Preparation method of light-controlled nano functional master batch

By mixing a modified coupling agent with an inorganic nanomaterial and a color regulator, an optical nanoregulator is prepared, which solves the problem of insufficient optical properties of existing masterbatch films and improves the optical and mechanical properties of the films.

CN120699286APending Publication Date: 2025-09-26GUIZHOU INST OF METALLURGY & CHEM ENG +2
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Patent Information

Application Number
CN202511019429.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-23
Publication Date
2025-09-26

AI Technical Summary

Technical Problem

When using existing masterbatches to prepare films, it is impossible to achieve precise control of light transmittance, resulting in insufficient optical properties of the film.

Method used

A modified coupling agent is mixed with an inorganic nanomaterial and a color regulator to prepare a light-nano regulator, which is then extruded through a twin-screw extruder and water-cooled to form a light-regulating nanofunctional masterbatch, which is then used to prepare a film in a film blowing machine.

Benefits of technology

The optical and mechanical properties of the film are improved, and precise control of light transmittance is achieved.

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Abstract

The invention relates to the technical field of high polymer materials, and particularly discloses a preparation method of a light-controlled nano functional master batch, which comprises the following steps: S1, taking materials: respectively taking a modified coupling agent, an inorganic nano material dispersing agent and a color regulating agent according to the mass ratio of (1-5): (50-200): (5-20); s2, preparing a light nano regulating agent, namely mixing the modified coupling agent and the inorganic nano material dispersing agent, stirring at a high speed for 1-2 minutes, adding the color regulating agent, and stirring at a high speed to prepare the light nano regulating agent; and S3, preparing the light-controlled nano functional master batch, namely sequentially adding 10-30 g of the light-controlled nano regulating agent, 450-500 g of a resin matrix, 2-8 g of polyethylene wax, 5-10 g of Fischer-Tropsch wax and 0.1-1 g of an antioxidant into a high-speed mixer, stirring for 3-8 minutes, uniformly mixing, extruding by a double-screw extruder at the rotating speed of 100-500 r / min under the temperature condition of 145-190 DEG C, and carrying out water-cooling grain-sized dicing, so as to prepare the light-controlled nano functional master batch. The prepared master batch is used for preparing a film and can improve the optical property and mechanical property of the film.
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Description

Technical Field

[0001] The present invention relates to the technical field of polymer materials, and in particular to a method for preparing light-regulated nano-functional masterbatch. Background Art

[0002] Functional masterbatches, developed in the 1980s as a plastics processing additive, consist of an excess of chemical additives, a carrier resin, and a dispersant. Through pre-mixing technology, pigments and additives are evenly dispersed in the carrier resin to form a granular material. The uniformity of functional masterbatches in film manufacturing ensures color stability and consistent performance.

[0003] To improve the mechanical properties of PE films produced using functional masterbatches, a Chinese invention patent application with application number "CN202311375510.2" discloses a filler masterbatch, its preparation method, and its application. The masterbatch comprises the following raw materials by weight: 8-10 parts of a silane coupling agent-grafted PUA resin; 2-3 parts of a dispersant; 2-3 parts of 2,6-di-tert-butyl-4-methylphenol; 20-25 parts of modified nano-calcium carbonate powder; 40-45 parts of modified nano-barium sulfate powder; 3-5 parts of a toughening resin; and 18-20 parts of a low-density PE resin. The silane coupling agent-grafted PUA resin in the filler masterbatch contains two chemically distinct groups: siloxane groups that react chemically with inorganic powders; and PUA segments that are PE-friendly and readily form hydrogen bonds with the PE resin. This silane coupling agent grafted onto PUA resin can improve the interfacial adhesion between inorganic powders and PE resin, significantly enhancing the mechanical properties of PE films made with it. While this masterbatch improves the mechanical properties of thin films, it has no specific effect on their optical properties. When used to make agricultural films, it is impossible to precisely control light transmittance. Summary of the Invention

[0004] The purpose of the present invention is to provide a method for preparing a light-regulated nano-functional masterbatch to solve the problem that when using existing masterbatches to prepare films, the optical properties of the film have no directionality and the transmittance of light cannot be precisely controlled.

[0005] In order to solve the above problems, the technical solutions provided are as follows: A method for preparing a light-regulated nano-functional masterbatch comprises the following steps: S1: Take the materials and take the modified coupling agent, inorganic nanomaterial dispersant and color control agent respectively according to the mass ratio of 1-5:50-200:5-20; S2: Preparation of the photo-nano control agent: first, the modified coupling agent and the inorganic nanomaterial dispersant are mixed and stirred at high speed for 1-2 minutes, and then the color control agent is added and stirred at high speed to prepare the photo-nano control agent; S3: Preparation of light-regulated nano-functional masterbatch: take 10-30g of light-regulated nano-control agent, 450-500g of resin matrix, 2-8g of polyethylene wax, 5-10g of Fischer-Tropsch wax, and 0.1-1g of antioxidant, add them into a high-speed mixer in sequence and stir for 3-8 minutes to mix evenly, extrude through a twin-screw extruder at a temperature of 145°C to 190°C and a speed of 100-500r / min, water-cooled and pelletized to prepare light-regulated nano-functional masterbatch.

[0006] The beneficial effect of the above technical solution is that: the color regulator is mixed with the inorganic nanomaterial dispersant to prepare the optical nanoregulator, and the color regulator can be well dispersed in the inorganic nanomaterial. The prepared optical nanoregulator is then used to prepare the masterbatch, which can improve the dispersibility of the masterbatch in the subsequent preparation of the film, thereby improving the optical and mechanical properties of the film.

[0007] Furthermore, the method also includes step S4: preparation of light-regulated nano-functional agricultural film, taking 3000 g of the resin matrix, adding 99 g of the functional masterbatch prepared in step S3 into a high-speed blender and mixing evenly, pouring the mixture into a film blowing machine with a melting temperature of 175°C and a die head temperature of 165°C to blow the film, and testing the film thickness.

[0008] Furthermore, the modified coupling agent in step S1 is composed of one or more of a titanate coupling agent, an aluminate coupling agent, a silicate coupling agent, calcium stearate, and zinc stearate.

[0009] Furthermore, the inorganic nanomaterial dispersant in step S1 is composed of one or more of CaCO3, SiO2, and BaSO4.

[0010] Furthermore, the color modifier in step S2 includes a red modifier, a blue modifier and a green modifier.

[0011] Furthermore, the red color regulator is composed of one or more of permanent red (PR-213), fluorescent red (MP13), and luminous red (MP14); the blue color regulator is composed of one or more of phthalocyanine blue, fluorescent blue (MP19), and luminous blue (MP20); and the green color regulator is light-fast orange (PO-38).

[0012] Furthermore, the resin matrix used in steps S3 and S4 is composed of one or more of low-density polyethylene, linear low-density polyethylene, high-density polyethylene, and polypropylene.

[0013] Furthermore, the antioxidant is composed of one or more of hindered phenol antioxidants 1010 and phosphite antioxidants 168. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 Schematic diagram of SEM characterization of the film prepared in Example 1; Figure 2 Schematic diagram of SEM characterization of the film prepared in Comparative Example 1; Figure 3 This is a schematic diagram of SEM characterization of the red control agent dispersed in nano-BaSO4 in Example 1; Figure 4 Schematic diagram of SEM characterization of the red control agent dispersed in nano-SiO2 in comparative example 2; Figure 5 Schematic diagram of SEM characterization of the red regulator dispersed in nano-CaCO3 in comparative example 3; DETAILED DESCRIPTION The following is further described in detail through specific implementation methods: The specific implementation process is as follows: Example 1 A method for preparing a light-regulated nano-functional masterbatch comprises the following steps: S1: Take the materials and take aluminate modified coupling agent, nano BaSO4 and red control agent respectively according to the mass ratio of 2:100:10; S2: Preparation of the photo-nano control agent: first, the aluminate-modified coupling agent and nano-BaSO4 were mixed and stirred at high speed for 1 minute, and then the red control agent was added and stirred at high speed to prepare the photo-nano control agent. The red control agent was luminous red (MP14). The aluminate-modified coupling agent and nano-BaSO4 can modify the red control agent. S3: Preparation of light-regulated nano-functional masterbatch: 20g of light-regulated nano-controller, 467g of linear low-density polyethylene, 5g of polyethylene wax, 8g of Fischer-Tropsch wax, and 0.5g of hindered phenol antioxidant 1010 are added to a high-speed mixer in sequence and stirred for 5 minutes to mix evenly. The mixture is extruded through a twin-screw extruder at a temperature of 145°C to 190°C and a speed of 300r / min, and water-cooled and pelletized to prepare light-regulated nano-functional masterbatch.

[0015] The prepared light-regulated nano-functional masterbatch was further prepared into agricultural film, and the performance of the agricultural film was tested. The preparation process of the agricultural film is as follows: S4: Preparation of light-regulated nano-functional agricultural film: 3000g of linear low-density polyethylene and 99g of the functional masterbatch prepared in step S3 were added to a high-speed blender and mixed thoroughly. The mixture was then poured into a film blowing machine with a melt temperature of 175°C and a die head temperature of 165°C for film blowing. The film thickness was measured, and the optical properties (including transmittance, haze, and film appearance) and mechanical properties (including elongation at break, tensile strength, and Young's modulus) of the film were tested. The test methods for the film's optical properties are described in GB / T2410-2008, Transparent Plastics - Determination of Transmittance and Haze. The test methods for the film's mechanical properties are described in GB / T13022-1991, Plastics - Test Methods for Tensile Properties of Films.

[0016] Example 2 The difference between Example 2 and Example 1 is that the red modifier added in step S2 is replaced by a blue modifier, and the blue modifier is luminous blue (MP20).

[0017] Example 3 The difference between Example 3 and Example 1 is that the red control agent added in step S2 is replaced by a green control agent, and the green control agent is light-fast orange (PO-38).

[0018] The optical performance test data of the films of Examples 1-3 are shown in Table 1 below: Table 1 Optical performance test data of films of Examples 1-3

[0019] The mechanical properties test data of the films of Examples 1-3 are shown in Table 2 below: Table 2 Mechanical properties test data of films of Examples 1-3

[0020] From the mechanical and optical performance data of the films prepared in Examples 1-3 in Table 1 and Table 2 above, it can be concluded that the film prepared using the red color regulator luminous red (MP14) used in Example 1 has the highest light transmittance and the strongest mechanical properties.

[0021] Comparative Example 1 The difference between Comparative Example 1 and Example 1 is that nano-BaSO4 is not added in step S2.

[0022] The films prepared in Example 1 and Comparative Example 1 were characterized by SEM. The SEM characteristics of the film in Example 1 are as follows: Figure 1 As shown, the SEM characterization of the film of Comparative Example 1 is as follows Figure 2 As shown by Figure 1 and Figure 2From the comparison, it can be seen that the film made of the light regulating agent modified with nano-BaSO4 in Example 1 has no apparent crystal points, while the film made of the light regulating agent not modified with nano-BaSO4 in Comparative Example 1 has a small amount of apparent crystal points.

[0023] Comparative Example 2 The difference between Comparative Example 2 and Example 1 is that the nano-BaSO4 added in step S2 is replaced by nano-SiO2.

[0024] Comparative Example 3 The difference between Comparative Example 3 and Example 1 is that the nano-BaSO4 added in step S2 is replaced by nano-CaCO3.

[0025] The SEM characterization results of the nano inorganic pigments in Example 1, Comparative Example 2 and Comparative Example 3 are as follows: Figure 3-5 As shown by Figure 3-5 Characterization images show that the agglomeration of Luminous Red (MP14) is significantly reduced after the organic pigment is dispersed in fine nano-inorganic materials. When Luminous Red (MP14) is dispersed in modified BaSO4, the functional particle size is smaller. Furthermore, increasing the red / blue light control capability requires a corresponding increase in the nano-inorganic material content. However, excessive nano-inorganic material content can lead to reduced transmittance. Modified BaSO4 dispersed in Luminous Red (MP14) achieves better results than modified SiO2 and CaCO3 dispersed in Luminous Red (MP14).

[0026] The above is only an embodiment of the present invention, and the common knowledge such as the specific structure and characteristics of the scheme is not described in detail here. It should be pointed out that for those skilled in the art, without departing from the structure of the present invention, several variations and improvements can be made, which should also be regarded as the scope of protection of the present invention, and these will not affect the effect of the implementation of the present invention and the practicality of the patent. The scope of protection required by this application shall be based on the content of its claims, and the specific implementation methods and other records in the specification can be used to interpret the content of the claims.

Claims

1. A method for preparing light-regulated nano-functional masterbatch, characterized in that: The following steps are involved: S1: Take the materials and take the modified coupling agent, inorganic nanomaterial dispersant and color control agent respectively according to the mass ratio of 1-5:50-200:5-20; S2: Preparation of the photo-nano control agent: first, the modified coupling agent and the inorganic nanomaterial dispersant are mixed and stirred at high speed for 1-2 minutes, and then the color control agent is added and stirred at high speed to prepare the photo-nano control agent; S3: Preparation of light-regulated nano-functional masterbatch: take 10-30g of light-regulated nano-control agent, 450-500g of resin matrix, 2-8g of polyethylene wax, 5-10g of Fischer-Tropsch wax, and 0.1-1g of antioxidant, add them into a high-speed mixer in sequence and stir for 3-8 minutes to mix evenly, extrude through a twin-screw extruder at a temperature of 145°C to 190°C and a speed of 100-500r / min, water-cooled and pelletized to prepare light-regulated nano-functional masterbatch.

2. The method for preparing a light-regulated nano-functional masterbatch according to claim 1, characterized in that: The process also includes step S4: preparation of light-regulated nano-functional agricultural film, taking 3000 g of the resin matrix, adding 99 g of the functional masterbatch prepared in step S3 into a high-speed blender and mixing them evenly, pouring them into a film blowing machine with a melting temperature of 175°C and a die head temperature of 165°C to blow the film, and testing the film thickness.

3. The method for preparing a light-regulated nano-functional masterbatch according to claim 2, characterized in that: The modified coupling agent in step S1 is composed of one or more of a titanate coupling agent, an aluminate coupling agent, a silicate coupling agent, calcium stearate, and zinc stearate.

4. The method for preparing a light-regulated nano-functional masterbatch according to claim 3, characterized in that: The inorganic nanomaterial dispersant in step S1 is composed of one or more of CaCO3, SiO2, and BaSO4.

5. The method for preparing a light-regulated nano-functional masterbatch according to claim 4, characterized in that: The color modifiers in step S2 include a red modifier, a blue modifier, and a green modifier.

6. The method for preparing a light-regulated nano-functional masterbatch according to claim 5, characterized in that: The red regulator is composed of one or more of permanent red, fluorescent red, and luminous red; the blue regulator is composed of one or more of phthalocyanine blue, fluorescent blue, and luminous blue; and the green regulator is sun-fast orange.

7. The method for preparing a light-regulated nano-functional masterbatch according to claim 6, characterized in that: The resin matrix used in steps S3 and S4 is composed of one or more of low-density polyethylene, linear low-density polyethylene, high-density polyethylene, and polypropylene.

8. The method for preparing a light-regulated nano-functional masterbatch according to claim 7, characterized in that: The antioxidant is composed of one or more of a hindered phenol antioxidant 1010 and a phosphite antioxidant 168.

Citation Information

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