CN115260680B - High-weather-resistance TPV composite material and preparation method thereof - Google Patents
High-weather-resistance TPV composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a high weather-resistant TPV composite material, which comprises the following steps: s1: carrying out surface activation treatment on the silicone rubber master batch particles; s2: sequentially adding aldehyde compounds and diamine for chemical reaction; then adding halogenated alkane to carry out quaternization grafting reaction; s3: carrying out anion exchange reaction on the modified silicone rubber and fluorine-containing anion salt to obtain modified silicone rubber; s4: kneading the mixture with a silicone rubber master batch and an additive, extruding and granulating to obtain a mixture A; s5: and mixing the modified fluoroplastic, the fluoroplastic master batch and the cross-linking agent to obtain a mixture B, and carrying out dynamic vulcanization on the mixture A and the mixture B to obtain the composite material. The TPV composite material not only has excellent mechanical properties and weather resistance, but also improves various properties such as antibacterial property, hydrophobicity and compatibility of the TPV composite material, and can meet the long-term use requirement of TPV products such as automobile window sealing strips and the like in a severe environment.
Description
Technical Field
The invention relates to the technical field of TPV composite materials, in particular to a high weather-resistant TPV composite material and a preparation method thereof.
Background
Thermoplastic dynamic vulcanizates (Thermoplastic Vulcanizate, TPV) are thermoplastic elastomers that use thermoplastic as the continuous phase and rubber as the dispersed phase. The TPV composite material is prepared by blending thermoplastic plastics and rubber and preparing a dynamic vulcanized thermoplastic elastomer by a dynamic vulcanization technology so as to realize the complementation of the performances of the thermoplastic plastics and the rubber, so that the composite material has more excellent performances, and is widely applied to important fields such as automobile industry, consumer goods, electronic and electric appliances, building industry and the like. Particularly, an automobile is used as a closed space, and a car window sealing strip is usually required to be used for sealing so as to prevent rainwater from leaking into the automobile and avoid influencing the quality of interior trim parts of the automobile; and the weatherstrip is often required to have long-term weather resistance in severe environments; however, the window sealing strip is also a place easy to store dirt and easy to grow bacteria, and has adverse effects on the air environment in the vehicle, so that the improvement of the performances such as antibiosis, hydrophobicity and the like is also a technical improvement point of long-term attention in the field.
Disclosure of Invention
In view of the shortcomings of the prior art, the invention aims to provide a high weather-resistant TPV composite material, so as to solve the problem that the conventional TPV composite material cannot achieve weather resistance, antibacterial property, hydrophobicity and other properties, and cannot meet long-term use requirements of TPV products such as automobile window sealing strips and the like in severe environments.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method for preparing a high weather resistant TPV composite material, the method comprising the steps of:
s1: the silicone rubber master batch particles are soaked in an activating agent for surface activation treatment, taken out and dried after being soaked for 12-24 hours, and dispersed in toluene solution to prepare a mixed solution with the mass concentration of 5-10%;
s2: sequentially adding aldehyde compounds and diamine into the mixed solution prepared in the step S1 to carry out chemical reaction; then, continuously adding halogenated alkane to carry out quaternization grafting reaction;
s3: after the reaction of the step S2 is finished, dispersing the silicon rubber particles in deionized water after filtering and washing, then adding fluorine-containing anion salt, and carrying out anion exchange reaction in an ion exchange column to obtain modified silicon rubber; the invention firstly activates hydroxyl on the surface of the silicone rubber master batch particles through a strong alkali solution, then carries out aldol condensation reaction with the added aldehyde compound, further carries out hydroxylamine reaction with the added diamine, and carries out quaternization grafting reaction with halogenated alkane, thereby improving the antibacterial property; the modified silicon rubber containing chlorine ions is obtained through a multi-step synthetic reaction route, and then the modified silicon rubber is subjected to anion exchange reaction with fluorine-containing anion salt, so that the modified silicon rubber is finally obtained. The modified silicone rubber master batch particles have excellent weather resistance, good antibacterial and hydrophobic properties, and can meet the long-term use requirements of TPV products such as automobile door and window sealing strips and the like under severe conditions. Physical migration of functional components in the TPV composite material is avoided by means of chemical grafting modification reaction, so that the long-term service life of the TPV composite material is prolonged.
S4: and (3) mixing the modified silicone rubber obtained in the step (S3), the silicone rubber master batch and the additive according to the mass ratio of 40-60: 40-60: 3-7, adding the mixture into a kneader at a certain temperature for kneading, and extruding and granulating the mixture by a screw extruder to obtain a mixture A;
s5: the modified fluoroplastic, the fluoroplastic master batch and the cross-linking agent are mixed according to the mass ratio of 40-60: 40-60: 1-5, mixing to obtain a mixture B, and mixing the mixture A obtained in the step S4 and the mixture B according to the mass ratio of 30-50: 100 are respectively fed into a double-screw extruder through different weightlessness equipment, are dynamically vulcanized at a certain melting temperature, and are pelletized through pelletizer equipment, so that the high weather-resistant TPV composite material is obtained.
Further, the activator is a mixed solution of 30-40% sodium hydroxide solution and ethylenediamine, and the mass ratio of the sodium hydroxide to the ethylenediamine is 3-5:1. According to the invention, the mixed solution of the sodium hydroxide solution and the ethylenediamine is used as an activating agent, on one hand, the inorganic alkali sodium hydroxide solution activates the surfaces of the silicone rubber master batch particles to obtain active site hydroxyl groups, and on the other hand, the addition of the organic alkali ethylenediamine further promotes the surface activation of the silicone rubber master batch particles to obtain the active site hydroxyl groups.
Further, the aldehyde compound is at least one of formaldehyde, benzaldehyde and paraldehyde. As a further preferable technical scheme, the aldehyde compound is formaldehyde.
Further, the diamine is at least one of dimethylamine, diethylamine or dipropylamine.
Further, the haloalkane is at least one of 2-chloro-1, 3-difluoropropane, 1-chloro-1-fluoroethane or 2-chloro-1, 3-tetrafluoro-propane. The halogenated alkane contains chlorine and fluorine elements, wherein the chlorine atom is more active than the fluorine atom, and is grafted on the nitrogen atom of the tertiary amino group of the modified silicone rubber to carry out quaternization reaction; and fluorine atoms introduced by the silicone rubber master batch particles play an effective role in hydrophobic and oleophobic.
Further, the additive is an inorganic filler or an antioxidant. The inorganic filler can be selected from calcium carbonate, diatomite, carbon black, etc., and the antioxidant can be selected from antioxidant 1010, antioxidant 1098, antioxidant 22462S, antioxidant 300, etc.
Further, the cross-linking agent is at least one of benzoyl peroxide, di-tert-butyl peroxide, dicumyl peroxide and dibenzoyl peroxide.
Further, the mass ratio of the silicone rubber master batch to the aldehyde compound is 100: 1-3, wherein the molar ratio of the aldehyde compound to diamine to halogenated alkane is 1:1 to 1.1:1 to 1.1.
Further, the modification method of the modified fluoroplastic comprises the following steps: adding deionized water, perfluorohexane-1-ammonium sulfonate, trifluorotrichloroethane and trimethyl vinyl ammonium bromide into a reaction kettle, stirring and sealing; introducing inert gas to 1.5-2 MPa, maintaining the pressure for 30min, and vacuumizing to-0.08 to-0.09 MPa; then slowly adding tetrafluoroethylene monomer and perfluoroethyl vinyl ether, stirring and heating to a reaction temperature of 50-120 ℃, and adding an initiator to react, wherein the pressure of a reaction kettle is 0.5-5 MPa; filtering, washing, drying, granulating, dispersing in deionized water, adding fluorine-containing anion salt, and performing anion exchange reaction in an ion exchange column to obtain the modified fluoroplastic. According to the modified fluoroplastic, the ammonium perfluorohexane-1-sulfonate is used as a dispersing agent, the trifluorotrichloroethane is used as a diluting agent, and through the reaction of trimethyl vinyl ammonium bromide, tetrafluoroethylene monomers and perfluoroethyl vinyl ether, quaternary ammonium salt functional groups and perfluoro groups are introduced into branched chains of the fluoroplastic, so that on one hand, the compatibility with a disperse phase compounded with modified silicone rubber is improved, and on the other hand, various properties of the TPV composite material, such as antibacterial property, hydrophobicity, weather resistance and the like, are further ensured.
In another aspect, the invention provides a high weather-resistant TPV composite material, which is prepared by the preparation method of the high weather-resistant TPV composite material.
The invention has the beneficial effects that:
according to the preparation method of the high weather-resistant TPV composite material, the modified fluoroplastic and the fluoroplastic master batch compounded mixture B are used as a continuous phase, and the modified silicone rubber and the silicone rubber master batch compounded mixture A are used as a disperse phase, and the high weather-resistant TPV composite material is obtained after dynamic vulcanization. The TPV composite material not only has excellent mechanical properties and weather resistance, but also improves various properties such as antibacterial property, hydrophobicity and compatibility of the TPV composite material, and can meet the long-term use requirements of TPV products such as automobile window sealing strips and the like in a severe environment.
Detailed Description
The following description is presented to enable one of ordinary skill in the art to make and use the invention. The preferred embodiments in the following description are by way of example only and other obvious variations will occur to those skilled in the art.
Example 1
The preparation method of the high weather-resistant TPV composite material comprises the following steps:
s1: the silicone rubber master batch particles are soaked in an activating agent for surface activation treatment, taken out and dried after being soaked for 12 hours, and dispersed in toluene solution to prepare a mixed solution with the mass concentration of 5 percent; the activator is mixed solution of 30% sodium hydroxide solution and ethylenediamine, and the mass ratio of the sodium hydroxide to the ethylenediamine is 3:1;
s2: and (2) sequentially adding formaldehyde and dimethylamine into the mixed solution prepared in the step (S1) to carry out chemical reaction, wherein the mass ratio of the silicone rubber master batch to the formaldehyde is 100:1, controlling the initial reaction temperature to be 10 ℃, and controlling formaldehyde to carry out aldol condensation reaction with the surface-activated silicone rubber master batch particles at the reaction temperature; heating to 60 ℃ to continue aldehyde-amine reaction, and then continuing to add 2-chloro-1, 3-difluoropropane to perform quaternization grafting reaction; the molar ratio of formaldehyde, dimethylamine and 2-chloro-1, 3-difluoropropane is 1:1.05:1.05;
s3: after the reaction of the step S2 is finished, dispersing the silicon rubber particles in deionized water after filtering and washing, then adding fluorine-containing anion salt, and carrying out anion exchange reaction in an ion exchange column to obtain modified silicon rubber;
s4: and (3) mixing the modified silicone rubber obtained in the step (S3), the silicone rubber master batch and the additive according to a mass ratio of 40:60:3, adding the mixture into a kneader at a certain temperature for kneading, and extruding and granulating the mixture by a screw extruder to obtain a mixture A; the additive comprises the following components in percentage by mass: 0.1 of calcium carbonate and an antioxidant 1010;
s5: the modified fluoroplastic, the fluoroplastic master batch and benzoyl peroxide are mixed according to the mass ratio of 60:40:1, mixing to obtain a mixture B, and mixing the mixture A and the mixture B obtained in the step S4 according to a mass ratio of 30:100 are respectively fed into a double-screw extruder through different weightlessness equipment, are dynamically vulcanized at the temperature of 190 ℃, and are pelletized through pelletizer equipment, so that the high weather-resistant TPV composite material is obtained.
The modification method of the modified fluoroplastic comprises the following steps: adding 50 parts by weight of deionized water, 12 parts by weight of ammonium perfluoro hexane-1-sulfonate, 50 parts by weight of trifluorotrichloroethane and 10 parts by weight of trimethyl vinyl ammonium bromide into a reaction kettle, stirring and sealing; introducing inert gas to 1.5MPa, maintaining the pressure for 30min, and vacuumizing to-0.08 MPa; then slowly adding tetrafluoroethylene monomer and perfluoroethyl vinyl ether, wherein the molar ratio of the tetrafluoroethylene monomer to the perfluoroethyl vinyl ether to the trimethyl vinyl ammonium bromide is 15:1:3, stirring and heating to the reaction temperature of 80 ℃, wherein the pressure of a reaction kettle is 1.5MPa, and adding 0.5 weight part of initiator sodium persulfate for reaction; filtering, washing, drying, granulating, dispersing in deionized water, adding fluorine-containing anion salt, and performing anion exchange reaction in an ion exchange column to obtain the modified fluoroplastic.
Example 2
The preparation method of the high weather-resistant TPV composite material comprises the following steps:
s1: the silicone rubber master batch particles are soaked in an activating agent for surface activation treatment, taken out and dried after being soaked for 18 hours, and dispersed in toluene solution to prepare a mixed solution with the mass concentration of 7 percent; the activator is mixed solution of 35% sodium hydroxide solution and ethylenediamine, and the mass ratio of the sodium hydroxide to the ethylenediamine is 4:1;
s2: and (2) sequentially adding formaldehyde and diethylamine into the mixed solution prepared in the step (S1) to carry out chemical reaction, wherein the mass ratio of the silicon rubber master batch to the formaldehyde is 100:2, controlling the initial reaction temperature to be 15 ℃, and controlling formaldehyde to carry out aldol condensation reaction with the surface-activated silicone rubber master batch particles at the reaction temperature; heating to 70 ℃ to continue aldehyde-amine reaction, and then continuing to add 1-chloro-1-fluoroethane to perform quaternization grafting reaction; the molar ratio of formaldehyde, diethylamine and 1-chloro-1-fluoroethane is 1:1.1:1.1;
s3: after the reaction of the step S2 is finished, dispersing the silicon rubber particles in deionized water after filtering and washing, then adding fluorine-containing anion salt, and carrying out anion exchange reaction in an ion exchange column to obtain modified silicon rubber;
s4: and (3) mixing the modified silicone rubber obtained in the step (S3), the silicone rubber master batch and the additive according to the mass ratio of 50:50:5, adding the mixture into a kneader at a certain temperature for kneading, and extruding and granulating the mixture by a screw extruder to obtain a mixture A; the additive comprises the following components in percentage by mass: 0.3 of diatomite and an antioxidant 1010;
s5: the modified fluoroplastic, the fluoroplastic master batch and benzoyl peroxide are mixed according to the mass ratio of 50:50:3, mixing to obtain a mixture B, and mixing the mixture A and the mixture B obtained in the step S4 according to a mass ratio of 40:100 are respectively fed into a double-screw extruder through different weightlessness equipment, are dynamically vulcanized at the temperature of 195 ℃, and are pelletized through pelletizer equipment, so that the high weather-resistant TPV composite material is obtained.
The modified fluoroplastic was the same as in example 1.
Example 3
The preparation method of the high weather-resistant TPV composite material comprises the following steps:
s1: the silicone rubber master batch particles are soaked in an activating agent for surface activation treatment, taken out and dried after being soaked for 24 hours, and dispersed in toluene solution to prepare a mixed solution with the mass concentration of 10 percent; the activator is mixed solution of sodium hydroxide solution with the mass concentration of 40% and ethylenediamine, and the mass ratio of the sodium hydroxide to the ethylenediamine is 5:1;
s2: adding formaldehyde and dipropylamine into the mixed solution prepared in the step S1 in sequence to carry out chemical reaction, wherein the mass ratio of the silicone rubber master batch to the formaldehyde is 100:3, controlling the initial reaction temperature to be 15 ℃, and controlling formaldehyde to carry out aldol condensation reaction with the surface-activated silicone rubber master batch particles at the reaction temperature; heating to 80 ℃ to continue aldehyde-amine reaction, and then continuing to add 2-chloro-1, 3-tetrafluoro-propane to perform quaternization grafting reaction; the molar ratio of formaldehyde to dipropylamine to 2-chloro-1, 3-tetrafluoro-propane is 1:1.1:1.1;
s3: after the reaction of the step S2 is finished, dispersing the silicon rubber particles in deionized water after filtering and washing, then adding fluorine-containing anion salt, and carrying out anion exchange reaction in an ion exchange column to obtain modified silicon rubber;
s4: and (3) mixing the modified silicone rubber obtained in the step (S3), the silicone rubber master batch and the additive according to a mass ratio of 60:40:7, adding the mixture into a kneader at a certain temperature for kneading, and extruding and granulating the mixture by a screw extruder to obtain a mixture A; the additive comprises the following components in percentage by mass: 0.5 carbon black and antioxidant 1010;
s5: the modified fluoroplastic, the fluoroplastic master batch and benzoyl peroxide are mixed according to the mass ratio of 40:60:5, mixing to obtain a mixture B, and mixing the mixture A and the mixture B obtained in the step S4 according to a mass ratio of 50:100 are respectively fed into a double-screw extruder through different weightlessness equipment, are dynamically vulcanized at the temperature of 200 ℃, and are pelletized through pelletizer equipment, so that the high weather-resistant TPV composite material is obtained.
The modified fluoroplastic was the same as in example 1.
Comparative example 1
The composition of the raw materials and the preparation method thereof of the high weather resistant TPV composite of this comparative example are substantially the same as those of example 1, except that the modified silicone rubber was not added to the TPV composite of this comparative example.
Comparative example 2
The composition of the raw materials and the preparation method of the high weather resistant TPV composite material of the comparative example are basically the same as those of the example 1, except that the modified fluoroplastic is not added to the TPV composite material of the comparative example.
The high weather resistant TPV composite materials prepared in examples 1 to 3 and comparative examples 1 to 2 were subjected to performance test, and the performance results are shown in Table 1:
wherein: tensile test: the materials were tested for mechanical properties (tensile strength, elongation at break) using a stretcher.
Antibacterial test: the antibacterial rate of the sample is detected by a dipping method, the experimental strain adopts escherichia coli, the sample is put into a 250ml conical flask filled with 70ml of PBS and 5ml of bacterial suspension, and the concentration of the bacterial suspension in the PBS is 1 multiplied by 10 4 -2×10 4 cfu/ml. After 1h of sample dipping, 0.5ml of sample solution is taken, properly diluted, cultured for 24h on an agar plate, and then viable bacteria count is carried out. No sample was used as a negative control. The average colony count change rate before and after the dipping was calculated to evaluate the antibacterial property.
TABLE 1
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention, which is defined by the appended claims.
Claims (9)
1. The preparation method of the high weather-resistant TPV composite material is characterized by comprising the following steps of:
s1: the silicone rubber master batch particles are soaked in an activating agent for surface activation treatment, taken out and dried after being soaked for 12-24 hours, and dispersed in toluene solution to prepare a mixed solution with the mass concentration of 5-10%;
s2: sequentially adding aldehyde compounds and diamine into the mixed solution prepared in the step S1 to carry out chemical reaction; then, continuously adding halogenated alkane to carry out quaternization grafting reaction;
s3: after the reaction of the step S2 is finished, dispersing the silicon rubber particles in deionized water after filtering and washing, then adding fluorine-containing anion salt, and carrying out anion exchange reaction in an ion exchange column to obtain modified silicon rubber;
s4: and (3) mixing the modified silicone rubber obtained in the step (S3), the silicone rubber master batch and the additive according to the mass ratio of 40-60: 40-60: 3-7, adding the mixture into a kneader at a certain temperature for kneading, and extruding and granulating the mixture by a screw extruder to obtain a mixture A;
s5: the modified fluoroplastic, the fluoroplastic master batch and the cross-linking agent are mixed according to the mass ratio of 40-60: 40-60: 1-5, mixing to obtain a mixture B, and mixing the mixture A obtained in the step S4 and the mixture B according to the mass ratio of 30-50: 100 are respectively fed into a double-screw extruder through different weightlessness equipment, are subjected to dynamic vulcanization at a certain melting temperature, and are subjected to pelletization through a pelletization machine equipment, so that the high weather-resistant TPV composite material is obtained;
the modification method of the modified fluoroplastic comprises the following steps: adding deionized water, perfluorohexane-1-ammonium sulfonate, trifluorotrichloroethane and trimethyl vinyl ammonium bromide into a reaction kettle, stirring and sealing; introducing inert gas to 1.5-2 MPa, maintaining the pressure for 30min, and vacuumizing to-0.08 to-0.09 MPa; then slowly adding tetrafluoroethylene monomer and perfluoroethyl vinyl ether, stirring and heating to a reaction temperature of 50-120 ℃, and adding an initiator to react, wherein the pressure of a reaction kettle is 0.5-5 MPa; filtering, washing, drying, granulating, dispersing in deionized water, adding fluorine-containing anion salt, and performing anion exchange reaction in an ion exchange column to obtain the modified fluoroplastic.
2. The method for preparing the high weather-resistant TPV composite material according to claim 1, wherein the activator is a mixed solution of 30-40% sodium hydroxide solution and ethylenediamine, and the mass ratio of the sodium hydroxide to the ethylenediamine is 3-5:1.
3. The method for preparing a high weather resistant TPV composite material according to claim 1, wherein the aldehyde compound is at least one of formaldehyde, benzaldehyde, and paraldehyde.
4. The method of preparing a high weatherable TPV composite according to claim 1, wherein the diamine is at least one of dimethylamine, diethylamine, or dipropylamine.
5. The method of preparing a high weatherable TPV composite according to claim 1, wherein the haloalkane is at least one of 2-chloro-1, 3-difluoropropane, 1-chloro-1-fluoroethane, or 2-chloro-1, 3-tetrafluoropropane.
6. The method of preparing a high weatherable TPV composite according to claim 1, wherein the additive is an inorganic filler or an antioxidant.
7. The method for preparing a high weatherable TPV composite according to claim 1, wherein the cross-linking agent is at least one of benzoyl peroxide, di-t-butyl peroxide, dicumyl peroxide.
8. The method for preparing the high weather resistant TPV composite material according to claim 1, wherein the mass ratio of the silicone rubber master batch to the aldehyde compound is 100: 1-3, wherein the molar ratio of the aldehyde compound to diamine to halogenated alkane is 1:1 to 1.1:1 to 1.1.
9. A high weather resistant TPV composite material, characterized in that the composite material is prepared by the method for preparing a high weather resistant TPV composite material according to any one of claims 1 to 8.
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| CN103396639A (en) * | 2013-07-19 | 2013-11-20 | 华南理工大学 | Dynamic vulcanized fluoroplastic/fluororubber/silicone rubber thermoplastic elastomer and preparation method thereof |
| CN106009449A (en) * | 2016-05-25 | 2016-10-12 | 北京化工大学 | High temperature-resistant oil-resistant thermoplastic vulcanizate and preparation method thereof |
| CN113480867A (en) * | 2021-07-27 | 2021-10-08 | 晶锋集团股份有限公司 | Novel fluorine material high-temperature-resistant control cable material and preparation method thereof |
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| KR20060135664A (en) * | 2003-12-15 | 2006-12-29 | 다우 코닝 코포레이션 | Fluoroplastic silicone vulcanizates |
| CN107141502B (en) * | 2017-05-31 | 2019-08-23 | 泰州度博迈医疗器械有限公司 | A kind of antibacterial silicon rubber, preparation method and applications |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103396639A (en) * | 2013-07-19 | 2013-11-20 | 华南理工大学 | Dynamic vulcanized fluoroplastic/fluororubber/silicone rubber thermoplastic elastomer and preparation method thereof |
| CN106009449A (en) * | 2016-05-25 | 2016-10-12 | 北京化工大学 | High temperature-resistant oil-resistant thermoplastic vulcanizate and preparation method thereof |
| CN113480867A (en) * | 2021-07-27 | 2021-10-08 | 晶锋集团股份有限公司 | Novel fluorine material high-temperature-resistant control cable material and preparation method thereof |
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