CN117089152A - High-toughness PVC material and preparation method thereof - Google Patents
High-toughness PVC material and preparation method thereof Download PDFInfo
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- CN117089152A CN117089152A CN202311137066.0A CN202311137066A CN117089152A CN 117089152 A CN117089152 A CN 117089152A CN 202311137066 A CN202311137066 A CN 202311137066A CN 117089152 A CN117089152 A CN 117089152A
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- 239000000463 material Substances 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000004800 polyvinyl chloride Substances 0.000 claims abstract description 66
- 229920000915 polyvinyl chloride Polymers 0.000 claims abstract description 65
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 32
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 32
- 239000002071 nanotube Substances 0.000 claims abstract description 22
- 239000012760 heat stabilizer Substances 0.000 claims abstract description 20
- 239000004014 plasticizer Substances 0.000 claims abstract description 19
- 238000001125 extrusion Methods 0.000 claims abstract description 18
- 239000000945 filler Substances 0.000 claims abstract description 17
- 239000000314 lubricant Substances 0.000 claims abstract description 17
- 239000004709 Chlorinated polyethylene Substances 0.000 claims abstract description 11
- TXFOLHZMICYNRM-UHFFFAOYSA-N dichlorophosphoryloxybenzene Chemical compound ClP(Cl)(=O)OC1=CC=CC=C1 TXFOLHZMICYNRM-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 96
- 239000000243 solution Substances 0.000 claims description 62
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 54
- 238000003756 stirring Methods 0.000 claims description 48
- 238000006243 chemical reaction Methods 0.000 claims description 40
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 32
- 238000001035 drying Methods 0.000 claims description 32
- 238000005406 washing Methods 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 238000001914 filtration Methods 0.000 claims description 24
- PXIPVTKHYLBLMZ-UHFFFAOYSA-N Sodium azide Chemical compound [Na+].[N-]=[N+]=[N-] PXIPVTKHYLBLMZ-UHFFFAOYSA-N 0.000 claims description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- PGNZIEKVQCKOBT-UHFFFAOYSA-N tetraazidomethane Chemical compound [N-]=[N+]=NC(N=[N+]=[N-])(N=[N+]=[N-])N=[N+]=[N-] PGNZIEKVQCKOBT-UHFFFAOYSA-N 0.000 claims description 20
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 16
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 14
- 239000004593 Epoxy Substances 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 10
- RIFGWPKJUGCATF-UHFFFAOYSA-N ethyl chloroformate Chemical compound CCOC(Cl)=O RIFGWPKJUGCATF-UHFFFAOYSA-N 0.000 claims description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 8
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 8
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 8
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 8
- 239000008116 calcium stearate Substances 0.000 claims description 8
- 235000013539 calcium stearate Nutrition 0.000 claims description 8
- 235000011089 carbon dioxide Nutrition 0.000 claims description 8
- 238000004090 dissolution Methods 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 229910000077 silane Inorganic materials 0.000 claims description 8
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 8
- 239000010456 wollastonite Substances 0.000 claims description 8
- 229910052882 wollastonite Inorganic materials 0.000 claims description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 7
- IICCLYANAQEHCI-UHFFFAOYSA-N 4,5,6,7-tetrachloro-3',6'-dihydroxy-2',4',5',7'-tetraiodospiro[2-benzofuran-3,9'-xanthene]-1-one Chemical compound O1C(=O)C(C(=C(Cl)C(Cl)=C2Cl)Cl)=C2C21C1=CC(I)=C(O)C(I)=C1OC1=C(I)C(O)=C(I)C=C21 IICCLYANAQEHCI-UHFFFAOYSA-N 0.000 claims description 6
- 229920002367 Polyisobutene Polymers 0.000 claims description 6
- 150000004996 alkyl benzenes Chemical class 0.000 claims description 6
- IRERQBUNZFJFGC-UHFFFAOYSA-L azure blue Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[S-]S[S-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] IRERQBUNZFJFGC-UHFFFAOYSA-L 0.000 claims description 6
- 229940049964 oleate Drugs 0.000 claims description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 6
- 229920000728 polyester Polymers 0.000 claims description 6
- 229930187593 rose bengal Natural products 0.000 claims description 6
- 229940081623 rose bengal Drugs 0.000 claims description 6
- STRXNPAVPKGJQR-UHFFFAOYSA-N rose bengal A Natural products O1C(=O)C(C(=CC=C2Cl)Cl)=C2C21C1=CC(I)=C(O)C(I)=C1OC1=C(I)C(O)=C(I)C=C21 STRXNPAVPKGJQR-UHFFFAOYSA-N 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 4
- 239000010702 perfluoropolyether Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 150000005846 sugar alcohols Polymers 0.000 claims description 4
- 235000013799 ultramarine blue Nutrition 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- QZCLKYGREBVARF-UHFFFAOYSA-N Acetyl tributyl citrate Chemical compound CCCCOC(=O)CC(C(=O)OCCCC)(OC(C)=O)CC(=O)OCCCC QZCLKYGREBVARF-UHFFFAOYSA-N 0.000 claims description 2
- 235000010469 Glycine max Nutrition 0.000 claims description 2
- 244000068988 Glycine max Species 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- APVVRLGIFCYZHJ-UHFFFAOYSA-N trioctyl 2-hydroxypropane-1,2,3-tricarboxylate Chemical compound CCCCCCCCOC(=O)CC(O)(C(=O)OCCCCCCCC)CC(=O)OCCCCCCCC APVVRLGIFCYZHJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229920000642 polymer Polymers 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 239000002861 polymer material Substances 0.000 abstract description 2
- 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 4
- 239000003063 flame retardant Substances 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229920001218 Pullulan Polymers 0.000 description 2
- 239000004373 Pullulan Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 235000019423 pullulan Nutrition 0.000 description 2
- FSDYDBAXNANUQE-UHFFFAOYSA-N tris(2,4-dichlorophenyl) phosphate Chemical compound ClC1=CC(Cl)=CC=C1OP(=O)(OC=1C(=CC(Cl)=CC=1)Cl)OC1=CC=C(Cl)C=C1Cl FSDYDBAXNANUQE-UHFFFAOYSA-N 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229920006280 packaging film Polymers 0.000 description 1
- 239000012785 packaging film Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
- C08L27/04—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 containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to the technical field of high polymer materials, and discloses a high-toughness PVC material and a preparation method thereof, wherein the PVC material is prepared from the following components in parts by weight: 120 parts of polyvinyl chloride, 10-15 parts of modified carbon nano tubes, 1-2 parts of toner, 3-5 parts of lubricant, 2-3 parts of plasticizer, 8-12 parts of filler and 2-4 parts of heat stabilizer, and the preparation method comprises the steps of mixing the components and then putting the components into an extruder for extrusion to obtain the high-toughness PVC material, wherein the invention has the advantages that: after the carbon nano tube is treated by strong acid, negative charges on the nano tube are carried to wrap the wall of the carbon nano tube to reduce agglomeration, so that the dispersibility is improved, a shell layer is formed by grafting phenyl dichlorophosphate and chlorinated polyethylene on the carbon nano tube, the flame retardance and high temperature resistance of the PVC material are improved, the shell layer and the PVC material have better compatibility, and the formed three-molecule polymer can effectively improve the toughness and transparency of the PVC material and has excellent temperature resistance, weather resistance, flame retardance and impact resistance.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a high-toughness PVC material and a preparation method thereof.
Background
Polyvinyl chloride is a polymer obtained by polymerizing vinyl chloride monomers under the action of an initiator such as peroxides and azo compounds or by a free radical polymerization mechanism under the action of light and heat, and vinyl chloride homopolymers and vinyl chloride copolymers are collectively called vinyl chloride resins. The composite material is widely applied to the aspects of building materials, industrial products, daily necessities, floor leathers, floor tiles, artificial leathers, pipes, wires and cables, packaging films, bottles, foaming materials, sealing materials, fibers and the like. The processing heat stability of the PVC material is poor, the PVC resin can be decomposed more quickly at the temperature of more than 150 ℃, the heat stabilizer can be added in the prior art, the PVC resin can be processed normally after the heat stabilizer is added, the adding amount of the heat stabilizer is more, on the one hand, the transparency of the final PVC material can be influenced, as disclosed in patent No. CN 104130528B, the preparation of the transparent environment-friendly PVC modified material is good in transparency, and the obtained PVC material cannot meet the requirement of toughness. Polyvinyl chloride (PVC) cable material is a multicomponent mixed material formed by taking PVC resin as a base and adding various complexing agents, and is widely applied to insulation and protection layer materials of cables due to the advantages of excellent mechanical property, good weather resistance, good electrical insulation performance and the like.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a high-toughness PVC material and a preparation method thereof, and the PVC material has the advantages of excellent temperature resistance, weather resistance, good flame retardant effect and excellent shock resistance.
(II) technical scheme
In order to achieve the above purpose, the present invention provides the following technical solutions: the high-toughness PVC material comprises, by weight, 120 parts of polyvinyl chloride, 10-15 parts of modified carbon nanotubes, 1-2 parts of toner, 3-5 parts of lubricant, 2-3 parts of plasticizer, 8-12 parts of filler and 2-4 parts of heat stabilizer.
Further, the heat stabilizer is a compound of colorful citric acid and calcium stearate; the filler is wollastonite treated by silane; the plasticizer is epoxy, polyester and polyalcohol; the lubricant is any one or more of polyethylene glycol ether, alkylbenzene, polyisobutene and perfluoropolyether; the toner is one or more of rose bengal, ultramarine blue, pram and ash.
Further, the preparation method of the modified carbon nano tube comprises the following steps:
(1) Adding the carbon nano tube into a mixed solution of sulfuric acid and nitric acid, performing ultrasonic dispersion for 0.5-1h at 20-25 ℃, heating to 100-120 ℃, condensing and refluxing for 2-4h, washing and drying to obtain carboxylated carbon nano tube;
(2) Dissolving carboxylated carbon nanotubes, triethylamine and acetone in deionized water at 0-3 ℃, adding ethyl chloroformate into the deionized water, stirring and reacting for 2-3 hours, dissolving sodium azide in the deionized water, dripping the deionized water into a reaction system, stirring and reacting for 1-2 hours, extracting, washing and drying to obtain carbon azide nanotubes, dissolving the carbon azide nanotubes in tertiary butanol, adding concentrated hydrochloric acid into the carbon azide, and reacting for 1-2 hours at the temperature of 30-40 ℃ to obtain the carbon azide nanotubes;
(3) Adding 1-2g of aminated carbon nano tube and 3.1-4.2g of methylene dichloride into a reactor, cooling dry ice and acetone to-70-60 ℃, continuously adding 0.63-0.74g of phenyl dichlorophosphate and 0.65-0.71g of triethylamine into the reactor, stirring for 1-2h, reacting at 20-25 ℃, evaporating, washing, filtering after the reaction is finished to obtain solid A, adding 1.2-1.4g of chlorinated polyethylene, 0.02-0.06g of tetrahydrofuran and 1.6-2.2g of solid A into the reactor, reacting at 20-25 ℃ for 20-24h, filtering and drying to obtain the modified carbon nano tube.
Further, the mass ratio of the carboxylated carbon nano tube to the triethylamine to the ethyl chloroformate to the sodium azide is 1:0.5-0.6:0.5-0.8:0.4-0.45.
Further, the volume ratio of sulfuric acid to nitric acid in the step (1) is 1:3-4.
Further, the preparation method of the citric acid billows comprises the following steps: adding citric acid into water for dissolution, adding sodium hydroxide for reaction for 15-20min at 60-80deg.C, adding gorgeous chloride into the saponified solution after the saponified solution is transparent, stirring for 30-40min, filtering, washing, and drying to obtain citric acid.
Further, the pH of the sodium hydroxide is adjusted to 9-10.
Further, the plasticizer epoxy is one or more of epoxy furfuryl oleate, epoxy soybean oleate and epoxy tall oleate; the polyesters are trioctyl citrate or acetyl tributyl citrate.
Further, the method comprises the following steps:
(1) Calculating the required amount of each component according to the weight portion ratio, and taking the raw materials of each component;
(2) Adding the components into a high-speed blender, starting the blender at a low speed, mixing at a high speed, stirring for 20-30min, reacting at 100-120 ℃ and stirring at 1000-1200r/min;
(3) And cooling and curing the uniformly mixed materials, putting the materials into an extruder for extrusion, and extruding and granulating by the extruder to obtain the high-toughness PVC material.
Further, the rotating speed of the screw is 30-40r/min, the temperature from the charging port to the first area of the extrusion die is 150-160 ℃, the temperature of the second area is 160-165 ℃, the temperature of the third area is 165-168 ℃, and the temperature of the fourth area is 170-175 ℃, so that the high-toughness PVC material is prepared.
(III) beneficial technical effects
According to the invention, the components are mixed and then put into an extruder for extrusion to obtain the high-toughness PVC material, after the carbon nano tube is treated by strong acid, negative charges on the nano tube are carried on the nano tube to wrap the wall of the carbon nano tube, agglomeration is reduced, dispersibility is improved, a shell layer is formed outside the nano tube by grafting the dichlorophenyl phosphate and the chlorinated polyethylene on the carbon nano tube, meanwhile, the dichlorophenyl phosphate has a good flame retardant effect, the flame retardance of the PVC material is improved, and as the shell layer is the chlorinated polyethylene and the PVC material have better compatibility, the three-molecule polymer is formed, so that the toughness and transparency of the PVC material are improved, and meanwhile, the PVC material has excellent heat resistance, weather resistance, flame retardance and impact resistance.
Drawings
Fig. 1 is a schematic diagram of the preparation of modified carbon nanotubes.
FIG. 2 is a scanning electron microscope image of a high-toughness PVC material.
Detailed Description
Example 1
The high-toughness PVC material of the embodiment comprises the following components in parts by weight
120 parts of polyvinyl chloride, 10 parts of modified carbon nano tubes, 1 part of toner, 3 parts of lubricant, 2 parts of plasticizer, 8 parts of filler and 2 parts of heat stabilizer.
The heat stabilizer is a combination of colorful citric acid and calcium stearate, the filler is wollastonite treated by silane, the plasticizer is epoxy, the lubricant is polyethylene glycol ether and alkylbenzene, and the toner is rose bengal or ultramarine.
The preparation method of the modified carbon nano tube comprises the following steps:
(1) Adding the carbon nano tube into a mixed solution of sulfuric acid and nitric acid in a volume ratio of 1:3, performing ultrasonic dispersion for 0.5h at 20 ℃, heating to 100 ℃, condensing and refluxing for 2h, washing and drying to obtain carboxylated carbon nano tube;
(2) Dissolving 10g of carboxylated carbon nano tube, 5g of triethylamine and acetone in deionized water at the temperature of 0 ℃, adding 5g of ethyl chloroformate into the solution, stirring the solution for reaction for 2 hours, dissolving 4g of sodium azide in the deionized water, dripping the solution into a reaction system, stirring the solution for reaction for 1 hour, extracting, washing and drying the solution to obtain carbon azide nano tube, dissolving the carbon azide nano tube in tertiary butanol, adding concentrated hydrochloric acid into the solution, and reacting the solution for 1 hour at the temperature of 30 ℃ to obtain the aminated carbon nano tube;
(3) Adding 1g of aminated carbon nano tube and 3.1g of methylene dichloride into a reactor, cooling dry ice and acetone to-70 ℃, continuously adding 0.63g of phenyl dichlorophosphate and 0.65g of triethylamine into the reactor, stirring for 1h, reacting at 20 ℃, evaporating, washing and filtering after the reaction is finished to obtain solid A, adding 1.2g of chlorinated polyethylene, 0.02g of tetrahydrofuran and 1.6g of solid A into the reactor, reacting at 20 ℃ for 20h, filtering and drying to obtain the modified carbon nano tube.
The preparation method of the citric acid billows comprises the following steps:
adding citric acid into water for dissolution, adding sodium hydroxide into the solution for reaction to adjust the pH to 9, reacting for 15min at the temperature of 60 ℃, adding gorgeous chloride into the saponified solution after the saponified solution is transparent, stirring for 30min, filtering, washing and drying to obtain the citric acid billows.
The preparation method of the high-toughness PVC material comprises the following steps:
(1) Calculating the required amount of each component according to the weight portion ratio, and taking the raw materials of each component;
(2) Adding the components into a high-speed blender, starting the blender at a low speed, mixing at a high speed, stirring for 20min, and stirring at a reaction temperature of 100 ℃ for 1000r/min;
(3) And (3) cooling and curing the uniformly mixed materials, putting the materials into an extruder for extrusion, wherein the rotating speed of a screw is 30r/min, extruding and granulating by the extruder from a charging port to an extrusion die at the temperature of 150 ℃ in the first region, 160 ℃ in the second region, 165 ℃ in the third region and 170 ℃ in the fourth region.
Example 2
The high-toughness PVC material of the embodiment comprises the following components in parts by weight
120 parts of polyvinyl chloride, 15 parts of modified carbon nano tubes, 2 parts of toner, 5 parts of lubricant, 3 parts of plasticizer, 12 parts of filler and 4 parts of heat stabilizer.
The heat stabilizer is a combination of colorful citric acid and calcium stearate, the filler is wollastonite treated by silane, the plasticizer is polyester, the lubricant is polyisobutene and perfluoropolyether, and the toner is pullulan and ash.
The preparation method of the modified carbon nano tube comprises the following steps:
(1) Adding the carbon nano tube into a mixed solution with the volume ratio of sulfuric acid to nitric acid of 1:4, performing ultrasonic dispersion for 1h at 25 ℃, heating to 120 ℃, condensing and refluxing for 4h, washing and drying to obtain carboxylated carbon nano tube;
(2) Dissolving 10g of carboxylated carbon nano tube, 6g of triethylamine and acetone in deionized water at the temperature of 3 ℃, adding 8g of ethyl chloroformate into the solution, stirring the solution for reaction for 3 hours, dissolving 4.5g of sodium azide in the deionized water, dripping the solution into a reaction system, stirring the solution for reaction for 2 hours, extracting, washing and drying the solution to obtain carbon azide nano tube, dissolving the carbon azide nano tube in tertiary butanol, adding concentrated hydrochloric acid into the solution, and reacting the solution at the temperature of 40 ℃ for 2 hours to obtain the aminated carbon nano tube;
(3) Adding 2g of aminated carbon nano tube and 4.2g of methylene dichloride into a reactor, cooling dry ice and acetone to-60 ℃, continuously adding 0.74g of phenyl dichlorophosphate and 0.71g of triethylamine into the reactor, stirring for 2 hours, reacting at 25 ℃, evaporating, washing and filtering after the reaction is finished to obtain solid A, adding 1.4g of chlorinated polyethylene, 0.06g of tetrahydrofuran and 2.2g of solid A into the reactor, reacting at 25 ℃ for 24 hours, filtering and drying to obtain the modified carbon nano tube.
The preparation method of the citric acid billows comprises the following steps:
adding citric acid into water for dissolution, adding sodium hydroxide into the water for reaction to adjust the pH to 10, reacting for 20min at the temperature of 80 ℃, adding gorgeous chloride into the saponified solution after the saponified solution is transparent, stirring for 40min, filtering, washing and drying to obtain the citric acid billows.
The preparation method of the high-toughness PVC material comprises the following steps:
(1) Calculating the required amount of each component according to the weight portion ratio, and taking the raw materials of each component;
(2) Adding the components into a high-speed blender, starting the blender at a low speed, mixing at a high speed, stirring for 30min, and stirring at a reaction temperature of 120 ℃ at a rotation speed of 1200r/min;
(3) And (3) cooling and curing the uniformly mixed materials, putting the materials into an extruder for extrusion, wherein the rotating speed of a screw is 40r/min, extruding and granulating by the extruder from a feed inlet to an extrusion die at the temperature of 160 ℃ in the first region, 165 ℃ in the second region, 165 ℃ in the third region and 165-168 ℃ in the fourth region, and obtaining the high-toughness PVC material.
Example 3
The high-toughness PVC material of the embodiment comprises the following components in parts by weight
120 parts of polyvinyl chloride, 12.5 parts of modified carbon nano tubes, 1.5 parts of toner, 4 parts of lubricant, 2.5 parts of plasticizer, 10 parts of filler and 3 parts of heat stabilizer.
The heat stabilizer is a combination of gorgeous citric acid and calcium stearate, the filler is wollastonite treated by silane, the plasticizer is polyalcohol, the lubricant is alkylbenzene and polyisobutene, and the toner is rose bengal, ultramarine blue and gray.
The preparation method of the modified carbon nano tube comprises the following steps:
(1) Adding the carbon nano tube into a mixed solution of sulfuric acid and nitric acid with the volume ratio of 1:3.5, performing ultrasonic dispersion for 0.75h at 22.5 ℃, heating to 110 ℃, condensing and refluxing for 3h, washing and drying to obtain carboxylated carbon nano tube;
(2) Dissolving 10g of carboxylated carbon nano tube, 5.5g of triethylamine and acetone in deionized water at the temperature of 1.5 ℃, adding 7.5g of ethyl chloroformate into the solution, stirring the solution to react for 2.5h, dissolving 4.25g of sodium azide in the deionized water, then dropwise adding the solution into a reaction system, stirring the solution to react for 1.5h, extracting, washing and drying the solution to obtain carbon azide nano tube, dissolving the carbon azide nano tube in tertiary butanol, adding concentrated hydrochloric acid into the solution, and reacting the solution for 1.5h at the temperature of 35 ℃ to obtain the aminated carbon nano tube;
(3) Adding 1.5g of aminated carbon nano-tube and 3.65g of methylene dichloride into a reactor, cooling dry ice and acetone to the temperature of minus 65 ℃, continuously adding 0.68g of phenyl dichlorophosphate and 0.68g of triethylamine into the reactor, stirring for 1.5h, reacting at the temperature of 22.5 ℃, evaporating, washing and filtering after the reaction is finished to obtain solid A, adding 1.3g of chlorinated polyethylene, 0.04g of tetrahydrofuran and 1.9g of solid A into the reactor, reacting at the temperature of 22.5 ℃ for 22h, filtering and drying to obtain the modified carbon nano-tube.
The preparation method of the citric acid billows comprises the following steps:
adding citric acid into water for dissolution, adding sodium hydroxide into the water for reaction to adjust the pH to 9.5, reacting for 17.5min at 70 ℃, adding gorgeous chloride into the saponified solution after the saponified solution is transparent, stirring for 35min, filtering, washing and drying to obtain the citric acid billows.
The preparation method of the high-toughness PVC material comprises the following steps:
(1) Calculating the required amount of each component according to the weight portion ratio, and taking the raw materials of each component;
(2) Adding the components into a high-speed blender, starting the blender at a low speed, mixing at a high speed, stirring for 25min, and stirring at a reaction temperature of 110 ℃ at a rotation speed of 1100r/min;
(3) And (3) cooling and curing the uniformly mixed materials, putting the materials into an extruder for extrusion, wherein the rotating speed of a screw is 35r/min, and extruding and granulating the materials from a feed inlet to an extrusion die at the temperature of 155 ℃ in a first region, 162.5 ℃ in a second region, 166.5 ℃ in a third region and 172.5 ℃ in a fourth region by using the extruder to prepare the high-toughness PVC material.
Example 4
The high-toughness PVC material of the embodiment comprises the following components in parts by weight
120 parts of polyvinyl chloride, 12.5 parts of modified carbon nano tubes, 1.5 parts of toner, 4 parts of lubricant, 2.5 parts of plasticizer, 10 parts of filler and 3 parts of heat stabilizer.
The heat stabilizer is a combination of gorgeous citric acid and calcium stearate, the filler is wollastonite treated by silane, the plasticizer is polyalcohol, the lubricant is alkylbenzene and polyisobutene, and the toner is rose bengal, ultramarine blue and gray.
The preparation method of the modified carbon nano tube comprises the following steps:
(1) Adding the carbon nano tube into a mixed solution with the volume ratio of sulfuric acid to nitric acid of 1:3, performing ultrasonic dispersion for 1h at 25 ℃, heating to 120 ℃, condensing and refluxing for 4h, washing and drying to obtain carboxylated carbon nano tube;
(2) Dissolving 10g of carboxylated carbon nano tube, 6g of triethylamine and acetone in deionized water at the temperature of 3 ℃, adding 8g of ethyl chloroformate into the solution, stirring the solution for reaction for 3 hours, dissolving 4.5g of sodium azide in the deionized water, dripping the solution into a reaction system, stirring the solution for reaction for 2 hours, extracting, washing and drying the solution to obtain carbon azide nano tube, dissolving the carbon azide nano tube in tertiary butanol, adding concentrated hydrochloric acid into the solution, and reacting the solution at the temperature of 40 ℃ for 2 hours to obtain the aminated carbon nano tube;
(3) Adding 1.5g of aminated carbon nano-tube and 3.65g of methylene dichloride into a reactor, cooling dry ice and acetone to the temperature of minus 65 ℃, continuously adding 0.68g of phenyl dichlorophosphate and 0.68g of triethylamine into the reactor, stirring for 1.5h, reacting at the temperature of 22.5 ℃, evaporating, washing and filtering after the reaction is finished to obtain solid A, adding 1.3g of chlorinated polyethylene, 0.04g of tetrahydrofuran and 1.9g of solid A into the reactor, reacting at the temperature of 22.5 ℃ for 22h, filtering and drying to obtain the modified carbon nano-tube.
The preparation method of the citric acid billows comprises the following steps:
adding citric acid into water for dissolution, adding sodium hydroxide into the solution for reaction to adjust the pH to 9, reacting for 15min at the temperature of 60 ℃, adding gorgeous chloride into the saponified solution after the saponified solution is transparent, stirring for 30min, filtering, washing and drying to obtain the citric acid billows.
The preparation method of the high-toughness PVC material comprises the following steps:
(1) Calculating the required amount of each component according to the weight portion ratio, and taking the raw materials of each component;
(2) Adding the components into a high-speed blender, starting the blender at a low speed, mixing at a high speed, stirring for 20min, and stirring at a reaction temperature of 100 ℃ for 1000r/min;
(3) And (3) cooling and curing the uniformly mixed materials, putting the materials into an extruder for extrusion, wherein the rotating speed of a screw is 30r/min, extruding and granulating by the extruder from a charging port to an extrusion die at the temperature of 150 ℃ in the first region, 160 ℃ in the second region, 165 ℃ in the third region and 170 ℃ in the fourth region.
Example 5
The high-toughness PVC material of the embodiment comprises the following components in parts by weight
120 parts of polyvinyl chloride, 15 parts of modified carbon nano tubes, 2 parts of toner, 5 parts of lubricant, 3 parts of plasticizer, 12 parts of filler and 4 parts of heat stabilizer.
The heat stabilizer is a combination of colorful citric acid and calcium stearate, the filler is wollastonite treated by silane, the plasticizer is polyester, the lubricant is polyisobutene and perfluoropolyether, and the toner is pullulan and ash.
The preparation method of the modified carbon nano tube comprises the following steps:
(1) Adding the carbon nano tube into a mixed solution of sulfuric acid and nitric acid with the volume ratio of 1:3.5, performing ultrasonic dispersion for 0.5h at 20 ℃, heating to 100 ℃, condensing and refluxing for 2h, washing and drying to obtain carboxylated carbon nano tube;
(2) Dissolving 10g of carboxylated carbon nano tube, 5g of triethylamine and acetone in deionized water at the temperature of 0 ℃, adding 5g of ethyl chloroformate into the solution, stirring the solution for reaction for 2 hours, dissolving 4g of sodium azide in the deionized water, dripping the solution into a reaction system, stirring the solution for reaction for 1 hour, extracting, washing and drying the solution to obtain carbon azide nano tube, dissolving the carbon azide nano tube in tertiary butanol, adding concentrated hydrochloric acid into the solution, and reacting the solution for 1 hour at the temperature of 30 ℃ to obtain the aminated carbon nano tube;
(3) Adding 1g of aminated carbon nano tube and 3.1g of methylene dichloride into a reactor, cooling dry ice and acetone to-70 ℃, continuously adding 0.63g of phenyl dichlorophosphate and 0.65g of triethylamine into the reactor, stirring for 1h, reacting at 20 ℃, evaporating, washing and filtering after the reaction is finished to obtain solid A, adding 1.2g of chlorinated polyethylene, 0.02g of tetrahydrofuran and 1.6g of solid A into the reactor, reacting at 20 ℃ for 20h, filtering and drying to obtain the modified carbon nano tube.
The preparation method of the citric acid billows comprises the following steps:
adding citric acid into water for dissolution, adding sodium hydroxide into the solution for reaction to adjust the pH to 9, reacting for 15min at the temperature of 60 ℃, adding gorgeous chloride into the saponified solution after the saponified solution is transparent, stirring for 30min, filtering, washing and drying to obtain the citric acid billows.
The preparation method of the high-toughness PVC material comprises the following steps:
(1) Calculating the required amount of each component according to the weight portion ratio, and taking the raw materials of each component;
(2) Adding the components into a high-speed blender, starting the blender at a low speed, mixing at a high speed, stirring for 25min, and stirring at a reaction temperature of 110 ℃ at a rotation speed of 1100r/min;
(3) And (3) cooling and curing the uniformly mixed materials, putting the materials into an extruder for extrusion, wherein the rotating speed of a screw is 35r/min, and extruding and granulating the materials from a feed inlet to an extrusion die at the temperature of 155 ℃ in a first region, 162.5 ℃ in a second region, 166.5 ℃ in a third region and 172.5 ℃ in a fourth region by using the extruder to prepare the high-toughness PVC material.
Comparative example 1
The high-toughness PVC material of the embodiment comprises the following components in parts by weight
120 parts of polyvinyl chloride, 10 parts of modified carbon nano tubes, 1 part of toner, 3 parts of lubricant, 2 parts of plasticizer, 8 parts of filler and 2 parts of heat stabilizer.
The heat stabilizer is a combination of colorful citric acid and calcium stearate, the filler is wollastonite treated by silane, the plasticizer is epoxy, the lubricant is polyethylene glycol ether and alkylbenzene, and the toner is rose bengal or ultramarine.
The preparation method of the modified carbon nano tube comprises the following steps:
(1) Adding the carbon nano tube into a mixed solution with the volume ratio of sulfuric acid to nitric acid of 1:3, performing ultrasonic dispersion for 0.5h at 20 ℃, heating to 100 ℃, condensing and refluxing for 2h, washing and drying to obtain carboxylated carbon nano tube;
(2) Dissolving 10g of carboxylated carbon nano tube, 6g of triethylamine and acetone in deionized water at the temperature of 3 ℃, adding 8g of ethyl chloroformate into the solution, stirring the solution for reaction for 3 hours, dissolving 4.5g of sodium azide in the deionized water, dripping the solution into a reaction system, stirring the solution for reaction for 2 hours, extracting, washing and drying the solution to obtain carbon azide nano tube, dissolving the carbon azide nano tube in tertiary butanol, adding concentrated hydrochloric acid into the solution, and reacting the solution at the temperature of 40 ℃ for 2 hours to obtain the aminated carbon nano tube;
(3) Adding 1g of aminated carbon nano tube and 3.1g of methylene dichloride into a reactor, cooling dry ice and acetone to-70 ℃, continuously adding 0.63g of phenyl dichlorophosphate and 0.65g of triethylamine into the reactor, stirring for 1h, reacting at 20 ℃, evaporating, washing and filtering after the reaction is finished to obtain solid A, adding 1.2g of chlorinated polyethylene and 1.6g of solid A into the reactor, reacting at 20 ℃ for 20h, filtering and drying to obtain the modified carbon nano tube.
The preparation method of the citric acid billows comprises the following steps:
adding citric acid into water for dissolution, adding sodium hydroxide into the water for reaction to adjust the pH to 10, reacting for 20min at the temperature of 80 ℃, adding gorgeous chloride into the saponified solution after the saponified solution is transparent, stirring for 40min, filtering, washing and drying to obtain the citric acid billows.
The preparation method of the high-toughness PVC material comprises the following steps:
(1) Calculating the required amount of each component according to the weight portion ratio, and taking the raw materials of each component;
(2) Adding the components into a high-speed blender, starting the blender at a low speed, mixing at a high speed, stirring for 25min, and stirring at a reaction temperature of 110 ℃ at a rotation speed of 1100r/min;
(3) And (3) cooling and curing the uniformly mixed materials, putting the materials into an extruder for extrusion, wherein the rotating speed of a screw is 35r/min, and extruding and granulating the materials from a feed inlet to an extrusion die at the temperature of 155 ℃ in a first region, 162.5 ℃ in a second region, 166.5 ℃ in a third region and 172.5 ℃ in a fourth region by using the extruder to prepare the high-toughness PVC material.
The transparency test is carried out by adopting an ICS83 standard, the flame retardant test is carried out by adopting an UL94 standard, the flame retardant grade reaches 4VA grade, the tensile strength is tested according to a GB/T8804.2-2003 standard, the elongation at break is tested according to a GB/T5836-1996 standard, and the impact strength is tested according to an MGB/T1043.1-2008 standard, and the test results are shown in Table 1.
TABLE 1
As shown in Table 1, the high-toughness PVC material prepared by the invention has high toughness, high flame retardance, high transparency and better tensile strength, elongation at break and impact strength, and can be applied to various occasions.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A high-toughness PVC material characterized by: 120 parts of polyvinyl chloride, 10-15 parts of modified carbon nano tubes, 1-2 parts of toner, 3-5 parts of lubricant, 2-3 parts of plasticizer, 8-12 parts of filler and 2-4 parts of heat stabilizer.
2. The high-toughness PVC material according to claim 1, wherein: the heat stabilizer is a compound of colorful citric acid and calcium stearate; the filler is wollastonite treated by silane; the plasticizer is epoxy, polyester and polyalcohol; the lubricant is any one or more of polyethylene glycol ether, alkylbenzene, polyisobutene and perfluoropolyether; the toner is one or more of rose bengal, ultramarine blue, pram and ash.
3. The high-toughness PVC material according to claim 1, wherein: the preparation method of the modified carbon nano tube comprises the following steps:
(1) Adding the carbon nano tube into a mixed solution of sulfuric acid and nitric acid, performing ultrasonic dispersion for 0.5-1h at 20-25 ℃, heating to 100-120 ℃, condensing and refluxing for 2-4h, washing and drying to obtain carboxylated carbon nano tube;
(2) Dissolving carboxylated carbon nanotubes, triethylamine and acetone in deionized water at 0-3 ℃, adding ethyl chloroformate into the deionized water, stirring and reacting for 2-3 hours, dissolving sodium azide in the deionized water, dripping the deionized water into a reaction system, stirring and reacting for 1-2 hours, extracting, washing and drying to obtain carbon azide nanotubes, dissolving the carbon azide nanotubes in tertiary butanol, adding concentrated hydrochloric acid into the carbon azide, and reacting for 1-2 hours at the temperature of 30-40 ℃ to obtain the carbon azide nanotubes;
(3) Adding 1-2g of aminated carbon nano tube and 3.1-4.2g of methylene dichloride into a reactor, cooling dry ice and acetone to-70-60 ℃, continuously adding 0.63-0.74g of phenyl dichlorophosphate and 0.65-0.71g of triethylamine into the reactor, stirring for 1-2h, reacting at 20-25 ℃, evaporating, washing, filtering after the reaction is finished to obtain solid A, adding 1.2-1.4g of chlorinated polyethylene, 0.02-0.06g of tetrahydrofuran and 1.6-2.2g of solid A into the reactor, reacting at 20-25 ℃ for 20-24h, filtering and drying to obtain the modified carbon nano tube.
4. A high toughness PVC material according to claim 3, wherein: the mass ratio of the carboxylated carbon nano tube to the triethylamine to the ethyl chloroformate to the sodium azide is 1:0.5-0.6:0.5-0.8:0.4-0.45.
5. A high toughness PVC material according to claim 3, wherein: the volume ratio of sulfuric acid to nitric acid in the step (1) is 1:3-4.
6. The high-toughness PVC material according to claim 2, wherein: the preparation method of the citric acid billows comprises the following steps: adding citric acid into water for dissolution, adding sodium hydroxide for reaction for 15-20min at 60-80deg.C, adding gorgeous chloride into the saponified solution after the saponified solution is transparent, stirring for 30-40min, filtering, washing, and drying to obtain citric acid.
7. The high-toughness PVC material according to claim 6, wherein: the pH of the sodium hydroxide is adjusted to 9-10.
8. The high-toughness PVC material according to claim 2, wherein: the plasticizer epoxy is one or more of epoxy furfuryl oleate, epoxy soybean oleate and epoxy tall oleate; the polyesters are trioctyl citrate or acetyl tributyl citrate.
9. The method of making a high toughness PVC material according to claims 1-8, wherein: the method comprises the following steps:
(1) Calculating the required amount of each component according to the weight portion ratio, and taking the raw materials of each component;
(2) Adding the components into a high-speed blender, starting the blender at a low speed, mixing at a high speed, stirring for 20-30min, reacting at 100-120 ℃ and stirring at 1000-1200r/min;
(3) And cooling and curing the uniformly mixed materials, putting the materials into an extruder for extrusion, and extruding and granulating by the extruder to obtain the high-toughness PVC material.
10. The method of preparing a high-toughness PVC material according to claim 9, wherein: the rotating speed of the screw is 30-40r/min, the temperature from the feed inlet to the first area of the extrusion die is 150-160 ℃, the temperature of the second area is 160-165 ℃, the temperature of the third area is 165-168 ℃, and the temperature of the fourth area is 170-175 ℃, so that the high-toughness PVC material is prepared.
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| CN109777007A (en) * | 2019-02-22 | 2019-05-21 | 华研(佛山)纳米材料有限公司 | A kind of carbon nanotube polyvinyl chloride composite materials and preparation method thereof |
| CN113524833A (en) * | 2021-07-19 | 2021-10-22 | 四川新明塑业有限公司 | Mining PVC-O pipe and preparation method thereof |
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| CN109777007A (en) * | 2019-02-22 | 2019-05-21 | 华研(佛山)纳米材料有限公司 | A kind of carbon nanotube polyvinyl chloride composite materials and preparation method thereof |
| CN113524833A (en) * | 2021-07-19 | 2021-10-22 | 四川新明塑业有限公司 | Mining PVC-O pipe and preparation method thereof |
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