CN111534013A - High-hydrophobicity antibacterial polypropylene material and preparation method thereof - Google Patents
High-hydrophobicity antibacterial polypropylene material and preparation method thereof Download PDFInfo
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- CN111534013A CN111534013A CN202010555414.6A CN202010555414A CN111534013A CN 111534013 A CN111534013 A CN 111534013A CN 202010555414 A CN202010555414 A CN 202010555414A CN 111534013 A CN111534013 A CN 111534013A
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- polypropylene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/26—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/42—Introducing metal atoms or metal-containing groups
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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Abstract
The invention discloses a high-hydrophobicity antibacterial polypropylene material and a preparation method thereof; the high-hydrophobicity antibacterial polypropylene material comprises the following components in parts by weight: 44-85 parts of polypropylene grafted siloxane copolymer; 7-20 parts of glass fiber; 1-10 parts of a compatilizer; 0.1 to 10 portions of inorganic filler; 1-5 parts of an antioxidant; 0.05 to 1 portion of other auxiliary agents; the siloxane group on the prepared polypropylene grafted siloxane copolymer can not only radically change the polarity of the surface of the polypropylene composition material and improve the hydrophobic property of the polypropylene composition material, but also can interact with glass fiber to improve the strength of the polypropylene material.
Description
Technical Field
The invention belongs to the field of high-molecular chemical synthesis, and particularly relates to a high-hydrophobicity antibacterial polypropylene material and a preparation method thereof.
Background
Polypropylene (PP) is a thermoplastic synthetic resin with excellent performance, and is colorless translucent thermoplastic light general-purpose plastic. The polypropylene has chemical resistance, heat resistance, electrical insulation, high-strength mechanical property, good high-wear-resistance processing property and the like, so that the polypropylene can be rapidly and widely developed and applied in a plurality of fields such as machinery, automobiles, electronic and electric appliances, buildings, textiles, packaging, agriculture, forestry, fishery, food industry and the like since the coming out. In recent years, with the rapid development of the industries such as packaging, electronics, automobiles and the like in China, the development of the industries in China is greatly promoted. And because of its plasticity, polypropylene materials are gradually replacing wooden products, and the mechanical functions of metals have been gradually replaced by high strength toughness and high wear resistance.
With the rapid development of domestic appliances in China, polypropylene materials are widely applied, such as dish-washing machines, refrigerators and the like, but the internal plastic parts of the domestic appliances are in a humid environment for a long time and are easy to breed bacteria.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a high-hydrophobicity antibacterial polypropylene material and a preparation method thereof, and the hydrophobic property and antibacterial property of the polypropylene material are improved.
The invention aims to provide a high-hydrophobicity antibacterial polypropylene material.
The invention also aims to provide a preparation method of the high-hydrophobicity antibacterial polypropylene material.
The above purpose of the invention is realized by the following technical scheme:
the high-hydrophobicity antibacterial polypropylene material comprises the following components in parts by weight:
the polypropylene grafted siloxane copolymer has a structure shown in a formula (I).
Wherein n is 100-5000.
The glass fiber is alkali-free glass fiber, the diameter is 15-20 μm, and the length is 6-10 mm.
The compatilizer is a polar monomer graft polymer, and the polymer is selected from one or more of polyethylene, polypropylene and ethylene-alpha-ethylene-octene copolymer; the polar monomer is selected from one or more of maleic anhydride and derivatives thereof, acrylic acid and ester derivatives thereof.
The inorganic filler is at least one of calcium carbonate, talcum powder, barium sulfate and red mud.
The antioxidant is at least one of an anti-aging agent 288, 2, 4-trimethyl-1, 3-dihydroquinoline and 2, 6-di-tert-butyl-4-methylphenol.
The other auxiliary agents are one or more of calcium stearate, zinc stearate and erucamide.
The reaction process and the preparation method of the polypropylene grafted siloxane copolymer are as follows:
1.4-Hydroxyphenyltrimethoxysilane was prepared.
NMF is used as a solvent, 4-iodophenol and triethoxy silicon are used as raw materials, 2-biphenyl) di-tert-butylphosphine and tris (dibenzylideneacetone) dipalladium are used as catalysts, and the reaction is carried out for 12 hours at 60 ℃ under the alkaline condition of (S) - (-) -2- (A- (I-propyl) methylamine) -1H-benzimidazole to obtain 4-hydroxyphenyl trimethoxy silane, wherein the molar ratio of the 4-iodophenol to the triethoxy silicon is 1: 1.5.
2. Preparation of polypropylene grafted Silicone copolymer.
N2Under protection, using toluene as solvent, carrying out acyl chlorination reaction on single-terminal hydroxyl polypropylene and succinyl chloride as raw materials, carrying out reflux reaction for 12h at 140 ℃, treating with anhydrous acetone after the reaction is finished, drying to obtain a polypropylene product with an acyl chloride group at the terminal, reacting the obtained single-terminal hydroxyl polypropylene acyl chlorination product with 4-hydroxyphenyl trimethoxy silane at 110 ℃ for 10h, and then saturating K2CO3Neutralizing the reaction solution to obtain the degradable polypropylene grafted sericin copolymer, wherein the molar ratio of the single-end hydroxyl polypropylene to the succinyl chloride is 1:200, and the mass ratio of the single-end hydroxyl polyacrylic chloride product to the 4-hydroxyphenyl trimethoxysilane is 1: 20.
A preparation method of the high-hydrophobicity antibacterial polypropylene material comprises the following steps:
the polypropylene grafted siloxane copolymer, the glass fiber, the compatilizer, the inorganic filler, the antioxidant and other auxiliary agents are mixed according to the proportion, and the length-diameter ratio is 36-40: 1, melting, mixing and dispersing at 180-250 ℃, adding glass fiber from a side feed port, extruding and granulating to obtain the high-hydrophobicity antibacterial polypropylene material.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the invention synthesizes the polypropylene grafted siloxane copolymer through organic reaction, siloxane group on the polypropylene grafted siloxane copolymer not only can radically change the polarity of the surface of the polypropylene composition material and improve the hydrophobic property of the polypropylene composition material, but also can interact with glass fiber to improve the strength of the polypropylene material.
Detailed Description
The present invention will be described in further detail with reference to specific examples, which are not intended to limit the present invention in any manner. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1
Preparation of 4-hydroxyphenyltrimethoxysilane.
4-iodophenol (1.10g,5mmol), triethoxysilane (1.23g,7.5mmol), (2-biphenyl) di-tert-butylphosphine (0.09g,0.3mmol), tris (dibenzylideneacetone) dipalladium (0.27g,0.3mmol) and (S) - (-) -2- (A- (I-propyl) methylamine) -1H-benzimidazole (0.03g,0.15mmol) were added to a 150mL flask, 50mL of LNMF was added via a one-shot syringe, the temperature was raised to 60 ℃ for 12H reaction, the product was purified by column chromatography using petroleum ether/ethyl acetate as the mobile phase, and vacuum drying was carried out at 45 ℃ to 4-hydroxyphenyltrimethoxysilane.
Example 2
Preparation of polypropylene grafted Silicone copolymer.
N2Under protection, single-terminal hydroxypolypropylene (0.85g,0.1mmol) and 50mL of toluene were added to a 100mL Schlenk flask, and stirred at 140 ℃ for 30min to be polymerizedAfter the materials are completely dissolved, adding succinyl chloride (3.10g,20mmol) to continue reacting for 12h at 140 ℃, treating with anhydrous acetone after the reaction is finished, drying to obtain a polypropylene product with an acyl chloride group at the end,
4-Hydroxyphenyltrimethoxysilane (0.43g,2mmol) and 10mL of dioxane were added to a 50mL round-bottomed flask, the temperature was raised to 80 ℃, the one-terminal hydroxypolyacryloylchlorination product (4.5mmol,5.0g) prepared in example 2 dissolved in 20mL of dioxane was gradually added dropwise, the temperature was raised to 110 ℃ for reaction for 10 hours, and the reaction solution was poured into anhydrous ethanol for precipitation and filtration. Washing with anhydrous ethanol for several times, washing with distilled water for several times, and changing to saturated K2CO3Washing the solution, and finally washing the solution to be neutral by using water. And (5) drying for 5h in vacuum to obtain the degradable polypropylene grafted sericin copolymer.
Example 3
And (3) preparing the high-hydrophobicity antibacterial polypropylene material.
According to the proportion (weight portion), 60 portions of polypropylene grafted siloxane copolymer, 20 portions of glass fiber, 8 portions of compatilizer, 10 portions of inorganic filler, 1 portion of antioxidant and 1 portion of other auxiliary agents are mixed according to the proportion that the length-diameter ratio is 36-40: 1, melting, mixing and dispersing at 180-250 ℃, adding glass fiber from a side feed port, extruding and granulating to obtain the high-hydrophobicity antibacterial polypropylene material.
The samples were injection molded into 100 x 3mm square plaques and the contact angles (theta angle) of the material with water were tested 6 times in parallel and were 145, 144, 143, 145, 147, 142 respectively.
Comparative example 1
According to the proportion (weight portion), 55 portions of polypropylene, 5 portions of 4-hydroxyphenyl trimethoxy silane, 20 portions of glass fiber, 8 portions of compatilizer, 10 portions of inorganic filler, 1 portion of antioxidant and 1 portion of other auxiliary agents are mixed according to the proportion that the length-diameter ratio is 36-40: 1, melting, mixing and dispersing at 180-250 ℃, adding glass fiber from a side feed port, and extruding and granulating. The samples were injection molded into 100 x 3mm square plaques and the contact angles (theta angle) of the material with water were tested 6 times in parallel and were 132, 133, 130, 127, 130, 128, 130, respectively.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. The high-hydrophobicity antibacterial polypropylene material is characterized by comprising the following components in parts by weight:
the polypropylene grafted siloxane copolymer has a structure shown in a formula (I):
wherein n is 100-5000.
2. The highly hydrophobic antibacterial polypropylene material according to claim 1, wherein the glass fiber is alkali-free glass fiber, and has a diameter of 15 μm to 20 μm and a length of 6mm to 10 mm.
3. The highly hydrophobic antibacterial polypropylene material as claimed in claim 1, wherein the compatibilizer is a polar monomer graft polymer selected from one or more of polyethylene, polypropylene, and ethylene- α -ethylene-octene copolymer; the polar monomer is selected from one or more of maleic anhydride and derivatives thereof, acrylic acid and ester derivatives thereof.
4. The highly hydrophobic antibacterial polypropylene material according to claim 1, wherein the inorganic filler is at least one of calcium carbonate, talc, barium sulfate and red mud.
5. The highly hydrophobic antibacterial polypropylene material according to claim 1, wherein the antioxidant is at least one of antioxidant 288, 2, 4-trimethyl-1, 3-dihydroquinoline, and 2, 6-di-tert-butyl-4-methylphenol.
6. The highly hydrophobic antibacterial polypropylene material as claimed in claim 1, wherein the other auxiliary agent is one or more of calcium stearate, zinc stearate and erucamide.
7. The preparation method of the highly hydrophobic antibacterial polypropylene material according to claim 1, comprising the steps of:
the polypropylene grafted siloxane copolymer, the glass fiber, the compatilizer, the inorganic filler, the antioxidant and other auxiliary agents are mixed according to the proportion, and the length-diameter ratio is 36-40: 1, melting, mixing and dispersing at 180-250 ℃, adding glass fiber from a side feed port, extruding and granulating to obtain the high-hydrophobicity antibacterial polypropylene material.
8. The polypropylene-grafted silicone copolymer according to claim 1, wherein the preparation method of the polypropylene-grafted silicone copolymer comprises the following steps:
(1) taking NMF as a solvent, 4-iodophenol and triethoxy silicon as raw materials, taking (2-biphenyl) di-tert-butylphosphine and tris (dibenzylideneacetone) dipalladium as catalysts, and reacting for 12H at 60 ℃ under the alkaline condition of (S) - (-) -2- (A- (I-propyl) methylamine) -1H-benzimidazole to obtain 4-hydroxyphenyl trimethoxy silane, wherein the molar ratio of the 4-iodophenol to the triethoxy silicon is 1: 1.5;
(2).N2under protection, using toluene as solvent, carrying out acyl chlorination reaction on single-terminal hydroxyl polypropylene and succinyl chloride as raw materials, carrying out reflux reaction at 140 ℃ for 12h, treating with anhydrous acetone after the reaction is finished, drying to obtain a polypropylene product with an acyl chloride group at the terminal, and obtaining the single-terminal hydroxyl polypropyleneReacting the acyl chloride product with 4-hydroxyphenyl trimethoxy silane at 110 deg.C for 10 hr to obtain saturated K2CO3Neutralizing the reaction solution to obtain a degradable polypropylene grafted sericin copolymer, wherein the molar ratio of single-end hydroxyl polypropylene to succinyl chloride is 1:200, and the mass ratio of a single-end hydroxyl polyacrylic chloride product to 4-hydroxyphenyl trimethoxysilane is 1: 20;
wherein n is 100-5000.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202010555414.6A CN111534013A (en) | 2020-06-17 | 2020-06-17 | High-hydrophobicity antibacterial polypropylene material and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111892775A (en) * | 2020-08-18 | 2020-11-06 | 闫镇达 | Polypropylene-siloxane blending lipophilic special material and preparation method thereof |
| CN112080151A (en) * | 2020-09-16 | 2020-12-15 | 彭军文 | Hydrophobic antibacterial rigid polypropylene material and preparation method thereof |
| CN112266541A (en) * | 2020-10-16 | 2021-01-26 | 张雪飞 | Nitrogen-phosphorus flame-retardant polypropylene material and preparation method thereof |
| CN113337036A (en) * | 2021-04-21 | 2021-09-03 | 日丰企业集团有限公司 | Modified polypropylene material and preparation method thereof |
| CN114316452A (en) * | 2022-01-04 | 2022-04-12 | 苏州浩纳新材料科技有限公司 | Super-hydrophobic foamed polypropylene and preparation method thereof |
-
2020
- 2020-06-17 CN CN202010555414.6A patent/CN111534013A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111892775A (en) * | 2020-08-18 | 2020-11-06 | 闫镇达 | Polypropylene-siloxane blending lipophilic special material and preparation method thereof |
| CN112080151A (en) * | 2020-09-16 | 2020-12-15 | 彭军文 | Hydrophobic antibacterial rigid polypropylene material and preparation method thereof |
| CN112266541A (en) * | 2020-10-16 | 2021-01-26 | 张雪飞 | Nitrogen-phosphorus flame-retardant polypropylene material and preparation method thereof |
| CN113337036A (en) * | 2021-04-21 | 2021-09-03 | 日丰企业集团有限公司 | Modified polypropylene material and preparation method thereof |
| CN114316452A (en) * | 2022-01-04 | 2022-04-12 | 苏州浩纳新材料科技有限公司 | Super-hydrophobic foamed polypropylene and preparation method thereof |
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Application publication date: 20200814 |