CN110423420B - High-strength high-temperature-resistant polyvinyl chloride material - Google Patents
High-strength high-temperature-resistant polyvinyl chloride material Download PDFInfo
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- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
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Abstract
The invention discloses a high-strength high-temperature-resistant polyvinyl chloride material which comprises the following raw materials in parts by weight: 100 parts of polyvinyl chloride, 35-45 parts of graphite, 10-15 parts of hexachlorocyclotriphosphazene, 40-50 parts of concentrated sulfuric acid with the mass fraction of 98%, 5-8 parts of potassium permanganate and 30% of H2O2 3-8 parts of polysilane aryne resin, 20-30 parts of SBS thermoplastic elastomer and 10-15 parts of benzoxazine. The modified redox graphene is used as a carrier, and the polyvinyl chloride material of the polysilane aryne resin and the SBS thermoplastic elastomer is compounded, so that the modified redox graphene has excellent tensile strength and high-temperature resistance.
Description
Technical Field
The invention relates to the technical field of polyvinyl chloride materials, in particular to a high-strength high-temperature-resistant polyvinyl chloride material.
Background
Polyvinyl chloride is a polymer polymerized by vinyl chloride monomers under the action of initiators such as peroxides and azo compounds or under the action of light and heat according to a free radical polymerization reaction mechanism, is white powder with an amorphous structure, has small branching degree, relative density of about 1.4, glass transition temperature of 77-90 ℃, starts to decompose at about 170 ℃, has poor stability to light and heat, can be decomposed to generate hydrogen chloride at more than 100 ℃ or after being exposed to sunlight for a long time, and further automatically catalyzes and decomposes to cause color change, and the physical and mechanical properties are also rapidly reduced, so that a novel polyvinyl chloride material can be produced; the existing polyvinyl chloride material has single function, and is not compatible with high temperature resistance and high strength well, so that the invention provides a high-strength high-temperature-resistant polyvinyl chloride material.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a high-strength high-temperature-resistant polyvinyl chloride material.
The invention provides a high strengthThe high-temperature resistant polyvinyl chloride material comprises the following raw materials in parts by weight: 100 parts of polyvinyl chloride, 35-45 parts of graphite, 10-15 parts of hexachlorocyclotriphosphazene, 40-50 parts of concentrated sulfuric acid with the mass fraction of 98%, 5-8 parts of potassium permanganate and 30% of H2O2 3-8 parts of polysilane aryne resin, 20-30 parts of SBS thermoplastic elastomer and 10-15 parts of benzoxazine.
A preparation method of a high-strength high-temperature-resistant polyvinyl chloride material comprises the following steps:
s1: adding graphite into 98% concentrated sulfuric acid, adding potassium permanganate, stirring, adding 30% H2O2Heating hexachlorocyclotriphosphazene in a water bath, pouring out supernatant, washing with hydrochloric acid with the mass fraction of 10%, suction filtering, and drying to obtain a material A;
s2: dispersing the material A in dimethyl amide for ultrasonic treatment, adding polyvinyl chloride into dimethyl amide solution in the ultrasonic treatment process, and then centrifugally drying to obtain a material B;
s3: mixing the material B with polysilane aryne resin, adding benzoxazine in the mixing process, heating in an oil bath, cooling, performing suction filtration, and drying a filter cake;
s4: plasticizing the filter cake and SBS thermoplastic elastomer at high temperature to obtain material C;
s5: cooling and tabletting the material C.
Preferably, in S1, H with the mass fraction of 30 percent is added during stirring2O2And the temperature of hexachlorocyclotriphosphazene is 80-100 ℃, the temperature of water bath heating is 55-65 ℃, and the water bath time is 1-2 hours.
Preferably, in S2, material A is dispersed in dimethyl amide for 1-2 hours of ultrasonic treatment, and is washed by deionized water before the last centrifugation, and is taken out and dried after being washed.
Preferably, in S3, the temperature of the oil bath is 100-120 ℃ for 2-4 hours, stirring is continued during the oil bath, and the vessel is repeatedly washed with a dimethylformamide solution before suction filtration.
Preferably, in S3 and S4, the material B and the filter cake are dried in a vacuum drying oven.
Preferably, in S4, the SBS thermoplastic elastomer is preheated for 1-2 hours before the high-temperature plastication, the preheating temperature is 120-140 ℃, and the high-temperature plastication temperature is 160-180 ℃, and the time is 2-3 hours.
Graphene is a two-dimensional honeycomb-shaped carbon nanomaterial formed by single-layer carbon atoms, is the basic building block dimension of all other graphite materials, is a novel material, and has a series of excellent physicochemical properties.
In the invention, in S1, graphite is used as a raw material to be subjected to oxidation reduction to prepare redox graphene (GO represents the redox graphene), potassium permanganate has strong oxidizing property in concentrated sulfuric acid, and the mass fraction of potassium permanganate is 30% of H2O2Forming reducing agent under acidic potassium permanganate, oxidation of graphite in potassium permanganate and H2O2GO is prepared under the reduction, GO has good mechanical properties, it can make its performance such as mechanical properties and barrier properties obtain very big improvement to fill a small amount of GO in polymer organic material, GO' S specific surface area is than great and its surface has many polar groups such as hydroxyl, carboxyl, this makes GO lamella agglomerate more easily in the composite material base member, but the dispersion degree is lower, in the S1, H2O2When graphite oxide is reduced, hexachlorocyclotriphosphazene is added to carry out surface modification on GO, the surface is smoother than that without modification, so that the interaction force between layers is weakened, the dispersibility in high polymer is improved, and the activity is improved.
In S2, the modified GO and the polyvinyl chloride polymer are prepared into a composite material, so that the mechanical property of the polyvinyl chloride is improved, meanwhile, the specific surface area of the GO is large, and the surface of the GO is provided with a plurality of polar groups similar to hydroxyl, carboxyl and the like, so that the GO can conveniently react with other materials with high heat resistance and high strength.
In S3, the polysilane aryne resin has extremely high heat resistance, and benzoxazine is added at the temperature of 100-120 ℃, the benzoxazine has good mechanical property, low water absorption and excellent thermal stability, the thermal decomposition temperature and the residue rate of benzoxazine with alkynyl are obviously improved compared with benzoxazine, the polysilane aryne resin can be used for hybridizing silicon-containing aryne resin, the viscosity is reduced after the reaction with a material B, the processing performance is excellent, and the bending strength is obviously improved.
The SBS thermoplastic elastomer in the S4 is a styrene-butadiene-styrene block copolymer, has the characteristics of excellent tensile strength, large surface friction coefficient, good processing performance and the like, is blended with the product in the S3 to obtain the modified redox graphene which is used as a carrier, is compounded with the polysilane aryne resin and the polyvinyl chloride material of the SBS thermoplastic elastomer, and has excellent tensile strength and high temperature resistance.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Example one
The embodiment provides a high-strength high-temperature-resistant polyvinyl chloride material which comprises the following raw materials in parts by weight: 100 parts of polyvinyl chloride, 35 parts of graphite, 10 parts of hexachlorocyclotriphosphazene, 40 parts of concentrated sulfuric acid with the mass fraction of 98%, 5 parts of potassium permanganate and 30% of H2O2 3 parts of polysilane aryne resin 20 parts, SBS thermoplastic elastomer 20 parts and benzoxazine 10 parts.
The preparation method comprises the following steps:
s1: adding graphite into 98% concentrated sulfuric acid, adding potassium permanganate, stirring, adding 30% H2O2Heating hexachlorocyclotriphosphazene in a water bath, pouring out supernatant, washing with hydrochloric acid with the mass fraction of 10%, suction filtering, and drying to obtain a material A;
s2: dispersing the material A in dimethyl amide for ultrasonic treatment, adding polyvinyl chloride into dimethyl amide solution in the ultrasonic treatment process, and then centrifugally drying to obtain a material B;
s3: mixing the material B with polysilane aryne resin, adding benzoxazine in the mixing process, heating in an oil bath, cooling, performing suction filtration, and drying a filter cake;
s4: plasticizing the filter cake and SBS thermoplastic elastomer at high temperature to obtain material C;
s5: cooling and tabletting the material C.
Example two
The embodiment provides a high-strength high-temperature-resistant polyvinyl chloride material which comprises the following raw materials in parts by weight: 100 parts of polyvinyl chloride, 45 parts of graphite, 15 parts of hexachlorocyclotriphosphazene, 50 parts of concentrated sulfuric acid with the mass fraction of 98%, 8 parts of potassium permanganate and 30% of H2O2 8 parts of polysilane aryne resin, 30 parts of SBS thermoplastic elastomer and 15 parts of benzoxazine;
the preparation method comprises the following steps:
s1: adding graphite into 98% concentrated sulfuric acid, adding potassium permanganate, stirring, adding 30% H2O2Heating hexachlorocyclotriphosphazene in a water bath, pouring out supernatant, washing with hydrochloric acid with the mass fraction of 10%, suction filtering, and drying to obtain a material A;
s2: dispersing the material A in dimethyl amide for ultrasonic treatment, adding polyvinyl chloride into dimethyl amide solution in the ultrasonic treatment process, and then centrifugally drying to obtain a material B;
s3: mixing the material B with polysilane aryne resin, adding benzoxazine in the mixing process, heating in an oil bath, cooling, performing suction filtration, and drying a filter cake;
s4: plasticizing the filter cake and SBS thermoplastic elastomer at high temperature to obtain material C;
s5: cooling and tabletting the material C.
EXAMPLE III
The embodiment provides a high-strength high-temperature-resistant polyvinyl chloride material which comprises the following raw materials in parts by weight: 100 parts of polyvinyl chloride, 37 parts of graphite, 11 parts of hexachlorocyclotriphosphazene, 42 parts of concentrated sulfuric acid with the mass fraction of 98%, 6 parts of potassium permanganate and 30% of H2O2 4 parts of polysilane aryne resin 23 parts, SBS thermoplastic elastomer 22 parts and benzoxazine 12 parts;
the preparation method comprises the following steps:
s1: adding graphite into 98% concentrated sulfuric acid, adding potassium permanganate, stirring, and stirringAdding 30 percent of H in mass fraction in the stirring process2O2Heating hexachlorocyclotriphosphazene in a water bath, pouring out supernatant, washing with hydrochloric acid with the mass fraction of 10%, suction filtering, and drying to obtain a material A;
s2: dispersing the material A in dimethyl amide for ultrasonic treatment, adding polyvinyl chloride into dimethyl amide solution in the ultrasonic treatment process, and then centrifugally drying to obtain a material B;
s3: mixing the material B with polysilane aryne resin, adding benzoxazine in the mixing process, heating in an oil bath, cooling, performing suction filtration, and drying a filter cake;
s4: plasticizing the filter cake and SBS thermoplastic elastomer at high temperature to obtain material C;
s5: cooling and tabletting the material C.
Example four
The embodiment provides a high-strength high-temperature-resistant polyvinyl chloride material which comprises the following raw materials in parts by weight: 100 parts of polyvinyl chloride, 42 parts of graphite, 13 parts of hexachlorocyclotriphosphazene, 47 parts of concentrated sulfuric acid with the mass fraction of 98%, 7 parts of potassium permanganate and 30% of H2O2 7 parts of polysilane aryne resin 28 parts, SBS thermoplastic elastomer 27 parts and benzoxazine 14 parts;
the preparation method comprises the following steps:
s1: adding graphite into 98% concentrated sulfuric acid, adding potassium permanganate, stirring, adding 30% H2O2Heating hexachlorocyclotriphosphazene in a water bath, pouring out supernatant, washing with hydrochloric acid with the mass fraction of 10%, suction filtering, and drying to obtain a material A;
s2: dispersing the material A in dimethyl amide for ultrasonic treatment, adding polyvinyl chloride into dimethyl amide solution in the ultrasonic treatment process, and then centrifugally drying to obtain a material B;
s3: mixing the material B with polysilane aryne resin, adding benzoxazine in the mixing process, heating in an oil bath, cooling, performing suction filtration, and drying a filter cake;
s4: plasticizing the filter cake and SBS thermoplastic elastomer at high temperature to obtain material C;
s5: cooling and tabletting the material C.
EXAMPLE five
The embodiment provides a high-strength high-temperature-resistant polyvinyl chloride material which comprises the following raw materials in parts by weight: 100 parts of polyvinyl chloride, 40 parts of graphite, 13 parts of hexachlorocyclotriphosphazene, 45 parts of concentrated sulfuric acid with the mass fraction of 98%, 6.5 parts of potassium permanganate and 30% of H2O26 parts of polysilane aryne resin 25 parts, SBS thermoplastic elastomer 25 parts and benzoxazine 12.5 parts;
the preparation method comprises the following steps:
s1: adding graphite into 98% concentrated sulfuric acid, adding potassium permanganate, stirring, adding 30% H2O2Heating hexachlorocyclotriphosphazene in a water bath, pouring out supernatant, washing with hydrochloric acid with the mass fraction of 10%, suction filtering, and drying to obtain a material A;
s2: dispersing the material A in dimethyl amide for ultrasonic treatment, adding polyvinyl chloride into dimethyl amide solution in the ultrasonic treatment process, and then centrifugally drying to obtain a material B;
s3: mixing the material B with polysilane aryne resin, adding benzoxazine in the mixing process, heating in an oil bath, cooling, performing suction filtration, and drying a filter cake;
s4: plasticizing the filter cake and SBS thermoplastic elastomer at high temperature to obtain material C;
s5: cooling and tabletting the material C.
Comparative example 1
The comparison example provides a high-strength high-temperature-resistant polyvinyl chloride material, and the difference with the example 5 is that SBS thermoplastic elastomer is removed;
the feed comprises the following raw materials in parts by weight: 100 parts of polyvinyl chloride, 40 parts of graphite, 13 parts of hexachlorocyclotriphosphazene, 45 parts of concentrated sulfuric acid with the mass fraction of 98%, 6.5 parts of potassium permanganate and 30% of H2O26 parts of polysilane aryne resin 25 parts and benzoxazine 12.5 parts;
the preparation method comprises the following steps:
s1: adding graphite into 98% concentrated sulfuric acid, adding potassium permanganate, stirring, adding 30% H2O2Heating hexachlorocyclotriphosphazene in a water bath, pouring out supernatant, washing with hydrochloric acid with the mass fraction of 10%, suction filtering, and drying to obtain a material A;
s2: dispersing the material A in dimethyl amide for ultrasonic treatment, adding polyvinyl chloride into dimethyl amide solution in the ultrasonic treatment process, and then centrifugally drying to obtain a material B;
s3: mixing the material B with polysilane aryne resin, adding benzoxazine in the mixing process, heating in an oil bath, cooling, performing suction filtration, and drying a filter cake to obtain a material C1;
s4: material C1 was cooled and tabletted.
Comparative example No. two
The comparison example provides a high-strength high-temperature-resistant polyvinyl chloride material, and the difference from the example 5 is that polysilane aryne resin and benzoxazine are removed;
the feed comprises the following raw materials in parts by weight: 100 parts of polyvinyl chloride, 40 parts of graphite, 13 parts of hexachlorocyclotriphosphazene, 45 parts of concentrated sulfuric acid with the mass fraction of 98%, 6.5 parts of potassium permanganate and 30% of H2O26 parts of SBS thermoplastic elastomer 25 parts;
the preparation method comprises the following steps:
s1: adding graphite into 98% concentrated sulfuric acid, adding potassium permanganate, stirring, adding 30% H2O2Heating hexachlorocyclotriphosphazene in a water bath, pouring out supernatant, washing with hydrochloric acid with the mass fraction of 10%, suction filtering, and drying to obtain a material A;
s2: dispersing the material A in dimethyl amide for ultrasonic treatment, adding polyvinyl chloride into dimethyl amide solution in the ultrasonic treatment process, and then centrifugally drying to obtain a material B;
s3: plasticizing the material B and SBS thermoplastic elastomer at high temperature to obtain a material C2;
s4: material C2 was cooled and tabletted.
The tensile strength, abrasion resistance, thermal expansion coefficient and thermal stability time at 200 degrees of comparative tests were carried out after the products obtained in example 1, example 2, example 3, example 4 and example 5, and the products obtained in comparative example one and comparative example two were left for one month, and the test results are shown in Table 1:
TABLE 1
| Tensile Strength (MPa) | Abrasion resistance (g/100 r) | Coefficient of thermal expansion (. times.10)-5/K） | Thermal stability time (min) at 200 DEG C | |
| Example one | 30.5 | 0.047 | 2.31 | 215 |
| Example two | 31.6 | 0.051 | 2.23 | 204 |
| EXAMPLE III | 30.8 | 0.054 | 2.22 | 208 |
| Example four | 29.8 | 0.051 | 2.43 | 211 |
| EXAMPLE five | 34.7 | 0.055 | 2.44 | 220 |
| Comparative example 1 | 27.5 | 0.033 | 2.35 | 223 |
| Comparative example No. two | 35.8 | 0.054 | 1.87 | 183 |
From the experimental data in table 1, it can be seen that the example is obviously higher in strength than comparative example 1, higher in heat resistance than comparative example 2, and the product obtained in the fifth example has the best performance, so that the polyvinyl chloride material prepared by the invention and using the modified redox graphene as a carrier, compounding the polysilane aryne resin and the SBS thermoplastic elastomer has excellent tensile strength and high temperature resistance.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. A preparation method of high-strength high-temperature-resistant polyvinyl chloride material is characterized in that,
the feed comprises the following raw materials in parts by weight: 100 parts of polyvinyl chloride, 35-45 parts of graphite, 10-15 parts of hexachlorocyclotriphosphazene, 40-50 parts of concentrated sulfuric acid with the mass fraction of 98%, 5-8 parts of potassium permanganate and 30% of H2O2 3-8 parts of polysilane aryne resin, 20-30 parts of SBS thermoplastic elastomer and 10-15 parts of benzoxazine;
the method comprises the following steps:
s1: adding graphite into 98% concentrated sulfuric acid, adding potassium permanganate, stirring, adding 30% H2O2Heating hexachlorocyclotriphosphazene in a water bath, pouring out supernatant, washing with hydrochloric acid with the mass fraction of 10%, suction filtering, and drying to obtain a material A;
s2: dispersing the material A in dimethyl amide for ultrasonic treatment, adding polyvinyl chloride into dimethyl amide solution in the ultrasonic treatment process, and then centrifugally drying to obtain a material B;
s3: mixing the material B with polysilane aryne resin, adding benzoxazine in the mixing process, heating in an oil bath, cooling, performing suction filtration, and drying a filter cake;
s4: plasticizing the filter cake and SBS thermoplastic elastomer at high temperature to obtain material C;
s5: cooling and tabletting the material C.
2. The method for preparing high-strength high-temperature-resistant polyvinyl chloride material according to claim 1, wherein in the step S1, 30% by weight of H is added during stirring2O2The temperature of the hexachlorocyclotriphosphazene and the hexachlorocyclotriphosphazene is 80-100 ℃, the temperature of the hexachlorocyclotriphosphazene and the hexachlorocyclotriphosphazene during water bath heating is 55-65 ℃, and the temperature of the hexachlorocyclotriphosphazene and the hexachlorocyclotriphosphazene during water bath heating isThe time is 1-2 hours.
3. The method for preparing a high-strength high-temperature resistant polyvinyl chloride material according to claim 1, wherein in the step S2, the material A is dispersed in dimethyl amide for 1-2 hours of ultrasonic treatment, and is washed with deionized water before the last centrifugation, and is taken out and dried after being washed.
4. The method as claimed in claim 1, wherein the temperature of the oil bath in S3 is 100-120 ℃ for 2-4 hours, the stirring is continued during the oil bath, and the vessel is repeatedly washed with dimethylformamide solution before suction filtration.
5. The method as claimed in claim 1, wherein in each of the steps S3 and S4, the material B and the filter cake are dried in a vacuum drying oven.
6. The method as claimed in claim 1, wherein in S4, the SBS thermoplastic elastomer is preheated for 1-2 hours before the high temperature plastication, the preheating temperature is 120-140 ℃, and the high temperature plastication temperature is 160-180 ℃ for 2-3 hours.
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2019
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