CN111040296B - Polyolefin composition with high mechanical property and preparation method thereof - Google Patents
Polyolefin composition with high mechanical property and preparation method thereof Download PDFInfo
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- 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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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/045—Polysiloxanes containing less than 25 silicon atoms
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
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- C08J5/18—Manufacture of films or sheets
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C—CHEMISTRY; METALLURGY
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- C08L2201/00—Properties
- C08L2201/04—Antistatic
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
Abstract
The invention discloses a polyolefin composition, which mainly comprises the following components: 20-100 parts of polyolefin resin, 1-60 parts of epoxy polyhedral oligomeric silsesquioxane, 0.1-5 parts of a cross-linking agent and 0.01-1 part of an auxiliary cross-linking agent. According to the invention, a small amount of epoxy polyhedral oligomeric silsesquioxane is added, and the polysilsesquioxane has a plurality of reactive groups, so that a mutually-crosslinked network structure can be formed with polypropylene resin under the action of a crosslinking agent, and the inorganic phase and the organic phase are combined through a strong chemical bond, so that the mechanical properties such as rigidity, impact strength and the like of the polyolefin material are improved.
Description
Technical Field
The invention relates to a polyolefin composition with high mechanical property and a preparation method thereof, belonging to the technical field of polyolefin functional master batch.
Background
The polypropylene PP is one of five general-purpose plastics, has rich raw material sources, low price, easy processing and forming and excellent product comprehensive performance, and is widely applied. PP is used as a semi-crystalline polymer material and has excellent performances such as higher rigidity, corrosion resistance, electrical insulation and the like. In general, polypropylene resins produced industrially have an isotactic structure content of about 95% and the balance of atactic or syndiotactic polypropylene. The polypropylene has a regular structure and high crystallization, the melting point of the polypropylene can reach 167 ℃, the polypropylene has good heat resistance, corrosion resistance, surface rigidity and scratch resistance, but the polypropylene is quickly transformed from a glassy state to a molten state, the melting range is narrow, the high elastic state range is very small, and the melt strength is small, so the polypropylene has low mechanical properties in plastic materials, and the tensile strength only reaches 30 MPa. Polypropylene with a larger isotactic index has higher tensile strength, but with the increase of the isotactic index, the impact strength of the material is reduced, thereby limiting the application of polypropylene.
Therefore, in order to enhance the mechanical properties, especially the impact strength, of the polypropylene material, other materials have been modified in the prior art, for example, in chinese patent CN103724809A, a brand new epoxy resin additive is prepared by using epoxy resin, diethanolamine, nylon 6, and ammonium acetate, and is used for enhancing the mechanical properties of the polypropylene material. However, the epoxy resin additive prepared by the invention is white block-shaped, and the polypropylene material is added after grinding, so that the following problems are caused: (1) since the particle diameter ratio of the aid is large, even if the grinding is carried out for a long time, a fine particle diameter cannot be obtained, so that the dispersibility of the aid in a material system is influenced, and the light transmittance of the material is influenced due to uneven dispersion; (2) because the assistant particles and the polypropylene material are physically blended, the complete and uniform distribution cannot be achieved, and thus, in a material system, some places have high mechanical properties, and some places have low mechanical properties, which causes unevenness.
Therefore, it is obvious that developing a new polyolefin composition with high mechanical properties, which has both good light transmittance and mechanical properties, has positive practical significance.
Disclosure of Invention
The invention aims to provide an antistatic heat-conducting polyolefin composition which simultaneously has good antistatic performance and high heat conductivity.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows: a polyolefin composition with high mechanical property mainly comprises the following components in parts by mass:
wherein the mass ratio of the polyolefin resin to the epoxy group polyhedral oligomeric silsesquioxane is 2.5-10: 1;
wherein the polyolefin resin is a polypropylene resin; the preparation method of the epoxy polyhedral oligomeric silsesquioxane is as follows:
(1) hydrolyzing vinyl trichlorosilane to obtain octavinyl polyhedral oligomeric silsesquioxane;
(2) and (2) epoxidizing the octavinyl polyhedral oligomeric silsesquioxane in the step (1) by using peroxyacetic acid to obtain the epoxy polyhedral oligomeric silsesquioxane.
Hereinbefore, the polyolefin resin may be 25 parts, 30 parts, 35 parts, 40 parts, 50 parts, 60 parts, 70 parts, 80 parts, 90 parts, 92 parts, 94 parts, 95 parts, 96 parts, 98 parts.
The epoxy polyhedral oligomeric silsesquioxane can be 12 parts, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, 56 parts, 58 parts and 59 parts.
Preferably, the mass ratio of the polyolefin resin to the epoxy group polyhedral oligomeric silsesquioxane is 2.5-10: 1, more preferably 3 to 5: 1, more preferably 4: 1.
the preparation method of the epoxy polyhedral oligomeric silsesquioxane can be represented by the following chemical reaction formula:
wherein, the epoxy polyhedral oligomeric silsesquioxane is abbreviated as epoxy-POSS.
Preferably, the particle size of the epoxy polyhedral oligomeric silsesquioxane is 5-20 nm. More preferably, the particle size of the epoxy polyhedral oligomeric silsesquioxane is 8-15 nm, and more preferably 10-12 nm.
In the above technical solution, the cross-linking agent is selected from one or more of tert-butyl peroxydicarbonate-2-ethylhexyl peroxybenzoate, tert-butyl peroxybenzoate, bis (tert-butylperoxycumene), 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane, dicumyl peroxide, triethylenetetramine and diethylenetriamine or diethylaminopropylamine.
In the above technical scheme, the auxiliary crosslinking agent is selected from one or more of triallyl cyanurate, triallyl isocyanurate, ethylene glycol dimethacrylate, trimethylolpropane trimethacrylate, divinylbenzene and propyl phthalate.
In the technical scheme, the mass ratio of the polyolefin resin to the functional filler is 3-5: 1.
the invention also claims a preparation method of the polyolefin composition with high mechanical property, which comprises the following steps: putting the components into a stirrer according to the proportion for stirring, and uniformly mixing; and putting the uniformly mixed materials into an extruder which is preheated to 150-200 ℃, and cooling, granulating and drying the extruded melt to obtain the polyolefin composition.
Preferably, the stirring speed is 120-180 r/min.
The invention also discloses an insulating heat-conducting transparent film prepared from the polyolefin composition.
The invention also discloses an insulating heat-conducting transparent plate prepared from the polyolefin composition.
The working mechanism of the invention is as follows: polypropylene has excellent electrical insulation, low water absorption and low water vapor transmission rate, but the mechanical property is poor; according to the invention, epoxy polyhedral oligomeric silsesquioxane is adopted, and the polysilsesquioxane has a plurality of reactive groups, and can form a mutually-crosslinked network structure with polypropylene resin under the action of a crosslinking agent, so that the inorganic phase and the organic phase are combined through strong chemical bonds, and the rigidity and the impact strength of the polyolefin material are improved; on the other hand, the epoxy polyhedral oligomeric silsesquioxane nano material has a unique cubic structure and high porosity, can be used as a functional filler to improve the mechanical properties such as tensile strength, rigidity and the like of polypropylene resin, accelerate the crystallization rate of the polypropylene resin and promote the grain size refinement, and has excellent dispersibility in polypropylene although the grain size is small, so that the polyolefin resin has good light transmittance.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
1. the invention develops a novel polyolefin composition, combines the excellent electrical insulation property, low water absorption rate and low water vapor transmission rate of polyolefin, and by adding a small amount of epoxy polyhedral oligomeric silsesquioxane, the polysilsesquioxane has a plurality of reactive groups, and can form a mutually-crosslinked network structure with polypropylene resin under the action of a crosslinking agent, so that the inorganic phase and the organic phase are combined through strong chemical bonds, the mechanical properties of the polyolefin material, such as rigidity, impact strength and the like, are improved, and a remarkable effect is achieved;
2. the invention realizes the combination of the inorganic phase and the organic phase through strong chemical bonds, and compared with the existing physical blending, the invention has no problems of inorganic particle agglomeration and weak binding force of two-phase interfaces;
3. in the polyolefin composition, the mass ratio of the polyolefin resin to the functional filler is 5-10: 1; therefore, the addition amount of the functional filler is very small, which is mainly benefited by the chemical bond combination between the inorganic phase and the organic phase, and the small addition amount not only can improve the mechanical property of the material, but also can enable the material to have better light transmittance;
4. the preparation method is simple and easy to implement, has low cost and is suitable for popularization and application.
Detailed Description
Example one
A polyolefin composition with high mechanical property mainly comprises the following steps:
weighing 100g of homopolymerized polypropylene, 10g of epoxy-POSS, 0.5g of 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane and 0.05g of trimethylolpropane trimethacrylate, adding the materials into a stirrer, stirring for 30min, then putting the mixture into a hopper of an extruder, controlling the temperature of each section of the extruder to be between 150 ℃ and 200 ℃ and the rotating speed of a screw to be 150r/min, cooling and molding a melt in a water tank after extrusion, drawing the melt into a granulator, granulating and drying.
Example two
A polyolefin composition with high mechanical property mainly comprises the following steps:
weighing 100g of homopolymerized polypropylene, 25g of epoxy-POSS, 0.5g of 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane and 0.05g of trimethylolpropane trimethacrylate, adding the materials into a stirrer, stirring for 30min, then putting the mixture into a hopper of an extruder, controlling the temperature of each section of the extruder to be between 150 ℃ and 200 ℃ and the rotating speed of a screw to be 150r/min, cooling and molding a melt in a water tank after extrusion, drawing the melt into a granulator, granulating and drying.
EXAMPLE III
A polyolefin composition with high mechanical property mainly comprises the following steps:
weighing 100g of homopolymerized polypropylene, 40g of epoxy-POSS, 0.5g of 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane and 0.05g of trimethylolpropane trimethacrylate, adding the materials into a stirrer, stirring for 30min, then putting the mixture into a hopper of an extruder, controlling the temperature of each section of the extruder to be between 150 ℃ and 200 ℃ and the rotating speed of a screw to be 150r/min, cooling and molding a melt in a water tank after extrusion, drawing the melt into a granulator, granulating and drying.
Comparative example 1
A polyolefin composition with high mechanical property mainly comprises the following steps:
125g of homopolymerized polypropylene, 0.5g of 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane and 0.05g of trimethylolpropane trimethacrylate are weighed and added into a stirrer to be stirred for 30min, then the mixture is put into a hopper of an extruder, the temperature of each section of the extruder is between 150 ℃ and 200 ℃, the rotating speed of a screw is 150r/min, a melt is extruded and then cooled and molded in a water tank, and the melt is pulled into a granulator to be granulated and then dried.
Comparative example No. two
A polyolefin composition with high mechanical property mainly comprises the following steps:
weighing 100g of homopolymerized polypropylene, 20g of epoxy resin, 5g of POSS, 0.5g of 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane and 0.05g of trimethylolpropane trimethacrylate, adding the materials into a stirrer, stirring for 30min, then putting the mixture into a hopper of an extruder, controlling the temperature of each section of the extruder to be between 150 ℃ and 200 ℃ and the rotating speed of a screw to be 150r/min, cooling and molding a melt in a water tank after extrusion, drawing the melt into a granulator, granulating and drying.
Comparative example No. three
Referring to the disclosure of Chinese patent CN103724809A, a polyolefin composition with high mechanical properties comprises the following main steps:
weighing 53 parts of epoxy resin, 11 parts of diethanolamine, 23 parts of nylon 6 and 0.8 part of ammonium acetate; adding nylon 6 into ammonium acetate to dissolve, adding epoxy resin and diethanolamine, mixing, adding excessive water until white precipitate is not generated, filtering the white precipitate, oven drying to obtain white block, and pulverizing to obtain white powder.
Weighing 100g of homopolymerized polypropylene, 25g of white powder, 0.5g of 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane and 0.05g of trimethylolpropane trimethacrylate, adding the materials into a stirrer, stirring for 30min, then putting the mixture into a hopper of an extruder, controlling the temperature of each section of the extruder to be between 150 ℃ and 200 ℃ and the rotating speed of a screw to be 150r/min, cooling and molding a melt in a water tank after extrusion, drawing the melt into a granulator, granulating and drying.
The above examples one to three and comparative examples one to three were added to polypropylene resins in an amount of 10% by mass, respectively, and test pieces required for the tests were prepared.
The polypropylene materials were tested for light transmittance (GB2410-1989), haze (GB2410-1989), tensile strength (GB/T1040-1992), and impact strength (GB/T1843-.
The properties are detailed in the following table:
| S1 | S2 | S3 | D1 | D2 | D3 | |
| light transmittance (%) | 96 | 96 | 94 | 96 | 86 | 88 |
| Haze (%) | 1.3 | 1.2 | 1.5 | 1.6 | 7.1 | 6.3 |
| Flexural Strength (MPa) | 36.4 | 37.6 | 37.5 | 25.2 | 28.8 | 30.1 |
| Tensile Strength (MPa) | 48.1 | 49.3 | 48.8 | 29.5 | 35.0 | 39 |
| Impact Strength (KJ/m)2) | 31 | 32 | 32 | 19 | 22 | 26 |
In the above table: s1 to S3 represent examples one to three, and D1 to D3 represent comparative examples one to three.
From the above table, it is found by comparing the performances of the first to third examples and the first comparative example that when the epoxy polyhedral oligomeric silsesquioxane is added into the resin material, the transparency and haze of the polypropylene resin are not greatly affected, the material still has a good transparent effect, and meanwhile, the mechanical properties of the material, such as bending strength, tensile strength, impact strength and the like, are greatly improved.
Compared with the comparative example I, the composite material directly prepared by using the epoxy resin and the polypropylene has the advantages of poor light transmission and haze and small improvement on mechanical properties such as rigidity of the material.
As can be seen from examples one to three, when 100g of homopolypropylene and 25g of epoxy-POSS were added as the material components, the combination of the materials was the best in all aspects, and the bending strength was 37.6MPa, the tensile strength was 49.3MPa, and the impact strength was 32KJ/m2And the light transmittance reaches 96 percent, so the polyolefin material is a transparent polyolefin material with good mechanical property.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A polyolefin composition of high mechanical properties, characterized in that: the adhesive mainly comprises the following components in parts by mass:
20-100 parts of polyolefin resin
1-60 parts of epoxy polyhedral oligomeric silsesquioxane
0.1-5 parts of cross-linking agent
0.01-1 part of assistant crosslinking agent
Wherein the mass ratio of the polyolefin resin to the epoxy group polyhedral oligomeric silsesquioxane is 2.5-10: 1;
wherein the polyolefin resin is a polypropylene resin; the preparation method of the epoxy polyhedral oligomeric silsesquioxane is as follows:
(1) hydrolyzing vinyl trichlorosilane to obtain octavinyl polyhedral oligomeric silsesquioxane;
(2) then epoxidizing the octavinyl polyhedral oligomeric silsesquioxane in the step (1) by using peroxyacetic acid to obtain the epoxy polyhedral oligomeric silsesquioxane;
the particle size of the epoxy polyhedral oligomeric silsesquioxane is 5-20 nm.
2. Polyolefin composition according to claim 1, characterized in that: the cross-linking agent is selected from one or more of tert-butyl peroxycarbonic acid-2-ethylhexyl ester, tert-butyl peroxybenzoate, bis (tert-butylperoxycumene), 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane, diisopropylbenzene hydroperoxide, triethylenetetramine, diethylenetriamine or diethylaminopropylamine.
3. Polyolefin composition according to claim 1, characterized in that: the auxiliary crosslinking agent is selected from one or more of triallyl cyanurate, triallyl isocyanurate, ethylene glycol dimethacrylate, trimethylolpropane trimethacrylate and divinyl benzene.
4. Polyolefin composition according to claim 1, characterized in that: the mass ratio of the polyolefin resin to the functional filler is preferably 3-5: 1.
5. a process for the preparation of a polyolefin composition having high mechanical properties, characterized in that it comprises the following steps: putting the components into a stirrer according to the proportion of claim 1, and stirring to mix uniformly; and putting the uniformly mixed materials into an extruder which is preheated to 150-200 ℃, and cooling, granulating and drying the extruded melt to obtain the polyolefin composition.
6. The method of claim 5, wherein: the stirring speed is 120-180 r/min.
7. An insulating, thermally conductive, transparent film prepared using the polyolefin composition of any of claims 1 to 4.
8. An insulating and heat-conducting transparent sheet prepared from the polyolefin composition of any one of claims 1 to 4.
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| CN114316439B (en) * | 2022-01-12 | 2023-07-18 | 青岛颐世保塑料有限公司 | High-fluidity high-rigidity environment-friendly flame-retardant PP modified material for livestock breeding deodorization equipment |
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