CN105837892B - It is a kind of to utilize carbon doping heat-conducting plastic of microwave treatment and preparation method thereof - Google Patents

It is a kind of to utilize carbon doping heat-conducting plastic of microwave treatment and preparation method thereof Download PDF

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Publication number
CN105837892B
CN105837892B CN201610212477.5A CN201610212477A CN105837892B CN 105837892 B CN105837892 B CN 105837892B CN 201610212477 A CN201610212477 A CN 201610212477A CN 105837892 B CN105837892 B CN 105837892B
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preparation
conducting plastic
heat
microwave treatment
carbon doping
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CN105837892A (en
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陈旭东
陶德良
刘林
杨金
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Guangdong Gunakai Material Technology Co Ltd
Guangdong New Material Research Institute Co Ltd
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Guangdong Gunakai Material Technology Co Ltd
Guangdong New Material Research Institute Co Ltd
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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
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/092—Polycarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/28—Treatment by wave energy or particle radiation
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/21—Urea; Derivatives thereof, e.g. biuret
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/315—Compounds containing carbon-to-nitrogen triple bonds
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/34—Heterocyclic compounds having nitrogen in the ring
    • C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
    • C08K5/3477—Six-membered rings
    • C08K5/3492—Triazines
    • C08K5/34922—Melamine; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10—Homopolymers or copolymers of propene
    • C08L23/12—Polypropene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/04—Homopolymers or copolymers of ethene
    • C08J2323/06—Polyethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/10—Homopolymers or copolymers of propene
    • C08J2323/12—Polypropene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2325/00—Characterised by the use 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 an aromatic carbocyclic ring; Derivatives of such polymers
    • C08J2325/02—Homopolymers or copolymers of hydrocarbons
    • C08J2325/04—Homopolymers or copolymers of styrene
    • C08J2325/06—Polystyrene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00—Characterised by the use 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; Derivatives of such polymers
    • C08J2327/02—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/04—Characterised by the use 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; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08J2327/06—Homopolymers or copolymers of vinyl chloride
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • C08J2377/06—Polyamides derived from polyamines and polycarboxylic acids

Abstract

Carbon doping heat-conducting plastic of microwave treatment and preparation method thereof is utilized the invention discloses a kind of.Its preparation method is：After fluoropolymer resin and micromolecular compound blending are stirred evenly, a certain amount of water is added, as in micro-wave oven, a period of time is heated using microwave, after small molecule is carbonized, takes out and dries, the material of gained is added directly into blending, extrusion molding in extruder, obtains finished product.The present invention preparation method with it is existing prepare the method for thermoplastic materials compared with, with technique is simple, yield is high, good heat conductivity, the advantages that structure diversification, its heat-conducting plastic prepared can be widely used in fields such as the fields such as transformer inductance, cooling electronic component, special cable, Electronic Packaging, heat conduction embedding.

Description

It is a kind of to utilize carbon doping heat-conducting plastic of microwave treatment and preparation method thereof
Technical field
The present invention relates to material chemistry technical field, and in particular to a kind of carbon doping heat-conducting plastic using microwave treatment and Its preparation method.
Background technology
In the last few years, as the progress of industrial production and science and technology, people propose higher property to Heat Conduction Material It can require.The heat transfer pipe of industrial wastewater is such as handled, has both needed material to have higher heat conductivility, while also requires material resistance toization Learn corrosion.On the other hand, with the miniaturization of electronic device, while also require that heat-removal mould, fin progressively minimize.But The preferable material of traditional heat conductivility, mostly metal material and inorganic non-metallic material, these materials or not corrosion-resistant, or add Complex process of work shaping or both.For the New Times to new material demand, high polymer material has excellent corrosion-resistant Performance and mechanical property, the visual field of people is progressed into, but pure high polymer material is usually inefficient, because high Molecular material is the non-conductor of heat mostly.
Plastics thermal conductivity factor very little, the existing method for improving plastics heat conductivility mainly have two kinds, first, synthesis tool There is the structural plastic of high thermal conductivity coefficient.Such as there is polyacetylene, polyaniline, the polypyrrole of Thermal conductivity, more grind Study carefully, be to concentrate on to be filled plastics with high heat conduction filler, obtained using the cooperative effect between two or more material The heat-conducting plastic that arrives is cheap, easy processing shaping, and some special dimensions are can apply to by appropriate PROCESS FOR TREATMENT.But For traditional method being filled with high heat conduction filler to plastics, due to most of high heat conduction filler be metal material or For inorganic non-metallic material, it is usually unsatisfactory with the interface cohesion of organic polymer resin material.The stone occurred in recent years Black alkene, due to high thermal conductivity, thermal conductivity is up to 3000 ~ 6 000 W/ (m K), gradually attracts much attention.But graphite Alkene preparation technology is complicated, synthesis cost is high, it is difficult to which high-volume synthesizes.
The content of the invention
The technical problem to be solved in the present invention is to provide one kind that is a kind of simple and easy to get and can manufacture using at microwave Carbon doping heat-conducting plastic of reason and preparation method thereof.
In order to solve the above-mentioned technical problem, the base case of first technical scheme provided by the invention is：One kind utilizes The preparation method of the carbon doping heat-conducting plastic of microwave treatment, including extrusion molding step, described extrusion molding step are gone back before Include carburising step：After first being mixed, stirred evenly by fluoropolymer resin and micromolecular compound, water is added, is done again after microwave heating It is dry.
Using a kind of preparation method of carbon doping heat-conducting plastic using microwave treatment of technical solution of the present invention, small molecule Compound is easily carbonized in the presence of microwave, the carbon point good heat conductivity of generation, can be used as heat filling, and polymer The polymer of some small-molecular-weights also can also be carried out partially carbonized in the effect of microwave in resin, be improved between polymer and carbon point Interface combination, strengthen heat-conductive characteristic, while be continuously increased the packing ratio of small molecule filler so that the carbon point of generation is poly- Heat conduction network chain is formed in compound matrix.In addition, fluoropolymer resin be carbonized jointly under microwave action with micromolecular compound it is same When, fluoropolymer resin is easily wrapped in inside by the carbon point of generation, and it is polymeric matrix that formation is internal, outside is what carbon point coated Structure so that material tentatively mixes, and is advantageous to follow-up coextrusion.Small molecule is first carbonized by microwave, then with polymerizeing For the preparation method of thing blending extrusion, this method and existing carbon doping heat-conducting plastic, its preparation method is simple and easy to get, and can criticize Amount production.
The preferred scheme one of first technical scheme, on base case, described micromolecular compound includes lemon The mixture of one of which or urea and citric acid in acid, melamine, dicyanodiamine, urea.
The preferred scheme two of first technical scheme, on base case, described fluoropolymer resin include polyethylene, The mixture of one of which or polypropylene and terylene in polyvinyl chloride, nylon66 fiber, polystyrene.
The preferred scheme three of first technical scheme, on base case or preferred scheme one or preferred scheme two, institute In the fluoropolymer resin and the mixed mixture of micromolecular compound stated, the ratio of micromolecular compound is at least 10%.
The preferred scheme four of first technical scheme, on base case or preferred scheme three, described polymer tree In fat and the mixed mixture of micromolecular compound, the ratio of micromolecular compound is 20%.
The preferred scheme five of first technical scheme, on preferred scheme four, microwave heats in described carburising step Time be 7 ~ 15min, dry be disposed in 12 DEG C of baking oven dry.
The preferred scheme six of first technical scheme, on preferred scheme four, described fluoropolymer resin and water plus Entering amount ratio is：100g：10~20ml.
The base case of second technical scheme provided by the invention, base case in first technical scheme, preferably Scheme one on the basis of one of them, utilizes the preparation method of the carbon doping heat-conducting plastic of microwave treatment into preferred scheme six Manufactured heat-conducting plastic.Using heat-conducting plastic made of the preparation method of the carbon doping heat-conducting plastic of this microwave treatment, for becoming The fields such as depressor inductance, cooling electronic component, special cable, Electronic Packaging, heat conduction embedding have good application value.
Brief description of the drawings
Fig. 1 is finished product thermal conductivity factor schematic diagram prepared by the embodiment of the present invention one.
Fig. 2 is finished product thermal conductivity factor schematic diagram prepared by the embodiment of the present invention two.
Fig. 3 is finished product thermal conductivity factor schematic diagram prepared by the embodiment of the present invention three.
Fig. 4 is finished product thermal conductivity factor schematic diagram prepared by the embodiment of the present invention four.
Fig. 5 is finished product thermal conductivity factor schematic diagram prepared by the embodiment of the present invention five.
Embodiment
Embodiment one：
100g polyethylene is mixed with citric acid, in the mixture of polyethylene and citric acid, the ratio difference of citric acid For：10%th, 15%, 20%, 25%, 20ml water is added, is placed in micro-wave oven, 7min is heated under 700mw microwaves, takes out after 120 Dried in DEG C baking oven, by the material extruder for shaping of gained, heat-conducting plastic finished product be made, and test its thermal conductivity factor, The result of test is respectively：2.216w/ (mk), 3.865w/ (mk), 5.124w/ (mk), 6.223w/ (mk), such as scheme Shown in 1, for the thermal conductivity factor of material under the conditions of the citric acid of different proportion.
Embodiment two：
100g polyvinyl chloride is mixed with melamine, in the mixture of polyvinyl chloride and melamine, melamine Ratio be respectively：10%th, 15%, 20%, 25%, 15ml water is added, is placed in micro-wave oven, is heated 10min under 700mw microwaves, take Go out after being dried in 120 DEG C of baking ovens, by the material extruder for shaping of gained, heat-conducting plastic finished product is made, and test it Thermal conductivity factor, the result of test are respectively：1.628w/(m·k)、3.059w/(m·k)、4.205w/(m·k)、5.109w/ (mk), as shown in Fig. 2 thermal conductivity factor for material under the conditions of the melamine of different proportion.
Embodiment three：
100g nylon66 fibers are mixed with dicyanodiamine, in nylon66 fiber and the mixture of dicyanodiamine, the ratio of dicyanodiamine Example be respectively：10%th, 15%, 20%, 25%, 18ml water is added, is placed in micro-wave oven, 15min is heated under 700mw microwaves, after taking-up Dried in 120 DEG C of baking ovens, by the material extruder for shaping of gained, heat-conducting plastic finished product is made, and test its heat conduction Coefficient, the result of test are respectively：2.523w/(m·k)、3.095w/(m·k)、3.511w/(m·k)、4.598w/(m· K), as shown in figure 3, thermal conductivity factor for material under the conditions of the dicyanodiamine of different proportion.
Example IV：
After 50g terylene and 50g polypropylene are mixed with urea, in the mixture of terylene, polypropylene and urea, urea Ratio is respectively：10%th, 15%, 20%, 25%, 10ml water is added, is placed in micro-wave oven, 7min is heated under 700mw microwaves, after taking-up Dried in 120 DEG C of baking ovens, the material of gained is used for extruder for shaping, heat-conducting plastic finished product is made, and test it and lead Hot coefficient, the result of test are respectively：1.578w/(m·k)、3.012w/(m·k)、3.615w/(m·k)、4.725w/(m· K), as shown in figure 4, thermal conductivity factor for material under the conditions of the urea of different proportion.
Embodiment five：
By 100g polystyrene respectively with urea/citric acid（1:1）After mixing, in polystyrene and urea/citric acid In mixture, the ratio of urea/citric acid is respectively：10%th, 15%, 20%, 25%, 10ml water is added, is placed in micro-wave oven, 10min is heated under 700mw microwaves, takes out after being dried in 120 DEG C of baking ovens, the material of gained is used for extruder for shaping, Heat-conducting plastic finished product is made, and tests its thermal conductivity factor, the result of test is respectively：2.005w/(m·k)、3.065w/(m· K), 3.489w/ (mk), 4.509w/ (mk), as shown in figure 5, being material under the conditions of urea/citric acid of different proportion Thermal conductivity factor.
Comparative example：
After 100g polyethylene is mixed with the graphite of different proportion respectively, in the mixture of polyethylene and graphite, graphite Ratio be respectively 20%, 40%, 60%, by the material extruder for shaping of gained, heat-conducting plastic finished product is made.Its heat conduction Coefficient is respectively：0.892 w/(m·k)、0.968w/(m·k)、1.109w/(m·k).
As can be seen here：One ~ embodiment of embodiments of the invention five, its thermal conductivity factor measured are superior to comparative example, and real When applying the ratio of the ratio of the micromolecular compound of one ~ embodiment of example five in the mixture more than 10%, its thermal conductivity factor is superior to The ratio of micromolecular compound is less than 10%；When the ratio ratio in the mixture of micromolecular compound is more than 20%, its Thermal conductivity factor is much better than below 20%.
For those skilled in the art, on the premise of technical solution of the present invention is not departed from, if can also make Dry modification and improvement, these should also be considered as protection scope of the present invention, these all without influence effect that the present invention implemented and Practical applicability.

Claims (8)

1. a kind of preparation method of carbon doping heat-conducting plastic using microwave treatment, including extrusion molding step, it is characterised in that Also include carburising step before described extrusion molding step：First mixed, stirred evenly by fluoropolymer resin and micromolecular compound Afterwards, water, re-dry after microwave heating are added；Described micromolecular compound includes citric acid, melamine, dicyanodiamine, urine The mixture of one of which or urea and citric acid in element.
2. the preparation method of the carbon doping heat-conducting plastic according to claim 1 using microwave treatment, it is characterised in that：Institute The fluoropolymer resin stated includes polyethylene, polyvinyl chloride, nylon66 fiber, the one of which in polystyrene or polypropylene and terylene Mixture.
3. the preparation method of the carbon doping heat-conducting plastic according to claim 1 or 2 using microwave treatment, its feature exist In：In described fluoropolymer resin and the mixed mixture of micromolecular compound, the ratio of micromolecular compound is at least 10%.
4. the preparation method of the carbon doping heat-conducting plastic according to claim 3 using microwave treatment, it is characterised in that：Institute In the fluoropolymer resin and the mixed mixture of micromolecular compound stated, the ratio of micromolecular compound is more than 20%.
5. the preparation method of the carbon doping heat-conducting plastic according to claim 4 using microwave treatment, it is characterised in that：Institute The time that microwave heats in the carburising step stated is 7~15min, dries and is disposed on drying in 12 DEG C of baking oven.
6. the preparation method of the carbon doping heat-conducting plastic according to claim 4 using microwave treatment, it is characterised in that：Institute The fluoropolymer resin and the addition ratio of water stated be：100g：10~20ml.
7. the preparation side of the carbon doping heat-conducting plastic using microwave treatment according to claim 1~2 or 5~6 any one Heat-conducting plastic made of method.
8. heat conduction made of the preparation method according to claim 3 using the carbon doping heat-conducting plastic of microwave treatment is moulded Material.
CN201610212477.5A 2016-04-07 2016-04-07 It is a kind of to utilize carbon doping heat-conducting plastic of microwave treatment and preparation method thereof Expired - Fee Related CN105837892B (en)

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Citations (2)

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CN102942175A (en) * 2012-11-23 2013-02-27 中国科学院长春光学精密机械与物理研究所 Application of carbon nanodots as water-soluble ratiometric fluorescent probe
CN104327288A (en) * 2007-10-01 2015-02-04 帝斯曼知识产权资产管理有限公司 Heat-processable thermally conductive polymer composition

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104327288A (en) * 2007-10-01 2015-02-04 帝斯曼知识产权资产管理有限公司 Heat-processable thermally conductive polymer composition
CN102942175A (en) * 2012-11-23 2013-02-27 中国科学院长春光学精密机械与物理研究所 Application of carbon nanodots as water-soluble ratiometric fluorescent probe

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