CN114957833A - Preparation method of high-performance graphene/polyethylene heat conduction pipe - Google Patents
Preparation method of high-performance graphene/polyethylene heat conduction pipe Download PDFInfo
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- CN114957833A CN114957833A CN202210567358.7A CN202210567358A CN114957833A CN 114957833 A CN114957833 A CN 114957833A CN 202210567358 A CN202210567358 A CN 202210567358A CN 114957833 A CN114957833 A CN 114957833A
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- 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
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
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- 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
- Y02P20/10—Process efficiency
Abstract
A preparation method of a high-performance graphene/polyethylene heat conduction pipe relates to a preparation method of a heat conduction pipe. In the first step of the method, the flake graphite is oxidized, intercalated and stripped through oxidation intercalation and high-temperature expansion to obtain thick graphene. And secondly, melting and blending the thick graphene sheets obtained in the first step with high heat-resistant Polyethylene (PERT) resin in an internal mixer and a screw extruder to obtain the graphene/polyethylene heat-conducting pipe. The thick graphene prepared by the invention has good heat conduction, reinforcing and toughening effects, the preparation method is simple, and the conditions are easy to control. The prepared heat conduction pipe has high heat conduction coefficient and excellent mechanical property, and has wide application value in the field of preparing high-performance heat conduction pipes.
Description
Technical Field
The invention relates to a preparation method of a heat conduction pipe, in particular to a preparation method of a high-performance graphene/polyethylene heat conduction pipe.
Background
The development of semiconductor manufacturing technology has led in recent decades to the integration and miniaturization of electronic components. However, with the rapid increase in performance of electronic devices, the removal of excess or residual heat is becoming an increasingly critical issue. The polymer composite material with light weight, multiple functions, low cost and high heat conductivity has wide application prospect as a heat dissipation element. One of the inherent characteristics of polymers is their extremely low thermal conductivity, which limits their use in certain conditions where higher thermal conductivity is required.
Graphene is a compound represented by sp 2 The bonded carbon atoms are arranged on a two-dimensional honeycomb latticeA single layer of material of (a). The first paper about graphene was published in 2004, and a two-dimensional material stably existing at room temperature was prepared for the first time, breaking the statement that the two-dimensional material cannot stably exist at room temperature, and a discoverer of the two-dimensional material obtains the nobel prize in physics in 2010. Since graphene has excellent mechanical and electrical properties and higher light transmittance, the graphene is a new member of a carbon family and is paid much attention, and a large number of researchers are researching and preparing single-layer or few-layer graphene in a large area; in the same way, many researchers are researching and preparing graphene powder materials, wherein a redox method is the most common method for preparing graphene powder at present and is also one of the most potential methods for realizing large-scale preparation of graphene powder. Graphene has a large specific surface area and a unique two-dimensional structure. The thermal conductivity coefficient of the single-layer graphene can reach 5300W/(m.K), and the single-layer graphene can be used as a thermal conductive filler to effectively improve the thermal conductivity of a polymer. However, most of the heat-conducting pipes prepared by using graphene oxide and flake graphite as heat-conducting fillers have poor mechanical properties and cannot be applied to the field of heat conduction in a large scale.
Disclosure of Invention
The invention aims to provide a preparation method of a high-performance graphene/polyethylene heat-conducting pipe, which comprises the steps of oxidizing, expanding and stripping crystalline flake graphite by a high-temperature expansion and mechanical stripping method to obtain thick graphene; the fusion intercalation is realized in the fusion blending process, the thick graphene is peeled into the thin graphene sheet, and the excellent mechanical performance is obtained while the thermal conductivity of the polyethylene heat-conducting pipe is effectively improved. The graphene/polyethylene heat-conducting pipe prepared by the invention has good heat-conducting property and mechanical property, so that the graphene/polyethylene heat-conducting pipe has potential application value in other fields such as heat-conducting ground heating pipes and heat-radiating materials.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a high-performance graphene/polyethylene heat conduction pipe comprises the following preparation processes:
the preparation of the thick graphene/polyethylene heat conduction pipe comprises two steps: firstly, carrying out oxidation intercalation and high-temperature expansion on flake graphite to obtain thick graphene; secondly, carrying out melt blending on the thick graphene and the high-heat-resistant polyethylene resin, and carrying out melt blending and extrusion molding to obtain a thick graphene/polyethylene heat-conducting pipe;
in the first step, the oxidant used in the preparation of the thick graphene is any one or a mixture of more of ammonium persulfate, potassium permanganate, potassium dichromate and nitric acid; the intercalation agent is one or more of sodium dodecyl sulfate, hexadecyl ammonium bromide, phosphoric acid, perchloric acid, sulfuric acid, boric acid and copper chloride; the reaction temperature is controlled between 20 and 40 ℃; the reaction time is controlled to be between 20 and 120 min; the high-temperature expansion temperature is 300-600 ℃; in the process of preparing the thick graphene, the temperature of a system needs to be controlled below 15 ℃ in a low-temperature stage, and the temperature needs to be controlled below 30 ℃ in a dilution process;
in the second step, the used high thermal conductivity polyethylene is one or more of XL1800, P382RA, SM5500 and SP980, and the melt blending temperature is controlled between 160 ℃ and 190 ℃; the extrusion molding temperature is controlled between 180 ℃ and 210 ℃; the mass ratio of the thick graphene to the high heat-resistant polyethylene is 0.01: 1-0.1: 1.
the invention has the advantages and effects that:
1. the preparation equipment of the thick graphene sheet has low requirement, the raw materials are easy to obtain, and the thick graphene sheet can be used for modifying polymer materials.
2. The thick graphene prepared by the method has better subsequent utilization value, and can be used for obtaining the graphene/polyolefin composite material.
3. The thick graphene prepared by the method is black solid powder, has good heat conduction, reinforcing and toughening effects, and effectively improves the heat conduction performance and the mechanical property of the polymer under the condition of low filling amount. The polymer has higher application value in the fields of heat conduction, reinforcement, toughening and the like of polymers in the future.
4. The graphene/polyethylene heat conduction material prepared by the invention has high heat conduction performance and excellent mechanical property, and has higher application value in the fields of heat conduction pipes, heat dissipation materials and the like.
Drawings
Fig. 1 is an enlarged photograph of a thick graphene structure prepared by the present invention.
Detailed Description
The present invention will be described in detail with reference to the embodiments shown in the drawings.
Example 1:
the first step is as follows: uniformly mixing 30mL of mixed acid (concentrated sulfuric acid: concentrated phosphoric acid = 2: 1) and 10g of flake graphite in an ice-water bath, slowly adding 5g of potassium permanganate into the mixed solution, ensuring that the temperature is lower than 15 ℃ in the process, heating the water bath to 35 ℃ after the addition is finished, and carrying out heat preservation reaction for 60 min; diluting the obtained mixed solution with water to 1L under ice bath condition, ensuring the temperature to be lower than 30 ℃, and adding H 2 O 2 And (3) 20mL, performing suction filtration and washing for 3 times, drying, and placing in a 500 ℃ high-temperature tube furnace for high-temperature expansion to obtain the thick graphene.
The second step is that: 3.6g of thick graphene and 180g of high heat-resistant polyethylene (PERT, P382 RA) are melted and mixed at 180 ℃, and the mixture is extruded to form the graphene/polyethylene composite material, wherein the thermal conductivity coefficient (lambda) of the graphene/polyethylene composite material is 0.4222W/(m.K), the tensile strength is 18.7MPa, the flexural modulus is 259.1MPa, and the impact strength is 36.9kJ/m 2 。
Example 2:
the first step is as follows: same as example 1
The second step is that: 5.4g of thick graphene and 180g of high heat-resistant polyethylene (PERT, P382 RA) are melted and mixed at 180 ℃, and the mixture is extruded to form the graphene/polyethylene composite material, wherein the thermal conductivity (lambda) of the graphene/polyethylene composite material is 0.5103W/(m.K), the tensile strength is 17.7MPa, the flexural modulus is 288.4MPa, and the impact strength is 32.3kJ/m 2 。
Example 3:
the first step is as follows: same as example 1
The second step is that: 9.0g of thick graphene and 180g of high heat-resistant polyethylene (PERT, P382 RA) are melted and mixed at 180 ℃, and the mixture is extruded to obtain the graphene/polyethylene composite material, wherein the thermal conductivity (lambda) of the graphene/polyethylene composite material is 0.6023W/(m.K), the tensile strength is 16.6MPa, the flexural modulus is 324.6MPa, and the impact strength is 25.0kJ/m 2 。
Claims (1)
1. A preparation method of a high-performance graphene/polyethylene heat conduction pipe is characterized by comprising the following preparation processes:
the preparation of the thick graphene/polyethylene heat conduction pipe comprises two steps: firstly, carrying out oxidation intercalation and high-temperature expansion on flake graphite to obtain thick graphene; secondly, carrying out melt blending on the thick graphene and the high-heat-resistant polyethylene resin, and carrying out melt blending and extrusion molding to obtain a thick graphene/polyethylene heat-conducting pipe;
in the first step, the oxidant used in the preparation of the thick graphene is any one or a mixture of more of ammonium persulfate, potassium permanganate, potassium dichromate and nitric acid; the intercalation agent is one or more of sodium dodecyl sulfate, hexadecyl ammonium bromide, phosphoric acid, perchloric acid, sulfuric acid, boric acid and copper chloride; the reaction temperature is controlled between 20 and 40 ℃; the reaction time is controlled to be between 20 and 120 min; the high-temperature expansion temperature is 300-600 ℃; in the process of preparing the thick graphene, the temperature of a system needs to be controlled below 15 ℃ in a low-temperature stage, and the temperature needs to be controlled below 30 ℃ in a dilution process;
in the second step, the used high thermal conductivity polyethylene is one or more of XL1800, P382RA, SM5500 and SP980, and the melt blending temperature is controlled between 160 ℃ and 190 ℃; the extrusion molding temperature is controlled between 180 ℃ and 210 ℃; the mass ratio of the thick graphene to the high heat-resistant polyethylene is 0.01: 1-0.1: 1.
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Citations (7)
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US20180339906A1 (en) * | 2015-11-16 | 2018-11-29 | Fudan University | Preparation method for large-size graphene oxide or graphene |
CN109354703A (en) * | 2018-08-27 | 2019-02-19 | 华南理工大学 | A kind of class graphene composite material preparation method in-situ inserted based on polymer graphite |
CN109665518A (en) * | 2017-10-16 | 2019-04-23 | 山东欧铂新材料有限公司 | A kind of preparation method of highly conductive graphene |
CN109824040A (en) * | 2019-03-14 | 2019-05-31 | 西南科技大学 | Quickly prepare expanded graphite method, wet process removing prepares graphene method |
CN112143072A (en) * | 2020-09-02 | 2020-12-29 | 新奥(内蒙古)石墨烯材料有限公司 | Graphene/polyethylene heat conduction material, preparation method thereof, pipe using heat conduction material and ground source heat pump |
CN113830757A (en) * | 2020-06-24 | 2021-12-24 | 四川烯时代新材料有限公司 | Method for preparing low-defect graphene by thermal stripping of low-graphite oxide after intercalation |
CN114763428A (en) * | 2021-01-14 | 2022-07-19 | 中国科学院大连化学物理研究所 | Method for preparing polymer and graphene composite material, composite material and base resin obtained by method |
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- 2022-05-24 CN CN202210567358.7A patent/CN114957833A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20180339906A1 (en) * | 2015-11-16 | 2018-11-29 | Fudan University | Preparation method for large-size graphene oxide or graphene |
CN109665518A (en) * | 2017-10-16 | 2019-04-23 | 山东欧铂新材料有限公司 | A kind of preparation method of highly conductive graphene |
CN109354703A (en) * | 2018-08-27 | 2019-02-19 | 华南理工大学 | A kind of class graphene composite material preparation method in-situ inserted based on polymer graphite |
CN109824040A (en) * | 2019-03-14 | 2019-05-31 | 西南科技大学 | Quickly prepare expanded graphite method, wet process removing prepares graphene method |
CN113830757A (en) * | 2020-06-24 | 2021-12-24 | 四川烯时代新材料有限公司 | Method for preparing low-defect graphene by thermal stripping of low-graphite oxide after intercalation |
CN112143072A (en) * | 2020-09-02 | 2020-12-29 | 新奥(内蒙古)石墨烯材料有限公司 | Graphene/polyethylene heat conduction material, preparation method thereof, pipe using heat conduction material and ground source heat pump |
CN114763428A (en) * | 2021-01-14 | 2022-07-19 | 中国科学院大连化学物理研究所 | Method for preparing polymer and graphene composite material, composite material and base resin obtained by method |
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