CN114410016B - Polypropylene composition, method for preparing toughened impact-resistant copolymer polypropylene resin, toughened impact-resistant copolymer polypropylene resin and application thereof - Google Patents
Polypropylene composition, method for preparing toughened impact-resistant copolymer polypropylene resin, toughened impact-resistant copolymer polypropylene resin and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of polypropylene, in particular to a polypropylene composition, a method for preparing a toughening impact-resistant copolymerized polypropylene resin, the toughening impact-resistant copolymerized polypropylene resin and application thereof, wherein the polypropylene composition comprises 100 parts by weight of copolymerized polypropylene, 0.01-0.2 part by weight of nucleating agent and 0.1-3 parts by weight of performance improver; the performance modifier comprises an imidazole-cured epoxy resin and a peroxide. The notch impact strength of the copolymer polypropylene resin provided by the invention is as high as 10kJ/m at normal temperature 2 The notched impact strength at-20 ℃ is up to 5.3kJ/m 2 The melt flow rate under the conditions of 230 ℃ and 2.16kg load is up to 43g/10min, and the high-toughness high-fluidity high-toughness high-strength plastic composite material has the advantages of good fluidity and high toughness, and can be directly used for producing products such as daily necessities, automobiles, household appliances and the like.
Description
Technical Field
The invention relates to the technical field of polypropylene, in particular to a polypropylene composition, a method for preparing toughened anti-impact copolymer polypropylene resin, the toughened anti-impact copolymer polypropylene resin and application thereof.
Background
Polypropylene is a semi-crystalline polymer with excellent comprehensive properties, and is widely applied in the fields of automobiles, household appliances, buildings, packaging, agriculture and the like. However, polypropylene has high notch sensitivity and low impact strength, and is particularly obvious at low temperature, which greatly limits further popularization and application of polypropylene.
The high-fluidity polypropylene can reduce the processing temperature, reduce the energy consumption, shorten the molding period and improve the production efficiency, and the high-impact copolymer polypropylene has higher added value and better impact resistance than the impact copolymer polypropylene, and can be widely applied to modified materials which are required to maintain good toughness, strength and high temperature resistance.
In the prior art, the melt flow rate and the impact resistance of the copolymerized polypropylene prepared by adopting the hydrogen preparation method are not high, and the requirements of the fields of automobiles, household appliances, buildings, packaging, agriculture and the like are hardly met. Therefore, it is necessary to improve the flowability and impact resistance of the polypropylene copolymer produced by the hydrogen blending method.
Disclosure of Invention
The invention aims to solve the problem that the melt flow rate and the impact resistance of the copolymerized polypropylene prepared by a hydrogen preparation method in the prior art are not high, and provides a polypropylene composition, a method for preparing a toughened impact-resistant copolymerized polypropylene resin, the toughened impact-resistant copolymerized polypropylene resin and application thereof.
In order to achieve the above object, the present invention provides a polypropylene composition, wherein the polypropylene composition comprises 100 parts by weight of copolymerized polypropylene, 0.01 to 0.2 parts by weight of a nucleating agent, and 0.1 to 3 parts by weight of a performance improver; the performance modifier comprises an imidazole-cured epoxy resin and a peroxide.
In a second aspect, the present invention provides a method of preparing a toughened impact copolymer polypropylene resin, the method comprising: the components in the polypropylene composition of the first aspect are mixed and then extruded and granulated in a double-screw extruder to obtain the toughened impact-resistant copolymerized polypropylene resin.
In a third aspect, the present invention provides a toughened impact copolymer polypropylene resin prepared by the method of the second aspect.
In a fourth aspect, the present invention provides an application of the toughened impact-resistant copolymer polypropylene resin in the field of daily necessities, automobiles or household appliances.
The notch impact strength of the toughened impact-resistant copolymer polypropylene resin provided by the invention is as high as 10kJ/m at normal temperature 2 The notched impact strength at-20 ℃ is up to 5.3kJ/m 2 The melt flow rate under the conditions of 230 ℃ and 2.16kg load is up to 43g/10min, and the high-toughness high-fluidity high-toughness high-strength plastic composite material has the advantages of good fluidity and high toughness, and can be directly used for producing products such as daily necessities, automobiles, household appliances and the like.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
As previously described, the present invention provides in a first aspect a polypropylene composition comprising 100 parts by weight of a copolymerized polypropylene, 0.01 to 0.2 parts by weight of a nucleating agent and 0.1 to 3 parts by weight of a performance improver; the performance modifier comprises an imidazole-cured epoxy resin and a peroxide.
The performance improver can improve the melt flow rate of polypropylene, is particularly effective for the copolymerized polypropylene which is not easy to obtain high melt flow rate by a hydrogen regulation method in the production process, can react with the impact copolymerized polypropylene, improves the impact resistance of the impact copolymerized polypropylene, obviously improves the normal-temperature notch impact strength, the low-temperature notch impact strength and the melt flow rate of the prepared polypropylene resin, and can be directly used for producing products such as daily necessities, automobiles, household appliances and the like.
In some preferred embodiments of the present invention, the polypropylene composition comprises 100 parts by weight of copolymerized polypropylene, 0.01 to 0.05 parts by weight of a nucleating agent, and 0.2 to 1 part by weight of a performance improver in order to further improve the flowability and impact resistance of the prepared polypropylene resin.
According to the present invention, in order to improve the melt flow rate and impact resistance of the polypropylene composition, it is preferable that the imidazole-cured epoxy resin is selected from at least one of 2-methylimidazole-cured diglycidyl phthalate, 2-phenylimidazole-cured diglycidyl phthalate, 2-methylimidazole-cured terephthalyl diglycidyl ester, 2-phenylimidazole-cured terephthalyl diglycidyl ester, 2-methylimidazole-cured bisphenol a diglycidyl ether, and 2-phenylimidazole-cured bisphenol a diglycidyl ether; preferably 2-methylimidazole-cured diglycidyl phthalate and/or 2-phenylimidazole-cured bisphenol A diglycidyl ether.
According to the present invention, in order to further improve the melt flow rate and impact resistance of the polypropylene composition, preferably, the peroxide is at least one selected from the group consisting of dicumyl peroxide, 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane and 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane; further preferred are 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane and/or 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane.
According to the present invention, it is further preferred that the weight ratio of the imidazole-cured epoxy resin to the peroxide is 1 to 50:1, for example, may be 1: 1. 5: 1. 10: 1. 15: 1. 20:1. 25: 1. 30: 1. 35: 1. 40: 1. 45: 1. 50:1 or any of the range of values consisting of any two ratios mentioned above, preferably from 5 to 20:1. under the above preferred conditions, the normal temperature notched impact strength, the low temperature notched impact strength and the melt flow rate of the polypropylene composition can be improved.
In a preferred embodiment of the present invention, in order to further improve the toughness of the polypropylene composition, the property improver is preferably selected from one of composition a consisting of 2-methylimidazole-cured diglycidyl phthalate and 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane, composition B consisting of 2-methylimidazole-cured diglycidyl phthalate and 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane, composition C consisting of 2-methylimidazole-cured terephthaloyl diglycidyl ester and 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane, and composition D consisting of 2-methylimidazole-cured terephthaloyl diglycidyl ester and 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane.
In the present invention, the method for preparing the performance improver may be known to those skilled in the art, and in a preferred embodiment of the present invention, the method for preparing the performance improver includes:
s1, dispersing an imidazole compound and epoxy resin in an organic solvent to obtain an oil phase;
s2, adding the oil phase into an aqueous solution containing sodium dodecyl sulfate, and reacting for 4 hours at 40 ℃ until dichloromethane is completely volatilized; and (3) obtaining a suspension, and centrifuging, washing and drying the suspension to obtain the imidazole-cured epoxy resin.
According to the invention, preferably the imidazole is selected from 2-methylimidazole and/or 2-phenylimidazole.
According to the present invention, preferably, the epoxy resin is selected from at least one of diglycidyl phthalate, terephthalyl diglycidyl ester, and bisphenol a diglycidyl ether.
According to the present invention, preferably, the organic solvent is methylene chloride.
According to the present invention, in order to further improve the rigidity index, such as flexural strength and flexural modulus, of the polypropylene composition, preferably, the nucleating agent is selected from at least one of talc, a metal carboxylate nucleating agent and an organophosphate nucleating agent; further preferably, the metal carboxylate nucleating agent is at least one selected from sodium benzoate, bis (p-tert-butylbenzoic acid) hydroxyaluminum, (1 r,2r,3s,4 s) -rel-bicyclo [2.2.1] hepta-2, 3-dicarboxylic acid disodium salt (nucleating agent HPN-68L), (1 r,2 s) -rel-1, 2-cyclohexanedicarboxylic acid calcium salt (nucleating agent HPN-20E), nucleating agent HPN-505, bis (4-tert-butylbenzoic acid) aluminum hydroxide (nucleating agent NAA-326); further preferably, the organophosphate nucleating agent is selected from at least one of the nucleating agents sodium 2,2' -methyl-bis- (4, 6-di-tert-butylphenyl) phosphate (nucleating agent NA-11), bis [2,2' -methyl-bis- (4, 6-di-tert-butylphenyl) phosphate ] hydroxyaluminum (nucleating agent NA-21), nucleating agent NA-27 and 2,2' -methylene-bis- (4, 6-di-tert-butylphenyl) phosphate (nucleating agent NAP-62).
In some preferred embodiments of the invention, the melt index of the polypropylene copolymer at 230℃and a load of 2.16kg is 21-30g/10min; under the above preferred conditions, the modifying effect of the property improver on the polypropylene composition is particularly remarkable.
According to the present invention, preferably, the polypropylene copolymer is prepared by a Novolen process, and under preferred conditions, the method for preparing the polypropylene copolymer comprises: in the presence of an NHP catalyst, contacting liquid propylene with ethylene for reaction to obtain polypropylene copolymer; wherein the reaction conditions include: the temperature is 70-85 ℃; the pressure is 2.5-3.5MPa; further preferably, the ethylene is used in an amount of 6-15wt% of the propylene, for example, 6wt%, 8wt%, 9wt%, 10wt%, 12wt%, 15wt% or any value in the range of any two values mentioned above, most preferably 9wt%.
According to the present invention, to further optimize the properties of the polypropylene composition, the polypropylene composition further comprises an antioxidant and an acid neutralizer; preferably, the polypropylene composition further comprises 0.05 to 0.5 parts by weight of an antioxidant and 0.01 to 0.2 parts by weight of an acid neutralizer based on 100 parts by weight of the copolymerized polypropylene.
According to the invention, preferably, the acid neutralizer is selected from calcium stearate and/or hydrotalcite.
According to the present invention, the antioxidant is selected from at least one of hindered phenol antioxidants and at least one of phosphite antioxidants; further preferably, the hindered phenol antioxidant is selected from at least one of pentaerythritol tetrakis [ beta- (3, 5-di-t-butyl-4-hydroxyphenyl) propionate (antioxidant 1010), 1,3, 5-tris (3, 5-di-t-butyl-4-hydroxybenzyl) isocyanuric acid (antioxidant 3114) and 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-t-butyl-4-hydroxybenzyl) benzene (antioxidant 330); preferably an antioxidant 1010.
Preferably, the phosphite antioxidant is selected from tris [2, 4-di-tert-butylphenyl ] phosphite (antioxidant 168) and/or tetrakis (2, 4-di-tert-butylphenyl) -4,4' -biphenylbisphosphite; preferably an antioxidant 168.
In a second aspect, the present invention provides a method of preparing a toughened impact copolymer polypropylene resin, the method comprising: the components in the polypropylene composition of the first aspect are mixed and then extruded and granulated in a double-screw extruder to obtain the toughened impact-resistant copolymerized polypropylene resin.
According to the invention, preferably, the extrusion temperature is 180-240 ℃.
The performance improver provided by the invention can be directly subjected to modification reaction with the polypropylene composition produced by the hydrogen regulating method in a double-screw extruder.
In a third aspect, the present invention provides a toughened impact copolymer polypropylene resin prepared by the method of the second aspect.
According to the present invention, preferably, the toughened impact copolymer polypropylene resin has a melt index of 38 to 45g/10min at 230℃under a load of 2.16 kg; the notched impact strength of the simply supported beam at 23 ℃ is more than or equal to 8kJ/m 2 The method comprises the steps of carrying out a first treatment on the surface of the The notched impact strength of the simply supported beam at the temperature of minus 20 ℃ is more than or equal to 4.8kJ/m 2 。
In a fourth aspect, the present invention provides an application of the toughened impact-resistant copolymer polypropylene resin in the field of daily necessities, automobiles or household appliances.
In the following examples, MI (melt index, 230 ℃ C., load 2.16 kg) was obtained using ISO 1133-2011 test; impact strength at 23℃was measured according to ISO 179-2010; impact strength at-20 ℃ is tested by the method of ISO 179-2010; tensile strength was tested using methods of ISO 527-2012; flexural modulus was tested using the method of ISO 178-2010; the heat distortion temperature is obtained by an ISO 75-2013 test; the crystallization temperature was measured using ISO 11357-2018.
1. The preparation method of the methyl imidazole cured diglycidyl phthalate comprises the following steps:
6g of 2-methylimidazole and 90g of diglycidyl phthalate were dispersed in 40mL of methylene chloride, and sonicated until the 2-methylimidazole and diglycidyl phthalate were completely dissolved, to obtain an oil phase.
The oil phase was added to 100mL of an aqueous solution of sodium dodecyl sulfate (0.1 wt%) and reacted at 40 ℃ for 4h until the dichloromethane was completely volatilized; and (3) obtaining a suspension, and centrifuging, washing and drying the suspension to obtain the methylimidazole solidified diglycidyl phthalate.
2. The preparation method of the 2-phenylimidazole solidified bisphenol A diglycidyl ether comprises the following steps:
6g of 2-phenylimidazole and 100g of bisphenol A diglycidyl ether were dispersed in 40mL of methylene chloride, and sonicated until the 2-phenylimidazole and bisphenol A diglycidyl ether were completely dissolved, yielding an oil phase.
The oil phase was added to 100mL of an aqueous solution of sodium dodecyl sulfate (0.1 wt%) and reacted at 40 ℃ for 4h until the dichloromethane was completely volatilized; and (3) obtaining a suspension, and centrifuging, washing and drying the suspension to obtain the 2-phenylimidazole solidified bisphenol A diglycidyl ether.
In the following examples, the composition of the modifier is shown in Table 1.
TABLE 1
Note that: * Weight ratio of imidazole cured epoxy resin to peroxide
Preparation example
Preparation of the copolymer polypropylene:
taking NHP as a catalyst, and carrying out polymerization reaction on liquid propylene with the purity of 99.7% and ethylene with the purity of 99.99% on a Novolen process gas-phase polymerization polypropylene device to obtain copolymer polypropylene;
the temperature of the polymerization reaction is 80 ℃; the pressure is 3.2MPa; the weight ratio of ethylene to propylene is 9:100; the melt index of the resulting copolymer polypropylene was 28g/10min.
Examples 1 to 22
Uniformly mixing the copolymerized polypropylene resin, the hindered phenol antioxidant, the phosphite antioxidant, the acid neutralizer, the nucleating agent and the performance improver, and then extruding and granulating in a double-screw extruder to obtain the toughened and impact-resistant copolymerized polypropylene resin, wherein the extrusion and granulating temperature is 230 ℃.
The amounts of the respective raw materials are shown in Table 2, and the physical properties of the resulting polypropylene copolymer resins are shown in Table 4.
TABLE 2
Comparative examples 1 to 15
The procedure of example 1 was followed except that the amounts of the respective raw materials were as shown in Table 3, and the physical properties of the resulting polypropylene copolymer resins were as shown in Table 4.
TABLE 3 Table 3
TABLE 4 Table 4
As can be seen from the results of Table 4, the melt flow rate and processability of the copolymer polypropylene resin obtained in the examples of the present invention are remarkably improved under the condition that the tensile strength and flexural modulus are substantially unchanged, relative to those of the copolymer polypropylene of the comparative exampleLifting; normal temperature simple beam notch impact strength not less than 8.2kJ/m 2 Compared with the polypropylene copolymer of the comparative example, the polypropylene copolymer is obviously improved by more than 40 percent; the polypropylene resin can be directly used for producing daily necessities, automobiles and household appliances without adding other auxiliary agents.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (13)
1. A polypropylene composition, characterized in that the polypropylene composition comprises 100 parts by weight of a copolymerized polypropylene, 0.01 to 0.2 parts by weight of a nucleating agent and 0.1 to 3 parts by weight of a performance improver;
the performance modifier comprises an imidazole-cured epoxy resin and a peroxide;
wherein the imidazole-cured epoxy resin is selected from at least one of 2-methylimidazole-cured diglycidyl phthalate, 2-phenylimidazole-cured diglycidyl phthalate, 2-methylimidazole-cured diglycidyl terephthalate, 2-phenylimidazole-cured diglycidyl terephthalate, 2-methylimidazole-cured bisphenol A diglycidyl ether and 2-phenylimidazole-cured bisphenol A diglycidyl ether;
the peroxide is at least one selected from dicumyl peroxide, 2, 5-dimethyl-2, 5-di (tertiary butyl peroxy) hexane and 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxynonane;
the weight ratio of the imidazole cured epoxy resin to the peroxide is 1-50:1, a step of;
the nucleating agent is at least one selected from talcum powder, metal carboxylate nucleating agent and organic phosphate nucleating agent.
2. The polypropylene composition according to claim 1, wherein the polypropylene composition comprises 100 parts by weight of copolymerized polypropylene, 0.01 to 0.05 parts by weight of a nucleating agent and 0.2 to 1 parts by weight of a performance improver.
3. Polypropylene composition according to claim 1, wherein the imidazole-cured epoxy resin is selected from 2-methylimidazole-cured diglycidyl phthalate and/or 2-phenylimidazole-cured bisphenol a diglycidyl ether.
4. The polypropylene composition according to claim 1, wherein the performance modifier is selected from one of composition a consisting of 2-methylimidazole-cured diglycidyl phthalate and 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane, composition B consisting of 2-methylimidazole-cured diglycidyl phthalate and 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane, composition C consisting of 2-phenylimidazole-cured bisphenol a diglycidyl ether and 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane, and composition D consisting of 2-phenylimidazole-cured bisphenol a diglycidyl ether and 3,6, 9-triethyl-3, 6, 9-trimethyl-1, 4, 7-triperoxonane.
5. The polypropylene composition according to any one of claim 1, wherein the metal carboxylate nucleating agent is selected from at least one of sodium benzoate, bis (p-tert-butylbenzoate) aluminum hydroxy, (1 r,2r,3s,4 s) -rel-bicyclo [2.2.1] hepta-2, 3-dicarboxylic acid disodium salt and (1 r,2 s) -rel-1, 2-cyclohexanedicarboxylic acid calcium salt;
and/or the organic phosphate nucleating agent is selected from nucleating agent sodium 2,2 '-methyl-bis- (4, 6-di-tert-butylphenyl) phosphate and/or bis [2,2' -methyl-bis- (4, 6-di-tert-butylphenyl) phosphate ] hydroxyaluminum.
6. The polypropylene composition according to any one of claims 1 to 5, wherein the copolymer polypropylene has a melt index of 21-30g/10min at 230 ℃ and under load of 2.16 kg.
7. The polypropylene composition according to any one of claims 1 to 5, wherein the polypropylene composition further comprises an antioxidant and an acid neutralizer.
8. The polypropylene composition according to claim 7, wherein the acid neutralizer is selected from calcium stearate and/or hydrotalcite.
9. The polypropylene composition according to claim 7, wherein the antioxidant is selected from at least one of hindered phenol antioxidants and at least one of phosphite antioxidants.
10. The polypropylene composition according to claim 9, wherein the hindered phenol antioxidant is selected from at least one of pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], 1,3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) isocyanuric acid and 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene;
and/or the phosphite antioxidant is selected from tris [2, 4-di-tert-butylphenyl ] phosphite and/or tetrakis (2, 4-di-tert-butylphenyl) -4,4' -biphenylbisphosphite.
11. A method of preparing a toughened impact copolymer polypropylene resin, the method comprising: mixing the components in the polypropylene composition according to any one of claims 1-10, and extruding and granulating in a twin-screw extruder to obtain the toughened impact copolymer polypropylene resin; the extrusion temperature is 180-240 ℃.
12. A toughened impact copolymer polypropylene resin prepared by the process of claim 11; the melt flow rate of the toughened impact copolymer polypropylene resin is 38-45g/10min under the conditions of 230 ℃ and load of 2.16 kg; the notched impact strength of the simply supported beam at 23 ℃ is more than or equal to 8kJ/m 2 The method comprises the steps of carrying out a first treatment on the surface of the The notched impact strength of the simply supported beam at the temperature of minus 20 ℃ is more than or equal to 4.8kJ/m 2 。
13. Use of the toughened impact co-polypropylene resin of claim 12 in the field of consumer goods and/or automobiles.
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| JPH0741634A (en) * | 1993-07-30 | 1995-02-10 | Tonen Corp | Molded article of polypropylene resin composition |
| CN1425709A (en) * | 2002-12-19 | 2003-06-25 | 上海交通大学 | Process for preparing dynamic cured epoxy resin/polypropylene blend |
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| JPH0741634A (en) * | 1993-07-30 | 1995-02-10 | Tonen Corp | Molded article of polypropylene resin composition |
| CN1425709A (en) * | 2002-12-19 | 2003-06-25 | 上海交通大学 | Process for preparing dynamic cured epoxy resin/polypropylene blend |
| CN1472246A (en) * | 2003-06-19 | 2004-02-04 | 上海交通大学 | Reinforced toughened polypropylene material preparing method |
| CN109776967A (en) * | 2019-02-24 | 2019-05-21 | 成都市水泷头化工科技有限公司 | A kind of polypropylene dedicated material and preparation method for bumper |
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| 江学良,张勇,张隐西.动态固化聚丙烯/环氧树脂共混物的制备工艺研究.中国塑料.2003,(10), * |
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