Polypropylene composition and polypropylene and process for the production thereof and luminary

By adding olefin maleic anhydride copolymer microspheres and white oil to a polypropylene composition, and utilizing contact mixing and melt blending techniques, the dispersion problem of microspheres in polypropylene was solved, resulting in polypropylene products with high haze, high light transmittance, and uniform surface, suitable for applications such as LED lighting bodies.

CN122103743APending Publication Date: 2026-05-29CHINA PETROLEUM & CHEMICAL CORP +3

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
CHINA PETROLEUM & CHEMICAL CORP
Filing Date
2024-11-29
Publication Date
2026-05-29

AI Technical Summary

Technical Problem

In the prior art, the olefin maleic anhydride binary copolymer microspheres have poor dispersibility in polypropylene, resulting in uneven mixing, easy dust generation, and difficulty in uniform dispersion in polypropylene materials, which affects light diffusion performance and aesthetics.

Method used

The polypropylene composition comprises a polypropylene matrix, olefin maleic anhydride copolymer microspheres, and white oil. The olefin maleic anhydride copolymer microspheres are uniformly dispersed in the polypropylene matrix through contact mixing and melt blending. White oil is used to coat the microspheres during the preparation process to improve dispersibility.

Benefits of technology

The process achieved uniform dispersion of olefin maleic anhydride copolymer microspheres in polypropylene, improving the haze and light transmittance of the product, resulting in a uniform surface without white spots, thus enhancing the product's aesthetics and application value.

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Abstract

The application relates to the field of high polymer materials, and discloses a polypropylene composition, a polypropylene and a preparation method of the polypropylene and a luminary; the polypropylene composition comprises a polypropylene matrix, olefin maleic anhydride copolymer microspheres and white oil, the content of the olefin maleic anhydride copolymer microspheres is 0.1-10 parts by weight relative to 100 parts by weight of the polypropylene matrix, and the content of the white oil is 0.5-4 parts by weight. The polypropylene product has high haze and high light transmittance, the surface is uniform and free of white spots, the material has excellent aesthetic degree, and has extremely high application value.
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Description

Technical Field

[0001] This invention relates to the field of polymer materials, specifically to a polypropylene composition, polypropylene, a method for preparing the same, and an illuminator. Background Technology

[0002] Olefin-maleic anhydride copolymer microspheres have numerous applications. They can be added to polyolefins as additives or fillers, exhibiting far better compatibility than common inorganic particles. They can improve many properties of polypropylene, such as light diffusion, polarity, and opening properties. CN112708020A discloses a maleic anhydride terpolymer microsphere, its preparation method, and its application. The copolymer microspheres are added to polyolefin materials as an opening agent, significantly improving the opening properties of polyolefin films.

[0003] However, due to the significant size and bulk density difference between the polymer microspheres and polypropylene particles, stratification occurs during large-scale mixing, making uniform mixing difficult and easily generating dust that poses environmental and health hazards. Therefore, how to uniformly mix the copolymer microspheres and polypropylene while avoiding dust generation, and ultimately ensure the microspheres are uniformly dispersed within the polypropylene material, remains a key technical challenge.

[0004] As the most promising lighting source, LEDs boast advantages such as robust structure, shock and impact resistance, fast light response, long lifespan, and low energy consumption—only 10% of that of incandescent bulbs. They are widely used in urban and residential lighting, electronics, automobiles, and various other industries, becoming ubiquitous in modern society. However, as a point light source, LEDs emit concentrated and intense light, leading to glare and uneven illumination. Therefore, in practical applications, light-diffusing materials are typically used to transform them into linear or surface light sources, making the light brighter and softer, reducing glare, and enhancing the aesthetics of the illuminated area.

[0005] Currently, light-diffusing materials for LEDs are mainly bulk scattering materials. These materials achieve light diffusion by adding scattering particles with different refractive indices to a transparent polymer matrix, causing multiple refractions of light as it passes through the interface. They offer advantages such as easily controllable transmittance and haze. Due to the high price and density of polycarbonate, inexpensive and low-density light-diffusing polypropylene materials are rapidly developing under the trend of automotive lightweighting. Maleic anhydride copolymer microspheres can be used as light diffusing agents to prepare light-diffusing polypropylene through melt blending.

[0006] CN114479260B discloses a heat-resistant light-diffusing polypropylene composition and its application, as well as a heat-resistant light-diffusing polypropylene and its preparation method and application; comprising the following components by weight: based on 100 parts by weight of polypropylene, the amount of maleic anhydride / N-phenylmaleimide / α-methylstyrene copolymer microspheres is 0.3-10 parts by weight, and the amount of organosilicon resin microspheres is 0.05-0.5 parts by weight. However, this method uses terpolymer microspheres, which are more expensive.

[0007] However, existing technologies suffer from poor dispersibility of olefin-maleic anhydride binary copolymer microspheres in polypropylene, making the research and development of a new polypropylene technology of great significance. Summary of the Invention

[0008] The purpose of this invention is to overcome the dispersion problem of olefin-maleic anhydride copolymer microspheres in polypropylene in the prior art, and to provide a polypropylene composition, polypropylene, a method for preparing the same, and an illuminator. The method of this invention enables the olefin-maleic anhydride copolymer microspheres to be better dispersed in the polypropylene matrix, and the polypropylene products containing the olefin-maleic anhydride copolymer microspheres (e.g., illuminators) have high haze, high light transmittance, and a uniform surface without white spots, resulting in excellent aesthetics and high application value.

[0009] To achieve the above objectives, a first aspect of the present invention provides a polypropylene composition comprising a polypropylene matrix, olefin maleic anhydride copolymer microspheres, and white oil, wherein the content of the olefin maleic anhydride copolymer microspheres is 0.1-10 parts by weight relative to 100 parts by weight of the polypropylene matrix, and the content of the white oil is 0.05-8 parts by weight.

[0010] A second aspect of the present invention provides a method for preparing polypropylene using the aforementioned polypropylene composition, wherein the method comprises:

[0011] (1) The polypropylene is brought into contact with white oil for a first mixing;

[0012] (2) The polypropylene coated with white oil obtained in step (1) is brought into contact with olefin maleic anhydride copolymer microspheres for a second mixing.

[0013] (3) Polypropylene is obtained by melt blending the mixture obtained in step (2).

[0014] A third aspect of the present invention provides a polypropylene prepared by the method described above.

[0015] A fourth aspect of the present invention provides an illumination body, wherein the material used to prepare the illumination body comprises polypropylene, wherein the polypropylene is the polypropylene described above.

[0016] Through the above technical solution, the method of the present invention enables the olefin maleic anhydride copolymer microspheres to be better dispersed in the polypropylene matrix. The polypropylene products containing the olefin maleic anhydride copolymer microspheres preferably have high haze, high light transmittance, and uniform surface without white spots. The products have excellent aesthetics and have extremely high application value. Attached Figure Description

[0017] Figure 1 Here is an SEM image of the surface morphology of the styrene-maleic anhydride copolymer microspheres prepared in Example 2.

[0018] Figure 2 This is the DSC curve of the styrene-maleic anhydride copolymer microspheres prepared in Example 2;

[0019] Figure 3 This is a photograph of a 1mm polypropylene sample prepared in Comparative Example 2.

[0020] Figure 4 This is a photograph of a 1mm sheet made from polypropylene prepared in Example 1. Detailed Implementation

[0021] The endpoints and any values ​​of the ranges disclosed herein are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.

[0022] As previously stated, a first aspect of the present invention provides a polypropylene composition comprising a polypropylene matrix, olefin maleic anhydride copolymer microspheres, and white oil, wherein the content of the olefin maleic anhydride copolymer microspheres is 0.1-10 parts by weight relative to 100 parts by weight of the polypropylene matrix, and the content of the white oil is 0.5-8 parts by weight.

[0023] According to the present invention, in a preferred embodiment, the content of the olefin maleic anhydride copolymer microspheres is 0.5-5 parts by weight and the content of the white oil is 0.5-4 parts by weight relative to 100 parts by weight of the polypropylene matrix; more preferably, the content of the olefin maleic anhydride copolymer microspheres is 2-4 parts by weight and the content of the white oil is 0.8-3 parts by weight relative to 100 parts by weight of the polypropylene matrix.

[0024] The inventors of this invention have discovered that using olefin-maleic anhydride copolymer microspheres, because these microspheres have the structure of maleic anhydride and exist in a spherical shape, can improve the polarity, light diffusion performance, and opening performance of polypropylene. Preferably, when the olefin-maleic anhydride copolymer microspheres are styrene-maleic anhydride copolymer microspheres, due to the large number of rigid ring structures, they can not only better improve the light diffusion performance, but also enhance the heat resistance of polypropylene.

[0025] According to the present invention, in the olefin-maleic anhydride copolymer microspheres, based on the total molar amount of each structural unit in the copolymer, the molar content of maleic anhydride structural units is 40-50 mol%, and the molar content of olefin structural units is 50-60 mol%. Preferably, in the olefin-maleic anhydride copolymer microspheres, based on the total molar amount of each structural unit in the copolymer, the molar content of maleic anhydride structural units is 45-50 mol%, and the molar content of olefin structural units is 50-55 mol%.

[0026] According to the present invention, the particle size of the olefin maleic anhydride copolymer microspheres is 500-2000 nm, preferably 1000-1500 nm.

[0027] According to the present invention, the method for preparing the olefin-maleic anhydride copolymer microspheres includes: reacting an olefin, maleic anhydride and a solvent in contact with each other under stirring conditions in the presence of an initiator to obtain olefin-maleic anhydride copolymer microspheres.

[0028] According to the present invention, the initiator is azobisisobutyronitrile and / or azobisisoheptanenitrile, preferably azobisisobutyronitrile.

[0029] According to the present invention, the solvent is isoamyl acetate or a mixture of hexane and acetone.

[0030] According to the present invention, the reaction conditions include: a temperature of 45-100°C and a time of 60-600 min; preferably, a temperature of 50-70°C and a time of 180-360 min.

[0031] According to the present invention, the olefin in the olefin maleic anhydride copolymer microspheres is a C4-C9 olefin; preferably, the olefin in the olefin maleic anhydride copolymer microspheres is one or more selected from styrene maleic anhydride copolymer microspheres, α-methylstyrene maleic anhydride copolymer microspheres, isobutylene maleic anhydride copolymer microspheres, and isobutylene maleic anhydride copolymer microspheres; more preferably, the olefin in the olefin maleic anhydride copolymer microspheres is styrene maleic anhydride copolymer microspheres.

[0032] According to a preferred embodiment of the present invention, the method for preparing the olefin (styrene) maleic anhydride copolymer microspheres includes: firstly dissolving olefin (styrene), maleic anhydride and initiator in a mixed solvent of isoamyl acetate or hexaneacetone to form a homogeneous solution, then reacting at 50-100°C for a period of time to obtain a copolymer emulsion suspension, and then obtaining the olefin (styrene) maleic anhydride copolymer microspheres after solid-liquid separation.

[0033] According to the present invention, the melt index of the polypropylene matrix at 230°C and a load of 2.16 kg is 2-70 g / 10 min, preferably 25-60 g / 10 min; more preferably 25-27 g / 10 min. In the present invention, the polypropylene can be homopolymer polypropylene and / or atactic polypropylene.

[0034] According to the present invention, the kinematic viscosity of the white oil at 40°C is 5-100 mm. 2 / s, preferably 20-70mm 2 / s. In this invention, the main components of the white oil are hydrocarbon compounds, including but not limited to: one or a mixture of several white oils selected from No. 5, No. 7, No. 10, No. 15, No. 26, No. 32, No. 46, No. 68, and No. 100.

[0035] According to the present invention, the polypropylene composition further includes an antioxidant, wherein the antioxidant may be a mixture of antioxidant 1010 and antioxidant 168 in a 1:1 ratio, and in the present invention, the amount of the antioxidant is 0.1-0.3 parts by weight relative to 100 parts by weight of the polypropylene.

[0036] A second aspect of the present invention provides a method for preparing polypropylene using the aforementioned polypropylene composition, wherein the method comprises:

[0037] (1) The polypropylene matrix is ​​brought into contact with white oil for the first mixing;

[0038] (2) The polypropylene coated with white oil obtained in step (1) is brought into contact with olefin maleic anhydride copolymer microspheres for a second mixing.

[0039] (3) Polypropylene is obtained by melt blending the mixture obtained in step (2).

[0040] According to the present invention, the polypropylene matrix may be polypropylene powder or polypropylene particles.

[0041] According to the present invention, the maleic anhydride olefin in the polypropylene is uniformly dispersed in the polypropylene matrix.

[0042] According to the present invention, in step (1), polypropylene granules or polypropylene powder and white oil are first mixed in contact and mixed evenly; wherein, the first mixing can be carried out at room temperature, and in the present invention, it can be mixed at a temperature of -20°C to 60°C for 0.1-30 min; preferably, it can be mixed at a temperature of 20°C to 60°C for 0.1-30 min; more preferably, it can be carried out at a stirring speed of 500-50000 rpm.

[0043] According to the present invention, in step (2), the polypropylene with white oil coating obtained in step (1) and the remaining components are placed in a high-speed mixer in a weight ratio for a second mixing, and the mixture is made uniform; wherein, the second mixing can be carried out at room temperature, and in the present invention, the mixing can be carried out at a temperature of -20°C to 60°C for 0.1-10 min; preferably, the mixing can be carried out at a temperature of 20°C to 60°C for 0.1-10 min; more preferably, the mixing can be carried out at a stirring speed of 500-50000 rpm.

[0044] In this invention, the equipment used for the first mixing and the second mixing in steps (1) and (2) is not specifically limited, as long as it ensures that the surface of the polypropylene powder or particles is coated with white oil; for example, in small-scale mixing, it can be simply mixed by shaking a bag, or a laboratory stirring paddle can be used. In a preferred embodiment of this invention, a high-speed mixer is used for mixing.

[0045] According to the present invention, in step (3), the mixture obtained in step (2) is melt-blended by an extruder to obtain polypropylene with uniformly dispersed styrene-maleic anhydride copolymer microspheres.

[0046] According to the present invention, in step (3), the temperature of the mixture obtained by the mixing process in the melt extrusion process is 170-250°C in each zone, and the residence time of the mixture is 1-10 min.

[0047] A third aspect of the present invention provides a polypropylene prepared by the method described above.

[0048] According to the present invention, the heat distortion temperature of the polypropylene is ≥50°C, and the light transmittance of the 1mm sample is ≥40%, and the haze is ≥60%; preferably, the heat distortion temperature of the polypropylene is 80-120°C, and the light transmittance of the 1mm sample is 60-95%, and the haze is 70-100%.

[0049] According to the present invention, the light transmittance of the 2mm sample is ≥30% and the haze is ≥60%; preferably, the light transmittance of the 2mm sample is 40-90% and the haze is 80-100%.

[0050] According to the present invention, the sheet product prepared using the polypropylene has no white spots on its surface.

[0051] A fourth aspect of the present invention provides an illumination body, wherein the material used to prepare the illumination body comprises polypropylene, wherein the polypropylene is the polypropylene described above.

[0052] According to the present invention, the illuminator is an LED lamp.

[0053] In this invention, since the size of the copolymer microspheres is larger than the wavelength of light, the polypropylene has high haze, good light transmittance, and good heat resistance, and can be used as a lampshade material in LED lamps, etc.

[0054] The present invention will be described in detail below through embodiments.

[0055] In the following examples and comparative examples:

[0056] Among the experimental materials:

[0057] Both the polypropylene Y26 powder and granules were purchased from Zhenhai Refining & Chemical Co., Ltd. The melt index was 25.8 g / 10 min at 230℃ and 2.16 kg; in addition, the weight average molecular weight was 110,000-130,000 g / mol.

[0058] The polypropylene M60ET granules were purchased from Zhenhai Refining & Chemical Co., Ltd., and had a melt index of 59.3 g / 10 min at 230℃ and 2.16 kg; in addition, the weight average molecular weight was 150,000-170,000.

[0059] The polypropylene T03 granules were purchased from Zhenhai Refining & Chemical Co., Ltd., and had a melt index of 2.1 g / 10 min at 230℃ and 2.16 kg; the weight-average molecular weight was 370,000-400,000.

[0060] All types of white oil are purchased from Guangdong Zhonghai Nanlian Energy Co., Ltd., and are all industrial-grade white oil.

[0061] Antioxidant 225 was purchased from Yingkou Fengguang New Materials Co., Ltd.

[0062] All other reagents used in the examples and comparative examples were commercially available.

[0063] The following instruments and measurement methods were used for determination:

[0064] Light transmittance and haze were tested using an NDH7000 haze meter manufactured by NIPPON DENSHOKU Electric Color Industry Co., Ltd. of Japan, in accordance with GB / T2410. The thicknesses of the polypropylene samples were 1 mm and 2 mm, and each set of data was tested 5 times and the average value was taken.

[0065] The morphology and size of the copolymer microspheres were observed and measured using an Axia ChemiSEMLoVAC scanning electron microscope manufactured by Thermo Fisher Scientific.

[0066] The glass transition temperature of the copolymer microspheres was measured using a differential scanning calorimeter (DSC 1) manufactured by Mettler Toledo, Switzerland.

[0067] The heat distortion temperature of polypropylene was tested using an HV6M heat distortion Vicat tester manufactured by Instron according to ISO-75 standard, with each set of data being tested 5 times and the average value taken.

[0068] The white spots on the sample were observed directly with the naked eye.

[0069] Preparation Example 1

[0070] 500 ml of isoamyl acetate was placed in a 1000 ml three-necked flask, and nitrogen gas was purged for 30 min to remove oxygen. 24.5 g of maleic anhydride and 26 g of styrene were added to the flask. After complete dissolution, 0.4 g of azobisisobutyronitrile (AIBN) was added, and the water bath temperature was raised to 70 °C, and the reaction was carried out for 7 h. After the reaction, the mixture was centrifuged at 10000 rpm for 10 min, the supernatant was removed, 500 ml of methanol was added, and the mixture was stirred for 0.5 h. After centrifugation, the supernatant was removed, and this process was repeated twice. Then, the mixture was vacuum dried at 140 °C for 24 h to obtain a styrene-maleic anhydride copolymer. The styrene-maleic anhydride copolymer microspheres, based on the total molar amount of each structural unit of the copolymer, have a maleic anhydride structural unit molar content of 50 mol% and a styrene structural unit molar content of 50 mol%. The particle size of the styrene-maleic anhydride copolymer microspheres is 800-1400 nm.

[0071] Preparation Example 2

[0072] The styrene-maleic anhydride copolymer was prepared using the same method as in Preparation Example 1, except that "isoamyl acetate" was replaced with "a mixed solvent of hexane and acetone, with a weight ratio of hexane to acetone of 2:1", resulting in the styrene-maleic anhydride copolymer; wherein, based on the total molar amount of each structural unit in the copolymer, the molar content of maleic anhydride structural units in the styrene-maleic anhydride copolymer microspheres is 50 mol%, the molar content of styrene structural units is 50 mol%, and the particle size of the styrene-maleic anhydride copolymer microspheres is 800-1300 nm.

[0073] Figure 1 Here are SEM images of the surface morphology of the styrene-maleic anhydride copolymer microspheres prepared in Example 2. Figure 1As can be seen from the test results, the copolymer microspheres prepared in Preparation Example 2 are mostly 0.8-1.3 μm in size, have smooth and uncontaminated surfaces, and have a particle size larger than the wavelength of visible light, so they can be used as a light diffusing agent for polypropylene.

[0074] Figure 2 This is a DSC curve of the styrene-maleic anhydride copolymer microspheres prepared in Example 2. Figure 2 Test results show that the glass transition temperature of the copolymer microspheres is about 215℃. The higher glass transition temperature can increase the heat distortion temperature of polypropylene and also ensure that polypropylene is not deformed by high-temperature shearing during processing.

[0075] Preparation Example 3

[0076] The styrene-maleic anhydride copolymer was prepared using the same method as in Preparation Example 1, except that "styrene" was replaced with "α-methylstyrene," resulting in an α-methylstyrene-maleic anhydride copolymer. In the α-methylstyrene-maleic anhydride copolymer microspheres, based on the total molar amount of each structural unit of the copolymer, the molar content of the maleic anhydride structural unit was 50 mol%, and the molar content of the α-methylstyrene structural unit was 50 mol%. The particle size of the α-methylstyrene-maleic anhydride copolymer microspheres was 1000-1600 nm.

[0077] Preparation Example 4

[0078] The styrene-maleic anhydride copolymer was prepared using the same method as in Preparation Example 1, except that "styrene" was replaced with "isobutylene," resulting in an isobutylene-maleic anhydride copolymer. In the isobutylene-maleic anhydride copolymer microspheres, based on the total molar amount of each structural unit of the copolymer, the molar content of the maleic anhydride structural unit was 50 mol%, and the molar content of the isobutylene structural unit was 50 mol%. The particle size of the isobutylene-maleic anhydride copolymer microspheres was 700-1200 nm.

[0079] Example 1

[0080] This embodiment illustrates polypropylene with uniformly dispersed olefin maleic anhydride copolymer microspheres prepared using the composition and preparation method of the present invention.

[0081] The polypropylene composition comprises: 10 kg of Y26 polypropylene granules and 0.1 kg of No. 26 white oil (kinematic viscosity of 26 mmHg at 40°C). 2 The styrene-maleic anhydride copolymer microspheres obtained in Preparation Example 2 were also included (s) and 0.2 kg.

[0082] Methods for preparing polypropylene include:

[0083] 10 kg of Y26 polypropylene granules and 0.1 kg of No. 26 white oil (kinematic viscosity of 26 mmHg at 40°C) were mixed. 2 The styrene-maleic anhydride copolymer microspheres obtained in Preparation Example 2 were added to a small laboratory high-speed mixer and stirred at 2500 rpm for 1 min. Then, 0.2 kg of the styrene-maleic anhydride copolymer microspheres were added to the high-speed mixer and stirred at 3000 rpm for 2 min. The resulting polypropylene particles with copolymer microspheres adhering to their surface were taken out and melt-blended and granulated through a twin-screw extruder to obtain polypropylene particles with uniformly dispersed styrene-maleic anhydride copolymer microspheres. The granulated sheet material was then injected into test samples according to the standard for testing.

[0084] Figure 4 This is a photograph of a 1mm sheet made from the polypropylene prepared in Example 1. Figure 4 These are photographs of the actual objects taken with a camera, from... Figure 4 It can be seen that there are no white spots on the surface of the sheet, which suggests that the styrene-maleic anhydride copolymer microspheres are uniformly dispersed inside the polypropylene matrix.

[0085] Example 2

[0086] This embodiment illustrates polypropylene with uniformly dispersed olefin maleic anhydride copolymer microspheres prepared using the composition and preparation method of the present invention.

[0087] The polypropylene composition comprises: 10 kg of Y26 polypropylene granules and 0.15 kg of No. 15 white oil (kinematic viscosity of 15 mm at 40°C). 2 / s) and 0.3 kg of styrene-maleic anhydride copolymer microspheres from Preparation Example 2.

[0088] Methods for preparing polypropylene include:

[0089] Polypropylene was prepared using the same method as in Example 1, except that "0.1 kg of No. 26 white oil" was replaced with "0.15 kg of No. 15 white oil (kinematic viscosity of 15 mmHg at 40°C)". 2 Replace “0.2 kg of styrene-maleic anhydride copolymer microspheres from Preparation Example 2” with “0.3 kg of styrene-maleic anhydride copolymer microspheres from Preparation Example 2” to obtain polypropylene particles with uniform dispersion of styrene-maleic anhydride copolymer microspheres. Inject the granulated sheet material into test samples according to the standard and test them.

[0090] Example 3

[0091] This embodiment illustrates polypropylene with uniformly dispersed olefin maleic anhydride copolymer microspheres prepared using the composition and preparation method of the present invention.

[0092] The polypropylene composition comprises: 10 kg of Y26 polypropylene granules and 0.35 kg of No. 68 white oil (kinematic viscosity of 68 mmHg at 40°C). 2 / s) and 0.15 kg of styrene-maleic anhydride copolymer microspheres from Preparation Example 2.

[0093] Methods for preparing polypropylene include:

[0094] Polypropylene was prepared using the same method as in Example 1, except that "0.1 kg of No. 26 white oil" was replaced with "0.35 kg of No. 68 white oil (kinematic viscosity of 68 mmHg at 40°C)". 2 Replace “0.2 kg of styrene-maleic anhydride copolymer microspheres from Preparation Example 2” with “0.15 kg of styrene-maleic anhydride copolymer microspheres from Preparation Example 2” to obtain polypropylene particles with uniform dispersion of styrene-maleic anhydride copolymer microspheres. Inject the granulated sheet material into test samples according to the standard and test them.

[0095] Example 4

[0096] This embodiment illustrates polypropylene with uniformly dispersed olefin maleic anhydride copolymer microspheres prepared using the composition and preparation method of the present invention.

[0097] The polypropylene composition comprises: 10 kg of Y26 polypropylene granules and 0.05 kg of No. 46 white oil (kinematic viscosity of 46 mmHg at 40°C). 2 / s) and 0.05 kg of styrene-maleic anhydride copolymer microspheres from Preparation Example 2.

[0098] Methods for preparing polypropylene include:

[0099] Polypropylene was prepared using the same method as in Example 1, except that "0.1 kg of No. 26 white oil" was replaced with "0.05 kg of No. 46 white oil (kinematic viscosity of 46 mmHg at 40°C)". 2 Replace “0.2 kg of styrene-maleic anhydride copolymer microspheres from Preparation Example 2” with “0.05 kg of styrene-maleic anhydride copolymer microspheres from Preparation Example 2”, replace the speed and time of the laboratory mini high-speed mixer from “2500 rpm for 1 min” to “4000 rpm for 1.5 min”, and replace the speed and time of the laboratory mini high-speed mixer after adding the styrene-maleic anhydride copolymer microspheres from “3000 rpm for 2 min” to “4000 rpm for 1.5 min”. This will result in polypropylene particles with uniform dispersion of styrene-maleic anhydride copolymer microspheres. The granulated sheet material will be injected into test samples according to the standard for testing.

[0100] Example 5

[0101] This embodiment illustrates polypropylene with uniformly dispersed olefin maleic anhydride copolymer microspheres prepared using the composition and preparation method of the present invention.

[0102] The polypropylene composition comprises: 10 kg of Y26 polypropylene granules and 0.1 kg of No. 5 white oil (kinematic viscosity of 5 mm at 40°C). 2 / s) and 0.1 kg of No. 100 white oil (kinematic viscosity of 100 mm at 40°C) 2 The mixture of ( / s) and 0.4 kg of the styrene-maleic anhydride copolymer microspheres of Preparation Example 2.

[0103] Methods for preparing polypropylene include:

[0104] Polypropylene was prepared using the same method as in Example 1, except that "0.1 kg of No. 26 white oil" was replaced with "0.1 kg of No. 5 white oil (kinematic viscosity of 5 mm at 40°C)". 2 / s) and 0.1 kg of No. 100 white oil (kinematic viscosity of 100 mm at 40°C) 2 The mixture was prepared by replacing "0.2 kg of styrene-maleic anhydride copolymer microspheres from Preparation Example 2" with "0.4 kg of styrene-maleic anhydride copolymer microspheres from Preparation Example 2". Polypropylene particles with uniform dispersion of styrene-maleic anhydride copolymer microspheres were obtained. The granulated sheet material was then injected into test samples according to the standard for testing.

[0105] Example 6

[0106] This embodiment illustrates polypropylene with uniformly dispersed olefin maleic anhydride copolymer microspheres prepared using the composition and preparation method of the present invention.

[0107] The polypropylene composition comprises: 10 kg of Y26 polypropylene granules and 0.05 kg of No. 10 white oil (kinematic viscosity of 10 mmHg at 40°C). 2 The styrene-maleic anhydride copolymer microspheres obtained in Preparation Example 1 were also prepared in 0.03 kg (s) and 0.03 kg (s).

[0108] Methods for preparing polypropylene include:

[0109] Polypropylene was prepared using the same method as in Example 1, except that "0.1 kg of No. 26 white oil" was replaced with "0.05 kg of No. 10 white oil (kinematic viscosity of 10 mmHg at 40°C)". 2 Replace “0.2 kg of styrene-maleic anhydride copolymer microspheres obtained in Preparation Example 2” with “0.03 kg of styrene-maleic anhydride copolymer microspheres obtained in Preparation Example 1”, and you will get polypropylene particles with styrene-maleic anhydride copolymer microspheres uniformly dispersed. The granulated sheet material is then injected into test samples according to the standard for testing.

[0110] Example 7

[0111] This embodiment illustrates polypropylene with uniformly dispersed olefin maleic anhydride copolymer microspheres prepared using the composition and preparation method of the present invention.

[0112] The polypropylene composition comprises: 10 kg of Y26 polypropylene powder and 0.3 kg of No. 46 white oil (kinematic viscosity of 46 mmHg at 40°C). 2 The styrene-maleic anhydride copolymer microspheres obtained in Preparation Example 2 were also prepared in 0.1 kg (s) and 0.1 kg (s).

[0113] Methods for preparing polypropylene include:

[0114] Polypropylene was prepared using the same method as in Example 1, except that "10 kg Y26 polypropylene granules" was replaced with "10 kg Y26 polypropylene powder", and "0.1 kg No. 26 white oil" was replaced with "0.3 kg No. 46 white oil (kinematic viscosity of 46 mmHg at 40°C)". 2 Replace “0.2 kg of styrene-maleic anhydride copolymer microspheres obtained in Preparation Example 2” with “0.1 kg of styrene-maleic anhydride copolymer microspheres obtained in Preparation Example 2”, and add 0.02 kg of antioxidant 225 at the same time. This will result in polypropylene particles with styrene-maleic anhydride copolymer microspheres uniformly dispersed. The granulated sheet material will be injected into test samples according to the standard for testing.

[0115] Example 8

[0116] This embodiment illustrates polypropylene with uniformly dispersed olefin maleic anhydride copolymer microspheres prepared using the composition and preparation method of the present invention.

[0117] The polypropylene composition comprises: 10 kg of T03 polypropylene granules and 0.1 kg of No. 26 white oil (kinematic viscosity of 26 mm at 40°C). 2 The styrene-maleic anhydride copolymer microspheres obtained in Preparation Example 2 were also included (s) and 0.2 kg.

[0118] Methods for preparing polypropylene include:

[0119] Polypropylene was prepared using the same method as in Example 1, except that "10 kg of Y26 polypropylene granules in Example 1" was replaced with "10 kg of T03 polypropylene granules". This resulted in polypropylene particles with polystyrene-maleic anhydride copolymer microspheres uniformly dispersed. The granulated sheet material was then injected into test samples according to standards for testing.

[0120] Example 9

[0121] This embodiment illustrates polypropylene with uniformly dispersed olefin maleic anhydride copolymer microspheres prepared using the composition and preparation method of the present invention.

[0122] The polypropylene composition comprises: 10 kg of M60ET polypropylene granules and 0.1 kg of No. 26 white oil (kinematic viscosity of 26 mm at 40°C). 2 The styrene-maleic anhydride copolymer microspheres obtained in Preparation Example 2 were also included (s) and 0.2 kg.

[0123] Methods for preparing polypropylene include:

[0124] Polypropylene was prepared using the same method as in Example 1, except that “Y26 polypropylene granules” was replaced with “M60ET polypropylene granules”, resulting in polypropylene particles with uniformly dispersed styrene-maleic anhydride copolymer microspheres. The granulated sheet material was then injected into test samples according to standards for testing.

[0125] Example 10

[0126] This embodiment illustrates polypropylene with uniformly dispersed olefin maleic anhydride copolymer microspheres prepared using the composition and preparation method of the present invention.

[0127] The polypropylene composition comprises: 10 kg of Y26 polypropylene granules and 0.5 kg of No. 32 white oil (kinematic viscosity of 32 mm at 40°C). 2 The styrene-maleic anhydride copolymer microspheres obtained in Preparation Example 2 were also prepared in 0.8 kg (s) and 0.8 kg (s).

[0128] Methods for preparing polypropylene include:

[0129] Polypropylene was prepared using the same method as in Example 1, except that: "0.1 kg of No. 26 white oil" was replaced with "0.5 kg of No. 32 white oil", "0.2 kg of styrene-maleic anhydride copolymer microspheres prepared in Preparation Example 2" was replaced with "0.8 kg of styrene-maleic anhydride copolymer microspheres prepared in Preparation Example 2", and "stirring at 2500 rpm for 1 min using a laboratory small high-speed mixer" was replaced with "stirring at 10000 rpm for 3 min". After adding the styrene-maleic anhydride copolymer microspheres, "stirring at 3000 rpm for 2 min using a laboratory small high-speed mixer" was replaced with "stirring at 10000 rpm for 5 min". This resulted in polypropylene particles with uniformly dispersed styrene-maleic anhydride copolymer microspheres. The granulated sheet material was then injected into test samples according to standards for testing.

[0130] Example 11

[0131] This embodiment illustrates polypropylene with uniformly dispersed olefin maleic anhydride copolymer microspheres prepared using the composition and preparation method of the present invention.

[0132] The polypropylene composition comprises: 10 kg of Y26 polypropylene granules and 0.1 kg of No. 26 white oil (kinematic viscosity of 26 mmHg at 40°C). 2 / s) and 0.1 kg of the α-methylstyrene maleic anhydride copolymer microspheres obtained in Preparation Example 3.

[0133] Methods for preparing polypropylene include:

[0134] Polypropylene was prepared using the same method as in Example 1, except that "0.2 kg of styrene-maleic anhydride copolymer microspheres prepared in Preparation Example 2" was replaced with "0.1 kg of α-methylstyrene-maleic anhydride copolymer microspheres obtained in Preparation Example 3". Polypropylene particles with uniform dispersion of α-methylstyrene-maleic anhydride copolymer microspheres were obtained. The granulated sheet material was injected into test samples according to the standard for testing.

[0135] Example 12

[0136] This embodiment illustrates polypropylene with uniformly dispersed olefin maleic anhydride copolymer microspheres prepared using the composition and preparation method of the present invention.

[0137] The polypropylene composition comprises: 10 kg of Y26 polypropylene granules and 0.1 kg of No. 26 white oil (kinematic viscosity of 26 mmHg at 40°C). 2 / s) and 0.1 kg of the isobutylene maleic anhydride copolymer microspheres obtained in Preparation Example 4.

[0138] Methods for preparing polypropylene include:

[0139] Polypropylene was prepared using the same method as in Example 1, except that "0.2 kg of styrene-maleic anhydride copolymer microspheres prepared in Preparation Example 2" was replaced with "0.1 kg of isobutylene-maleic anhydride copolymer microspheres obtained in Preparation Example 4". Polypropylene particles with uniform dispersion of isobutylene-maleic anhydride copolymer microspheres were obtained. The granulated sheet material was injected into test samples according to the standard for testing.

[0140] Comparative Example 1

[0141] The polypropylene composition comprises: 10 kg of Y26 polypropylene granules and 1 kg of styrene-maleic anhydride copolymer microspheres obtained in Preparation Example 2.

[0142] Methods for preparing polypropylene include:

[0143] 10 kg of Y26 polypropylene granules and 1 kg of styrene-maleic anhydride copolymer microspheres were added to a small laboratory high-speed mixer and stirred at 5000 rpm for 10 min. The mixture was then removed and melt-extruded into granules on a twin-screw extruder. As a result, polypropylene particles containing copolymer microspheres could not be obtained because the two could not be mixed evenly.

[0144] Comparative Example 2

[0145] The polypropylene composition comprises: 10 kg of Y26 polypropylene granules and 0.2 kg of styrene-maleic anhydride copolymer microspheres obtained in Preparation Example 2.

[0146] Methods for preparing polypropylene include:

[0147] 10 kg of Y26 polypropylene granules and 0.2 kg of styrene-maleic anhydride copolymer microspheres were fed into the main side feed port of a twin-screw extruder. After melt extrusion granulation, the granulated material was injected into test samples according to standards for testing.

[0148] Figure 3 This is a photograph of a 1mm polypropylene sample prepared in Comparative Example 2. Figure 3 It can be seen that directly blending styrene-maleic anhydride copolymer microspheres with polypropylene produces a large number of white spots, indicating that the styrene-maleic anhydride copolymer microspheres are not uniformly dispersed in polypropylene.

[0149] Comparative Example 3

[0150] The polypropylene composition comprises: 10 kg of Y26 polypropylene granules and 0.1 kg of No. 26 white oil (kinematic viscosity of 26 mmHg at 40°C). 2 The styrene-maleic anhydride copolymer microspheres prepared in Example 2 were also prepared in 3 kg (s) and 3 kg (s).

[0151] Methods for preparing polypropylene include:

[0152] Polypropylene was prepared using the same method as in Example 1, except that "0.2 kg of styrene-maleic anhydride copolymer microspheres prepared in Preparation Example 2" was replaced with "3 kg of styrene-maleic anhydride copolymer microspheres prepared in Preparation Example 2" to obtain polypropylene particles containing styrene-maleic anhydride copolymer microspheres. The granulated material was then injected into test samples according to standards for testing.

[0153] Comparative Example 4

[0154] The polypropylene composition comprises: 10 kg of Y26 polypropylene granules and 0.03 kg of No. 26 white oil (kinematic viscosity of 26 mmHg at 40°C). 2 The styrene-maleic anhydride copolymer microspheres obtained in Preparation Example 2 were also included (s) and 0.2 kg.

[0155] Methods for preparing polypropylene include:

[0156] Polypropylene was prepared using the same method as in Example 1, except that "0.1 kg of No. 26 white oil" was replaced with "0.03 kg of No. 26 white oil" to obtain polypropylene particles containing styrene-maleic anhydride copolymer microspheres. The granulated material was then injected into test samples according to standards for testing.

[0157] Comparative Example 5

[0158] The polypropylene composition comprises: 10 kg of Y26 polypropylene granules and 1 kg of No. 26 white oil (kinematic viscosity of 26 mm at 40°C). 2 The styrene-maleic anhydride copolymer microspheres obtained in Preparation Example 2 were also included (s) and 0.2 kg.

[0159] Methods for preparing polypropylene include:

[0160] Polypropylene was prepared using the same method as in Example 1, except that "0.1 kg of No. 26 white oil" was replaced with "1 kg of No. 26 white oil". It was found that there was too much white oil, and after coating the particles, a large amount of residue caused the olefin maleic anhydride copolymer microspheres to clump together, causing blockage after entering the screw and making extrusion granulation impossible.

[0161] Test case

[0162] Table 1 lists the surface white spots on 1 mm and 2 mm samples prepared from polypropylene using Examples 1-12 and Comparative Examples 1-5.

[0163] The haze, transmittance, and heat distortion temperature of 1 mm and 2 mm polypropylene samples prepared using Examples 1-12 and Comparative Examples 1-5 are listed in Table 2.

[0164] Table 1

[0165]

[0166]

[0167] Note: "-" in the table indicates that the component is not present, that is, the amount added is 0.

[0168] Table 2

[0169]

[0170]

[0171] It should be noted in Table 1 that "-" indicates that the test could not detect any data.

[0172] As can be seen from the results in Table 1, the polypropylene prepared by the present invention can uniformly disperse olefin maleic anhydride copolymer microspheres in the polypropylene matrix. Directly mixing olefin maleic anhydride copolymer microspheres with polypropylene cannot result in granulation. Side feeding through an extruder still leads to the generation of a large number of white spots. The polypropylene sheet prepared after using the white oil of the present invention has no white spots on its surface, and the preferred solution has significantly better results.

[0173] As can be seen from the results in Table 2, the polypropylene prepared using styrene-maleic anhydride copolymer microspheres, white oil, and polypropylene has good light diffusion effect, achieving both high haze and high light transmittance, and also has a high heat distortion temperature.

[0174] The preferred embodiments of the present invention have been described in detail above; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various technical features in any other suitable manner. These simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.

Claims

1. A polypropylene composition, characterized in that, The polypropylene composition comprises a polypropylene matrix, olefin maleic anhydride copolymer microspheres, and white oil, wherein the content of the olefin maleic anhydride copolymer microspheres is 0.1-10 parts by weight relative to 100 parts by weight of the polypropylene matrix, and the content of the white oil is 0.5-8 parts by weight.

2. The composition according to claim 1, wherein, The content of the olefin maleic anhydride copolymer microspheres is 0.5-5 parts by weight relative to 100 parts by weight of the polypropylene matrix, and the content of the white oil is 0.5-4 parts by weight.

3. The composition according to claim 2, wherein, The content of the olefin maleic anhydride copolymer microspheres is 2-4 parts by weight relative to 100 parts by weight of the polypropylene matrix, and the content of the white oil is 0.8-3 parts by weight.

4. The composition according to claim 1, wherein, In the olefin-maleic anhydride copolymer microspheres, based on the total molar amount of each structural unit in the copolymer, the molar content of the maleic anhydride structural unit is 40-50 mol%, and the molar content of the olefin structural unit is 50-60 mol%.

5. The composition according to claim 4, wherein, In the olefin-maleic anhydride copolymer microspheres, based on the total molar amount of each structural unit of the copolymer, the molar content of the maleic anhydride structural unit is 45-50 mol%, and the molar content of the olefin structural unit is 50-55 mol%.

6. The composition according to claim 1, wherein, The particle size of the olefin maleic anhydride copolymer microspheres is 500-2000 nm.

7. The composition according to any one of claims 1-6, wherein, The method for preparing the olefin-maleic anhydride copolymer microspheres includes: reacting olefin, maleic anhydride and solvent in the presence of an initiator to obtain olefin-maleic anhydride copolymer microspheres.

8. The composition according to claim 7, wherein, The initiator is azobisisobutyronitrile and / or azobisisoheptanenitrile; And / or, the solvent is a mixture of isoamyl acetate or hexaneacetone; And / or, the reaction conditions include: a temperature of 45-100°C and a time of 60-600 min.

9. The composition according to any one of claims 1-6, wherein, The olefin maleic anhydride copolymer microspheres contain olefins that are C4-C9 olefins.

10. The composition according to claim 9, wherein, The olefin in the olefin maleic anhydride copolymer microspheres is one or more of styrene maleic anhydride copolymer microspheres, α-methylstyrene maleic anhydride copolymer microspheres, and isobutylene maleic anhydride copolymer microspheres.

11. The composition according to claim 10, wherein, The olefin in the olefin-maleic anhydride copolymer microspheres is styrene-maleic anhydride copolymer microspheres.

12. The composition according to claim 1, wherein, The polypropylene matrix has a melt flow index of 2-70 g / 10 min at 230°C and 2.16 kg. And / or, the kinematic viscosity of the white oil at 40°C is 5-100 mm. 2 / s.

13. The composition according to claim 12, wherein, The polypropylene matrix has a melt flow index of 25-60 g / 10 min at 230°C and 2.16 kg. And / or, the kinematic viscosity of the white oil at 40°C is 20-70 mm. 2 / s.

14. The composition according to claim 13, wherein, The polypropylene matrix has a melt index of 25-27 g / 10 min at 230°C and 2.16 kg.

15. A method for preparing polypropylene using the polypropylene composition according to any one of claims 1-14, characterized in that, The method includes: (1) The polypropylene matrix is ​​brought into contact with white oil for the first mixing; (2) The polypropylene coated with white oil obtained in step (1) is brought into contact with olefin maleic anhydride copolymer microspheres for a second mixing. (3) Polypropylene is obtained by melt blending the mixture obtained in step (2).

16. The method according to claim 15, wherein, The conditions for the first mixing include mixing at a temperature of -20°C to 60°C for 0.1-30 minutes; And / or, the conditions for the second mixing include: mixing at a temperature of -20°C to 60°C for 0.1-10 min.

17. A polypropylene prepared by the method of claim 15 or 16.

18. The polypropylene according to claim 17, wherein, The heat distortion temperature of the polypropylene is ≥50℃, and the light transmittance of the 1mm sample is ≥40%, and the haze is ≥60%.

19. The polypropylene according to claim 18, wherein, The heat distortion temperature of the polypropylene is 80-120℃, and the light transmittance of the 1mm sample is 60-95%, and the haze is 70-100%.

20. The polypropylene according to any one of claims 17-19, wherein, The sheet products prepared using the polypropylene described above have no white spots on their surface.

21. A lighting body, characterized in that, The material used to prepare the illuminator includes polypropylene, wherein the polypropylene is the polypropylene as described in any one of claims 17-20.

22. The illuminator according to claim 21, wherein, The lighting element is an LED light.