CN112358675A - Polypropylene composition and preparation method thereof - Google Patents
Polypropylene composition and preparation method thereof Download PDFInfo
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- CN112358675A CN112358675A CN202010942463.5A CN202010942463A CN112358675A CN 112358675 A CN112358675 A CN 112358675A CN 202010942463 A CN202010942463 A CN 202010942463A CN 112358675 A CN112358675 A CN 112358675A
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Abstract
The invention discloses a polypropylene composition, which comprises the following components in parts by weight: 100 parts of polypropylene resin; 5-50 parts of silicon dioxide-containing inorganic powder grafted by quaternary phosphonium salt. The addition of the silicon dioxide-containing inorganic powder grafted by the quaternary phosphonium salt not only can enable the polypropylene composition to have long-acting antibacterial performance, but also can enable the polypropylene composition to be endowed with flame retardant performance and antistatic performance by the silicon dioxide-containing inorganic powder grafted by the quaternary phosphonium salt.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a polypropylene composition and a preparation method thereof.
Background
With the increasing demand for light weight of automobiles, polypropylene (PP) materials are widely used in automobile parts, including bumpers, instrument panels, door panels, pillars, and various decorative parts, due to their characteristics of low specific gravity, excellent mechanical properties, low cost, and easy processing. With the development of the automobile industry, the requirements on automobile materials are higher and higher, and with the rise of the requirements of people on antibiosis and virus resistance, the Jili automobile provides a new automobile antibiosis standard, which is a great revolution to the automobile industry, and has epoch-making significance as an automobile material supplier to provide materials with antibiosis effect for T1 or a host factory.
However, the addition of a common antibacterial agent causes the reduction of other properties of the polypropylene material, which is caused by the following two reasons: 1. the toughness or strength of some biological antibacterial agents is poor, so that the mechanical property of the polypropylene material can be influenced after the biological antibacterial agents are added; 2. quaternary phosphonium salts have been reported as antibacterial agents to be added to polypropylene composites, but the use of quaternary phosphonium salts in polyolefin composites has been less explored because of their poor heat resistance and their significant decomposition during melt processing, which affects performance.
Disclosure of Invention
The invention aims to provide a polypropylene composition with a long-acting antibacterial function and the advantage of good heat resistance.
The invention is realized by the following technical scheme:
the polypropylene composition comprises the following components in parts by weight: 100 parts of polypropylene resin; 5-50 parts of silicon dioxide-containing inorganic powder grafted by quaternary phosphonium salt.
The polypropylene resin has a melt index in the range of 5 to 120g/10min (2.16kg, 230 ℃). The polypropylene resin may be a homo-polypropylene or a co-polypropylene.
The quaternary phosphonium salt grafted silica-containing inorganic powder is at least one of quaternary phosphonium salt grafted talcum powder, quaternary phosphonium salt grafted mica powder and quaternary phosphonium salt grafted glass fiber powder, and the grafting rate of the quaternary phosphonium salt is 5-25 wt%.
Preferably, the branching ratio of the quaternary phosphonium salt in the silicon dioxide-containing inorganic powder grafted by the quaternary phosphonium salt is 10-25 wt%.
The quaternary phosphonium salt is 3-bromopropyl triphenyl quaternary phosphonium salt.
The preparation method of the quaternary phosphonium salt grafted inorganic powder containing silicon dioxide comprises the following steps:
(1) grafting gamma-chloropropyltrimethoxysilane or gamma-chloropropyltriethoxysilane to the surface of inorganic powder containing silicon dioxide;
(2) then carrying out amination reaction with polyethyleneimine or polypropyleneimine;
(3) and then the product is reacted with 3-bromopropyltriphenyl quaternary phosphonium salt through microwave heating to obtain the inorganic powder containing silicon dioxide grafted by the quaternary phosphonium salt.
Specifically, adding inorganic powder containing silicon dioxide into a toluene solution with the weight 0.5-1 time of that of the inorganic powder containing silicon dioxide, adding water with the weight 0.5-1 time of that of the inorganic powder containing silicon dioxide, adding gamma-chloropropyltrimethoxy or gamma-chloropropyltriethoxysilane (silane coupling agent) to react for 4-8h at the temperature of 80-110 ℃ under normal pressure, and grafting the gamma-chloropropyltrimethoxy or gamma-chloropropyltriethoxysilane to the surface of the inorganic powder containing silicon dioxide; and then carrying out an amination reaction with polyethyleneimine or polypropylene imine at 70-90 ℃, carrying out microwave heating reaction on the product and 3-bromopropyltriphenyl quaternary phosphonium salt in an aqueous solution for 16-24h, controlling the temperature at 30-50 ℃ and the pressure at 1-4pa, and filtering and drying after the reaction is finished to obtain the silicon dioxide-containing inorganic powder grafted by the quaternary phosphonium salt.
The reaction formula of the silica-containing inorganic powder grafted with a quaternary phosphonium salt obtained by reacting gamma-chloropropyltrimethoxysilane, polyethyleneimine and 3-bromopropyltriphenylquaternary phosphonium salt is shown below. Wherein, silica represents silica-containing inorganic powder.
The average particle diameter of the silicon dioxide-containing inorganic powder grafted by the quaternary phosphonium salt is 800 meshes-5000 meshes.
In order to increase the toughness of the polypropylene composition, an amount of toughening agent may be added. 0-50 parts of toughening agent is also included according to the parts by weight; the toughening agent is selected from one or more of ethylene-octene copolymers.
In order to improve melt processability, a certain amount of processing aid may be added. 0-3 parts of processing aid is also included according to the parts by weight; the processing aid is selected from one or more of a lubricant and an antioxidant.
The lubricant is selected from acetamide. An optional designation is EBS 50.
The antioxidant is at least one selected from pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris [2, 4-di-tert-butylphenyl ] phosphite, n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate and didodecanediol thiodipropionate.
The common trade name of pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] is SONOX 1010; a common designation for tris [ 2.4-di-tert-butyl benzene ] phosphite is SONOX 168.
Specifically, the weight ratio of SONOX 1010: SONOX168 =2: 1.
The preparation method of the polypropylene composite material comprises the following steps: according to the proportion, the components are uniformly mixed by a high-speed mixer and then extruded and granulated by a double-screw extruder (the temperature of a zone 1 is 80-120 ℃, the temperature of a zone 2-5 is 180-200 ℃ and the temperature of the other zone is 200-230 ℃) to obtain the polypropylene composition.
The invention has the following beneficial effects:
according to the invention, the quaternary phosphonium salt is grafted to the surface of inorganic powder containing silicon dioxide, so that the defects of poor thermal stability and poor dispersibility of the quaternary phosphonium salt are overcome, the quaternary phosphonium salt has good dispersibility in a polypropylene composition resin matrix, and can bear the high temperature of polypropylene melting, and the antibacterial effect of the polypropylene composition is greatly improved. Moreover, the polypropylene composition contains a large amount of silicon and phosphorus (quaternary phosphonium functional groups), the silicon and phosphorus are synergistic in flame retardance, the flame retardance is good, and meanwhile, the quaternary phosphonium has strong antistatic property, so that the polypropylene composition is endowed with strong antistatic performance.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The raw materials used in the examples and comparative examples are as follows:
polypropylene resin a: melt flow rate 20g/10min, 2.16kg, 230 ℃, homo-polypropylene, PP 9018.
Polypropylene resin B: melt flow rate 40g/10min, 2.16kg, 230 ℃, copolypropylene, PP SP 179.
Quaternary phosphonium salt grafted talc a: the grafting rate of the quaternary phosphonium salt is 13 +/-1 wt%, and the average grain size is 1250 meshes, and the quaternary phosphonium salt is prepared by a method described in the section of the invention content;
quaternary phosphonium salt grafted talc B: the grafting rate of the quaternary phosphonium salt is 8 +/-1 wt%, and the average grain size is 1250 meshes, and the quaternary phosphonium salt is prepared by a method described in the section of the invention content;
quaternary phosphonium salt grafted talc C: the grafting rate of the quaternary phosphonium salt is 3 +/-1 wt%, and the average grain size is 1250 meshes, and the quaternary phosphonium salt is prepared by a method described in the section of the invention content;
quaternary phosphonium salt grafted mica powder: the grafting rate of the quaternary phosphonium salt is 18 +/-1 wt%, and the average grain size is 1250 meshes, and the quaternary phosphonium salt is prepared by a method described in the section of the invention content;
quaternary phosphonium salt grafted glass fiber powder: the grafting rate of the quaternary phosphonium salt is 7 +/-1 wt%, and the average particle size is 800 meshes, and the quaternary phosphonium salt is prepared by a method recorded in the section of 'invention contents';
quaternary phosphonium salt antibacterial agents: bis (1, 2-dicyanodipheylene) palladium (II) -benzyltriphenylphosphonium salt;
talc powder: FQ-5C, TYT-3000A, HTPUlTra 5;
mica powder: YM-SW 500;
glass fiber powder: glass fiber CS 10-03-508A;
ethylene-octene copolymer: POE 7447;
lubricant: an EBS 50;
antioxidant: the weight ratio of SONOX 1010: SONOX168 =2: 1;
examples and comparative examples preparation methods of polypropylene composites: according to the proportion, the components are uniformly mixed by a high-speed mixer and then extruded and granulated by a double-screw extruder (the temperature of a zone 1 is 80-120 ℃, the temperature of a zone 2-5 is 180-200 ℃, and the temperature of the other zone is 200-230 ℃) to obtain the polypropylene composition.
The performance test method comprises the following steps:
(1) the antibacterial rate is as follows: the samples were injection moulded into 100 x 3mm square plates and the antibacterial (%) of the material was tested according to ISO 22196.
(2) Flame retardancy: the sample band limit oxygen index is tested according to GB/T2406-2008 plastic combustion performance test method-oxygen index method.
(3) Antistatic property: referring to GB/T1410-2006 test sample plate surface resistivity, the lower the surface resistivity, the better the antistatic performance.
TABLE 1 composition ratios (parts by weight) and performance test results for polypropylene compositions of examples 1-7
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | |
| Polypropylene resin A | 100 | 100 | 100 | 100 | 100 | 100 | |
| Polypropylene resin B | 100 | ||||||
| Quaternary phosphonium salt grafted talcum powder A | 5 | 15 | 25 | 35 | 50 | 25 | 25 |
| Lubricant agent | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | |
| Antioxidant agent | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | |
| Ethylene-octene copolymer | 10 | ||||||
| Antibacterial ratio (%) | 95 | 98 | 99 | ＞99 | ＞99 | 99 | 99 |
| Limiting oxygen index (%) | 21 | 25 | 27 | 30 | 33 | 27 | 27 |
| Surface resistance (omega) | 1011 | 1010 | 109 | 108 | 107 | 109 | 109 |
From example 6/7, it is understood that the addition of POE, an antioxidant and a lubricant in a small amount does not cause significant changes in the antibacterial ratio, flame retardancy and surface resistance.
TABLE 2 composition ratios (parts by weight) and performance test results for polypropylene compositions of examples 8-10
| Example 8 | Example 9 | Example 10 | |
| Polypropylene resin | 100 | 100 | 100 |
| Quaternary phosphonium salt grafted talcum powder B | 25 | ||
| Quaternary phosphonium salt grafted mica powder | 25 | ||
| Quaternary phosphonium salt grafted glass fiber powder | 25 | ||
| Lubricant agent | 0.1 | 0.1 | 0.1 |
| Antioxidant agent | 0.2 | 0.2 | 0.2 |
| Antibacterial ratio (%) | ＞99 | 96 | 97 |
| Limiting oxygen index (%) | 28 | 27 | 27 |
| Surface resistance (omega) | 109 | 1010 | 1010 |
As shown in example 3/8/9/10, the graft ratio of the quaternary phosphonium salt is preferably 10 to 25wt%
Table 3: comparative example Polypropylene composition Each component proportion (parts by weight) and each performance test result
| Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Polypropylene resin | 100 | 100 | 100 |
| Quaternary phosphonium salt grafted talcum powder A | 2 | ||
| Quaternary phosphonium salt grafted talcum powder C | 25 | ||
| Quaternary phosphonium salt antibacterial agent | 3.25 | ||
| Talcum powder | 21.75 | 15 | |
| Lubricant agent | 0.1 | 0.1 | 0.1 |
| Antioxidant agent | 0.2 | 0.2 | 0.2 |
| Antibacterial rate | 40 | 26 | 76 |
| Limiting oxygen index | 20 | 18 | 18 |
| Surface resistance | 1012 | 1012 | 1012 |
As can be seen from comparative example 1, the grafting weight percentage of the quaternary phosphonium salt in the quaternary phosphonium salt grafted talcum powder is at least 5wt% or more, so that good antibacterial, flame retardant and antistatic technical effects can be achieved.
As can be seen from comparative example 2, the thermal stability of the quaternary phosphonium salt antibacterial agent is low, and the resulting polypropylene composition is not only poor in antibacterial effect but also has no technical effect of enhancing flame retardance.
Claims (10)
1. The polypropylene composition is characterized by comprising the following components in parts by weight: 100 parts of polypropylene resin; 5-50 parts of silicon dioxide-containing inorganic powder grafted by quaternary phosphonium salt.
2. The polypropylene composition according to claim 1, wherein the polypropylene resin has a melt index in the range of 5 to 120g/10min (2.16kg, 230 ℃).
3. The polypropylene composition according to claim 1, wherein the quaternary phosphonium salt grafted silica-containing inorganic powder is at least one selected from quaternary phosphonium salt grafted talc powder, quaternary phosphonium salt grafted mica powder and quaternary phosphonium salt grafted glass fiber powder, and the grafting ratio of the quaternary phosphonium salt is 5wt% to 25 wt%.
4. The polypropylene composition according to claim 1, wherein the quaternary phosphonium salt grafted silica-containing inorganic powder has a grafting ratio of the quaternary phosphonium salt of 10wt% to 25 wt%.
5. The polypropylene composition of claim 1, wherein the quaternary phosphonium salt is 3-bromopropyltriphenylphosphonium salt.
6. The polypropylene composition according to claim 1, wherein the quaternary phosphonium salt-grafted silica-containing inorganic powder has an average particle size of 800 mesh to 5000 mesh.
7. The polypropylene composite of claim 1, further comprising 0 to 50 parts by weight of a toughening agent; the toughening agent is selected from ethylene-octene copolymer.
8. The polypropylene composite according to claim 1, further comprising 0 to 3 parts by weight of a processing aid; the processing aid is selected from one or more of a lubricant and an antioxidant.
9. The polypropylene composite according to claim 1, wherein the quaternary phosphonium salt grafted silica-containing inorganic powder is prepared by:
(1) grafting gamma-chloropropyltrimethoxysilane or gamma-chloropropyltriethoxysilane to the surface of inorganic powder containing silicon dioxide;
(2) then carrying out amination reaction with polyethyleneimine or polypropyleneimine;
(3) and then the product is reacted with 3-bromopropyltriphenyl quaternary phosphonium salt through microwave heating to obtain the inorganic powder containing silicon dioxide grafted by the quaternary phosphonium salt.
10. A process for the preparation of a polypropylene composite according to any one of claims 1 to 9, characterized in that it comprises the following steps: according to the proportion, the components are uniformly mixed by a high-speed mixer and then extruded and granulated by a double-screw extruder (the temperature of a zone 1 is 80-120 ℃, the temperature of a zone 2-5 is 180-200 ℃ and the temperature of the other zone is 200-230 ℃) to obtain the polypropylene composition.
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| CN103418433A (en) * | 2012-05-16 | 2013-12-04 | 中国石油化工股份有限公司 | Loading type quaternary phosphonium catalyst, manufacturing method and application thereof |
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| CN104862812A (en) * | 2014-10-11 | 2015-08-26 | 青岛欣展塑胶有限公司 | Antibiosis-functionalized PTT polyester fibers and preparation method therefor |
| CN105177758A (en) * | 2015-10-26 | 2015-12-23 | 太仓市双宇化纤有限公司 | Antistatic polyacrylonitrile/polyaniline composite fiber material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103418433A (en) * | 2012-05-16 | 2013-12-04 | 中国石油化工股份有限公司 | Loading type quaternary phosphonium catalyst, manufacturing method and application thereof |
| CN103881193A (en) * | 2012-12-21 | 2014-06-25 | 青岛欣展塑胶有限公司 | Polyethylene antibacterial mildew-resistant master batch and preparation method thereof |
| CN104862812A (en) * | 2014-10-11 | 2015-08-26 | 青岛欣展塑胶有限公司 | Antibiosis-functionalized PTT polyester fibers and preparation method therefor |
| CN105177758A (en) * | 2015-10-26 | 2015-12-23 | 太仓市双宇化纤有限公司 | Antistatic polyacrylonitrile/polyaniline composite fiber material and preparation method thereof |
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