CN112143103A - Cage-type silsesquioxane modified polypropylene composite material and preparation method thereof - Google Patents
Cage-type silsesquioxane modified polypropylene composite material and preparation method thereof Download PDFInfo
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- CN112143103A CN112143103A CN202011021812.6A CN202011021812A CN112143103A CN 112143103 A CN112143103 A CN 112143103A CN 202011021812 A CN202011021812 A CN 202011021812A CN 112143103 A CN112143103 A CN 112143103A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/24—Crystallisation aids
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Abstract
The invention discloses a cage type silsesquioxane modified polypropylene composite material which is prepared from the following components in parts by weight: 0.1-10 parts of cage type silsesquioxane, 89-99.8 parts of polypropylene and 0.1-1 part of antioxidant; the structural formula of the cage-type silsesquioxane is one of the following structural formulas:
Description
Technical Field
The invention belongs to the technical field of modification of high polymer materials, and particularly relates to a polyhedral oligomeric silsesquioxane (POSS) modified polypropylene composite material and a preparation method thereof.
Background
Polypropylene is a common thermoplastic resin, and is widely used in various fields of life due to its excellent properties. However, polypropylene plastics also have some performance defects, and in order to further expand the application fields, the polypropylene plastics are generally required to be modified. The nucleating agent modification has been widely concerned in the industrial and scientific research fields because of the advantages of simple processing, remarkable and stable effect, simplicity, flexibility and the like. Polypropylene is a semi-crystalline polymer, and its crystallization speed affects its production cycle, crystal size, and thus other properties of polypropylene. Increasing the crystallization rate of polypropylene has become a hot spot for research in industry and academia. The addition of the nucleating agent can effectively improve the crystallization temperature, so that the supercooling degree of the polymer is improved in the actual processing process, and the crystallization speed of the polymer is effectively improved.
Cage type silsesquioxane (POSS) is a nano organic-inorganic hybrid material. The surface of the POSS has organic groups with extremely strong structural design, and the application of POSS in various fields is increased. Due to the ultra-strong structure designability, POSS containing certain special functions can be used as a nucleating agent of a semi-crystalline polymer, the crystallization process is accelerated, and the processing performance of the semi-crystalline polymer is improved.
Disclosure of Invention
The invention aims to provide a cage type silsesquioxane modified polypropylene composite material.
The second purpose of the invention is to provide a preparation method of the cage type silsesquioxane modified polypropylene composite material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a cage type silsesquioxane modified polypropylene composite material, which is prepared from the following components in parts by weight: 0.1-10 parts of cage type silsesquioxane, 89-99.8 parts of polypropylene and 0.1-1 part of antioxidant;
the structural formula of the cage-type silsesquioxane (POSS) is one or more of the following structural formulas:
R1、R2、R3、R4、R5、R6、R7、R8、R9、R10、R11、R12each independently selected from H, C1-18At least one of alkyl, phenyl, vinyl, epoxy, cyclohexyl, sodium ion, lithium ion, and potassium ion.
The cage type silsesquioxane modified polypropylene composite material is prepared from the following components in parts by weight:
2 parts of cage type silsesquioxane, 97.8 parts of polypropylene and 0.2 part of antioxidant;
or 3 parts of cage type silsesquioxane, 96.8 parts of polypropylene and 0.2 part of antioxidant.
The polypropylene is homo-polypropylene or co-polypropylene.
The molecular weight of the homo-or co-polypropylene is (1-100) x 104g·mol-1The Polymer Dispersion Index (PDI) is from 2 to 30 and the Melt Flow Index (MFI) is from 1 to 100g/10min (230 ℃ C., 2.16 Kg).
The antioxidant is a mixture of an antioxidant 1010 and an antioxidant 168, and the weight part ratio of the antioxidant 1010 to the antioxidant 168 is 1: 1.
The second aspect of the invention provides a preparation method of the cage-type silsesquioxane modified polypropylene composite material, which comprises the following steps: melting, mixing and extruding the cage-type silsesquioxane, the polypropylene and the antioxidant on a double-screw extruder according to the proportion, granulating and carrying out injection molding to obtain the cage-type silsesquioxane modified polypropylene composite material.
The melting, mixing and extruding adopts seven-stage heating, the temperature is 160-270 ℃, the temperature of each stage is preferably 190 ℃, 200 ℃, 190 ℃, and the feeding rotating speed and the main engine rotating speed are respectively 20-200 revolutions/min and 20-200 revolutions/min; preferably, the feeding speed and the main machine speed are respectively 20 revolutions per minute and 200 revolutions per minute.
The temperature of each injection molding section is 180 ℃, 210 ℃ and 220 ℃, the injection molding time is 15s, the pressure is maintained for 15s, and the cooling is 25 s.
Due to the adoption of the technical scheme, the invention has the following advantages and beneficial effects:
the cage type silsesquioxane modified polypropylene composite material effectively improves the crystallization property of polypropylene. The polyhedral oligomeric silsesquioxane serves as a nucleating agent of a matrix, so that the nucleating efficiency of the polypropylene is greatly improved, the crystallization rate of the polypropylene is increased, and the crystallization temperature of the polypropylene can be increased by 1-15 ℃ when the addition amount of the polyhedral oligomeric silsesquioxane is 0.1-10 wt%.
The cage type silsesquioxane modified polypropylene composite material greatly improves the crystallization temperature of polypropylene, promotes the crystallization of polypropylene and improves the mechanical property of polypropylene.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
The crystallization behavior of polypropylene is characterized by a Differential Scanning Calorimeter (DSC). The test atmosphere was nitrogen and the samples weighed 3-5 mg. The test procedure was as follows: heating to 200 ℃ at a speed of 10 ℃/min, and keeping the temperature for 5min to eliminate the thermal history of the sample. Then the temperature is reduced to 50 ℃ at the speed of 10 ℃/min to obtain the crystallization curve of the polypropylene. The flexural modulus in the examples of the present invention was injection-molded according to the ASTM D-638 standard (type I was used for the sample specification), and the tensile strength was injection-molded and tested according to the ASTM D-638 standard. The characterization of the heat distortion temperature is tested according to ISO75-2, and the heat distortion temperature is measured in a flat placing mode, the heating rate is 2 ℃/mm, and the load is 0.45 MPa.
The raw material used in the embodiment of the invention is homo-polypropylene or co-polypropylene with the molecular weight of (1-100) x 104g·mol-1The Polymer Dispersion Index (PDI) is from 2 to 30 and the Melt Flow Index (MFI) is from 1 to 100g/10min (230 ℃ C., 2.16 Kg).
The structural formula of the cage-type silsesquioxane (POSS) used in the embodiment of the invention is one or more of the following structural formulas:
R1、R2、R3、R4、R5、R6、R7、R8、R9、R10、R11、R12each independently selected from H, C1-18At least one of alkyl, phenyl, vinyl, epoxy, cyclohexyl, sodium ion, lithium ion, and potassium ion.
Example 1
2 parts by weight of heptapolymethyltriol lithium polyhedral oligomeric silsesquioxane (POSS) (the structure is 2 in the structural formula 1-8 of the polyhedral oligomeric silsesquioxane, wherein a substituent R1-7Is methyl, R8-10The preparation method comprises the following steps of (1) melting, mixing and extruding, granulating and injection molding for lithium ions purchased from hybrid plastics company of America under the product number of SO1457), 0.1 part by weight of antioxidant 1010, 0.1 part by weight of antioxidant 168 and 97.8 parts by weight of homopolymerized polypropylene on a double-screw extruder to obtain the cage-type silsesquioxane modified polypropylene composite material, wherein the melting, mixing and extruding adopts seven-section heating, the temperature of each section is 190 ℃, 200 ℃, 190 ℃, and the feeding rotating speed and the main machine rotating speed are respectively 20 revolutions/min and 200 revolutions/min; the temperature of each injection molding section is 180 ℃, 210 ℃ and 220 ℃, the injection molding time is 15s, the pressure is maintained for 15s, and the cooling is 25 s.
Example 2
1 part by weight of heptamethicone lithium polyhedral oligomeric silsesquioxane (POSS) (the structure is 2 in the structural formula 1-8 of the polyhedral oligomeric silsesquioxane, wherein a substituent R1-7Is methyl, R8-10Is lithium ion, purchased from hybrid plastics of America under the product number SO1457, 1 part by weight of heptapoly cyclohexyl trisilol cage type silsesquioxane (the structure of the cage type silsesquioxane is 2 in the structural formula 1-8, wherein the substituent R is1-7Is cyclohexyl, R8-10H, purchased from hybrid plastics company of America under the product number of MS0830), 0.1 part by weight of antioxidant 1010, 0.1 part by weight of antioxidant 168 and 97.8 parts by weight of homopolymerized polypropylene are melted, mixed, extruded and granulated on a double-screw extruder to obtain the cage-type silsesquioxane modified polypropylene composite materialThe material is prepared by adopting seven-section heating in the melting, mixing and extruding process, wherein the temperature of each section is 190 ℃, 200 ℃, 190 ℃, and the feeding rotating speed and the main machine rotating speed are respectively 20 revolutions per minute and 200 revolutions per minute; the temperature of each injection molding section is 180 ℃, 210 ℃ and 220 ℃, the injection molding time is 15s, the pressure is maintained for 15s, and the cooling is 25 s.
Example 3
2 parts by weight of heptapolymethyltriol lithium polyhedral oligomeric silsesquioxane (POSS) (the structure is 2 in the structural formula 1-8 of the polyhedral oligomeric silsesquioxane, wherein a substituent R1-7Is methyl, R8-10Is lithium ion, purchased from hybrid plastics of America under the product number SO1457, 1 weight part of hexa-phenyl trisilol cage type silsesquioxane (the structure of the cage type silsesquioxane is 3 in the structural formula 1-8, wherein the substituent R is1-8Is phenyl, R9-12H, purchased from hybrid plastics company of America, with the product number of SO1460), 0.1 part by weight of antioxidant 1010, 0.1 part by weight of antioxidant 168 and 96.8 parts by weight of homopolymerized polypropylene are melted, mixed and extruded on a double-screw extruder, and then are granulated and injected to obtain the cage-type silsesquioxane modified polypropylene composite material, wherein the melting, mixing and extrusion adopts seven-section heating, the temperature of each section is 190 ℃, 200 ℃, 190 ℃, and the feeding speed and the main engine speed are respectively 20 revolutions per minute and 200 revolutions per minute; the temperature of each injection molding section is 180 ℃, 210 ℃ and 220 ℃, the injection molding time is 15s, the pressure is maintained for 15s, and the cooling is 25 s.
Comparative example 1
Melting, mixing and extruding 0.1 part by weight of antioxidant 1010, 0.1 part by weight of antioxidant 168 and 99.8 parts by weight of homopolymerized polypropylene on a double-screw extruder, granulating and injecting to obtain a homopolymerized polypropylene compound, wherein the melting, mixing and extruding adopts seven-section heating, the temperature of each section is 190 ℃, 200 ℃, 190 ℃, and the feeding rotating speed and the main machine rotating speed are respectively 20 revolutions per minute and 200 revolutions per minute; the temperature of each injection molding section is 180 ℃, 210 ℃ and 220 ℃, the injection molding time is 15s, the pressure is maintained for 15s, and the cooling is 25 s.
The crystallization behavior and mechanical properties of examples 1 to 3 and comparative example 1 are shown in Table 1:
TABLE 1
As can be seen from the data in Table 1, the crystallization temperature of examples 1 to 3 is increased compared with that of comparative example 1, the supercooling degree required by crystallization is reduced, the flexural modulus and the tensile strength of examples 1 to 3 are increased compared with that of comparative example 1, and the cage-type silsesquioxane modified polypropylene composite material prepared in the embodiment of the invention can promote the crystallization of polypropylene, can effectively regulate and control the crystallization process of polypropylene, and is a high-efficiency nucleating agent.
Comparative example 2
Example 1 of the patent application with publication number CN103571057A as comparative example 2 is as follows:
100 parts of homopolymerized polypropylene, 0.004 part of nucleating agent eight (2, 2' -methylene-bis (4, 6-di-tert-butylphenol)) ethyl ammonium phosphate cage type silsesquioxane, 0.1 part of antioxidant 1010 and 0.1 part of antioxidant 168 are uniformly mixed in a high-speed mixer for 3 minutes, the obtained mixture is melted and blended in a double-screw extruder, cooled and cut into granules, and standard sample strips are prepared by an injection molding method, wherein the properties are shown in Table 2.
TABLE 2
As can be seen from the experimental data of comparative example 2 in Table 2 and examples 1 to 3 and comparative example 1 in Table 1, the effect of the present invention is superior to that of the prior patent, and the tensile strength, flexural modulus and heat distortion temperature of polypropylene are greatly improved.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The cage type silsesquioxane modified polypropylene composite material is characterized by being prepared from the following components in parts by weight: 0.1-10 parts of cage type silsesquioxane, 89-99.8 parts of polypropylene and 0.1-1 part of antioxidant;
the structural formula of the cage-type silsesquioxane is one or more of the following structural formulas:
R1、R2、R3、R4、R5、R6、R7、R8、R9、R10、R11、R12each independently selected from H, C1-18At least one of alkyl, phenyl, vinyl, epoxy, cyclohexyl, sodium ion, lithium ion, and potassium ion.
2. The cage type silsesquioxane modified polypropylene composite of claim 1, wherein the cage type silsesquioxane modified polypropylene composite is prepared from the following components in parts by weight:
2 parts of cage type silsesquioxane, 97.8 parts of polypropylene and 0.2 part of antioxidant.
3. The cage type silsesquioxane modified polypropylene composite of claim 1, wherein the cage type silsesquioxane modified polypropylene composite is prepared from the following components in parts by weight:
3 parts of cage type silsesquioxane, 96.8 parts of polypropylene and 0.2 part of antioxidant.
4. The cage silsesquioxane-modified polypropylene composite of claim 1, wherein the polypropylene is a homo-polypropylene or a co-polypropylene.
5. The cage type silsesquioxane-modified polypropylene composite according to claim 4, wherein the homo-or co-polypropylene has a molecular weight of (1-100) x 104g·mol-1The polymer has a dispersity index of 2-30 and a melt flow index of 1-100g/10 min.
6. The cage-type silsesquioxane modified polypropylene composite material as claimed in claim 1, wherein the antioxidant is a mixture of an antioxidant 1010 and an antioxidant 168, and the weight part ratio of the antioxidant 1010 to the antioxidant 168 is 1: 1.
7. A method for preparing the cage type silsesquioxane modified polypropylene composite material as claimed in any one of claims 1 to 6, wherein the method comprises the following steps: melting, mixing and extruding the cage-type silsesquioxane, the polypropylene and the antioxidant on a double-screw extruder according to the proportion, granulating and carrying out injection molding to obtain the cage-type silsesquioxane modified polypropylene composite material.
8. The preparation method of the cage-type silsesquioxane modified polypropylene composite material as claimed in claim 7, wherein the melt mixing extrusion is performed by heating in seven stages at 160-270 ℃, and the feeding speed and the main machine speed are 20-200 rpm and 20-200 rpm, respectively.
9. The method for preparing the polyhedral oligomeric silsesquioxane modified polypropylene composite material as claimed in claim 8, wherein the melt mixing extrusion is performed by heating in seven stages at 190 ℃, 200 ℃, 190 ℃, and at 20 rpm and 200 rpm respectively.
10. The method for preparing the cage-type silsesquioxane modified polypropylene composite material according to claim 7, wherein the injection molding temperature of each stage is 180 ℃, 210 ℃, 220 ℃, the injection molding time is 15s, the pressure is maintained for 15s, and the cooling time is 25 s.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113502020A (en) * | 2021-08-06 | 2021-10-15 | 山东京博石油化工有限公司 | POSS/polypropylene foam material and preparation method thereof |
| CN113621194A (en) * | 2021-08-20 | 2021-11-09 | 安徽瑞琦塑胶科技有限公司 | Wear-resistant high-strength plastic particles produced by using waste plastics |
| CN116144102A (en) * | 2021-11-19 | 2023-05-23 | 广东中塑新材料有限公司 | High-toughness polypropylene material and preparation method thereof |
| CN116574329A (en) * | 2023-05-25 | 2023-08-11 | 博特尔包装(江苏)有限公司 | Preparation process of stretch-resistant polypropylene packaging film |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113502020A (en) * | 2021-08-06 | 2021-10-15 | 山东京博石油化工有限公司 | POSS/polypropylene foam material and preparation method thereof |
| CN113621194A (en) * | 2021-08-20 | 2021-11-09 | 安徽瑞琦塑胶科技有限公司 | Wear-resistant high-strength plastic particles produced by using waste plastics |
| CN116144102A (en) * | 2021-11-19 | 2023-05-23 | 广东中塑新材料有限公司 | High-toughness polypropylene material and preparation method thereof |
| CN116144102B (en) * | 2021-11-19 | 2024-05-28 | 广东中塑新材料有限公司 | High-toughness polypropylene material and preparation method thereof |
| CN116574329A (en) * | 2023-05-25 | 2023-08-11 | 博特尔包装(江苏)有限公司 | Preparation process of stretch-resistant polypropylene packaging film |
| CN116574329B (en) * | 2023-05-25 | 2023-12-08 | 博特尔包装(江苏)有限公司 | Preparation process of stretch-resistant polypropylene packaging film |
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Application publication date: 20201229 |