CN113999344B - Metallocene-catalyzed alpha-olefin polymer grafted polypropylene and preparation method thereof - Google Patents
Metallocene-catalyzed alpha-olefin polymer grafted polypropylene and preparation method thereof Download PDFInfo
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- CN113999344B CN113999344B CN202111258852.7A CN202111258852A CN113999344B CN 113999344 B CN113999344 B CN 113999344B CN 202111258852 A CN202111258852 A CN 202111258852A CN 113999344 B CN113999344 B CN 113999344B
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Abstract
The invention belongs to the technical field of grafting modification of high polymer materials, and particularly relates to an alpha-olefin polymer grafted polypropylene catalyzed by metallocene and a preparation method thereof. The invention adopts a solid phase method to make polypropylene, metallocene catalyzed alpha-olefin oligomer and initiator undergo the grafting reaction for 10-300 min at 25-200 ℃ under the atmosphere of protective gas to prepare metallocene catalyzed alpha-olefin polymer grafted polypropylene; wherein the addition amount of the metallocene catalyzed alpha-olefin oligomer is 0.1 to 10 weight percent of the polypropylene. The impact strength of the grafted modified polypropylene prepared by the method is improved by 122%, the tensile yield stress is improved by 32%, the flexural modulus is improved by 20%, and the preparation method is simple, the preparation conditions are easy to control, the reaction conditions are mild, and the grafted modified polypropylene is suitable for mass production.
Description
Technical Field
The invention belongs to the technical field of grafting modification of high polymer materials, and particularly relates to an alpha-olefin polymer grafted polypropylene catalyzed by metallocene and a preparation method thereof.
Background
Polypropylene (PP) is a crystalline polymer with a regular structure, is low in cost, strong in corrosion resistance and excellent in physical properties, and is widely applied to various aspects in production and life of buildings, energy sources, chemical industry, transportation and the like. Common polypropylene products are all linear structures, have relatively narrow relative molecular mass distribution and low melt strength, and have poor anti-sagging performance, so that the polymers are limited in the processing procedures of thermoforming, extrusion coating, calendaring, foaming and the like. Accordingly, efforts have been made to increase the melt strength of the alloy over the past decades.
At present, the multifunctional monomer used for the grafting modification of the polypropylene is mainly a small molecular monomer such as acrylic ester, maleic anhydride and analogues thereof, vinyl siloxane and styrene and analogues thereof, but the improvement of the mechanical properties of the modified polypropylene is not obvious.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide the metallocene-catalyzed alpha-olefin polymer grafted polypropylene and the preparation method thereof, and compared with the polypropylene raw material, the impact strength of the grafted modified polypropylene prepared by the invention is improved by 122 percent, the tensile yield stress is improved by 32 percent, and the flexural modulus is improved by 20 percent.
Based on the above purpose, the technical scheme adopted by the invention is as follows:
In a first aspect, the present invention provides a process for the preparation of a metallocene-catalyzed, alpha-olefin polymer grafted polypropylene comprising the steps of:
The polypropylene, the metallocene catalyzed alpha-olefin oligomer and an initiator are subjected to grafting reaction for 10 to 300 minutes at the temperature of between 25 and 200 ℃ in the atmosphere of protective gas to prepare the metallocene catalyzed alpha-olefin polymer grafted polypropylene; the addition amount of the metallocene catalyzed alpha-olefin oligomer is 0.1 to 10 weight percent of the polypropylene.
The metallocene-catalyzed alpha-olefin oligomer is a mixture of the oligomerization alpha-olefins with different polymerization degrees, shows a uniform comb structure, does not have short side chains, contains unsaturated double bonds, has good compatibility with polypropylene, and can be used for grafting modification of polypropylene.
According to the invention, under the action of the initiator, the metallocene catalyzed alpha-olefin oligomer is grafted to the polypropylene, so that the mechanical property of the prepared modified polypropylene is obviously improved, the impact strength is improved by 122%, the tensile yield stress is improved by 32%, and the flexural modulus is improved by 20%.
In addition, the conventional methods for graft modification of polypropylene include a solution method, a melt method and a solid phase method. The solution method is to dissolve the polymer in a proper solvent, and the grafting reaction is carried out in the solution, so that the solution grafting method has serious environmental pollution, high production cost and complex post-treatment of the product, and needs a large amount of organic solvent and recovery. The melting method is to introduce the monomer into the polymer melt to graft the monomer onto the polypropylene main chain, the melting method has the advantages of higher reaction temperature, serious side reaction, difficult removal of residual monomer and poor product quality guarantee. The invention adopts a solid phase method for grafting modification of polypropylene, and the polypropylene is directly contacted with a modifier and an initiator for reaction, so that the reaction is carried out under the condition of being lower than the melting point of the polymer, the reaction temperature is mild, the investment cost is low, the solvent is not required to be recovered, the advantages of the existing melting method and the solution method are combined, the defects of the melting method and the solution method are overcome, the efficiency and the energy conservation are realized, and the development and application prospect is good.
Further, the metallocene-catalyzed alpha-olefin oligomer comprises at least one of an alpha-olefin polymer having a degree of polymerization of from 2 to 10, the metallocene-catalyzed alpha-olefin oligomer having a kinematic viscosity of from 2 to 200cSt at 100 ℃.
It has been found by experimentation that the increase in the kinematic viscosity of the metallocene-catalyzed alpha-olefin oligomer is detrimental to its graft modification reaction with polypropylene, so that the kinematic viscosity of the metallocene-catalyzed alpha-olefin oligomer is preferably at 200 cSt.
Further, the alpha-olefin in the alpha-olefin polymer is any one of C6-C20 carbon chain length.
Further, the α -olefin is octene.
Experiments show that the long carbon chain metallocene catalyzed alpha-olefin oligomer is difficult to graft on polypropylene, but the long carbon chain structure can enhance entanglement among polypropylene molecules, so that the inter-microcrystal connection tends to be tight, and the improvement on the physical properties of the composition is more remarkable.
Further, the metallocene-catalyzed alpha-olefin oligomer is added in an amount of 0.1wt% to 5wt% of the polypropylene.
The proper addition amount of the metallocene catalyzed alpha-olefin oligomer is 0.1 to 5 weight percent, and the mechanical property of the final grafted and modified polypropylene is not obviously improved by further addition.
Further, the initiator is a peroxide initiator, and the peroxide initiator comprises at least one of dicumyl peroxide, di-tert-butyl peroxide, benzoyl peroxide, 2, 4-dichloro benzoyl peroxide, tert-butyl peroxylaurate, 2, 5-dimethyl-2, 5-di (tert-butyl peroxy) hexane, di-tert-butyl peroxyisopropyl), tert-butylcumene peroxide, tert-butyl peroxybenzoate and tert-butyl peroxyacetate.
Further, the addition amount of the initiator is 0.1 to 10 weight percent of the polypropylene.
Further, the polypropylene is polypropylene pellets or polypropylene powder, preferably polypropylene powder.
In a second aspect, the present invention provides a metallocene-catalyzed, alpha-olefin polymer grafted polypropylene prepared by the above-described preparation process.
Further, the grafting rate of the metallocene catalyzed alpha-olefin polymer on the polypropylene is 0.55 to 1.28 percent; the tensile yield stress of the alpha-olefin polymer grafted polypropylene catalyzed by the metallocene is 24.8-32.1 MPa; the flexural modulus is 1210-1380 MPa; the notch impact strength of the simply supported beam is 16.8-20.7 KJ/m 2.
Compared with the prior art, the invention has the following beneficial effects:
The invention adopts a solid phase method to introduce the metallocene catalyzed alpha-olefin polymer into the molecular structure of polypropylene, the tensile strength, the bending strength and the impact strength of the obtained grafted polypropylene are all improved, the comprehensive performance of the material is excellent, and the grafted polypropylene can be widely applied to the fields of automobiles, buildings, medical appliances, cables, packages, household appliances and the like; in addition, the preparation method of the grafted modified polypropylene is simple, the process conditions are easy to control, the energy consumption is low, the method is suitable for the existing industrial production process flow, and continuous production can be realized.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples. It will be appreciated by persons skilled in the art that the specific embodiments described herein are for purposes of illustration only and are not intended to be limiting.
The test methods used in the examples are conventional methods unless otherwise specified; the materials, reagents and the like used, unless otherwise specified, are all commercially available. Wherein, the polypropylene powder and the metallocene catalyzed alpha-olefin polymer used in the invention are all derived from China petrochemical metallocene company.
Example 1
The embodiment provides a preparation method of a metallocene-catalyzed alpha-olefin polymer grafted polypropylene, which comprises the steps of adding 2000g of polypropylene powder, 6g of benzoyl peroxide and 100g of a metallocene-catalyzed 1-octene polymer (kinematic viscosity at 100 ℃ for 20 cSt) into a reaction kettle, stirring and mixing for 30min under a nitrogen protection state, heating to 90 ℃ for grafting reaction for 120min to obtain a grafting mixture, repeatedly washing the grafting mixture with absolute ethyl alcohol, extracting with acetone for 24h, and drying to obtain a grafting product, namely the metallocene-catalyzed alpha-olefin polymer grafted polypropylene.
The metallocene catalyzed alpha-olefin polymer grafted polypropylene prepared by the method is added into a double screw extruder to be extruded, cooled and granulated to prepare grafted modified polypropylene powder or granules, the grafted modified polypropylene powder or granules are prepared into a standard style by an injection method to be tested, the tensile property is tested by referring to the GB/T1040 standard, the bending property is tested by referring to the GB/T9341 standard, the impact property is tested by referring to the GB/T1843 standard, and the grafting rate of the product is expressed in terms of the weight ratio of the modifier. The results are shown in Table 1, with the modifiers in Table 1 referring to metallocene-catalyzed alpha-olefin polymers.
Example 2
The embodiment provides a preparation method of a metallocene-catalyzed alpha-olefin polymer grafted polypropylene, which comprises the steps of adding 2000g of polypropylene powder, 6g of benzoyl peroxide and 100g of a metallocene-catalyzed 1-octene polymer (kinematic viscosity at 100 ℃ C. 40 cSt) into a reaction kettle, stirring and mixing for 30min under a nitrogen protection state, heating to 100 ℃ for grafting reaction for 150min to obtain a grafting mixture, repeatedly washing the grafting mixture with absolute ethyl alcohol, extracting with acetone for 24h, and drying to obtain a grafting product, namely the metallocene-catalyzed alpha-olefin polymer grafted polypropylene.
The metallocene catalyzed alpha-olefin polymer grafted polypropylene prepared by the method is added into a double screw extruder to be extruded, cooled and granulated to prepare grafted modified polypropylene powder or granules, the grafted modified polypropylene powder or granules are prepared into a standard style by an injection method to be tested, the tensile property is tested by referring to the GB/T1040 standard, the bending property is tested by referring to the GB/T9341 standard, the impact property is tested by referring to the GB/T1843 standard, and the grafting rate of the product is expressed in terms of the weight ratio of the modifier. The results are shown in Table 1, with the modifiers in Table 1 referring to metallocene-catalyzed alpha-olefin polymers.
Example 3
The embodiment provides a preparation method of a metallocene-catalyzed alpha-olefin polymer grafted polypropylene, which comprises the steps of adding 2000g of polypropylene powder, 8g of benzoyl peroxide and 120g of a metallocene-catalyzed 1-octene polymer (100 cSt) into a reaction kettle, stirring and mixing for 30min under a nitrogen protection state, heating to 120 ℃ for grafting reaction for 150min to obtain a grafting mixture, repeatedly washing the grafting mixture with absolute ethyl alcohol, extracting with acetone for 24h, and drying to obtain a grafting product, namely the metallocene-catalyzed alpha-olefin polymer grafted polypropylene.
The metallocene catalyzed alpha-olefin polymer grafted polypropylene prepared by the method is added into a double screw extruder to be extruded, cooled and granulated to prepare grafted modified polypropylene powder or granules, the grafted modified polypropylene powder or granules are prepared into a standard style by an injection method to be tested, the tensile property is tested by referring to the GB/T1040 standard, the bending property is tested by referring to the GB/T9341 standard, the impact property is tested by referring to the GB/T1843 standard, and the grafting rate of the product is expressed in terms of the weight ratio of the modifier. The results are shown in Table 1, with the modifiers in Table 1 referring to metallocene-catalyzed alpha-olefin polymers.
Example 4
The embodiment provides a preparation method of a metallocene-catalyzed alpha-olefin polymer grafted polypropylene, which comprises the steps of adding 2000g of polypropylene powder, 10g of dicumyl peroxide and 80g of a metallocene-catalyzed 1-hexene polymer (kinematic viscosity at 100 ℃ for 20 cSt) into a reaction kettle, stirring and mixing for 30min under a nitrogen protection state, heating to 110 ℃ for grafting reaction for 90min to obtain a grafting mixture, repeatedly washing the grafting mixture with absolute ethyl alcohol, extracting with acetone for 24h, and drying to obtain a grafting product, namely the metallocene-catalyzed alpha-olefin polymer grafted polypropylene.
The metallocene catalyzed alpha-olefin polymer grafted polypropylene prepared by the method is added into a double screw extruder to be extruded, cooled and granulated to prepare grafted modified polypropylene powder or granules, the grafted modified polypropylene powder or granules are prepared into a standard style by an injection method to be tested, the tensile property is tested by referring to the GB/T1040 standard, the bending property is tested by referring to the GB/T9341 standard, the impact property is tested by referring to the GB/T1843 standard, and the grafting rate of the product is expressed in terms of the weight ratio of the modifier. The results are shown in Table 1, with the modifiers in Table 1 referring to metallocene-catalyzed alpha-olefin polymers.
Example 5
The embodiment provides a preparation method of a metallocene-catalyzed alpha-olefin polymer grafted polypropylene, which comprises the steps of adding 2000g of polypropylene powder, 10g of dicumyl peroxide and 80g of a metallocene-catalyzed 1-decene polymer (kinematic viscosity of 20cSt at 100 ℃) into a reaction kettle, stirring and mixing for 30min under a nitrogen protection state, heating to 110 ℃ for grafting reaction for 90min to obtain a grafting mixture, repeatedly washing the grafting mixture with absolute ethyl alcohol, extracting with acetone for 24h, and drying to obtain a grafting product, namely the metallocene-catalyzed alpha-olefin polymer grafted polypropylene.
The metallocene catalyzed alpha-olefin polymer grafted polypropylene prepared by the method is added into a double screw extruder to be extruded, cooled and granulated to prepare grafted modified polypropylene powder or granules, the grafted modified polypropylene powder or granules are prepared into a standard style by an injection method to be tested, the tensile property is tested by referring to the GB/T1040 standard, the bending property is tested by referring to the GB/T9341 standard, the impact property is tested by referring to the GB/T1843 standard, and the grafting rate of the product is expressed in terms of the weight ratio of the modifier. The results are shown in Table 1, with the modifiers in Table 1 referring to metallocene-catalyzed alpha-olefin polymers.
Example 6
The embodiment provides a preparation method of a metallocene-catalyzed alpha-olefin polymer grafted polypropylene, which comprises the steps of adding 2000g of polypropylene powder, 8g of benzoyl peroxide and 40g of a metallocene-catalyzed 1-octene polymer (kinematic viscosity at 100 ℃ for 20 cSt) into a reaction kettle, stirring and mixing for 30min under a nitrogen protection state, heating to 120 ℃ for grafting reaction for 120min to obtain a grafting mixture, repeatedly washing the grafting mixture with absolute ethyl alcohol, extracting with acetone for 24h, and drying to obtain a grafting product, namely the metallocene-catalyzed alpha-olefin polymer grafted polypropylene.
The metallocene catalyzed alpha-olefin polymer grafted polypropylene prepared by the method is added into a double screw extruder to be extruded, cooled and granulated to prepare grafted modified polypropylene powder or granules, the grafted modified polypropylene powder or granules are prepared into a standard style by an injection method to be tested, the tensile property is tested by referring to the GB/T1040 standard, the bending property is tested by referring to the GB/T9341 standard, the impact property is tested by referring to the GB/T1843 standard, and the grafting rate of the product is expressed in terms of the weight ratio of the modifier. The results are shown in Table 1, with the modifiers in Table 1 referring to metallocene-catalyzed alpha-olefin polymers.
Example 7
The embodiment provides a preparation method of a metallocene-catalyzed alpha-olefin polymer grafted polypropylene, which comprises the steps of adding 2000g of polypropylene powder, 10g of dicumyl peroxide and 150g of a metallocene-catalyzed 1-octene polymer (kinematic viscosity at 100 ℃ for 20 cSt) into a reaction kettle, stirring and mixing for 30min under a nitrogen protection state, heating to 120 ℃ for grafting reaction for 120min to obtain a grafting mixture, repeatedly washing the grafting mixture with absolute ethyl alcohol, extracting with acetone for 24h, and drying to obtain a grafting product, namely the metallocene-catalyzed alpha-olefin polymer grafted polypropylene.
The metallocene catalyzed alpha-olefin polymer grafted polypropylene prepared by the method is added into a double screw extruder to be extruded, cooled and granulated to prepare grafted modified polypropylene powder or granules, the grafted modified polypropylene powder or granules are prepared into a standard style by an injection method to be tested, the tensile property is tested by referring to the GB/T1040 standard, the bending property is tested by referring to the GB/T9341 standard, the impact property is tested by referring to the GB/T1843 standard, and the grafting rate of the product is expressed in terms of the weight ratio of the modifier. The results are shown in Table 1, with the modifiers in Table 1 referring to metallocene-catalyzed alpha-olefin polymers.
Meanwhile, the performance of the polypropylene raw material which is not subjected to grafting modification is detected as a comparison example, and the result is shown in the table 1, and the table 1 shows that the tensile yield stress, the flexural modulus and the impact strength of the polypropylene grafted and modified by the alpha-olefin polymer catalyzed by the metallocene are improved relative to the polypropylene raw material, the improvement of the impact strength is particularly remarkable, and the impact strength is improved by 81% -122% relative to the polypropylene raw material.
In addition, the grafting rate of the example 1 is obviously higher than that of the example 2 and the example 3, and the impact strength is not obviously different, so that the viscosity of the modifier is increased, and the dispersion of the polypropylene material is not facilitated, and the grafting modification is not facilitated.
Example 1 showed no significant difference in grafting ratio and various performance indexes as compared with examples 6 and 7, indicating that the change in the amount of modifier added has little effect on grafting ratio and various properties of the composition in the case of sufficient modifier addition; compared with example 4, the grafting rate of example 1 is not significantly different, and the grafting rate of example 1 is higher than that of example 5, which shows that small molecules are more easily grafted on the polypropylene main chain, and the long-chain branched structure is introduced, so that entanglement effect among PP molecules is increased, the connection among microcrystals tends to be tight, the performance of the composition is improved more obviously, and the impact strength of example 5 is obviously better than that of other examples.
Table 1 performance test index of modified polypropylene of examples 1 to 7
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (7)
1. A process for the preparation of a metallocene-catalyzed, alpha-olefin polymer grafted polypropylene comprising the steps of:
The polypropylene, the metallocene catalyzed alpha-olefin oligomer and an initiator are subjected to grafting reaction for 10 to 300 minutes at the temperature of between 90 and 120 ℃ in the atmosphere of protective gas to prepare the metallocene catalyzed alpha-olefin polymer grafted polypropylene;
The addition amount of the metallocene catalyzed alpha-olefin oligomer is 0.1 to 10 weight percent of the polypropylene; the metallocene-catalyzed alpha-olefin oligomer comprises at least one of an alpha-olefin polymer having a degree of polymerization of 2 to 10; the metallocene-catalyzed alpha-olefin oligomer has a kinematic viscosity at 100 ℃ of from 2 to 200 cSt; the alpha-olefin in the alpha-olefin polymer is any one of C6-C20 carbon chain length.
2. The process of claim 1 wherein the α -olefin is octene.
3. The method of claim 1, wherein the metallocene-catalyzed alpha-olefin oligomer is added in an amount of 0.1wt% to 5wt% of the polypropylene.
4. The method of claim 1, wherein the initiator is a peroxide initiator comprising at least one of dicumyl peroxide, di-t-butyl peroxide, benzoyl peroxide, 2, 4-dichlorobenzoyl peroxide, t-butyl peroxylaurate, 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane, di-t-butylperoxy isopropyl), t-butylcumene peroxide, t-butyl peroxybenzoate, and t-butyl peroxyacetate.
5. The preparation method according to claim 1, wherein the initiator is added in an amount of 0.1 to 10wt% of the polypropylene.
6. The method of claim 1, wherein the polypropylene is polypropylene pellets or polypropylene powder.
7. A metallocene-catalyzed alpha-olefin polymer grafted polypropylene produced by the process of any of claims 1-6.
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