, and together improves the mechanical properties and thermodynamic properties of the product. DETAILED DESCRIPTION

[0036] The present application is further described in detail below in combination with examples and comparative examples, and the raw materials involved in the present application can be obtained by market purchase.

[0037] Examples

[0038] Example 1

[0039] In this embodiment, the nucleating agent composition is prepared according to the following steps:

[0040] (1) Preparation of multi-layer graphene:

[0041] Preparation of expanded graphite: 1ml of 98wt% concentrated sulfuric acid is mixed with 0.1ml of hydrogen peroxide solution and 0.1ml of ammonium disulfate solution to form a treatment solution, while stirring the treatment solution, 2g of graphite is continuously added in small amounts, after 30min of reaction, a large amount of water (water temperature <10℃) is continuously stirred to achieve the purpose of activation, and the activated graphite is transported to a drying machine for drying to obtain pretreated graphite, the drying temperature is 120-160℃, and the moisture content is ≤5%; the pretreated graphite is granulated by a granulator, and the average mesh number is controlled at 200-300 meshes; the granulated material is calcined at a temperature of 600-800℃ to obtain expanded graphite;

[0042] The above expanded graphite is placed in a 75wt% ethanol solution, and air is rapidly expanded between the graphite layers by ultrasonic airization under 40KHz ultrasonic waves, so as to break and disperse the multi-layer graphene;

[0043] Preparation of polytetrafluoroethylene: the polytetrafluoroethylene sheets to be treated are placed in a plasma generation device, and plasma surface modification is performed in an ammonia atmosphere zone, with a treatment power of 200W and a treatment time of 15min. After drying and grinding, surface-modified polytetrafluoroethylene with an average particle size of 3nm is obtained.

[0044] (2) The above 3g multi-layer graphene is placed in 1L deionized water, and ultrasonic treatment is performed for 3h to obtain a multi-layer graphene suspension; 7g of the above polytetrafluoroethylene is added to the suspension and stirred at 70°C for 1h to form a mixed solution. After the reaction is completed, centrifugal separation is performed, and the product is washed with distilled water and dried to constant weight to obtain a nucleating agent composition.

[0045] Example 2

[0046] The difference between this example and Example 1 is that in this example, (3) the above 4g multi-layer graphene is placed in 1L deionized water, and ultrasonic treatment is performed for 3h to obtain a multi-layer graphene suspension; 6g of the above polytetrafluoroethylene is added to the suspension and stirred at 70°C for 1h to form a mixed solution. After the reaction is completed, centrifugal separation is performed, and the product is washed with distilled water and dried to constant weight to obtain a nucleating agent composition.

[0047] Example 3

[0048] The difference between this example and Example 1 is that in this example, (3) the above 2g multi-layer graphene is placed in 1L deionized water, and ultrasonic treatment is performed for 3h to obtain a multi-layer graphene suspension; 8g of the above polytetrafluoroethylene is added to the suspension and stirred at 70°C for 1h to form a mixed solution. After the reaction is completed, centrifugal separation is performed, and the product is washed with distilled water and dried to constant weight to obtain a nucleating agent composition.

[0049] Example 4

[0050] In this example, the nucleating agent composition is prepared according to the following steps:

[0051] (1) Preparation of multi-layer graphene:

[0052] Preparation of expanded graphite: 1 ml of 98 wt% concentrated sulfuric acid is mixed with 0.1 ml of hydrogen peroxide solution and 0.1 ml of ammonium disulfate solution to form a treatment solution. 2 g of graphite is continuously added to the treatment solution under stirring for 30 min. A large amount of water (water temperature <10°C) is continuously added under stirring for the purpose of activation. The activated graphite is dried in a drying machine at a temperature of 120-160°C to obtain pretreated graphite with a moisture content of ≤5%. The pretreated graphite is granulated in a granulator to obtain a mean particle size of 200-300 mesh. The granulated graphite is calcined at a temperature of 600-800°C to obtain expanded graphite.

[0053] The expanded graphite is placed in a 75 wt% ethanol solution. The interlayer air of the graphite is rapidly expanded, broken and dispersed to obtain multi-layer graphene by ultrasonic airization under 40 KHz ultrasonic wave.

[0054] Preparation of polytetrafluoroethylene: The treated nano-polytetrafluoroethylene powder is immersed in a polyethylene glycol / ethanol solution with a molecular weight of 1000 and a polyethylene glycol concentration of 80%. The powder is taken out after immersion at room temperature for 3 h, dried at 75°C to remove the solvent, and then placed in a plasma generating device for surface modification in an ammonia atmosphere at a treatment power of 200 W for 15 min. The polyethylene glycol not grafted onto the polytetrafluoroethylene is removed by washing with deionized water. The dried and ground product has an average particle size of 3 nm.

[0055] (2) The 3 g of multi-layer graphene is placed in 1 L of deionized water and ultrasonically treated for 3 h to obtain a multi-layer graphene suspension. 7 g of the above polytetrafluoroethylene is added to the suspension and stirred at 70°C for 1 h to form a mixture. After the reaction is completed, the product is washed with distilled water and dried to constant weight to obtain a nucleating agent composition.

[0056] Example 5

[0057] In this example, the nucleating agent composition is prepared according to the following steps:

[0058] (1) Preparation of multi-layer graphene:

[0059] Preparation of expanded graphite: 1 ml of 98 wt% concentrated sulfuric acid is mixed with 0.1 ml of hydrogen peroxide solution and 0.1 ml of ammonium disulfate solution to form a treatment solution. 2 g of graphite is continuously added to the treatment solution while stirring, and after 30 min, a large amount of water (water temperature <10°C) is continuously added while stirring to achieve the purpose of activation. The activated graphite is dried in a dryer to obtain pretreated graphite, with a drying temperature of 120-160°C and moisture content of ≤5%. The pretreated graphite is granulated using a granulator, with an average mesh size controlled at 200-300 mesh. The granulated material is calcined at a temperature of 600-800°C to obtain expanded graphite.

[0060] The expanded graphite is placed in a 75 wt% ethanol solution, and the interlayer air of the graphite is rapidly expanded, broken and dispersed to form multi-layer graphene using ultrasonic airization in a 40 KHz ultrasonic environment.

[0061] (2) Preparation of polytetrafluoroethylene: The polytetrafluoroethylene sheet to be treated is immersed in a polyethylene glycol / ethanol solution with a molecular weight of 1000 and a polyethylene glycol concentration of 80%. After soaking at room temperature for 3 h, the sheet is taken out, dried at 75°C to remove the solvent, and then placed in a plasma generating device for surface modification in an ammonia atmosphere zone. The treatment power is 200 W, and the treatment time is 15 min. Then, the polyethylene glycol not grafted onto the polytetrafluoroethylene is removed by washing with deionized water. After drying and grinding, surface-modified polytetrafluoroethylene with an average particle size of 3 nm is obtained.

[0062] (3) The above 3 g of multi-layer graphene is placed in 1 L of deionized water and ultrasonicated for 3 h to obtain a multi-layer graphene suspension. 7 g of the above polytetrafluoroethylene is added to the suspension and stirred at 70°C for 1 h to form a mixed solution. After the reaction is completed, centrifugal separation is performed, and the product is washed with distilled water and dried to constant weight to obtain a nucleating agent composition A.

[0063] (4) 6.5 g of nucleating agent composition A and 0.4 g of KH550 are dispersed in a mixture of 300 ml of deionized water and 600 ml of ethanol, and then reacted at 80°C for 4 h to obtain a modified mixed solution A. 3.5 g of 1,3:2,4-di(p-methylbenzylidene)sorbitol is added to anhydrous ethanol and stirred until completely dissolved to obtain a mixed solution B. The mixed solution B is added to the mixed solution A, ultrasonically dispersed for 30 min, and then mixed and added to a spray dryer for spray drying. The inlet air temperature is 150°C, and the outlet air temperature is 80°C. The nucleating agent composition is prepared.

[0064] Example 6

[0065] The difference between this example and Example 5 is that in this example, (4) 4.5 g of nucleating agent composition A and 0.4 g of KH550 are dispersed in a mixed solution of 300 ml of deionized water and 600 ml of ethanol, and then reacted at 80°C for 4 h to obtain modified mixed solution A; 5.5 g of 1,3:2,4-di(p-methylbenzylidene)sorbitol is added to anhydrous ethanol and stirred until completely dissolved to obtain mixed solution B; mixed solution B is added to mixed solution A and ultrasonically dispersed for 30 min, and then added to a spray dryer for spray drying after mixing, with an inlet air temperature of 150°C and an outlet air temperature of 80°C, to obtain a nucleating agent composition.

[0066] Example 7

[0067] The difference between this example and Example 5 is that in this example, (4) 4.5 g of nucleating agent composition A and 0.4 g of KH550 are dispersed in a mixed solution of 300 ml of deionized water and 600 ml of ethanol, and then reacted at 80°C for 4 h to obtain modified mixed solution A; 5.5 g of 1,3:2,4-di(p-methylbenzylidene)sorbitol is added to anhydrous ethanol and stirred until completely dissolved to obtain mixed solution B; mixed solution B is added to mixed solution A and ultrasonically dispersed for 30 min, and then added to a spray dryer for spray drying after mixing, with an inlet air temperature of 150°C and an outlet air temperature of 80°C, to obtain a nucleating agent composition.

[0068] Comparative Example

[0069] Comparative Example 1

[0070] The nucleating agent of this comparative example is multi-layer graphene, and the preparation method of the multi-layer graphene is as follows:

[0071] Preparation of expanded graphite: 1 ml of 98 wt% concentrated sulfuric acid, 0.1 ml of hydrogen peroxide solution, and 0.1 ml of ammonium disulfate solution are mixed to form a treatment solution. While stirring the treatment solution, 2 g of graphite is continuously added in small amounts. After 30 min of reaction, a large amount of water (water temperature <10°C) is continuously stirred to achieve the purpose of activation. The activated graphite is dried in a drying machine at a temperature of 120-160°C to obtain pretreated graphite with a water content of ≤5%. The pretreated graphite is granulated using a granulator to control the average mesh size to 200-300 mesh. The granulated material is calcined at a temperature of 600-800°C to obtain expanded graphite.

[0072] The above expanded graphite is placed in a 75 wt% ethanol solution, and the interlayer air of the graphite is rapidly expanded, broken, and dispersed into multi-layer graphene under the action of ultrasonic air in a 40 KHz ultrasonic environment.

[0073] Comparative Example 2

[0074] The nucleating agent of the present comparative example is polytetrafluoroethylene powder, and the preparation method of the polytetrafluoroethylene powder is as follows: the polytetrafluoroethylene to be treated is dried and ground to obtain polytetrafluoroethylene powder with an average particle size of 3 nm.

[0075] Comparative Example 3

[0076] The nucleating agent of the present comparative example is a mixture of 4 g of multilayer graphene and 6 g of nano-polytetrafluoroethylene powder. (The preparation method of the multilayer graphene is the same as that of Comparative Example 1, and the preparation method of the polytetrafluoroethylene is the same as that of Comparative Example 2)

[0077] Comparative Example 4

[0078] The nucleating agent of the present comparative example is a mixture of 1.95 g of multilayer graphene, 4.55 g of nano-polytetrafluoroethylene powder, and 3.5 g of 1,3:2,4-di(p-methylbenzylidene)sorbitol. (The preparation method of the multilayer graphene is the same as that of Comparative Example 1, and the preparation method of the polytetrafluoroethylene is the same as that of Comparative Example 2)

[0079] Application

[0080] 1.5 g of the nucleating agent of each of the examples and comparative examples was added to 1000 g of block copolymerized polypropylene J641, and after uniform mixing and stirring in a high-speed mixer, the mixture was extruded and pelletized by a twin-screw extruder, and then injection-molded into standard sample strips, which were used as the test samples. The extrusion temperature was 280±10°C, and the temperature of each section of the injection molding machine was 300-350°C.

[0081] Performance Test Method

[0082] The test was performed under the conditions of (23±2) °C and relative humidity (RH) of (50±5) % according to GB 2918-1998 (Standard Environment for Conditioning and Testing of Plastic Test Specimens), and the conditioning time of the test specimen was 48 h.

[0083] I. Mechanical Property Test

[0084] The sample strips prepared from each of the examples and comparative examples were tested for impact strength according to GB / T 1843-1996 (Plastic Izod Impact Test Method), and the test results are shown in Table 1.

[0085] The sample strips prepared from each of the examples and comparative examples were tested for flexural modulus according to GB / T 9341-2000 (Determination of Flexural Properties of Plastics), and the test results are shown in Table 1.

[0086] II. Thermal Property Test

[0087] The sample strips prepared from each of the examples and comparative examples were tested for heat distortion temperature according to GB / T 1634-2004 (Determination of Load Deflection Temperature of Plastics), and the test results are shown in Table 1.

[0088] Table 1 Performance test data table of examples 1-7 and comparative examples 1-4

[0089]

[0090] In combination with example 1 and comparative examples 1-3 and with reference to table 1, it can be seen that the mechanical and thermal properties of example 1 are better than those of comparative examples 1-3, which shows that by inserting polytetrafluoroethylene into the multi-layer graphene sheets, the application not only plays a synergistic effect of polytetrafluoroethylene and graphene as nucleating agent, but also inhibits the agglomeration of graphene itself, thereby promoting its dispersion in the resin and improving the mechanical and thermal properties of the product.

[0091] In combination with examples 1 and 4 and with reference to table 1, it can be seen that by introducing polyethylene glycol on the surface of polytetrafluoroethylene, the application can effectively improve the surface activity of polytetrafluoroethylene, and through plasma treatment, on the one hand, the grafting of polytetrafluoroethylene and polyethylene glycol is realized, and on the other hand, the change of the surface structure of polytetrafluoroethylene and polyethylene glycol improves the adhesion, which is conducive to the adhesion of polytetrafluoroethylene on graphene, further improves the combination of polytetrafluoroethylene and multi-layer graphene, and improves the mechanical and thermal properties of the product.

[0092] In combination with example 5 and comparative example 4 and with reference to table 1, it can be seen that the nucleating agent composition prepared by the application can fully play the nucleating effect of the three by inserting polytetrafluoroethylene into multi-layer graphene and then effectively combining it with sorbitol nucleating agent, which has better crystallization effect on the resin than simply mixing polytetrafluoroethylene, multi-layer graphene and sorbitol nucleating agent to form a nucleating agent combination, and improves the mechanical and thermal properties of the product.

[0093] The specific embodiments are only an explanation of the application, and are not a limitation of the application. Those skilled in the art can make modifications to the embodiments without creative contribution after reading the specification, but as long as the modifications are within the scope of the claims of the application, they are protected by the patent law.

Claims

1. A nucleating agent composition characterized in that, The nucleating agent composition comprises polytetrafluoroethylene and multilayer graphene, the polytetrafluoroethylene is interpenetrated in the multilayer graphene sheet, and the polytetrafluoroethylene is obtained by plasma treatment under a nitrogen-containing atmosphere; The mass ratio of the polytetrafluoroethylene to the multilayer graphene is (6-8):(2-4). The preparation method of the multilayer graphene comprises the following steps: graphite is subjected to oxidation treatment and then high-temperature expansion to obtain expanded graphite; and the expanded graphite is placed in an ethanol solution and subjected to ultrasonic treatment to obtain the multilayer graphene. The polytetrafluoroethylene is obtained by plasma treatment in the presence of a nitrogen-containing gas atmosphere and polyethylene glycol.

2. The nucleating agent composition of claim 1, wherein The nucleating agent composition further comprises a sorbitol nucleating agent, and the sorbitol nucleating agent is one or more of bis-1,3:2,4-(4'-propylbenzylidene)-1-propyl sorbitol, 1,3:2,4-dibenzylidene sorbitol, 1,3:2,4-di(p-methylbenzylidene) sorbitol, and 1,3:2,4-di(3,4-dimethylene benzylidene) sorbitol.

3. The method of producing the nucleating agent composition according to claim 1, characterized by, The multilayer graphene is added into deionized water to obtain a suspension, and polytetrafluoroethylene is mixed, washed, and dried to interpenetrate the polytetrafluoroethylene in the multilayer graphene sheet to obtain the nucleating agent composition.

4. The method of producing the nucleating agent composition according to claim 2, characterized by, The nucleating agent composition comprises the following steps: The multilayer graphene is added into deionized water to obtain a suspension, and polytetrafluoroethylene is mixed, washed, and dried to interpenetrate the polytetrafluoroethylene in the multilayer graphene sheet to obtain the nucleating agent composition A. The nucleating agent composition A is modified by using a silane coupling agent and dispersed in water to obtain a mixed solution A; The sorbitol nucleating agent is added into an alcohol solvent to be dissolved to obtain a mixed solution B; the mass ratio of the sorbitol nucleating agent to the nucleating agent composition A is (35-75):(25-65). The mixed solution B is added into the mixed solution A, ultrasonically dispersed, and then spray dried to obtain the nucleating agent composition.

5. The method for producing a nucleating agent composition according to claim 4, characterized by, The silane coupling agent is an amino silane coupling agent.

6. Use of the nucleating agent composition according to any one of claims 1 to 2, characterized in that The nucleating agent composition is used for preparing one or more of polypropylene, polyethylene, polylactic acid, and polyurethane.

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