CN104004294A - Preparation method of graphene-modified hard polyvinyl chloride composite tubing - Google Patents
Preparation method of graphene-modified hard polyvinyl chloride composite tubing Download PDFInfo
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- CN104004294A CN104004294A CN201410190681.2A CN201410190681A CN104004294A CN 104004294 A CN104004294 A CN 104004294A CN 201410190681 A CN201410190681 A CN 201410190681A CN 104004294 A CN104004294 A CN 104004294A
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Abstract
The invention provides a preparation method of a graphene-modified hard polyvinyl chloride composite tubing. The preparation method comprises the following steps of 1, modified graphene powder preparation, 2, modified graphene powder/polypropylene blended master batch preparation, and 3, graphene-modified hard polyvinyl chloride composite tubing preparation. The preparation method fully utilizes the existing equipment used in the hard polyvinyl chloride composite tubing industry, can obviously improve tubing mechanical strength and aging resistance only by use of a small amount of graphene powder, and has a low cost, obvious effects and good practicality.
Description
Technical field
The present invention relates to plastic conduit field, specifically refer to a kind of preparation method of the rigid polyvinyl chloride composite pipe with Graphene modification.
Background technology
Hard polyethylene pipe occupies critical role in numerous plastic pipes.Because it has that intensity is good, acid-alkali-corrosive-resisting, insulativity is good, fluid transportation performance is good, tubing is easy to connect, secondary processing is convenient, sufficient raw and the advantage such as cheap, is widely used in the fields such as building water supply and drainage, Chemical Manufacture, mine ventilation and cable penetration pipe.But hard polyethylene pipe also exists such as the shortcoming under poor heat stability, the low particularly cold condition of resistance to impact shock, therefore how to improve its shock resistance is the focus of paying close attention in the industry always.
The appearance of Graphene has brought hope to cracking of this difficult problem.Graphene is current known the highest (the breaking tenacity 130GPa of mechanical strength in the world, Young's modulus 1.0TPa), the thinnest (thickness 0.3nm), conduction (resistivity 10-6 Ω cm, a little less than the argent of conduction), the performance such as heat conduction (under room temperature, thermal conductivity reaches 5000W/mk, exceedes the diamond that current known thermal conductivity is the highest).These excellent properties of Graphene, make Graphene very likely become the material that improves plastic conduit over-all properties.
Although report or the patent of Graphene polymer composites occur (as application number ZL201110313859.4, ZL201310034290.7, ZL201110337141.9 etc.), but really Graphene also can be had to have not been reported of lifting to correlated performance for pipeline material.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art provides a kind of preparation method of the rigid polyvinyl chloride composite pipe with Graphene modification, and the rigid polyvinyl chloride composite pipe of preparing by present method has good shock resistance and thermostability.
The present invention is achieved through the following technical solutions: a kind of preparation method of the rigid polyvinyl chloride composite pipe with Graphene modification, its step comprises: (1) is by 1 × 10
-3the surface treatment agent of-1 parts by weight, is added in 1-1000 parts by weight solvent, adds the graphene powder of 1-100 parts by weight after the two is stirred, and ultrasonic dispersion after mixture high-speed stirring is made to modified graphene dispersion liquid; Also after spheroidal graphite, make modified graphene powder by dry this modified graphene dispersion liquid again; (2) by the modified graphene powder of the 0.1-10 parts by weight described in step (1), join in the polyvinyl chloride (PVC) RESINS of 100 parts by weight, add again the thermo-stabilizer of 1-10 parts by weight, the lubricant of 0.1-5 parts by weight, the auxiliary agent of the filler of 5-50 parts by weight and 1-20 parts by weight, after blending dispersion, extruding pelletization makes modified graphene powder/rigid polyvinyl chloride blend composition again; (3) the modified graphene powder/rigid polyvinyl chloride blend composition described in step (2) is added extrusion moulding in polychloroethylene pipes forcing machine make the rigid polyvinyl chloride composite pipe with Graphene modification.
Described surface treatment agent is one or more in silane coupling agent, titanate coupling agent, octadecylamine, isocyanic acid.
Described solvent is ethanol/water solution or ethanol/acetum.
Described polyvinyl chloride is tubing grade PVC resin, comprises SG-5, SG-6 or SG-7 type resin.
Described thermo-stabilizer is one or more in base lead salt class, metal soap, organic tin, epoxy compounds class, rare earth compound.
Described lubricant is one or more in fatty acid ester, lipid acid, fatty alcohol, fatty amide, metallic soap, paraffin, polyethylene wax, oxidic polyethylene dispersing agent for wax.
Described filler comprises one or more in calcium carbonate, talcum powder, titanium dioxide.
Described auxiliary agent comprises one or more in chlorinatedpolyethylene (CPE), MBS (MBS), ACR, tinting material.
Mixing in described step (2) utilizes Z-shaped kneader, high-speed mixer, mill or Banbury mixer to mix.
Extruding pelletization in described step (2) utilizes parallel double-screw extruder, conical double screw extruder or single screw extrusion machine to carry out.
Rigid polyvinyl chloride composite pipe with Graphene modification of the present invention can be applied to building to/drainage pipe, municipal tubing, industrial pipes, chemical industry tubing, protecting pipe field etc.The present invention makes full use of existing equipment in rigid polyvinyl chloride composite pipe industry, only need on formula, utilize the graphene powder of a small amount of modification aspect shock resistance and thermal stability, obviously promoting tubing, cost is low, and successful has very strong practicality.
Brief description of the drawings
Fig. 1 is preparation method's schematic flow sheet of the present invention.
Embodiment
By the following specific examples further illustrate the invention, preparation method's flow process of the present invention as shown in Figure 1:
Embodiment 1
(1) preparation of modified graphene powder: by the silane coupling agent of 1 parts by weight, add 100 parts by weight ethanol/water solution (ethanol: water=95:5, weight ratio) in, after stirring, add the graphene powder of 10 parts by weight, after high-speed stirring, ultrasonic dispersion makes modified graphene dispersion liquid again; After again this dispersion liquid being fully dried, utilize ball mill to make modified graphene powder;
(2) preparation of modified graphene powder/polypropene blended master batch: by the modified graphene powder of 1 parts by weight described in (1), join in the acrylic resin of 100 parts by weight, add again the thermo-stabilizer base lead salt of 1 parts by weight, the lubricant fatty acid ester of 1 parts by weight, lipid acid, fatty alcohol mixture, the filler-calcium carbonate of 10 parts by weight, the auxiliary agent chlorinatedpolyethylene (CPE) of 1 parts by weight, utilize Banbury mixer blending dispersion, again blend is joined to extruding pelletization in twin screw extruder and make modified graphene powder/rigid polyvinyl chloride blend composition, described polyvinyl chloride (PVC) RESINS is SG-5 type resin,
(3) with the preparation of the rigid polyvinyl chloride composite pipe of Graphene modification: add extrusion moulding in polychloroethylene pipes forcing machine to make the rigid polyvinyl chloride composite pipe 1 with Graphene modification the modified graphene powder/rigid polyvinyl chloride blend composition described in step (2).
Embodiment 2
(1) preparation of modified graphene powder: by the titanate coupling agent of 0.001 parts by weight, add 1 parts by weight ethanol/acetum (ethanol: acetic acid=95:5, weight ratio) in, after stirring, add the graphene powder of 1 parts by weight, after high-speed stirring, ultrasonic dispersion makes modified graphene dispersion liquid again; After again this dispersion liquid being fully dried, utilize ball mill to make modified graphene powder;
(2) preparation of modified graphene powder/polypropene blended master batch: by the modified graphene powder of 0.1 parts by weight described in (1), join in the acrylic resin of 100 parts by weight, add again the thermo-stabilizer metallic soap of 5 parts by weight, the lubricant fatty amide of 0.1 parts by weight and metallic soap mixture, the filler talcum powder of 5 parts by weight, auxiliary agent MBS (MBS) and the coloring agent mixture of 10 parts by weight, utilize Z-shaped kneader blending dispersion, again blend is joined to extruding pelletization in single screw extrusion machine and make modified graphene powder/rigid polyvinyl chloride blend composition, described polyvinyl chloride (PVC) RESINS is SG-6 type resin,
(3) with the preparation of the rigid polyvinyl chloride composite pipe of Graphene modification: add extrusion moulding in polychloroethylene pipes forcing machine to make the rigid polyvinyl chloride composite pipe 2 with Graphene modification the modified graphene powder/rigid polyvinyl chloride blend composition described in step (2).
Embodiment 3
(1) preparation of modified graphene powder: by the octadecylamine of 0.8 parts by weight and isocyanic acid coupling agent, add 1000 parts by weight ethanol/water solution (ethanol: water=95:5, weight ratio) in, after stirring, add the graphene powder of 100 parts by weight, after high-speed stirring, ultrasonic dispersion makes modified graphene dispersion liquid again; After again this dispersion liquid being fully dried, utilize ball mill to make modified graphene powder;
(2) preparation of modified graphene powder/polypropene blended master batch: by the modified graphene powder of 10 parts by weight described in (1), join in the acrylic resin of 100 parts by weight, add again the thermo-stabilizer organotin of 8 parts by weight, lubricant paraffin and the polyethylene wax mixture of 5 parts by weight, the filler titanium dioxide of 50 parts by weight, the auxiliary agent A CR of 20 parts by weight and coloring agent mixture, utilize mill blending dispersion, again blend is joined to extruding pelletization in Planetary Screw Extruder and make modified graphene powder/rigid polyvinyl chloride blend composition, described polyvinyl chloride (PVC) RESINS is SG-7 type resin,
(3) with the preparation of the rigid polyvinyl chloride composite pipe of Graphene modification: add extrusion moulding in polychloroethylene pipes forcing machine to make the rigid polyvinyl chloride composite pipe 3 with Graphene modification the modified graphene powder/rigid polyvinyl chloride blend composition described in step (2).
Embodiment 4
(1) preparation of modified graphene powder: by the octadecylamine of 0.1 parts by weight and isocyanic acid coupling agent, add 500 parts by weight ethanol/water solution (ethanol: water=95:5, weight ratio) in, after stirring, add the graphene powder of 50 parts by weight, after high-speed stirring, ultrasonic dispersion makes modified graphene dispersion liquid again; After again this dispersion liquid being fully dried, utilize ball mill to make modified graphene powder;
(2) preparation of modified graphene powder/polypropene blended master batch: by the modified graphene powder of 5 parts by weight described in (1), join in the acrylic resin of 100 parts by weight, add again thermo-stabilizer epoxy compounds and the rare earth compound of 10 parts by weight, the lubricant oxidation polyethylene wax of 3 parts by weight, the filler-calcium carbonate of 30 parts by weight, the auxiliary agent A CR of 5 parts by weight, utilize high-speed mixer blending dispersion, again blend is joined to extruding pelletization in Planetary Screw Extruder and make modified graphene powder/rigid polyvinyl chloride blend composition, described polyvinyl chloride (PVC) RESINS is SG-5 type resin,
(3) with the preparation of the rigid polyvinyl chloride composite pipe of Graphene modification: add extrusion moulding in polychloroethylene pipes forcing machine to make the rigid polyvinyl chloride composite pipe 4 with Graphene modification the modified graphene powder/rigid polyvinyl chloride blend composition described in step (2).
The present invention prepares the rigid polyvinyl chloride composite pipe with modified graphene of gained, with respect to the rigid polyvinyl chloride composite pipe that does not add Graphene, tensile strength has improved 20%, shock strength has improved 60%, ageing resistance has improved 20%, and this tubing has also possessed the functions such as antistatic, heat conduction in addition.
Other unaccounted part is prior art.
Claims (10)
1. by a preparation method for the rigid polyvinyl chloride composite pipe of Graphene modification, its step comprises: (1) is by 1 × 10
-3the surface treatment agent of-1 parts by weight, is added in 1-1000 parts by weight solvent, adds the graphene powder of 1-100 parts by weight after the two is stirred, and ultrasonic dispersion after mixture high-speed stirring is made to modified graphene dispersion liquid; Also after spheroidal graphite, make modified graphene powder by dry this modified graphene dispersion liquid again; (2) by the modified graphene powder of the 0.1-10 parts by weight described in step (1), join in the polyvinyl chloride (PVC) RESINS of 100 parts by weight, add again the thermo-stabilizer of 1-10 parts by weight, the lubricant of 0.1-5 parts by weight, the auxiliary agent of the filler of 5-50 parts by weight and 1-20 parts by weight, after blending dispersion, extruding pelletization makes modified graphene powder/rigid polyvinyl chloride blend composition again; (3) the modified graphene powder/rigid polyvinyl chloride blend composition described in step (2) is added extrusion moulding in polychloroethylene pipes forcing machine make the rigid polyvinyl chloride composite pipe with Graphene modification.
2. the preparation method who uses according to claim 1 the rigid polyvinyl chloride composite pipe of Graphene modification, is characterized in that: described surface treatment agent is one or more in silane coupling agent, titanate coupling agent, octadecylamine, isocyanic acid.
3. the preparation method who uses according to claim 1 the rigid polyvinyl chloride composite pipe of Graphene modification, is characterized in that: described solvent is ethanol/water solution or ethanol/acetum.
4. the preparation method who uses according to claim 1 the rigid polyvinyl chloride composite pipe of Graphene modification, is characterized in that: described polyvinyl chloride is tubing grade PVC resin, comprises SG-5, SG-6 or SG-7 type resin.
5. the preparation method who uses according to claim 1 the rigid polyvinyl chloride composite pipe of Graphene modification, is characterized in that: described thermo-stabilizer is one or more in base lead salt, metallic soap, organotin, epoxy compounds, rare earth compound.
6. the preparation method who uses according to claim 1 the rigid polyvinyl chloride composite pipe of Graphene modification, is characterized in that: described lubricant is one or more in fatty acid ester, lipid acid, fatty alcohol, fatty amide, metallic soap, paraffin, polyethylene wax, oxidic polyethylene dispersing agent for wax.
7. the preparation method who uses according to claim 1 the rigid polyvinyl chloride composite pipe of Graphene modification, is characterized in that: described filler comprises one or more in calcium carbonate, talcum powder, titanium dioxide.
8. the preparation method who uses according to claim 1 the rigid polyvinyl chloride composite pipe of Graphene modification, is characterized in that: described auxiliary agent comprises one or more in chlorinatedpolyethylene, MBS, ACR, tinting material.
9. the preparation method who uses according to claim 1 the rigid polyvinyl chloride composite pipe of Graphene modification, is characterized in that: the mixing in described step (2) utilizes Z-shaped kneader, high-speed mixer, mill or Banbury mixer to mix.
10. the preparation method who uses according to claim 1 the rigid polyvinyl chloride composite pipe of Graphene modification, is characterized in that: the extruding pelletization in described step (2) utilizes parallel double-screw extruder, conical double screw extruder or single screw extrusion machine to carry out.
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| CN201410190681.2A CN104004294A (en) | 2014-05-07 | 2014-05-07 | Preparation method of graphene-modified hard polyvinyl chloride composite tubing |
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Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104448074A (en) * | 2014-12-09 | 2015-03-25 | 厦门凯纳石墨烯技术有限公司 | Special modified graphene for polymerization of vinyl chloride |
| CN104817787A (en) * | 2015-05-05 | 2015-08-05 | 济宁利特纳米技术有限责任公司 | Antistatic plastic modified by functionalized graphene oxide and preparation method thereof |
| CN104843683A (en) * | 2015-04-09 | 2015-08-19 | 浙江泰索科技有限公司 | Method for modifying graphene by aqueous titanate |
| CN104844795A (en) * | 2015-04-09 | 2015-08-19 | 浙江泰索科技有限公司 | High strength thermal conductivity nylon 6 and preparation method thereof |
| CN105086200A (en) * | 2015-04-29 | 2015-11-25 | 宁波职业技术学院 | Graphene modified PVC material |
| CN105131450A (en) * | 2015-08-21 | 2015-12-09 | 宁波华安建材冶炼有限公司 | Graphene modified polyvinyl chloride material and preparation method thereof |
| CN105504587A (en) * | 2016-01-06 | 2016-04-20 | 青岛崂山管业科技有限公司 | Graphene PVC drainage pipe and preparation method thereof |
| CN105949679A (en) * | 2016-07-08 | 2016-09-21 | 江苏金材科技有限公司 | High-strength building formwork and production method thereof |
| CN106479085A (en) * | 2016-10-17 | 2017-03-08 | 黄宇 | A kind of high-impact Graphene modifying character for PVC material |
| CN107325438A (en) * | 2017-06-29 | 2017-11-07 | 江苏凯威药用包装有限公司 | It is a kind of for pvc material of medical package and preparation method thereof |
| CN107383693A (en) * | 2016-08-22 | 2017-11-24 | 广东纳路纳米科技有限公司 | A kind of modified white graphite alkene composite ganoine polychloroethylene pipes and preparation method thereof |
| CN107477272A (en) * | 2017-09-29 | 2017-12-15 | 江苏瑞腾涂装科技有限公司 | A kind of steel-plastics composite pipe |
| CN107739482A (en) * | 2017-10-31 | 2018-02-27 | 广西旭腾实业集团有限公司 | High-performance polyvinyl chloride pipe based on graphene and preparation method thereof |
| CN108003494A (en) * | 2017-11-16 | 2018-05-08 | 山东鲁泰控股集团有限公司 | A kind of environmental protection antistatic plate timber-used graphene modified hard PVC plastic and preparation method |
| CN108440866A (en) * | 2018-03-23 | 2018-08-24 | 长沙天卓塑胶有限公司 | A kind of preparation method of plastic tube |
| CN108948587A (en) * | 2018-07-24 | 2018-12-07 | 常州达奥新材料科技有限公司 | A kind of dedicated bloom modified master of transparent PVC boardy product |
| CN109251429A (en) * | 2018-08-08 | 2019-01-22 | 多凌新材料科技股份有限公司 | The graphene/carbon nano-tube master batch and its preparation method that are easily dispersed in PVC and application |
| CN109627624A (en) * | 2018-10-24 | 2019-04-16 | 山东鲁泰控股集团有限公司石墨烯高分子复合材料研发中心 | A kind of production line of graphene modified PVC resin |
| CN113637273A (en) * | 2021-08-31 | 2021-11-12 | 浙江同正管道技术有限公司 | Graphene reinforced PVC pipe and preparation method thereof |
| CN114957881A (en) * | 2022-05-16 | 2022-08-30 | 山东鲁泰控股集团有限公司石墨烯高分子复合材料研发中心 | Flame-retardant antistatic soft PVC material and preparation method thereof |
| CN115124797A (en) * | 2022-08-22 | 2022-09-30 | 鄂尔多斯市东澳管业有限公司 | Graphene composite rigid polyvinyl chloride pipe and preparation method thereof |
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| CN104448074A (en) * | 2014-12-09 | 2015-03-25 | 厦门凯纳石墨烯技术有限公司 | Special modified graphene for polymerization of vinyl chloride |
| CN104844795B (en) * | 2015-04-09 | 2017-12-29 | 浙江泰索科技有限公司 | A kind of high-strength heat conduction nylon 6 and preparation method thereof |
| CN104843683A (en) * | 2015-04-09 | 2015-08-19 | 浙江泰索科技有限公司 | Method for modifying graphene by aqueous titanate |
| CN104844795A (en) * | 2015-04-09 | 2015-08-19 | 浙江泰索科技有限公司 | High strength thermal conductivity nylon 6 and preparation method thereof |
| CN105086200A (en) * | 2015-04-29 | 2015-11-25 | 宁波职业技术学院 | Graphene modified PVC material |
| CN104817787A (en) * | 2015-05-05 | 2015-08-05 | 济宁利特纳米技术有限责任公司 | Antistatic plastic modified by functionalized graphene oxide and preparation method thereof |
| CN104817787B (en) * | 2015-05-05 | 2018-07-03 | 济宁利特纳米技术有限责任公司 | A kind of functionalization graphene is modified anti-static plastic and preparation method thereof |
| CN105131450A (en) * | 2015-08-21 | 2015-12-09 | 宁波华安建材冶炼有限公司 | Graphene modified polyvinyl chloride material and preparation method thereof |
| CN105504587A (en) * | 2016-01-06 | 2016-04-20 | 青岛崂山管业科技有限公司 | Graphene PVC drainage pipe and preparation method thereof |
| CN105949679A (en) * | 2016-07-08 | 2016-09-21 | 江苏金材科技有限公司 | High-strength building formwork and production method thereof |
| CN107383693A (en) * | 2016-08-22 | 2017-11-24 | 广东纳路纳米科技有限公司 | A kind of modified white graphite alkene composite ganoine polychloroethylene pipes and preparation method thereof |
| CN106479085A (en) * | 2016-10-17 | 2017-03-08 | 黄宇 | A kind of high-impact Graphene modifying character for PVC material |
| CN107325438A (en) * | 2017-06-29 | 2017-11-07 | 江苏凯威药用包装有限公司 | It is a kind of for pvc material of medical package and preparation method thereof |
| CN107477272A (en) * | 2017-09-29 | 2017-12-15 | 江苏瑞腾涂装科技有限公司 | A kind of steel-plastics composite pipe |
| CN107739482A (en) * | 2017-10-31 | 2018-02-27 | 广西旭腾实业集团有限公司 | High-performance polyvinyl chloride pipe based on graphene and preparation method thereof |
| CN108003494A (en) * | 2017-11-16 | 2018-05-08 | 山东鲁泰控股集团有限公司 | A kind of environmental protection antistatic plate timber-used graphene modified hard PVC plastic and preparation method |
| CN108440866A (en) * | 2018-03-23 | 2018-08-24 | 长沙天卓塑胶有限公司 | A kind of preparation method of plastic tube |
| CN108948587A (en) * | 2018-07-24 | 2018-12-07 | 常州达奥新材料科技有限公司 | A kind of dedicated bloom modified master of transparent PVC boardy product |
| CN109251429A (en) * | 2018-08-08 | 2019-01-22 | 多凌新材料科技股份有限公司 | The graphene/carbon nano-tube master batch and its preparation method that are easily dispersed in PVC and application |
| CN109251429B (en) * | 2018-08-08 | 2021-05-11 | 多凌新材料科技股份有限公司 | Graphene/carbon nanotube master batch easy to disperse in PVC (polyvinyl chloride), and preparation method and application thereof |
| CN109627624A (en) * | 2018-10-24 | 2019-04-16 | 山东鲁泰控股集团有限公司石墨烯高分子复合材料研发中心 | A kind of production line of graphene modified PVC resin |
| CN113637273A (en) * | 2021-08-31 | 2021-11-12 | 浙江同正管道技术有限公司 | Graphene reinforced PVC pipe and preparation method thereof |
| CN114957881A (en) * | 2022-05-16 | 2022-08-30 | 山东鲁泰控股集团有限公司石墨烯高分子复合材料研发中心 | Flame-retardant antistatic soft PVC material and preparation method thereof |
| CN114957881B (en) * | 2022-05-16 | 2024-03-15 | 山东鲁泰控股集团有限公司石墨烯高分子复合材料研发中心 | Flame-retardant antistatic soft PVC material and preparation method thereof |
| CN115124797A (en) * | 2022-08-22 | 2022-09-30 | 鄂尔多斯市东澳管业有限公司 | Graphene composite rigid polyvinyl chloride pipe and preparation method thereof |
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Application publication date: 20140827 |
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