CN110746703A - High-rigidity high-toughness polypropylene composition and preparation method thereof - Google Patents
High-rigidity high-toughness polypropylene composition and preparation method thereof Download PDFInfo
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Abstract
The invention provides a heightA high-rigidity and high-toughness polypropylene composition and a preparation method thereof belong to the technical field of polypropylene materials. The high-rigidity high-toughness polypropylene composition has the melt flow rate of more than 35g/10min, the ethylene mass content of more than 7 percent, the rubber mass content of more than 15 percent and the notch impact strength of a simply supported beam of more than 7kJ/m at room temperature2The bending modulus is more than 1500Mpa, the product is odorless, and the preparation method is mainly used for automobiles, household appliances and thin-wall injection molding products, is based on the Innovene gas-phase polypropylene process, has simple steps, and is easy for industrial application.
Description
Technical Field
The invention belongs to the technical field of polypropylene materials, and relates to a high-rigidity high-toughness polypropylene composition and a preparation method thereof.
Background
The high-crystalline polypropylene is high-crystallinity, high-crystallization temperature, high rigidity and high heat resistance polypropylene resin prepared by adding an efficient nucleating agent on the basis of high-stereoregularity homopolymerized polypropylene, and has wide application in occasions such as electric appliance parts, houses and the like. Belongs to a high-end product in polypropylene. Impact polypropylene is prepared by adding a certain amount of an ethylene-propylene rubber component to a continuous phase of homopolypropylene, typically by reactor techniques. The existence of the dispersed rubber phase plays a role in absorbing stress, so that the impact resistance of the material is greatly improved, and particularly the low-temperature impact resistance is obviously improved. The impact-resistant polypropylene is widely applied to a plurality of fields such as automobiles, household appliances, home furnishing and the like.
If the rigidity of the high-crystalline polypropylene and the toughness of the impact polypropylene are combined, the development of the high-crystalline impact polypropylene inevitably improves the performance of the polypropylene injection molding product fundamentally, reduces the material consumption, and avoids the adverse factors of cost increase and the like caused by blending glass fiber, inorganic filler and the like.
The companies such as SK, Barcel (BASELL) and the like are developing the high-crystallization impact polypropylene technology, and once the popularized products such as BX3900, BX3920, 540V and the like come into the market, the high-crystallization impact polypropylene technology can be widely recognized by users, and the selling price is more than 1500 yuan/ton higher than that of the common impact polypropylene. It is expected that the high-crystalline impact polypropylene must replace the existing high-crystalline polypropylene and impact polypropylene to a great extent and become the leading brand of the polypropylene resin for injection molding in the future.
At present, the main means for improving the rigidity of the impact-resistant polypropylene at home is to blend a certain amount of glass fiber or add a large amount of inorganic components such as calcium carbonate and the like, which causes the problems of great reduction of the impact resistance, increase of the density, reduction of the processing performance, color change and the like of the material. The direct production has high technical index and high production difficulty, and the product quality is still not ideal although some domestic enterprises do corresponding work.
Disclosure of Invention
In order to overcome the above disadvantages and shortcomings of the prior art, the present invention provides a high rigidity and high toughness polypropylene composition and a preparation method thereof, so as to obtain a polypropylene material with good fluidity, high crystallinity, good rigidity, impact resistance and no odor.
In order to achieve the purpose, the invention adopts the technical scheme that: in a first aspect, the invention provides a high-rigidity high-toughness polypropylene composition, the melt flow rate of which is more than 35g/10min, the ethylene mass content of which is more than 7%, the rubber mass content of which is more than 15%, and the notch impact strength of a simply supported beam at room temperature of which is more than 7kJ/m2The flexural modulus is more than 1500Mpa, and the polypropylene powder mainly comprises impact-resistant copolymerized polypropylene powder and an auxiliary agent, wherein the auxiliary agent comprises an antioxidant, an auxiliary antioxidant, an acid acceptor and a nucleating agent. Wherein, the room temperature refers to the temperature of the environment, and is generally 23 ℃. Under the conditions of the melt flow rate and the impact strength, the bending modulus of the traditional product is less than 1300 MPa; if the product is filled with stiffening materials such as calcium carbonate and the like to improve the flexural modulus of the product, the impact strength of the product is reduced by 10 to 15 percent. However, the composition of the present invention breaks this bottleneck by having a melt flow rate of greater than 35g/10min, greater than 7kJ/m2Has a flexural modulus of more than 1500MPa, in addition to the impact strength of (A).
As a preferable embodiment of the composition, the melt flow rate of the composition is 35-45 g/10min, the mass content of ethylene is 8-12%, and the mass content of rubber is 15-22%.
In a second aspect, the present invention also provides a method for preparing the above composition, which comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a catalyst, an electron donor and a cocatalyst into a first reactor, and reacting to obtain polypropylene powder;
(2) transferring the polypropylene powder obtained in the step (1) to a second reactor, and reacting with hydrogen and ethylene to obtain impact-resistant co-polypropylene powder;
(3) uniformly mixing the impact-resistant co-polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid acceptor and a nucleating agent to obtain a mixture;
(4) extruding the mixture obtained in the step (3) through an extruder to obtain the polypropylene composition. The preparation method comprises the step of combining the impact-resistant copolymerized polypropylene powder with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent to obtain a melt with a flow rate of more than 35g/10min, an ethylene mass content of more than 7%, a rubber mass content of more than 15%, and a simple beam notch impact strength of more than 7kJ/m at room temperature2The flexural modulus of the composition is more than 1500MPa, while the melt flow rate of the polypropylene material obtained by the preparation method described in CN109111643A is less than 35g/10min, the flexural modulus is less than 1200MPa, and the performance is obviously inferior to that of the composition described in the invention.
As a preferable embodiment of the production method of the present invention, the atomic ratio of Al, Mg and Si in the reaction system in the step (1) is Al: mg: si ═ 4:1: 1.
In the step (1), the volume concentration of hydrogen in the first reactor is 0.5-1.2%, the reaction pressure is 2.05-2.35Mpa, and the reaction temperature is 70-80 ℃.
In the step (2), the volume concentration of hydrogen in the second reactor is 0.1-0.3%, the volume concentration of ethylene is 10-30%, the reaction pressure is 2.05-2.35Mpa, and the reaction temperature is 65-75 ℃.
As a preferred embodiment of the preparation method of the present invention, in the step (3), the weight ratio of the impact-resistant copolymerized polypropylene powder, the antioxidant, the auxiliary antioxidant, the acid scavenger and the nucleating agent is: antioxidant: auxiliary antioxidant: acid-absorbing agent: the nucleating agent is 100: 0.05-0.15: 0.1-0.15: 0.01-0.05: 0.2-0.3.
In the step (3), the antioxidant is 3- (3, 5-bis-butyl-4-hydroxycyclohexyl) propionate, the auxiliary antioxidant is tris (2, 4-di-tert-butylphenyl) phosphite, the acid acceptor is hydrotalcite, and the nucleating agent is sodium 2, 2' -methylenebis (4, 6-di-tert-butylphenyl) phosphate.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the polypropylene composition has high fluidity, high crystallinity, high rigidity and impact resistance;
(2) the polypropylene composition has good processing performance and impact resistance, and can be used in the fields of household appliances, automobiles and the like, in particular to injection molding products of automotive interior parts and large thin-wall containers.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 75 ℃ and the volume concentration of hydrogen in the reactor to be 0.83 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 70 ℃, the volume concentration of hydrogen in the reactor to be 0.16%, and the volume concentration of ethylene to be 18%, so as to obtain impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.05:0.1:0.05:0.2 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to obtain the high-rigidity high-toughness polypropylene composition. The properties of the high rigidity and high toughness polypropylene composition obtained in this example are shown in Table 1.
Example 2
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 76 ℃ and the volume concentration of hydrogen in the reactor to be 0.86% to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 69 ℃, the volume concentration of hydrogen in the reactor to be 0.22%, and the volume concentration of ethylene to be 16%, so as to obtain impact-resistant copolymerized polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.05:0.1:0.05:0.2 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to obtain the high-rigidity high-toughness polypropylene composition. The properties of the high rigidity and high toughness polypropylene composition obtained in this example are shown in Table 1.
Example 3
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 75 ℃ and the volume concentration of hydrogen in the reactor to be 0.80 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 70 ℃, the volume concentration of hydrogen in the reactor to be 0.15%, and the volume concentration of ethylene to be 16%, so as to obtain impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.05:0.1:0.05:0.2 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
Example 4
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 70 ℃ and the volume concentration of hydrogen in the reactor to be 0.86 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 69 ℃, controlling the volume concentration of hydrogen in the reactor to be 0.22% and the volume concentration of ethylene to be 16%, and obtaining impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.05:0.1:0.05:0.2 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
Example 5
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 80 ℃ and the volume concentration of hydrogen in the reactor to be 0.86 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 69 ℃, controlling the volume concentration of hydrogen in the reactor to be 0.22% and the volume concentration of ethylene to be 16%, and obtaining impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.05:0.1:0.05:0.2 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
Example 6
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 76 ℃ and the volume concentration of hydrogen in the reactor to be 0.5 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 69 ℃, controlling the volume concentration of hydrogen in the reactor to be 0.11% and the volume concentration of ethylene to be 16%, and obtaining impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.05:0.1:0.05:0.2 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
Example 7
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 76 ℃ and the volume concentration of hydrogen in the reactor to be 1.2 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 69 ℃, controlling the volume concentration of hydrogen in the reactor to be 0.3% and the volume concentration of ethylene to be 16%, and obtaining impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.05:0.1:0.05:0.2 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
Example 8
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 76 ℃ and the volume concentration of hydrogen in the reactor to be 0.86 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 65 ℃, the volume concentration of hydrogen in the reactor to be 0.22%, and the volume concentration of ethylene to be 16%, so as to obtain impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.05:0.1:0.05:0.2 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
Example 9
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 76 ℃ and the volume concentration of hydrogen in the reactor to be 0.86 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 75 ℃, controlling the volume concentration of hydrogen in the reactor to be 0.22% and the volume concentration of ethylene to be 16%, and obtaining impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.05:0.1:0.05:0.2 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
Example 10
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 76 ℃ and the volume concentration of hydrogen in the reactor to be 0.86 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 69 ℃, the volume concentration of hydrogen in the reactor to be 0.22%, and the volume concentration of ethylene to be 10%, so as to obtain impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.05:0.1:0.05:0.2 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
Example 11
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 76 ℃ and the volume concentration of hydrogen in the reactor to be 0.86 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 69 ℃, the volume concentration of hydrogen in the reactor to be 0.22%, and the volume concentration of ethylene to be 30%, so as to obtain impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.05:0.1:0.05:0.2 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
Example 12
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 76 ℃ and the volume concentration of hydrogen in the reactor to be 0.86 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 69 ℃, controlling the volume concentration of hydrogen in the reactor to be 0.22% and the volume concentration of ethylene to be 16%, and obtaining impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.09:0.1:0.05:0.2 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
Example 13
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 76 ℃ and the volume concentration of hydrogen in the reactor to be 0.86 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 69 ℃, controlling the volume concentration of hydrogen in the reactor to be 0.22% and the volume concentration of ethylene to be 16%, and obtaining impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.15:0.1:0.05:0.2 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
Example 14
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 76 ℃ and the volume concentration of hydrogen in the reactor to be 0.86 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 69 ℃, controlling the volume concentration of hydrogen in the reactor to be 0.22% and the volume concentration of ethylene to be 16%, and obtaining impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.05:0.12:0.05:0.2 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
Example 15
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 76 ℃ and the volume concentration of hydrogen in the reactor to be 0.86 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 69 ℃, controlling the volume concentration of hydrogen in the reactor to be 0.22% and the volume concentration of ethylene to be 16%, and obtaining impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.05:0.15:0.05:0.2 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
Example 16
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 76 ℃ and the volume concentration of hydrogen in the reactor to be 0.86 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 69 ℃, controlling the volume concentration of hydrogen in the reactor to be 0.22% and the volume concentration of ethylene to be 16%, and obtaining impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.05:0.1:0.01:0.2 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
Example 17
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 76 ℃ and the volume concentration of hydrogen in the reactor to be 0.86 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 69 ℃, controlling the volume concentration of hydrogen in the reactor to be 0.22% and the volume concentration of ethylene to be 16%, and obtaining the impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing 100:0.05:0.1:0.025:0.2 of nucleating agent to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
Example 18
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 76 ℃ and the volume concentration of hydrogen in the reactor to be 0.86 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 69 ℃, controlling the volume concentration of hydrogen in the reactor to be 0.22% and the volume concentration of ethylene to be 16%, and obtaining impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.05:0.1:0.05:0.25 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
Example 19
One embodiment of the preparation method of the high-rigidity high-toughness polypropylene composition is disclosed. The preparation method comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a Ziegler Natta catalyst, an electron donor and a cocatalyst into a first reactor, and controlling the atomic number ratio of Al, Mg and Si in a reaction system to be Al: mg: controlling the reaction pressure of the first reactor to be 2.2MPa, the reaction temperature to be 76 ℃ and the volume concentration of hydrogen in the reactor to be 0.86 percent to obtain polypropylene powder, wherein Si is 4:1: 1;
(2) allowing the polypropylene powder obtained in the step (1) to enter a second reactor through an airlock system, controlling the reaction pressure of the second reactor to be 2.2MPa, the reaction temperature to be 69 ℃, controlling the volume concentration of hydrogen in the reactor to be 0.22% and the volume concentration of ethylene to be 16%, and obtaining impact-resistant co-polypropylene powder;
(3) mixing the impact-resistant copolymerized polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid absorbent and a nucleating agent according to the weight ratio: antioxidant: auxiliary antioxidant: acid-absorbing agent: uniformly mixing the nucleating agent with the ratio of 100:0.05:0.1:0.05:0.3 to obtain a mixture;
(4) and (4) extruding the mixture obtained in the step (3) and an auxiliary agent through an extruder to prepare the high-rigidity high-toughness polypropylene composition. The properties are shown in Table 1.
In examples 1-19, the antioxidant was 3- (3, 5-bis-butyl-4-hydroxycyclohexyl) propionate (1010), the auxiliary antioxidant was tris (2, 4-di-tert-butylphenyl) phosphite (168), the acid scavenger was hydrotalcite, and the nucleating agent was sodium 2, 2' -methylenebis (4, 6-di-tert-butylphenyl) phosphate.
Examples of effects
The high rigidity and high toughness polypropylene compositions obtained in examples 1 to 19 were subjected to the following performance tests:
(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.
TABLE 1 Polypropylene component contents and Performance indices obtained in examples 1-19
The results in Table 1 show that the polypropylene materials produced by the hydrogen-regulated production process in examples 1-19 have melt flow rate of more than 35g/10min, ethylene content of more than 7%, rubber content of more than 15%, and notched impact strength of a simply supported beam of more than 7kJ/m at room temperature2The flexural modulus is more than 1500MPa, the material is odorless, and the processing requirements of automobile and household electrical appliance materials are met.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. The high-rigidity high-toughness polypropylene composition is characterized in that the melt flow rate of the composition is more than 35g/10min, the ethylene mass content is more than 7%, the rubber mass content is more than 15%, and the notch impact strength of a simply supported beam at room temperature is more than 7kJ/m2The flexural modulus is more than 1500Mpa, and the polypropylene powder mainly comprises impact-resistant copolymerized polypropylene powder and an auxiliary agent, wherein the auxiliary agent comprises an antioxidant, an auxiliary antioxidant, an acid acceptor and a nucleating agent.
2. The composition according to claim 1, wherein the composition has a melt flow rate of 35 to 45g/10min, an ethylene content of 8 to 12% by mass and a rubber content of 15 to 22% by mass.
3. A process for the preparation of a composition according to claim 1 or 2, characterized in that it comprises the following steps:
(1) adopting an Innovene gas-phase polypropylene process, taking propylene as reaction gas, adding a catalyst, an electron donor and a cocatalyst into a first reactor, and reacting to obtain polypropylene powder;
(2) transferring the polypropylene powder obtained in the step (1) to a second reactor, and reacting with hydrogen and ethylene to obtain impact-resistant co-polypropylene powder;
(3) uniformly mixing the impact-resistant co-polypropylene powder obtained in the step (2) with an antioxidant, an auxiliary antioxidant, an acid acceptor and a nucleating agent to obtain a mixture;
(4) extruding the mixture obtained in the step (3) through an extruder to obtain the composition.
4. The production method according to claim 3, wherein the atomic number ratio of Al, Mg and Si in the reaction system in the step (1) is Al: mg: si ═ 4:1: 1.
5. The method according to claim 3, wherein in the step (1), the hydrogen volume concentration in the first reactor is 0.5 to 1.2%, the reaction pressure is 2.05 to 2.35MPa, and the reaction temperature is 70 to 80 ℃.
6. The method according to claim 3, wherein in the step (2), the volume concentration of hydrogen in the second reactor is 0.1 to 0.3%, the volume concentration of ethylene is 10 to 30%, the reaction pressure is 2.05 to 2.35MPa, and the reaction temperature is 65 to 75 ℃.
7. The preparation method according to claim 3, wherein in the step (3), the weight ratio of the impact co-polypropylene powder, the antioxidant, the auxiliary antioxidant, the acid absorbent and the nucleating agent is as follows: antioxidant: auxiliary antioxidant: acid-absorbing agent: the nucleating agent is 100: 0.05-0.15: 0.1-0.15: 0.01-0.05: 0.2-0.3.
8. The preparation method according to claim 3, wherein in the step (3), the antioxidant is 3- (3, 5-bis-butyl-4-hydroxycyclohexyl) propionate, the auxiliary antioxidant is tris (2, 4-di-tert-butylphenyl) phosphite, the acid scavenger is hydrotalcite, and the nucleating agent is sodium 2, 2' -methylenebis (4, 6-di-tert-butylphenyl) phosphate.
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