CN112745583B - High-gloss impact-resistant polypropylene composition and preparation method thereof - Google Patents
High-gloss impact-resistant polypropylene composition and preparation method thereof Download PDFInfo
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Abstract
The invention provides a high-gloss impact-resistant polypropylene composition, and a preparation method and application thereof. The invention provides a preparation method of a high-gloss impact-resistant polypropylene composition, which comprises the following steps: mixing propylene, a catalyst, an electron donor and a cocatalyst, and carrying out a first polymerization reaction to obtain polypropylene slurry; mixing the polypropylene slurry with ethylene, and carrying out a second polymerization reaction to obtain a polypropylene copolymer powder; mixing the copolymerized polypropylene powder, the antioxidant, the auxiliary antioxidant, the acid absorbing agent and the nucleating agent to obtain a mixture; and extruding and granulating the mixture to obtain the polypropylene composition. The high-gloss impact-resistant polypropylene composition prepared according to the invention has excellent gloss, rigidity and toughness, and can be used in the fields of household appliances, automobiles and the like, in particular to injection molding products of household appliance shells, bases and automobile exterior trimming parts.
Description
Technical Field
The invention relates to the field of polypropylene compositions, in particular to a preparation method and application of a high-gloss impact-resistant polypropylene composition.
Background
The high-crystallinity high-gloss polypropylene is high-crystallinity, high-crystallization temperature, high rigidity and high-gloss polypropylene resin prepared by adding an efficient nucleating agent on the basis of high-stereoregularity homopolymerized polypropylene, has wide application in the occasions of household parts, houses and the like, and the high-gloss polypropylene in the market is basically homopolymerized polypropylene at present and has the problems of low toughness, easiness in collision and the like. A modification factory adds a certain amount of toughening agents such as POE (polyolefin elastomer), rubber particles and the like into the homopolymerized polypropylene continuous phase, so that the impact resistance of the material is improved to a certain extent, but the dispersing effect of the toughening agents in downstream enterprises is poor, and the influence on the glossiness of the product is large.
If the combination of the glossiness and the toughness of the polypropylene is realized, the high-gloss impact-resistant polypropylene is developed, so that the performance of a polypropylene injection molding product is fundamentally improved, and the home appliance and automobile product has excellent appearance and good service performance.
Disclosure of Invention
The first purpose of the invention is to provide a high-gloss impact-resistant polypropylene resin produced by a hydrogen conditioning method, which has high glossiness, good toughness and no odor. The polypropylene resin material provided by the invention can be directly used for manufacturing the shell and the base of the household appliance without modification, thereby reducing intermediate links and lowering the production cost.
The second purpose of the invention is to provide a method for producing high-gloss impact-resistant polypropylene resin by using a hydrogen regulation method.
In a first aspect, the present invention provides a process for preparing a high gloss impact polypropylene composition comprising:
step A: mixing propylene and a catalyst system, and carrying out a first polymerization reaction to obtain polypropylene slurry, wherein the catalyst system comprises a catalyst, an electron donor and a cocatalyst;
and B: mixing the polypropylene slurry with ethylene, and carrying out a second polymerization reaction to obtain a polypropylene copolymer powder;
and C: mixing the copolymerized polypropylene powder, the antioxidant, the auxiliary antioxidant, the acid absorbing agent and the nucleating agent to obtain a mixture;
step D: and extruding and granulating the mixture to obtain the polypropylene composition.
According to some embodiments of the invention, the catalyst system has Al/Mg ═ 3.5 to 4.5 and Al/Si ═ 3.5 to 4.5.
According to a preferred embodiment of the invention, in the catalyst system, Al/Mg-4 and Al/Si-4.
According to one embodiment of the invention, the catalyst system comprises the procatalyst titanium tetrachloride, the procatalyst carrier MgCl 2 The electron donor isobutyl dimethoxy silane and the cocatalyst triethyl aluminum.
According to some embodiments of the invention, the hydrogen concentration in the first polymerization reaction is 0.1 to 0.5%.
According to some embodiments of the invention, the pressure of the first polymerization reaction is 3.4 ± 0.15MPa.
According to some embodiments of the invention, the temperature of the first polymerization reaction is 70 to 75 ℃.
According to some embodiments of the invention, the pressure of the second polymerization reaction is 1.2 ± 0.1 MPa.
According to some embodiments of the invention, the temperature of the second polymerization reaction is 75-80 ℃.
According to some embodiments of the invention, the hydrogen concentration in the second polymerization reaction is between 0.1 and 0.3%.
According to some embodiments of the invention, the ethylene concentration in the second polymerization reaction is between 20 and 30%.
According to some embodiments of the invention, the first polymerization reaction is carried out in a loop reactor.
According to some embodiments of the invention, the second polymerization reaction is carried out in a gas phase reactor.
According to some embodiments of the present invention, the copolymerized polypropylene powder has a melt flow rate greater than 10g/10 min.
According to some embodiments of the present invention, in step C, the polypropylene is 100 parts, the antioxidant is 0.05-0.15 part, the auxiliary antioxidant is 0.1-0.15 part, the acid acceptor is 0.01-0.05 part, and the nucleating agent is 0.2-0.3 part by weight.
According to some embodiments of the invention, the antioxidant is selected from 3- (3, 5-bis-butyl-4-hydroxycyclohexyl) propionate.
According to some embodiments of the invention, the secondary antioxidant is selected from tris (2, 4-di-tert-butylphenyl) phosphite.
According to some embodiments of the invention, the acid scavenger is selected from calcium stearate.
According to some embodiments of the invention, the nucleating agent is selected from substituted aryl phosphate salts.
According to a preferred embodiment of the invention, the nucleating agent is selected from substituted aryl sodium phosphates or substituted aryl heterocyclic sodium phosphates.
In a second aspect, the present invention provides a polypropylene composition obtained according to the preparation method of the first aspect.
According to some embodiments of the invention, the polypropylene composition has a melt flow rate of greater than 10g/10min, an ethylene content of greater than 5%, and a rubber content of greater than 10%.
According to some embodiments of the invention, the polypropylene composition has a melt flow rate of 10 to 15g/10min, an ethylene content of 5 to 10% and a rubber content of 10 to 20%.
According to some embodiments of the invention, the polypropylene composition has a simple beam notched impact strength of greater than 7kJ/m at room temperature 2 。
According to some embodiments of the invention, the polypropylene composition has a flexural modulus of greater than 1600 MPa.
According to some embodiments of the invention, the polypropylene composition has a gloss at 60 ° of more than 80%.
In a third aspect, the invention provides a use of the polypropylene composition obtained by the preparation method according to the first aspect or the polypropylene composition according to the second aspect in the electric and automotive industry.
The invention mainly aims at the fields of household appliances and automobiles, and provides a high-gloss impact-resistant polypropylene resin which has the following advantages compared with the prior art:
(1) the polypropylene resin prepared by the invention has high glossiness, high rigidity and impact resistance;
(2) the polypropylene resin prepared by the invention is tested according to GB3682, and has a melt index of more than 10g/10min, and the test conditions are as follows: the temperature is 230 ℃, and the load is 2.16 kg;
(3) the polypropylene resin prepared by the invention is tested according to GB/T9341, and the flexural modulus is more than 1600 MPa;
(4) in the invention, a hydrogen regulation method is adopted to replace a degradation method to produce the ultrahigh-fluidity high-crystallization impact polypropylene material, and high-gloss impact polypropylene copolymer with melt flow rate of more than or equal to 10g/10min is prepared by controlling reaction conditions in the polymerization process. Adding antioxidant, acid absorbent and nucleating agent, extruding and granulating to obtain the final product with melt flow rate not less than 10g/10min, ethylene content greater than 5%, rubber content greater than 10%, and impact strength greater than 7KJ/m 2 The flexural modulus is more than 1600MPa, and the glossiness at 60 ℃ is more than 80%.
(5) The polypropylene resin prepared by the invention has excellent glossiness, rigidity and toughness, and can be used in the fields of household appliances, automobiles and the like, in particular to injection molding products of household appliance shells, bases and automobile exterior trimming parts.
Detailed Description
The present invention will be described in more detail by way of examples, but the following examples are merely illustrative of the present invention and are not intended to limit the present invention, and therefore any changes within the meaning and scope equivalent to the claims of the present invention should be construed as being included in the scope of the claims.
In the following examples, the antioxidant was 3- (3, 5-Bitbutyl-4-hydroxycyclohexyl) propionic acid pentaerythritol ester (1010).
The auxiliary antioxidant is tris (2, 4-di-tert-butylphenyl) phosphite (168).
The acid absorbent is calcium stearate.
The nucleating agent is substituted aryl sodium phosphate.
The polymer related data in the examples were obtained according to the following test methods:
(1) melt Flow Rate (MFR): measured according to GB3682 at 230 ℃ under a load of 2.16 kg.
(2) Ethylene content: determined by known FTIR tests based on calibration with 13C-NMR.
(3) Rubber content: determined according to GB/T24282-.
(4) Tensile yield strength: measured according to GB/T1040.
(5) Impact strength of the simply supported beam notch: measured according to GB/T1043.1.
(6) Flexural modulus: measured according to GB/T9341.
Example 1
(1) Adopting Spheripol polypropylene process, using propylene as raw material, feeding 30 tons of propylene per hour, and adding titanium tetrachloride as catalyst and MgCl as carrier 2 Adding electron donor isobutyl dimethoxysilane and cocatalyst triethyl aluminum into a loop reactor, feeding 2kg of catalyst per hour, controlling Al/Mg to be 4 and Al/Si to be 4, controlling the reaction pressure of the loop reactor to be 3.4MPa, controlling the reaction temperature to be 70 ℃, and controlling the hydrogen concentration in the reactor to be 0.1 percent to obtain the polypropylene slurry.
(2) And (2) feeding the polypropylene slurry material obtained in the step (1) into a gas phase reactor, controlling the reaction pressure of the gas phase reactor to be 1.2MPa, the reaction temperature to be 75 ℃, and controlling the ethylene concentration in the reactor to be 20 percent, thus obtaining the copolymerized polypropylene powder with the melt flow rate of 10.2g/10 min.
(3) Uniformly mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid acceptor and a nucleating agent, wherein the mass composition is as follows:
polypropylene: 100 parts of antioxidant: 0.05 part of auxiliary antioxidant: 0.1 part, acid acceptor: 0.05 part, nucleating agent: 0.2 part.
(4) Extruding the mixture obtained in the step (3) through an extruder at 220 ℃ to prepare the high-gloss impact-resistant polypropylene composition. The properties are shown in Table 1.
Example 2
(1) Adopting Spheripol polypropylene process, using propylene as raw material, feeding 30 tons of propylene per hour, and adding titanium tetrachloride as catalyst and MgCl as carrier 2 Adding electron donor isobutyl dimethoxysilane and cocatalyst triethyl aluminum into a loop reactor, feeding 2kg of catalyst per hour, controlling Al/Mg to be 4 and Al/Si to be 4, controlling the reaction pressure of the loop reactor to be 3.4MPa, controlling the reaction temperature to be 70 ℃, and controlling the hydrogen concentration in the reactor to be 0.11 percent to obtain the polypropylene slurry.
(2) And (2) feeding the polypropylene slurry material obtained in the step (1) into a gas phase reactor, controlling the reaction pressure of the gas phase reactor to be 1.2MPa, the reaction temperature to be 76 ℃, and controlling the ethylene concentration in the reactor to be 21 percent, thus obtaining the copolymerized polypropylene powder with the melt flow rate of 10.7g/10 min.
(3) Uniformly mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid acceptor and a nucleating agent, wherein the mass composition is as follows:
polypropylene: 100 parts of antioxidant: 0.05 part of auxiliary antioxidant: 0.1 part, acid acceptor: 0.05 part, nucleating agent: 0.2 part.
(4) Extruding the mixture obtained in the step (4) through an extruder at 220 ℃ to prepare the high-gloss impact-resistant polypropylene composition. The properties are shown in Table 1.
Example 3
(1) Adopting Spheripol polypropylene process, using propylene as raw material, feeding 30 tons of propylene per hour, and adding titanium tetrachloride as catalyst and MgCl as carrier 2 Adding electron donor isobutyl dimethoxysilane and cocatalyst triethyl aluminum into a loop reactor, feeding 2kg of catalyst per hour, controlling Al/Mg to be 4 and Al/Si to be 4, controlling the reaction pressure of the loop reactor to be 3.4MPa, controlling the reaction temperature to be 71 ℃, and controlling the hydrogen concentration in the reactor to be 0.13 percent to obtain the polypropylene slurry.
(2) And (2) feeding the polypropylene slurry material obtained in the step (1) into a gas phase reactor, controlling the reaction pressure of the gas phase reactor to be 1.2MPa, the reaction temperature to be 75 ℃, and controlling the ethylene concentration in the reactor to be 24 percent, thus obtaining the copolymerized polypropylene powder with the melt flow rate of 11.3g/10 min.
(3) Uniformly mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid acceptor and a nucleating agent, wherein the mass composition is as follows:
polypropylene: 100 parts of antioxidant: 0.05 part of auxiliary antioxidant: 0.1 part, acid acceptor: 0.05 part, nucleating agent: 0.2 part.
(4) Extruding the mixture obtained in the step (4) through an extruder at 220 ℃ to prepare the high-gloss impact-resistant polypropylene composition. The properties are shown in Table 1.
Example 4
(1) Adopting Spheripol polypropylene process, using propylene as raw material, feeding 30 tons of propylene per hour, and adding titanium tetrachloride as catalyst and MgCl as carrier 2 Adding an electron donor of isobutyl dimethoxysilane and a cocatalyst of triethyl aluminum into a loop reactor, feeding 2kg of catalyst per hour, controlling Al/Mg to be 4 and Al/Si to be 6, controlling the reaction pressure of the loop reactor to be 3.4MPa, controlling the reaction temperature to be 70 ℃, and controlling the hydrogen concentration in the reactor to be 0.1 percent to obtain the polypropylene slurry.
(2) And (2) feeding the polypropylene slurry material obtained in the step (1) into a gas phase reactor, controlling the reaction pressure of the gas phase reactor to be 1.2MPa, the reaction temperature to be 75 ℃, and controlling the ethylene concentration in the reactor to be 20 percent, thus obtaining the copolymerized polypropylene powder with the melt flow rate of 9.3g/10 min.
(3) Uniformly mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid acceptor and a nucleating agent, wherein the mass composition is as follows:
polypropylene: 100 parts of antioxidant: 0.05 part of auxiliary antioxidant: 0.1 part, acid acceptor: 0.05 part, nucleating agent: 0.2 part.
(4) Extruding the mixture obtained in the step (3) through an extruder at 220 ℃ to prepare the high-gloss impact-resistant polypropylene composition. The properties are shown in Table 1.
Example 5
(1) Adopting Spheripol polypropylene process, using propylene as raw material, feeding 30 tons of propylene per hour, and adding titanium tetrachloride as catalyst and MgCl as carrier 2 Electron donorAdding butyl dimethoxysilane and a cocatalyst of triethyl aluminum into a loop reactor, feeding 2kg of catalyst per hour, controlling Al/Mg to be 4 and Al/Si to be 4, controlling the reaction pressure of the loop reactor to be 3.4MPa, controlling the reaction temperature to be 70 ℃, and controlling the hydrogen concentration in the reactor to be 0.6 percent to obtain the polypropylene slurry.
(2) And (2) feeding the polypropylene slurry material obtained in the step (1) into a gas phase reactor, controlling the reaction pressure of the gas phase reactor to be 1.2MPa, the reaction temperature to be 75 ℃, and controlling the ethylene concentration in the reactor to be 20 percent, thus obtaining the copolymerized polypropylene powder with the melt flow rate of 34.6g/10 min.
(3) Uniformly mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid acceptor and a nucleating agent, wherein the mass composition is as follows:
polypropylene: 100 parts of antioxidant: 0.05 part of auxiliary antioxidant: 0.1 part, acid acceptor: 0.05 part, nucleating agent: 0.2 part.
(4) Extruding the mixture obtained in the step (3) through an extruder at 220 ℃ to prepare the high-gloss impact-resistant polypropylene composition. The properties are shown in Table 1.
TABLE 1
The results in the table show that the melt flow rate of the polypropylene material produced by the hydrogen-blending production process in the embodiment is greater than 10g/10min, the ethylene content is greater than 5%, the rubber content is greater than 10%, the notch impact strength of the simply supported beam at room temperature is greater than 7kJ/m2, the flexural modulus is greater than 1600MPa, the glossiness at 60 ℃ is greater than 80%, and the material is odorless and meets the processing requirements of automobile and household appliance materials.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
Claims (5)
1. A method of making a high gloss impact polypropylene composition comprising:
step A: mixing propylene and a catalyst system, and carrying out a first polymerization reaction to obtain polypropylene slurry, wherein the catalyst system comprises a catalyst, an electron donor and a cocatalyst;
and B, step B: mixing the polypropylene slurry with ethylene, and carrying out a second polymerization reaction to obtain a polypropylene copolymer powder;
and C: mixing the copolymerized polypropylene powder, the antioxidant, the auxiliary antioxidant, the acid absorbing agent and the nucleating agent to obtain a mixture;
step D: extruding and granulating the mixture to obtain the polypropylene composition;
wherein, in the catalyst system, Al/Mg =3.5-4.5, Al/Si = 3.5-4.5;
and/or the hydrogen concentration in the first polymerization reaction is 0.1-0.5%;
the preparation method adopts a Spheripol polypropylene process;
the pressure of the first polymerization reaction is 3.4 +/-0.15 MPa, and the temperature is 70-75 ℃;
the pressure of the second polymerization reaction is 1.2 +/-0.1 MPa, and the temperature is 75-80 ℃;
in the second polymerization reaction, the concentration of hydrogen is 0.1-0.3%, and/or the concentration of ethylene is 20-30%;
the first polymerization reaction is carried out in a loop reactor; and/or the second polymerization reaction is carried out in a gas phase reactor; and/or the melt flow rate of the copolymerized polypropylene powder is more than 10g/10 min;
In the step C, 100 parts of polypropylene, 0.05-0.15 part of antioxidant, 0.1-0.15 part of auxiliary antioxidant, 0.01-0.05 part of acid acceptor and 0.2-0.3 part of nucleating agent by weight.
2. The process according to claim 1, wherein in step C, the antioxidant is selected from the group consisting of 3- (3, 5-bis-butyl-4-hydroxycyclohexyl) propionic acid pentaerythritol ester; and/or the secondary antioxidant is selected from tris (2, 4-di-tert-butylphenyl) phosphite; and/or the acid scavenger is selected from calcium stearate; and/or the nucleating agent is selected from substituted aryl phosphate salts.
3. A polypropylene composition obtainable by the process according to claim 1 or 2, wherein the polypropylene composition has a melt flow rate of more than 10g/10min, an ethylene content of more than 5% and a rubber content of more than 10%; and/or the impact strength of the simple beam gap at room temperature is more than 7kJ/m 2 (ii) a And/or a flexural modulus greater than 1600 Mpa; and/or 60 o The lower gloss is greater than 80%.
4. The polypropylene composition according to claim 3, wherein the polypropylene composition has a melt flow rate of 10 to 15g/10min, an ethylene content of 5 to 10% and a rubber content of 10 to 20%.
5. Use of the polypropylene composition obtained according to the preparation process of claim 1 or 2 or of the polypropylene composition according to claim 3 or 4 in the household and automotive industry.
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