CN112724580A - High-fluidity high-impact halogen-free flame-retardant polypropylene material and preparation method and application thereof - Google Patents
High-fluidity high-impact halogen-free flame-retardant polypropylene material and preparation method and application thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
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Abstract
The invention discloses a high-fluidity high-impact halogen-free flame-retardant polypropylene material, a preparation method and application thereof. Therefore, the high-fluidity high-impact halogen-free flame-retardant polypropylene material prepared by the invention has good flame-retardant property, good fluidity, strong toughness and rigidity, and excellent impact property and antistatic property.
Description
Technical Field
The invention relates to the technical field of modification of high polymer materials, and particularly relates to a high-fluidity high-impact halogen-free flame-retardant polypropylene material, and a preparation method and application thereof.
Background
The main components of the flame-retardant modified polypropylene material, such as a phosphorus-nitrogen flame-retardant system, are composed of a dehydrating agent (acid source), a char forming agent (char source) and an expanding agent (gas source), the flame-retardant mechanism is to promote the polymer to form char, and a layer of expanded porous homogeneous char layer is formed on the surface of the material, so that the functions of heat insulation, oxygen isolation, smoke suppression and molten drop prevention are achieved, and the purpose of flame retardance is achieved.
However, the halogen-free flame retardant contains hydrophilic functional groups such as polyhydroxy, amino and the like, which causes poor compatibility with polypropylene and seriously affects the toughness of the modified polypropylene material, if the elastomer is added for modification, too many elastomers can cause the reduction of the rigidity and the fluidity of the material, too few elastomers have unobvious toughening, and the rigidity and toughness balance cannot be achieved, and the halogen-free flame retardant also causes the deterioration of the fluidity of the material, which is not favorable for injection molding of the material.
For example, chinese patent CN201910267586.0 (published japanese 2019.8.2) discloses an ultrahigh-fluidity halogen-free flame-retardant polypropylene composite material and a preparation method thereof, the halogen-free flame-retardant polypropylene composite material is prepared from polypropylene, piperazine pyrophosphate flame retardant, compatilizer such as polypropylene grafted maleic anhydride, hyperdispersant, high aspect ratio filler and other components, and can improve the fluidity of the flame-retardant material to a certain extent, but the impact property of the material is poor.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defect and the defect that the existing halogen-free flame-retardant polypropylene material cannot have good fluidity and impact property at the same time, and provides a high-fluidity high-impact halogen-free flame-retardant polypropylene material which not only has good fluidity, but also has excellent impact property, toughness, rigidity and good antistatic property.
The invention also aims to provide a preparation method of the high-flow high-impact halogen-free flame-retardant polypropylene material.
The invention also aims to provide application of the high-flow high-impact halogen-free flame-retardant polypropylene material.
The above purpose of the invention is realized by the following technical scheme:
a high-fluidity high-impact halogen-free flame-retardant polypropylene material comprises the following components in parts by mass:
wherein the flow modifier is a stearylamine-based multipolymer; the interface modifier is one or more of N, N-bis-hydroxyethyl alkylamide, stearic acid diethanolamide, oleic acid diethanolamide, laureth-4 and polyethylene glycol stearate.
The invention takes polypropylene as a matrix material, and then adds a certain proportion of flow modifier and interface modifier for compounding, because the interface modification auxiliary agent contains alkyl chain segments, the compatibility with the polypropylene matrix and the toughening agent is better, in addition, the interface modifier also contains polyhydroxy group, which can interact with the halogen-free flame retardant through Van der Waals force, thereby improving the compatibility of the halogen-free flame retardant in the system, in addition, the flow modifier is also used as an internal lubricant, the flow property of the material can be greatly improved, meanwhile, the mechanical property of the material is not influenced, so the flow modifier, the interface modifier and the toughening agent can play a role in synergistically improving the fluidity of the halogen-free flame-retardant polypropylene material, the interface modification auxiliary agent and the toughening agent have a synergistic toughening effect, the material has excellent impact performance, the rigidity and toughness are balanced, and the flame retardant property can be well exerted. The added interface modifier contains groups of polyamino and hydroxyl, and is matched with the halogen-free flame retardant, and the combination of hydrogen bonds and moisture in the air is utilized, so that a water film is easily formed on the surface of a product, the surface resistivity is reduced, static charge leakage is accelerated, and an antistatic effect is achieved.
Preferably, the composition comprises the following components in parts by mass:
preferably, the interface modifier is one or more of N, N-bis-hydroxyethyl alkylamide, stearic acid diethanolamide and oleic acid diethanolamide.
Preferably, the melt flow rate of the polypropylene at 230 ℃ and 2.16kg is 20-50 g/10 min. The polypropylene resin selected by the invention has better fluidity and is beneficial to molding processing.
More preferably, the melt flow rate of the polypropylene at 230 ℃ and 2.16kg is 20-30 g/10 min.
Preferably, the polypropylene is one or more of homo-polypropylene, propylene-ethylene block copolymer, propylene-ethylene random copolymer and propylene-1-butylene random block.
More preferably, the polypropylene is a propylene-ethylene block copolymer.
Preferably, the halogen-free flame retardant is one or more of a mixture of piperazine pyrophosphate and melamine pyrophosphate, a mixture of piperazine pyrophosphate and melamine polyphosphate, and a mixture of high molecular weight ammonium polyphosphate and triazine charring agent.
More preferably, the halogen-free flame retardant is a mixture of piperazine pyrophosphate and melamine pyrophosphate.
Preferably, the melt index of the toughening agent is 1-15 g/10 min. The toughening agent of the invention is beneficial to molding processing.
More preferably, the melt index of the toughening agent is 6-10 g/10 min.
The toughening agent of the invention comprises but is not limited to one or more of ethylene-octene copolymer, ethylene-butene copolymer, ethylene-propylene triblock copolymer, styrene-butadiene-styrene block copolymer or maleic anhydride graft thereof.
Preferably, the toughening agent is a copolymer of ethylene-octene.
Preferably, the anti-dripping agent also comprises one or more of a main antioxidant, a secondary antioxidant, an anti-dripping aid, a lubricant and other processing aids.
Preferably, the method further comprises the following steps of:
the primary antioxidant of the present invention includes, but is not limited to, one or more of tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (Irganox 1010), tris (3, 5-di-tert-butyl-4-hydroxybenzyl) isocyanurate (antioxidant 3114), 1, 3, 5-tris (4-tert-butyl-3-hydroxy-2.6-dimethylbenzyl) isocyanurate (Cyanox1790), ethylenebis (oxyethylene) bis [3- (5-tert-butyl-4-hydroxy-m-tolyl) propionate ] (Irganox24), and 3, 9-bis [1, 1-dimethyl-2- [ (3-tert-butyl-4-hydroxy-5-methylphenyl) propionyloxy ] ethyl ] -2,4,8, 10-tetraoxaspiro [5.5] undecane (Suilizer GA 80/k-AO 80) Several kinds of them.
The auxiliary antioxidant comprises but is not limited to one or more of 1, 3, 5-tri (4-tert-butyl-3-hydroxy-2, 6-dimethylbenzyl) isocyanurate, diethylene glycol bis-beta- (3-tert-butyl-4-hydroxy-5-methylphenyl), pentaerythritol bis (2, 4-tert-butylphenyl) diphosphite and thioester antioxidants.
The anti-dripping auxiliary agent comprises but is not limited to one or more of uncoated polytetrafluoroethylene, polytetrafluoroethylene with an outer layer coated with a layer of SAN or PMMA, PS, and a copolymer of polytetrafluoroethylene.
The lubricant of the present invention includes, but is not limited to, one or more of polyethylene wax, polypropylene wax, ethylene bis stearamide, 5-butyl oxazole-2, 4-dione, calcium stearate, magnesium stearate, and the like.
The other processing aids include, but are not limited to, calcium stearate (CaSt), zinc stearate, and one or more of stearic acid, magnesium stearate, and Ethylene Bis Stearamide (EBS).
The preparation method for protecting the high-fluidity high-impact halogen-free flame-retardant polypropylene material comprises the following steps:
uniformly mixing polypropylene, a halogen-free flame retardant, a toughening agent, a flow modifier, an interface modifier, a main antioxidant, an auxiliary antioxidant, an anti-dripping auxiliary agent and a lubricant, melting and blending, extruding and granulating, and drying to obtain the high-flow high-impact halogen-free flame retardant polypropylene material.
Preferably, the rotation speed of the melt blending is 250-350 rpm.
Preferably, the temperature of each section of screw rod during extrusion is 150-160 ℃ in the first zone, 160-170 ℃ in the second zone, 180-190 ℃ in the third zone, 180-190 ℃ in the fourth zone, 180-190 ℃ in the fifth zone, 190-200 ℃ in the mouth mold, 300-500 r/min of the main engine rotation speed and lower than 0.1MPa of vacuum degree.
The invention also protects the application of the high-flow high-impact halogen-free flame-retardant polypropylene material in preparing a flame-retardant material. The high-fluidity high-impact halogen-free flame-retardant polypropylene material disclosed by the invention has good fluidity, excellent toughness, rigidity and impact resistance, and the flame-retardant property reaches V-0 level.
Compared with the prior art, the invention has the beneficial effects that:
the invention takes polypropylene as a matrix material, and then adds a certain proportion of flow modifier and interface modifier, because the interface modifier contains alkyl chain segment and polyhydroxy group, the compatibility with polypropylene, toughening agent and halogen-free flame retardant is better, the flow modifier can be used as an internal lubricant to greatly improve the flow property of the material, the flow modifier and the interface modifier are compounded and the toughening agent can synergistically improve the fluidity of each component in the system, the interface modification auxiliary agent and the toughening agent play a role in synergistic toughening, and simultaneously the mechanical property of the material is hardly influenced, thereby realizing the balance of rigidity and toughness. Therefore, the high-fluidity high-impact halogen-free flame-retardant polypropylene material prepared by the invention has good flame-retardant property, good fluidity, strong toughness and rigidity, and excellent impact property and antistatic property.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the present invention is not limited to the examples in any way. The starting reagents employed in the examples of the present invention are, unless otherwise specified, those that are conventionally purchased.
The raw materials used in the respective examples and comparative examples:
polypropylene: propylene-ethylene block copolymer, PP EP548R, melt flow index: 26.0g/10min (230 ℃ @2.16kg) Zhonghai shell brand;
halogen-free flame retardant: piperazine pyrophosphate and melamine pyrophosphate mixture, FP-2200, aldrich japan;
a toughening agent: ethylene-octene copolymer POE 8137 (melt index: 13g/10min, 190 ℃/2.16kg), Dow chemical;
flow modifier: stearamide multipolymer, SP500, Guangzhou entropy energy Innovation materials GmbH;
an interface modifier: n, N-bis-hydroxyethyl alkylamides, dendrimers, A4-66, Waishahen molecular New materials, Inc.;
main antioxidant: pentaerythrityl tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], Irganox1010, BASF, germany;
auxiliary antioxidant: pentaerythritol bis (2, 4-tert-butylphenyl) diphosphite, Irganox 168, Pasteur BASF, Germany;
anti-dripping aid: polytetrafluoroethylene, SN80-SA7, Guangzhou entropy energy Innovative materials shares, Inc.;
lubricant: ethylene bis stearamide, EBS B40, guangzhou runfeng chemical ltd.
Example 1
A high-flow high-impact halogen-free flame-retardant polypropylene material comprises the components in parts by mass as shown in the following table 1.
The preparation method of the high-flow high-impact halogen-free flame-retardant polypropylene material comprises the following steps:
uniformly mixing polypropylene, a halogen-free flame retardant, a toughening agent, a flow modifier, an interface modifier, a main antioxidant, an auxiliary antioxidant, an anti-dripping auxiliary agent and a lubricant, and then mixing for 3 minutes in a high-speed mixer; carrying out melt blending on the mixed mixture by adopting a double-screw extruder, wherein the feeding speed of the double-screw extruder is 350 rpm; the temperatures of the screws of the sections of the double-screw extruder from the feed inlet to the head are preferably 160 ℃ in the first zone, 170 ℃ in the second zone, 190 ℃ in the third zone, 190 ℃ in the fourth zone, 190 ℃ in the fifth zone, 200 ℃ in the neck mold, 500r/min of the rotating speed of the main machine and lower than 0.1MPa of vacuum degree. The components are uniformly mixed by screw shearing and mixing, and then are granulated and dried to obtain the composite material.
Examples 2 to 9 and comparative examples 1 to 7
The preparation method of the halogen-free flame-retardant polypropylene material of each example and the comparative example is the same as that of example 1, and the components and the parts by mass thereof are shown in the following table 1:
TABLE 1 Components and parts by mass of examples and comparative examples
Performance testing
1. Test method
(1) Melt flow rate: according to ISO 1133-2005, the test conditions are 230 ℃ and 2.16 Kg;
(2) tensile strength: the test is carried out according to ISO 527 standard, the test sample is a type I test sample, and the test equipment is a tensile testing machine Z020 of Zwick company in Germany;
(3) flexural strength, flexural modulus: the test is carried out according to ISO 178 standard, the size of a sample is 4mm multiplied by 10mm multiplied by 80mm, and the test equipment is a bending tester Z005 of Zwick Roell company in Germany;
(4) notched izod impact strength: the test was carried out according to ISO 180 standard, with specimen dimensions of 4mm by 10mm by 80mm and a notch depth of 2 mm. The test equipment is an impact tester HIT2.7P from Zwick roll, germany;
(5) and (3) surface resistivity test: according to GB/T1410-2006.
(6) And (3) testing the combustion grade: test bar size according to UL 94-2016: a 125mm × 12.5mm × 1.5mm sample strip, test equipment Plastics HVUL h.v.f.c burner, usa ATLAS;
2. test results
TABLE 2 results of the performance test of each example and comparative example
The results in Table 2 show that the flame retardant performance can reach V-0 level, and the data of each embodiment of the invention show that the interface modification auxiliary agent and the toughening agent have a synergistic toughening effect, and have high toughness and rigidity, high impact strength and good fluidity. The examples 1-2 have good fluidity, toughness and rigidity under the condition of low content of the toughening agent, the flame retardance can reach V-0 level, and the impact performance is improved to a certain extent compared with comparative examples 1 and 2; examples 3-5 by adding the flow modifier, the interface modification auxiliary agent and the toughening agent to interact, higher fluidity, toughness and rigidity are obtained, the impact resistance is greatly improved, and the surface resistance of the material of example 6 can be reduced to 10+11And has good antistatic effect. In examples 7 to 9, the synergistic effect of the interfacial modification auxiliary and the toughening agent can be achieved, and the high impact modified material can be obtained. From the structure of the interface modification auxiliary agent, the N, N-bis-hydroxyethyl alkylamide is replaced by stearic acid diethanolamide, oleic acid diethanolamide, laureth-4 and polyethylene glycol with similar structuresOne or more of stearate has equivalent effect. Since the toughening effect of 7 parts of toughening agent, 1.0 part of interface modifier and flow modifier in example 6 is close to the effect of 15 parts of toughening agent in comparative example 4, and the fluidity of example 6 is more excellent than that of comparative example 4, it is proved that the flow property and mechanical property of the halogen-free flame retardant polypropylene can be improved by adding the interface modifier and flow modifier with specific proportions, and when the mass content of the interface modifier and flow modifier is 0.6%, the melt flow rate of the halogen-free flame retardant polypropylene material is close to that of the polypropylene resin substrate, and the fluidity is excellent.
Compared with the comparative example 1, the flow modifier and the interface modifier are not added, and the halogen-free flame retardant contains a large amount of hydroxyl and amino, so that the compatibility of each component in the system is poor, the melt index is reduced, and the fluidity is poor; compared with the comparative examples 2-4, the toughening agent of the ethylene-octene copolymer with different contents is added, and the toughening agent does not contain a flow modifier and an interface modifier, so that the toughening effect of the toughening agent of the ethylene-octene copolymer with the addition amount of more than or equal to 10 percent is obvious, but the flow property, the tensile strength and the bending strength of the material are also obviously reduced; in comparative examples 5-6, by adding the interfacial modifier with different contents and the ethylene-octene copolymer toughening agent to perform synergistic effect, the bending modulus and the tensile strength of the material can be improved, the surface resistance is reduced, but the impact property of the material is reduced, the rigidity and toughness balance of the material cannot be ensured, the fluidity is not improved, and the surface resistance is still higher; comparative example 7 the flowability of the material was improved by adding only the flow modifier, but the tensile strength and flexural modulus of the material were lower and the surface resistance was higher.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The high-fluidity high-impact halogen-free flame-retardant polypropylene material is characterized by comprising the following components in parts by mass:
wherein the flow modifier is a stearylamine-based multipolymer; the interface modifier is one or more of N, N-bis-hydroxyethyl alkylamide, stearic acid diethanolamide, oleic acid diethanolamide, laureth-4 and polyethylene glycol stearate.
2. The high-flow high-impact halogen-free flame-retardant polypropylene material according to claim 1, which comprises the following components in parts by mass:
3. the high-flow high-impact halogen-free flame-retardant polypropylene material as claimed in claim 1 or 2, wherein the interfacial modifier is one or more of N, N-bis-hydroxyethyl alkylamide, stearic acid diethanolamide and oleic acid diethanolamide.
4. The high-flow high-impact halogen-free flame-retardant polypropylene material as claimed in claim 1, wherein the melt flow rate of the polypropylene at 230 ℃ and 2.16kg is 20-50 g/10 min.
5. The high-fluidity high-impact halogen-free flame-retardant polypropylene material according to claim 1, wherein the polypropylene is one or more of homo-polypropylene, propylene-ethylene block copolymer, propylene-ethylene random copolymer and propylene-1-butene random block.
6. The high-flow high-impact halogen-free flame retardant polypropylene material according to claim 1, wherein the halogen-free flame retardant is one or more of piperazine pyrophosphate and melamine pyrophosphate mixture, piperazine pyrophosphate and melamine polyphosphate mixture, high molecular weight ammonium polyphosphate and triazine charring agent mixture.
7. The high-flow high-impact halogen-free flame-retardant polypropylene material as claimed in claim 1, wherein the melt index of the toughening agent is 1-15 g/10 min.
8. The high-fluidity high-impact halogen-free flame-retardant polypropylene material as claimed in claim 1, further comprising one or more of a primary antioxidant, a secondary antioxidant, an anti-dripping aid, a lubricant and other processing aids.
9. The preparation method of the high-flow high-impact halogen-free flame-retardant polypropylene material as claimed in any one of claims 1 to 8, characterized by comprising the following steps:
uniformly mixing polypropylene, a halogen-free flame retardant, a toughening agent, a flow modifier and an interface modifier, melting and blending, extruding and granulating, and drying to obtain the high-flow high-impact halogen-free flame retardant polypropylene material.
10. The use of the high flow high impact halogen-free flame retardant polypropylene material of any one of claims 1 to 8 in the preparation of flame retardant materials.
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