CN112852092A - Super-hydrophobic wear-resistant polypropylene film and preparation method thereof - Google Patents
Super-hydrophobic wear-resistant polypropylene film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a super-hydrophobic wear-resistant polypropylene film and a preparation method thereof; the super-hydrophobic wear-resistant polypropylene film is formed by dissolving super-hydrophobic wear-resistant polypropylene block copolymer granules in a mixed solvent of xylene, toluene and benzene; according to the invention, the polymer with a hydrophobic effect and the wear-resistant agent are blocked on the polypropylene molecular chain, so that the polypropylene material has super-hydrophobicity and wear resistance, and the hydrophobic molecule and the wear-resistant agent are combined with the polypropylene in a covalent bond manner, so that the problems of poor compatibility of the hydrophobic agent and the wear-resistant agent with the polymer and easy loss of the hydrophobic agent and the wear-resistant agent are solved by adding the hydrophobic agent and the wear-resistant agent into the polypropylene base material in a physical mixing method.
Description
Technical Field
The invention belongs to the field of high polymer materials, and particularly relates to a super-hydrophobic wear-resistant polypropylene film and a preparation method thereof.
Background
The polypropylene has low price, environmental protection, wide application, excellent mechanical property, heat resistance, electrical property, chemical stability and weather resistance; the super-hydrophobic material taking polypropylene as a matrix has wide application in the aspects of self-cleaning materials, drag reduction coatings, corrosion resistance, water resistance, fog resistance, pollution prevention and the like; the polypropylene has good physical, mechanical and chemical properties and easy processing performance, and is light in weight, low in price and easy to recover, so that the polypropylene is widely applied to interior and exterior trimming parts of automobiles; however, the wear resistance of the polypropylene material is poor, and parts which are easily subjected to continuous friction from the outside, such as brake lamp housings, horn covers and the like, can be damaged due to friction, so that the attractiveness of an automobile is directly influenced, the application of the polypropylene material in automobile ornaments is seriously influenced, and the polypropylene material needs to be improved to meet the wear resistance requirement of products.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a super-hydrophobic wear-resistant polypropylene film and a preparation method thereof, wherein a polymer with a hydrophobic effect and a wear-resistant agent are blocked on a polypropylene molecular chain, so that a polypropylene material has super-hydrophobicity and wear resistance, the hydrophobic molecule and the wear-resistant agent are combined with polypropylene in a covalent bond mode, the problems that the hydrophobic agent and the wear-resistant agent are added into a polypropylene base material in a physical mixing method, the compatibility of the hydrophobic agent and the wear-resistant agent with the polymer is poor, and the hydrophobic agent and the wear-resistant agent are easy to run off are solved, and the super-hydrophobic property and the wear-resistant property have a synergistic.
The invention aims to provide a super-hydrophobic wear-resistant polypropylene film.
The invention also aims to provide a preparation method of the super-hydrophobic wear-resistant polypropylene film.
The above purpose of the invention is realized by the following technical scheme:
the preparation method of the super-hydrophobic wear-resistant polypropylene film comprises the following steps:
weighing 40-60 g of super-hydrophobic wear-resistant polypropylene block copolymer granules, and dissolving the granules in 1000ml of mixed solvent of xylene, toluene and benzene at 160 ℃, wherein the volume ratio of the three is 5:3:2, so as to form a polypropylene solution with the concentration of 40 mg/ml; and then, a polypropylene solution is spread on a glass substrate by adopting a tape casting method, the glass substrate is dried for 50 hours at 120 ℃ under the environment that the relative humidity is 80% and the concentration of ethanol steam is 13%, ethanol steam and water vapor in air are permeated into the surface of the polypropylene solution during drying to form honeycomb-shaped holes, so that a super-hydrophobic surface is obtained, and the obtained film is the super-hydrophobic wear-resistant polypropylene film.
The structural formula of the super-hydrophobic wear-resistant polypropylene block copolymer is shown as the following formula (I):
in the formula, the value of n is 100-500, the value of m is 5-10, and the value of p is 10-20.
The preparation method of the super-hydrophobic wear-resistant polypropylene block copolymer comprises the following steps:
(1) and (3) preparing a polypropylene macromolecular chain transfer agent.
Taking tetrahydrofuran as a solvent, RAFT reagent 4-cyano-4- (thiobenzoyl) valeric acid and SOCl2Performing acyl chlorination reaction to obtain 4-cyano-4- (thiobenzoyl) valeryl chloride, and performing esterification reaction on single-end hydroxyl polypropylene and 4-cyano-4- (thiobenzoyl) valeryl chloride by using toluene as a solvent and pyridine as an acid-binding agent to obtain the polypropylene macromolecule transfer agent.
Wherein the 4-cyano-4- (thiobenzoyl) pentanoic acid is reacted with SOCl2The molar ratio of the single-end hydroxyl polypropylene is 1:1: 5.
(2) And (3) preparing a super-hydrophobic polypropylene block copolymer.
Taking dioxane as a solvent, a silane coupling agent as a monomer, a polypropylene macromolecular chain transfer agent as a chain transfer agent and azodiisobutyronitrile as an initiator, and reacting for 2-8 hours at 70-80 ℃ under the conditions of no water, no oxygen and nitrogen protection to obtain the super-hydrophobic polypropylene block copolymer.
Wherein the silane coupling agent has the following structure:
wherein the molar ratio of the polypropylene macromolecular chain transfer agent, the azobisisobutyronitrile and the silane coupling agent is 1:10: 1000.
Wherein the concentration of the silane coupling agent is 1 mol/L.
(3) And (3) preparing the super-hydrophobic wear-resistant polypropylene block copolymer.
Reacting for 2-6 hours at 70-80 ℃ under the conditions of no water, no oxygen and nitrogen protection by using dioxane as a solvent, a wear-resisting agent as a monomer, a super-hydrophobic polypropylene block copolymer as a chain transfer agent and azodiisobutyronitrile as an initiator to obtain the super-hydrophobic wear-resisting polypropylene block copolymer.
Wherein the anti-wear agent has the following structure:
wherein the molar ratio of the super-hydrophobic polypropylene block copolymer, the azodiisobutyronitrile and the wear-resisting agent is 1:10: 1000.
Wherein the concentration of the anti-wear agent is 1 mol/L.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention provides a super-hydrophobic wear-resistant polypropylene film, which is characterized in that a polypropylene molecule is provided with hydrophobicity by blocking a silane coupling agent on a polypropylene molecule chain, and the polypropylene molecule is provided with wear resistance by blocking a wear-resistant agent on the polypropylene molecule chain, so that the super-hydrophobic property and the wear resistance have a synergistic effect.
(2) The invention provides a super-hydrophobic wear-resistant polypropylene film, hydrophobic molecules and a wear-resistant agent are combined with polypropylene in a covalent bond mode, and the problems that the hydrophobic agent and the wear-resistant agent are poor in compatibility with a polymer and the hydrophobic agent and the wear-resistant agent are easy to lose are solved by adding the hydrophobic agent and the wear-resistant agent into a polypropylene base material in a physical mixing method.
Drawings
FIG. 1 is a nuclear magnetic hydrogen spectrum diagram of a super-hydrophobic wear-resistant polypropylene block copolymer.
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
Adding 4-cyano-4- (thiobenzoyl) valeric acid (5.0mmol) into a 50ml bottle with stirrer, adding 20ml anhydrous tetrahydrofuran THF with syringe, and slowly adding thionyl chloride SOCl dropwise under stirring2(50.0mmol), the oil bath temperature was raised to 75 ℃ and refluxed for 2.5h, after the reaction was complete, SOCl was removed by distillation under reduced pressure2And THF to give a yellow oily product, which was dissolved in an appropriate amount of toluene solution.
The single-terminal hydroxyl polypropylene PP-OH (0.8mmol) was charged into a 100mL flask equipped with a stirrer, and after purging nitrogen three times, the mixture was stirred under N2Adding 30ml of anhydrous toluene in the atmosphere, continuously stirring, slowly heating the oil bath to 70 ℃, adding 1.5ml of pyridine after the polymer is completely dissolved, slowly dropwise adding the yellow oily product dissolved in the toluene solution after 40min, reacting for 3h at 80 ℃, cooling the product to room temperature, continuously dissolving/precipitating with toluene/methanol twice, and drying at 50 ℃ in vacuum to constant weight to obtain the polypropylene macromolecule transfer agent, wherein the yield is 73.6%.
Example 2
Respectively adding the polypropylene macromolecular chain transfer agent (0.1mmol) prepared in example 1, a silane coupling agent (10mmol), AIBN (0.01mmol) and 5mL of dioxane into a 10mL Schlenk bottle with a stirrer, setting the oil bath temperature to 75 ℃, placing the Schlenk bottle into an oil bath reaction kettle for polymerization after three liquid nitrogen freezing-air extraction-unfreezing cycles, immediately taking out the Schlenk bottle after 3 hours of reaction, placing the Schlenk bottle into liquid nitrogen for cooling, repeatedly precipitating a crude product in anhydrous ether, filtering precipitates, and drying in vacuum to obtain the super-hydrophobic polypropylene block copolymer with the yield of 72.8%.
Example 3
Respectively adding the super-hydrophobic polypropylene block copolymer (0.1mmol) prepared in example 2, an anti-wear agent (10mmol), AIBN (0.01mmol) and 5mL dioxane into a 10mL Schlenk bottle with a stirrer, setting the oil bath temperature to 75 ℃, placing the Schlenk bottle into an oil bath reaction kettle for polymerization after three liquid nitrogen freezing-air extraction-unfreezing cycles, immediately taking out the Schlenk bottle after 3 hours of reaction, placing the bottle into liquid nitrogen for cooling, repeatedly precipitating a crude product in anhydrous diethyl ether, filtering precipitates, and drying in vacuum to obtain the super-hydrophobic wear-resistant polypropylene block copolymer with the yield of 67.9%.
Example 4
Weighing 40 g of super-hydrophobic wear-resistant polypropylene block copolymer granules, and dissolving the granules in 1000ml of mixed solvent of xylene, toluene and benzene at 160 ℃, wherein the volume ratio of the three is 5:3:2, so as to form a polypropylene solution with the concentration of 40 mg/ml; and then, a polypropylene solution is spread on a glass substrate by adopting a tape casting method, the glass substrate is dried for 50 hours at 120 ℃ under the environment that the relative humidity is 80% and the concentration of ethanol steam is 13%, ethanol steam and water vapor in the air are permeated into the surface of the polypropylene solution during drying to form honeycomb-shaped holes, so that a super-hydrophobic surface is obtained, and the obtained film is the super-hydrophobic film polypropylene film.
Example 5
Weighing 50 g of super-hydrophobic wear-resistant polypropylene block copolymer granules, and dissolving the granules in 1000ml of mixed solvent of xylene, toluene and benzene at 160 ℃, wherein the volume ratio of the three is 5:3:2, so as to form a polypropylene solution with the concentration of 40 mg/ml; and then, a polypropylene solution is spread on a glass substrate by adopting a tape casting method, the glass substrate is dried for 50 hours at 120 ℃ under the environment that the relative humidity is 80% and the concentration of ethanol steam is 13%, ethanol steam and water vapor in the air are permeated into the surface of the polypropylene solution during drying to form honeycomb-shaped holes, so that a super-hydrophobic surface is obtained, and the obtained film is the super-hydrophobic film polypropylene film.
Example 6
Weighing 60 g of super-hydrophobic wear-resistant polypropylene block copolymer granules, and dissolving the granules in 1000ml of mixed solvent of xylene, toluene and benzene at 160 ℃, wherein the volume ratio of the three is 5:3:2, so as to form a polypropylene solution with the concentration of 40 mg/ml; and then, a polypropylene solution is spread on a glass substrate by adopting a tape casting method, the glass substrate is dried for 50 hours at 120 ℃ under the environment that the relative humidity is 80% and the concentration of ethanol steam is 13%, ethanol steam and water vapor in the air are permeated into the surface of the polypropylene solution during drying to form honeycomb-shaped holes, so that a super-hydrophobic surface is obtained, and the obtained film is the super-hydrophobic film polypropylene film.
Comparative example 1
Weighing 40 g of polypropylene granules, and dissolving the polypropylene granules in 1000ml of mixed solvent of xylene, toluene and benzene at 160 ℃, wherein the volume ratio of the three is 5:3:2, so as to form a polypropylene solution with the concentration of 40 mg/ml; and then, a polypropylene solution is spread on a glass substrate by adopting a tape casting method, the glass substrate is dried for 50 hours at 120 ℃ in an environment with the relative humidity of 80% and the concentration of ethanol steam of 13%, ethanol steam and water steam in the air are permeated into the surface of the polypropylene solution during drying to form honeycomb-shaped holes, so that a super-hydrophobic surface is obtained, and the obtained film is the polypropylene film.
Comparative example 2
Weighing 50 g of polypropylene granules and 50 g of silane coupling agent, dissolving the granules and the silane coupling agent in 1000ml of mixed solvent of xylene, toluene and benzene at 160 ℃, wherein the volume ratio of the granules to the solvent is 5:3:2, so as to form a polypropylene solution with the concentration of 40 mg/ml; and then, a polypropylene solution is spread on a glass substrate by adopting a tape casting method, the glass substrate is dried for 50 hours at 120 ℃ in an environment with the relative humidity of 80% and the concentration of ethanol steam of 13%, ethanol steam and water steam in the air are permeated into the surface of the polypropylene solution during drying to form honeycomb-shaped holes, so that a super-hydrophobic surface is obtained, and the obtained film is the polypropylene film.
Comparative example 3
Weighing 60 g of polypropylene granules and 60 g of wear-resistant agent, and dissolving the granules and the wear-resistant agent in 1000ml of mixed solvent of xylene, toluene and benzene at 160 ℃, wherein the volume ratio of the granules to the solvent is 5:3:2, so as to form a polypropylene solution with the concentration of 40 mg/ml; and then, a polypropylene solution is spread on a glass substrate by adopting a tape casting method, the glass substrate is dried for 50 hours at 120 ℃ in an environment with the relative humidity of 80% and the concentration of ethanol steam of 13%, ethanol steam and water steam in the air are permeated into the surface of the polypropylene solution during drying to form honeycomb-shaped holes, so that a super-hydrophobic surface is obtained, and the obtained film is the polypropylene film.
And (3) testing the wear resistance: injection moulding a sample with dimensions of 150 × 100 × 3.2mm, according to test method SAEJ 948: 2003, test conditions: grinding the wheel: CS-10, load: the abrasion and surface whitening of the material after the test were identified at 500 g/wheel for a total of 250 revolutions.
Tensile strength was determined according to standard HG/T2580-; the bending strength is measured according to the standard GB/T12585-2001; and (3) testing the impact strength of the simply supported beam: the test specimens were 80 x 6 x 4mm in size and the depth of the indentations was one third of the thickness of the test specimens, according to ISO 179.
And (3) hydrophobic property test: the wettability of the film surface was tested using an OCAH200 contact angle tester.
Table 1 shows the abrasion resistance and the hydrophobic property of the superhydrophobic abrasion-resistant polypropylene film.
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 (10)
1. The super-hydrophobic wear-resistant polypropylene film is characterized by being formed by dissolving super-hydrophobic wear-resistant polypropylene block copolymer granules in a mixed solvent of dimethylbenzene, methylbenzene and benzene, wherein the super-hydrophobic wear-resistant polypropylene block copolymer has a structure shown in a formula (I):
in the formula, the value of n is 100-500, the value of m is 5-10, and the value of p is 10-20.
2. The super-hydrophobic abrasion-resistant polypropylene film according to claim 1, wherein the preparation method of the super-hydrophobic abrasion-resistant polypropylene block copolymer comprises the following steps:
(1) taking tetrahydrofuran as a solvent, RAFT reagent 4-cyano-4- (thiobenzoyl) valeric acid and SOCl2Performing acyl chlorination reaction to obtain 4-cyano-4- (thiobenzoyl) valeryl chloride, and performing esterification reaction on single-end hydroxyl polypropylene and 4-cyano-4- (thiobenzoyl) valeryl chloride by using toluene as a solvent and pyridine as an acid-binding agent to obtain a polypropylene macromolecule transfer agent;
(2) reacting for 2-8 hours at 70-80 ℃ under the conditions of no water, no oxygen and nitrogen protection by using dioxane as a solvent, a silane coupling agent as a monomer, a polypropylene macromolecular chain transfer agent as a chain transfer agent and azodiisobutyronitrile as an initiator to obtain a super-hydrophobic polypropylene block copolymer;
(3) reacting for 2-6 hours at 70-80 ℃ under the conditions of no water, no oxygen and nitrogen protection by using dioxane as a solvent, a wear-resisting agent as a monomer, a super-hydrophobic polypropylene block copolymer as a chain transfer agent and azodiisobutyronitrile as an initiator to obtain the super-hydrophobic wear-resisting polypropylene block copolymer.
3. The super-hydrophobic abrasion-resistant polypropylene film as claimed in claim 2, wherein the super-hydrophobic abrasion-resistant polypropylene block copolymer is prepared by reacting 4-cyano-4- (thiobenzoyl) valeric acid with SOCl in step (1)2The molar ratio of the single-end hydroxyl polypropylene is 1:1: 5.
4. The super-hydrophobic abrasion-resistant polypropylene film according to claim 2, wherein in the preparation method of the super-hydrophobic abrasion-resistant polypropylene block copolymer, in the step (2), the silane coupling agent has the following structure:
5. the super-hydrophobic abrasion-resistant polypropylene film according to claim 2, wherein in the preparation method of the super-hydrophobic abrasion-resistant polypropylene block copolymer, in the step (2), the molar ratio of the polypropylene macromolecular chain transfer agent, the azobisisobutyronitrile and the silane coupling agent is 1:10: 1000.
6. The super-hydrophobic abrasion-resistant polypropylene film according to claim 2, wherein the super-hydrophobic abrasion-resistant polypropylene block copolymer is prepared by the method that in the step (2), the concentration of the silane coupling agent is 1 mol/L.
7. The super-hydrophobic abrasion-resistant polypropylene film according to claim 2, wherein in the step (3), the preparation method of the super-hydrophobic abrasion-resistant polypropylene block copolymer comprises the following steps:
8. the super-hydrophobic abrasion-resistant polypropylene film according to claim 2, wherein in the preparation method of the super-hydrophobic abrasion-resistant polypropylene block copolymer, in the step (3), the molar ratio of the super-hydrophobic polypropylene block copolymer, the azobisisobutyronitrile and the abrasion-resistant agent is 1:10: 1000.
9. The super-hydrophobic abrasion-resistant polypropylene film according to claim 2, wherein the super-hydrophobic abrasion-resistant polypropylene block copolymer is prepared in step (3) with an abrasion-resistant agent concentration of 1 mol/L.
10. The method for preparing the super-hydrophobic abrasion-resistant polypropylene film according to claim 1, comprising the following steps:
weighing 40-60 g of super-hydrophobic wear-resistant polypropylene block copolymer granules, and dissolving the granules in 1000ml of mixed solvent of xylene, toluene and benzene at 160 ℃, wherein the volume ratio of the three is 5:3:2, so as to form a polypropylene solution with the concentration of 40 mg/ml; and then, a polypropylene solution is spread on a glass substrate by adopting a tape casting method, the glass substrate is dried for 50 hours at 120 ℃ under the environment that the relative humidity is 80% and the concentration of ethanol steam is 13%, ethanol steam and water vapor in air are permeated into the surface of the polypropylene solution during drying to form honeycomb-shaped holes, so that a super-hydrophobic surface is obtained, and the obtained film is the super-hydrophobic wear-resistant polypropylene film.
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| CN114957763A (en) * | 2022-07-08 | 2022-08-30 | 江苏三乔智能科技有限公司 | Super-hydrophobic wear-resistant polypropylene coating and preparation method thereof |
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| CN114957763A (en) * | 2022-07-08 | 2022-08-30 | 江苏三乔智能科技有限公司 | Super-hydrophobic wear-resistant polypropylene coating and preparation method thereof |
| CN114957763B (en) * | 2022-07-08 | 2023-04-14 | 江苏三乔智能科技有限公司 | Super-hydrophobic wear-resistant polypropylene coating and preparation method thereof |
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