CN113462102B - Polyvinyl chloride composite material and preparation method thereof - Google Patents
Polyvinyl chloride composite material and preparation method thereof Download PDFInfo
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- CN113462102B CN113462102B CN202110951160.4A CN202110951160A CN113462102B CN 113462102 B CN113462102 B CN 113462102B CN 202110951160 A CN202110951160 A CN 202110951160A CN 113462102 B CN113462102 B CN 113462102B
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- polyionic liquid
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- 229920000915 polyvinyl chloride Polymers 0.000 title claims abstract description 82
- 239000004800 polyvinyl chloride Substances 0.000 title claims abstract description 82
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims description 10
- 229920000831 ionic polymer Polymers 0.000 claims description 60
- 239000007788 liquid Substances 0.000 claims description 60
- 239000000463 material Substances 0.000 claims description 43
- 239000000203 mixture Substances 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 38
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 26
- -1 tetrafluoroborate Chemical compound 0.000 claims description 26
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000002243 precursor Substances 0.000 claims description 22
- 238000001291 vacuum drying Methods 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 17
- 239000004014 plasticizer Substances 0.000 claims description 17
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 17
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 17
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 13
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 3
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 2
- RAXXELZNTBOGNW-UHFFFAOYSA-O Imidazolium Chemical compound C1=C[NH+]=CN1 RAXXELZNTBOGNW-UHFFFAOYSA-O 0.000 claims description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 150000002367 halogens Chemical class 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000002002 slurry Substances 0.000 description 19
- 239000011248 coating agent Substances 0.000 description 11
- 238000000576 coating method Methods 0.000 description 11
- 239000000243 solution Substances 0.000 description 11
- 239000002904 solvent Substances 0.000 description 10
- 239000000758 substrate Substances 0.000 description 10
- 238000000926 separation method Methods 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 8
- 239000011521 glass Substances 0.000 description 8
- 239000011259 mixed solution Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000003566 sealing material Substances 0.000 description 5
- NXQMCAOPTPLPRL-UHFFFAOYSA-N 2-(2-benzoyloxyethoxy)ethyl benzoate Chemical compound C=1C=CC=CC=1C(=O)OCCOCCOC(=O)C1=CC=CC=C1 NXQMCAOPTPLPRL-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- ZFMQKOWCDKKBIF-UHFFFAOYSA-N bis(3,5-difluorophenyl)phosphane Chemical compound FC1=CC(F)=CC(PC=2C=C(F)C=C(F)C=2)=C1 ZFMQKOWCDKKBIF-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- KAIPKTYOBMEXRR-UHFFFAOYSA-N 1-butyl-3-methyl-2h-imidazole Chemical compound CCCCN1CN(C)C=C1 KAIPKTYOBMEXRR-UHFFFAOYSA-N 0.000 description 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- XKBGEWXEAPTVCK-UHFFFAOYSA-M methyltrioctylammonium chloride Chemical compound [Cl-].CCCCCCCC[N+](C)(CCCCCCCC)CCCCCCCC XKBGEWXEAPTVCK-UHFFFAOYSA-M 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/10—Metal compounds
- C08K3/14—Carbides
-
- 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
- C08K7/00—Use of ingredients characterised by shape
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention belongs to the technical field of high molecular compounds, and particularly relates to a polyvinyl chloride composite material. The composite material comprises polyvinyl chloride and michael. The invention obviously improves the low temperature resistance and the mechanical property of the polyvinyl chloride.
Description
Technical Field
The invention belongs to the technical field of high molecular compounds, and particularly relates to a polyvinyl chloride composite material and a preparation method thereof.
Background
In recent years, with the development of society, sealing materials and flexible pipes for electric wires, cables, refrigerators, freezers, and residential doors and windows have become more and more popular, and the demand for such sealing materials and flexible pipes has been increasing, and the requirements for such sealing materials and flexible pipes have been increasing, particularly in terms of flexibility, wear resistance, and low temperature resistance.
Polyvinyl chloride is one of general-purpose resins, has the characteristics of low price, excellent flame retardant property, excellent insulation property, corrosion resistance, wide raw material sources and the like, is a plastic material with the largest domestic yield and the lowest price at present, can be used for hard products and soft products, and can be used for preparing the sealing material and the soft pipe (the latest research progress of polyvinyl chloride modification, wang Jiangong and the like, chemical intermediates, no. 6 of 2010, no. 1 of the left column of the page 19, no. 1 to No. 6 of the section, and the published day 12 and 31 of 2010), the development and the application of hard polyvinyl chloride impact modifier-acrylate copolymer (ACR-BM), hodgkin and the like, polyvinyl chloride, no. 1 of 1986, no. 1 to No. 2 of the abstract, and the published day 12 and 31 of 1986).
However, at present, the low temperature resistance of polyvinyl chloride is poor, and the low temperature embrittlement temperature is about-15 ℃, so that the sealing material and the flexible pipe made of the polyvinyl chloride as the base material have poor low temperature resistance.
Disclosure of Invention
In view of the above, the present invention aims to provide a polyvinyl chloride composite material having a remarkable low temperature resistance.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the composite material comprises polyvinyl chloride and michael.
The michael (MXene) is a class of metal carbide and metal nitride materials with two-dimensional layered structure.
Further, the composite material also comprises a polyion liquid mixture.
Further, the polyionic liquid mixture comprises polyionic liquid and a plasticizer.
Further, the polyionic liquid includes, but is not limited to, imidazolium polyionic liquid, quaternary ammonium polyionic liquid, pyrrole polyionic liquid, halogen polyionic liquid or tetrafluoroborate polyionic liquid.
Further, the plasticizer includes, but is not limited to, glycol fatty acid ester, dipentaerythritol ester, glycol (including polyglycidyl alcohol) benzoate, ethylene carbonate, or propylene carbonate.
Further, the mass ratio of the polyion liquid to the plasticizer is 2-5:1-10.
Furthermore, the mixture ratio of the polyvinyl chloride, the michael and the polyion liquid is 50-80 percent, 5-10 percent and 15-40 percent in percentage by mass.
Further, the thickness of the composite material is 50-250 μm.
The invention also aims to protect the preparation method of the composite material, which comprises the following steps:
preparing a michael material: adding titanium aluminum carbide into hydrofluoric acid, stirring, performing centrifugal separation, washing, filtering, drying and grinding to obtain a powdery pre-polymer of a mikelene material;
adding a precursor of a powdery michael material into dimethyl sulfoxide for ultrasonic stripping, then mixing with polyvinyl chloride, stirring to fully dissolve the polyvinyl chloride, then uniformly adding the polyvinyl chloride into a polytetrafluoroethylene mold, and performing vacuum drying to obtain the polytetrafluoroethylene material.
Further, the preparation method of the composite material also comprises the following steps:
preparation of polyion liquid mixture: mixing the polyion liquid and the plasticizer, adding the mixture into tetrahydrofuran, and uniformly stirring to obtain a polyion liquid mixture;
dissolving the precursor of the powdery michael material in a polyion liquid mixture after ultrasonic separation, and then mixing the solution with polyvinyl chloride.
Further, the preparation method of the composite material comprises the following steps:
preparing a michael material: adding titanium aluminum carbide into hydrofluoric acid, stirring, centrifuging, washing, filtering, drying and grinding the obtained precipitate to obtain a powdery pre-polymer of a michael material;
preparation of polyion liquid mixture: mixing the polyion liquid and the plasticizer, adding the mixture into tetrahydrofuran, and uniformly stirring to obtain a polyion liquid mixture;
adding a precursor of a powdery michael material into dimethyl sulfoxide for ultrasonic stripping, dissolving in a polyion liquid mixture, and stirring; and mixing the solution with polyvinyl chloride, stirring to fully dissolve the polyvinyl chloride, uniformly adding the polyvinyl chloride into a polytetrafluoroethylene mold, and performing vacuum drying to obtain the polytetrafluoroethylene composite material.
The invention has the beneficial effects that:
the invention obviously improves the low temperature resistance of the polyvinyl chloride.
The invention further improves the mechanical property of the polyvinyl chloride.
The preparation method is simple.
Detailed Description
The examples are provided for better illustration of the present invention, but the present invention is not limited to the examples. Therefore, those skilled in the art should make insubstantial modifications and adaptations to the embodiments of the present invention in light of the above teachings and remain within the scope of the invention.
In the invention, the low-temperature embrittlement temperature is tested by using B-type sample strips according to GB5470-2008 determination of embrittlement temperature by plastic impact method, and the number of the samples is 10.
The detection method of the tensile strength comprises the following steps:
1) The measuring tool measures the length and width of the faying surface of the test piece to the accuracy of 0.05mm.
2) The test specimen is symmetrically clamped in the upper and lower clamps, and the distance from the clamping position to the overlapping end is (50 + 1) mm.
3) The test instrument was started and loaded at a steady speed over (5 s 1) mm/min, the maximum load of shear failure of the test specimen was recorded, and the type of adhesive failure (cohesive failure, adhesive failure, metal failure) was recorded. In the formula of σ t = p/(bxd), σ t is tensile strength (MPa); p is the maximum load (N); b is the specimen width (mm); d is the specimen thickness (mm). Note that the area used in the calculation is the original cross-sectional area of the specimen at the fracture, not the post-fracture port cross-sectional area.
Example 1:
the microphone/polyvinyl chloride composite material comprises the following steps:
in a glass vessel, 2.66g of polyionic liquid (1-butyl-3-methylimidazole) and 1.43g of plasticizer (phthalic acid ester) were weighed out, dissolved in 10ml of tetrahydrofuran, and stirred for 6 hours to obtain a polyionic liquid mixture.
Slowly adding 1.0g of aluminum titanium carbide into an aqueous solution with the mass percent concentration of 50% HF, quickly stirring for 12h, and then carrying out centrifugal separation, washing, filtering, vacuum drying and grinding to obtain powdery precursor polymer of the microphone material.
Adding the precursor of the powdery microphone material into 10ml of dimethyl sulfoxide for ultrasonic stripping for 30min, then adding the polyion liquid mixture into the microphone material subjected to ultrasonic stripping, mixing and stirring for more than 24 hours to obtain a mixed solution A. And adding 5g of polyvinyl chloride into the solution A, stirring for more than 1h to fully dissolve the polyvinyl chloride to obtain a microphone/polyvinyl chloride composite material slurry, coating the slurry on a polytetrafluoroethylene film or an electrode substrate by using a coater, standing for 30min, volatilizing redundant solvent, and then carrying out vacuum drying at the temperature of 75 ℃ for 8h to finally obtain the microphone/polyvinyl chloride composite material.
Example 2:
the microphone/polyvinyl chloride composite material comprises the following steps:
1.34g of polyionic liquid (trioctylmethylammonium chloride), 2.66g of plasticizer (dipentaerythritol hexacarboxylate) were weighed in a glass container, dissolved in 10ml of tetrahydrofuran and stirred for 6 hours to obtain a polyionic liquid mixture. Slowly adding 1.0g of aluminum titanium carbide into an aqueous solution with the mass percent concentration of 50% HF, quickly stirring for 12h, and then carrying out centrifugal separation, washing, filtering, vacuum drying and grinding to obtain powdery precursor polymer of the microphone material.
Adding the precursor of the powdery microphone material into 10ml of dimethyl sulfoxide for ultrasonic stripping for 30min, then adding the polyion liquid mixture into the microphone material subjected to ultrasonic stripping, mixing and stirring for more than 24 hours to obtain a mixed solution A. And adding 5g of polyvinyl chloride into the solution A, stirring for more than 1h to fully dissolve the polyvinyl chloride to obtain a microphone/polyvinyl chloride composite material slurry, coating the slurry on a polytetrafluoroethylene film or an electrode substrate by using a coater, standing for 30min, volatilizing redundant solvent, and then carrying out vacuum drying at the temperature of 75 ℃ for 8h to finally obtain the microphone/polyvinyl chloride composite material.
Example 3:
the microphone/polyvinyl chloride composite material comprises the following steps:
0.067g of polyion liquid (N-methyl-N-propyl pyrrole bistrifluoromethylsulfonimide) and 0.034g of plasticizer (diethylene glycol dibenzoate) were weighed out in a glass container, dissolved in 10ml of tetrahydrofuran and stirred for 6 hours to obtain a polyion liquid mixture. 0.1g of aluminum titanium carbide was slowly added to an aqueous solution containing 50% by mass of HF, and after rapid stirring for 12 hours, the mixture was subjected to centrifugal separation, washing, filtration, vacuum drying, and grinding to obtain a powdery precursor of a microphone material.
Adding the precursor of the powdery microphone material into 10ml of dimethyl sulfoxide for ultrasonic stripping for 30min, then adding the polyion liquid mixture into the microphone material subjected to ultrasonic stripping, mixing and stirring for more than 24 hours to obtain a mixed solution A. And adding 9.85g of polyvinyl chloride into the solution A, stirring for more than 1h to fully dissolve the polyvinyl chloride to obtain a microphone/polyvinyl chloride composite material slurry, coating the slurry on a polytetrafluoroethylene film or an electrode substrate by using a coater, standing for 30min, volatilizing redundant solvent, and then carrying out vacuum drying at the temperature of 75 ℃ for 8h to finally obtain the microphone/polyvinyl chloride composite material.
Example 4:
the microphone/polyvinyl chloride composite material comprises the following steps:
0.067g of polyionic liquid (trifluoromethanesulfonic acid) and 0.034g of plasticizer (dioctyl adipate) were weighed out in a glass container and dissolved in 10ml of tetrahydrofuran and stirred for 6 hours to obtain a polyionic liquid mixture. 0.05g of aluminum titanium carbide was slowly added to an aqueous solution containing 50% by mass of HF, and after rapid stirring for 12 hours, the mixture was subjected to centrifugal separation, washing, filtration, vacuum drying, and grinding to obtain a powdery precursor of a microphone material.
Adding the precursor of the powdery microphone material into 10ml of dimethyl sulfoxide for ultrasonic stripping for 30min, then adding the polyion liquid mixture into the microphone material subjected to ultrasonic stripping, mixing and stirring for more than 24 hours to obtain a mixed solution A. And adding 9.85g of polyvinyl chloride into the solution A, stirring for more than 1h to fully dissolve the polyvinyl chloride to obtain a microphone/polyvinyl chloride composite material slurry, coating the slurry on a polytetrafluoroethylene film or an electrode substrate by using a coater, standing for 30min, volatilizing redundant solvent, and then carrying out vacuum drying at the temperature of 75 ℃ for 8h to finally obtain the microphone/polyvinyl chloride composite material.
Example 5:
the microphone/polyvinyl chloride composite material comprises the following steps:
0.067g of polyionic liquid (trifluoromethanesulfonic acid) and 0.034g of plasticizer (dioctyl adipate) were weighed out in a glass container and dissolved in 10ml of tetrahydrofuran and stirred for 6 hours to obtain a polyionic liquid mixture. Slowly adding 0.52g of aluminum titanium carbide into an aqueous solution of HF with a mass percent concentration of 50%, rapidly stirring for 12h, centrifuging, washing, filtering, vacuum drying, and grinding to obtain a powdery precursor polymer of the microphone material.
Adding the precursor of the powdery microphone material into 10ml of dimethyl sulfoxide for ultrasonic stripping for 30min, then adding the polyion liquid mixture into the microphone material subjected to ultrasonic stripping, mixing and stirring for more than 24 hours to obtain a mixed solution A. And adding 9.85g of polyvinyl chloride into the solution A, stirring for more than 1h to fully dissolve the polyvinyl chloride to obtain a microphone/polyvinyl chloride composite material slurry, coating the slurry on a polytetrafluoroethylene film or an electrode substrate by using a coater, standing for 30min, volatilizing redundant solvent, and then carrying out vacuum drying at the temperature of 75 ℃ for 8h to finally obtain the microphone/polyvinyl chloride composite material.
Example 6:
the microphone/polyvinyl chloride composite material comprises the following steps:
0.067g of polyionic liquid (trifluoromethanesulfonic acid) and 0.034g of plasticizer (dioctyl adipate) were weighed out in a glass container and dissolved in 10ml of tetrahydrofuran and stirred for 6 hours to obtain a polyionic liquid mixture. 1.11g of aluminum titanium carbide was slowly added to an aqueous solution containing 50% by mass of HF, and after rapid stirring for 12 hours, the mixture was subjected to centrifugal separation, washing, filtration, vacuum drying, and grinding to obtain a powdery precursor of a microphone material.
Adding the precursor of the powdery microphone material into 10ml of dimethyl sulfoxide for ultrasonic stripping for 30min, then adding the polyion liquid mixture into the microphone material subjected to ultrasonic stripping, mixing and stirring for more than 24 hours to obtain a mixed solution A. And adding 9.85g of polyvinyl chloride into the solution A, stirring for more than 1h to fully dissolve the polyvinyl chloride to obtain a microphone/polyvinyl chloride composite material slurry, coating the slurry on a polytetrafluoroethylene film or an electrode substrate by using a coater, standing for 30min, volatilizing redundant solvent, and then carrying out vacuum drying at the temperature of 75 ℃ for 8h to finally obtain the microphone/polyvinyl chloride composite material.
Example 7:
the microphone/polyvinyl chloride composite material comprises the following steps:
in a glass container, 0.33g of polyionic liquid (lithium tetrafluoroborate) and 0.17g of plasticizer (propylene carbonate) were weighed out, dissolved in 10ml of tetrahydrofuran, and stirred for 6 hours to obtain a polyionic liquid mixture. 0.5g of aluminum titanium carbide was slowly added to an aqueous solution containing 50% by mass of HF, and after rapid stirring for 12 hours, the mixture was subjected to centrifugal separation, washing, filtration, vacuum drying, and grinding to obtain a powdery precursor of a microphone material.
Adding the precursor of the powdery microphone material into 10ml of dimethyl sulfoxide for ultrasonic stripping for 30min, then adding the polyion liquid mixture into the microphone material subjected to ultrasonic stripping, mixing and stirring for more than 24 hours to obtain a mixed solution A. And adding 9.0g of polyvinyl chloride into the solution A, stirring for more than 1h to fully dissolve the polyvinyl chloride to obtain a mike-alkene/polyvinyl chloride composite material slurry, then coating the slurry on a polytetrafluoroethylene film or an electrode substrate by using a coating device, standing for 30min, volatilizing redundant solvent, and then carrying out vacuum drying for 8h at the temperature of 75 ℃ to finally obtain the mike-alkene/polyvinyl chloride composite material.
Comparative example 1:
the polyvinyl chloride/polyion liquid composite material comprises the following steps:
in a glass container, 2.66g of polyionic liquid (lithium tetrafluoroborate) and 1.34g of plasticizer (diethylene glycol dibenzoate) were weighed out, dissolved in 10ml of tetrahydrofuran and stirred for 6 hours to obtain a polyionic liquid mixture.
And then adding 5.0g of polyvinyl chloride into the polyion liquid mixture, stirring for more than 1h to fully dissolve the polyvinyl chloride, then coating the slurry on a polytetrafluoroethylene film or an electrode substrate by using a coater, standing for 30min, volatilizing redundant solvent, and then drying in vacuum for 8h at the temperature of 75 ℃ to finally obtain the polyvinyl chloride composite material.
Comparative example 2:
the microphone/polyvinyl chloride composite material comprises the following steps:
1.0g of aluminum titanium carbide was slowly added to an aqueous solution containing 50% by mass of HF, and after rapid stirring for 12 hours, the mixture was subjected to centrifugal separation, washing, filtration, drying, and grinding to obtain a powdery precursor of a microphone material.
Adding the precursor of the powdery mike alkene material into 10ml of dimethyl sulfoxide for ultrasonic stripping for 30min, then adding 10ml of tetrahydrofuran into the mike alkene material after ultrasonic stripping, mixing and stirring for more than 24 hours, and obtaining a mixed solution A.
And adding 5g of polyvinyl chloride into the solution A, stirring for more than 1h to fully dissolve the polyvinyl chloride to obtain a microphone/polyvinyl chloride composite material slurry, then coating the slurry on a polytetrafluoroethylene film or an electrode substrate by using a coater, standing for 30min, volatilizing redundant solvent, and then carrying out vacuum drying for 8h at the temperature of 75 ℃ to finally obtain the microphone/polyvinyl chloride composite material.
Comparative example 3:
the polyvinyl chloride material comprises the following steps:
and adding 5g of polyvinyl chloride into 10ml of tetrahydrofuran solution, stirring for more than 1h to fully dissolve the polyvinyl chloride to obtain polyvinyl chloride material slurry, then coating the slurry on a polytetrafluoroethylene film or an electrode substrate by using a coater, standing for 30min, volatilizing redundant solvent, and then carrying out vacuum drying for 8h at the temperature of 75 ℃ to finally obtain the polyvinyl chloride material.
Performance detection
The low-temperature embrittlement temperature and the tensile strength of the materials obtained in examples 1 to 5 and comparative examples 1 to 3 were measured, and the results are shown in table 1.
TABLE 1 Performance test results
| Source | Low temperature embrittlement temperature/. Degree.C | Tensile strength/MPa |
| Example 1 | -64 | 17.4 |
| Example 2 | -64.1 | 17.5 |
| Example 3 | -68 | 18.9 |
| Example 4 | -65 | 18.0 |
| Example 5 | -68 | 19.4 |
| Example 6 | -65 | 17.2 |
| Example 7 | -69 | 19.3 |
| Comparative example 1 | -43 | 15.3 |
| Comparative example 2 | -35 | 14.6 |
| Comparative example 3 | -16 | 14.3 |
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (5)
1. The composite material comprises polyvinyl chloride and is characterized by also comprising a michael and polyionic liquid mixture, wherein the polyionic liquid mixture comprises polyionic liquid and a plasticizer, the ratio of the polyvinyl chloride to the michael to the polyionic liquid mixture is 50-98.5 percent to 0.5-10 percent to 1-40 percent, and the mass ratio of the polyionic liquid to the plasticizer is 1-5:2-10.
2. The composite material of claim 1, wherein the polyionic liquid comprises an imidazolium polyionic liquid, a quaternary ammonium polyionic liquid, a pyrrole polyionic liquid, a halogen polyionic liquid, or a tetrafluoroborate polyionic liquid.
3. The composite material of claim 1, wherein the plasticizer comprises a glycol fatty acid ester, a dipentaerythritol ester, a glycol benzoate, an ethylene carbonate, or a propylene carbonate.
4. A method for preparing a composite material according to any one of claims 1 to 3, characterized in that it comprises the following steps:
preparing a michael material: adding titanium aluminum carbide into hydrofluoric acid, stirring, centrifuging, washing, filtering, drying and grinding the obtained precipitate to obtain a powdery pre-polymer of a michael material;
preparation of polyion liquid mixture: mixing the polyion liquid and the plasticizer, adding the mixture into tetrahydrofuran, and uniformly stirring to obtain a polyion liquid mixture;
ultrasonically separating a precursor of a powdery michael material, dissolving the precursor into a polyion liquid mixture, mixing the solution with polyvinyl chloride, then mixing with polyvinyl chloride, stirring to fully dissolve the polyvinyl chloride, then uniformly adding the polyvinyl chloride into a polytetrafluoroethylene mold, and performing vacuum drying to obtain the composite material.
5. The method of claim 4, comprising the steps of:
adding a precursor of a powdery michael material into dimethyl sulfoxide for ultrasonic stripping, dissolving in a polyion liquid mixture, and stirring; and mixing the solution with polyvinyl chloride, stirring to fully dissolve the polyvinyl chloride, uniformly adding the polyvinyl chloride into a polytetrafluoroethylene mold, and performing vacuum drying to obtain the polytetrafluoroethylene composite material.
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Denomination of invention: Polyvinyl chloride composite materials and their preparation methods Granted publication date: 20230314 Pledgee: Agricultural Bank of China Limited Jieyang City Branch Pledgor: JIEYANG SHENGLUBAO FOOTWARE Ltd. Registration number: Y2024980009080 |