CN109762226A - Composite heat conducting material and its preparation method and application - Google Patents
Composite heat conducting material and its preparation method and application Download PDFInfo
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- CN109762226A CN109762226A CN201811490041.8A CN201811490041A CN109762226A CN 109762226 A CN109762226 A CN 109762226A CN 201811490041 A CN201811490041 A CN 201811490041A CN 109762226 A CN109762226 A CN 109762226A
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Abstract
The present invention relates to composite heat conducting material and its preparation method and application, the composite heat conducting material by mixing material be irradiated it is cross-linking modified be made, the mixing material includes the composition of following mass fraction: 20~100 parts by weight of heat filling；100 parts by weight of polyvinyl resin；0.4~1.6 parts by weight of coupling agent；2~8 parts by weight of White Carbon black, composite heat conducting material are mainly used in the raw material of electric heating device fabrication.Composite heat conducting material of the invention, pass through the cooperation of polyvinyl resin and heat filling, improve the capacity of heat transmission of itself, and white carbon black is added on this basis, further thermal coefficient is improved to 0.51~0.55, while increasing radiation parameter appropriate, crosslink material is made to generate the gel of high-content, to improve the breaking strength and elongation at break of itself, enhance the mechanical property of itself.
Description
Technical field
The invention belongs to technical field of composite materials, in particular to composite heat conducting material and its preparation method and application.
Background technique
Tubing used in ground heating system is mainly plastic pipe currently on the market, with PE-X (crosslinked polyethylene), PE-RT
Based on (heat-proof polythene), PP-R (atactic copolymerized polypropene), crosslinking aluminum plastic composite pipe and PB (polybutene) etc..Plastic conduit with
Metallic conduit, which is compared, has many advantages, such as corrosion-resistant, non-corrosive, light-weight, easy for installation, long service life, but high molecular material
Thermal coefficient generally there was only 0.3W/mK or so, it is far short of what is expected with metal material compared with, thus have that heat dissipation is slow to imitate with heat exchange
The low problem of rate.
In order to meet the cooling requirements of floor heating pipe, need to introduce the filler with high thermal conductivity coefficient in polyolefin substrate,
Such as metal (metal oxide) class, ceramic-like, charcoal class heat filling.To make heat filling form certain thermally conductive chain, thermally conductive
Net, the loading of raising heat filling simply, although heating conduction has a preferable improvement, the mechanical property of composite material,
Other comprehensive performances such as processing performance have greater loss.Aluminium powder is added as heat filling in Wang Liangliang etc. in PP, is prepared for
Heat-conductive composite material, the results showed that heat filling amount increases, and the thermal conductivity of composite material is greatly improved while also reducing
Mechanical performance.(referring to Wang Liangliang, Tao Guoliang, the research of Thermal Conductivity of Aluminum Powder/PP Composite, plastics industry, 2003,
12:47-54).
White carbon black is divided into precipitated silica and fume colloidal silica by production method.White carbon black is mainly used as natural rubber
With reinforcing agent, the toothpaste abrasives of synthetic rubber etc..White carbon black is one of ultra tiny New Inorganic Materials of extremely important high-tech,
White carbon black partial size is small, and large specific surface area, superficial attractive forces are strong, and surface can be big, and chemical purity is high, superior stability, reinforcement
Property, thickening property and thixotropy, show unique characteristics in numerous subjects and field, do not replace.
Theoretically, white carbon black is applied to that its mechanical performance can be increased on polyolefin substrate, then cooperates and has height
The filler of thermal coefficient coefficient, can obtain the composite material for having good comprehensive performance, but at present and have no for this technology
The more mature research carried out.
Summary of the invention
The purpose of the present invention is in order to solve the above problem, the present invention provides one kind and has both good heating conduction and mechanical property
The composite heat conducting material of energy.
According to an aspect of the present invention, a kind of composite heat conducting material is provided, which is passed through by mixing material
Radiation crosslinking modified to be made, mixing material includes the composition of following mass fraction: 20~100 parts by weight of heat filling；
100 parts by weight of polyvinyl resin；0.4~1.6 parts by weight of coupling agent；2~8 parts by weight of White Carbon black.
Wherein, mixing material includes the composition of following mass fraction: 40~60 parts by weight of heat filling；Polyethylene
100 parts by weight of resin；0.8~1.2 parts by weight of coupling agent；4~6 parts by weight of White Carbon black.
Wherein, irradiation dose is 600~200kGy, preferably 100~190kGy.
Wherein, white carbon black is Fumed silica.
Wherein, heat filling includes the one or more of filler in metal, ceramic-like filler and carbons filler；Polyethylene tree
Rouge includes one of high density polyethylene (HDPE), medium density polyethylene, low density polyethylene (LDPE) and linear low density polyethylene etc. or several
Kind；Preferably low density polyethylene (LDPE) LG-SP980；Coupling agent includes vinyltriethoxysilane, ethylenediamine propyl triethoxy
Silane dredges propyl trimethoxy silicane, ethylenediamine hydroxypropyl methyl dimethoxysilane, amine propyl-triethoxysilicane, KH-550
Series, methacryloxypropyl trimethoxy silane, glycidyl ether oxypropyltrimethoxysilane, dimerization di(2-ethylhexyl)phosphate
One or more of different monooctyl ester, magnesium stearate and titanate coupling agent, preferably KH-550.
Wherein, the partial size of heat filling is 25 μm；Polyvinyl resin is preferably low density polyethylene (LDPE) LG-SP980；Coupling agent
Preferably KH-550.
Wherein, the mode of irradiation includes radioactive cobalt x ray irradiation x and electron accelerator irradiation.
According to another aspect of the present invention, the preparation method of the composite heat conducting material is provided, comprising the following steps: will fix
The heat filling of proportion is mixed with coupling agent, obtains the heat filling of coupling processing；By polyvinyl resin in 140 DEG C of mills, so
Heat filling and white carbon black after the coupling processing of fixed mixing ratio is added afterwards are kneaded at 140 DEG C, are cut bottom sheet, are obtained mixing material
Piece；Mixing material material piece is irradiated crosslinking, composite heat conducting material is made.
According to the third aspect of the invention we, application of the composite heat conducting material in electric heating equipment is provided.
White carbon black, the free hydroxyl and polyethylene molecule on white carbon black surface is added in the present invention in polyvinyl Heat Conduction Material
Physics and chemical bonding are formd under certain irradiation dose, Molecular Adsorption layer is formed on surface, constitutes white carbon black and gather
The three-dimensional net structure that ethylene molecule joins together, so that the deformation of polyethylene molecular chain is effectively limited, to play increasing
Pretend use.The free hydroxyl and heat filling on the white carbon black surface in addition added form physics and chemical bonding, improve and lead
The dispersibility of hot filler, while enhancing the building of heat filling thermal conducting path, enhance the thermal conductivity of composite material.
The invention has the following advantages:
Composite heat conducting material of the invention improves the thermally conductive energy of itself by the cooperation of polyvinyl resin and heat filling
Thermal coefficient is further improved to 0.51~0.55, while increasing irradiation appropriate by power, and add white carbon black on this basis
Condition, the gel for making crosslink material generate high-content enhance itself to improve the breaking strength and elongation at break of itself
Mechanical property.
Specific embodiment
The illustrative embodiments of the disclosure are described in more detail below.Although showing showing for the disclosure in specification
Example property embodiment, it being understood, however, that may be realized in various forms the disclosure without should be by embodiments set forth herein
It is limited.It is to be able to thoroughly understand the disclosure on the contrary, providing these embodiments, and can be by the model of the disclosure
It encloses and is fully disclosed to those skilled in the art.
1 composite heat conducting material X1 of embodiment
Composite heat conducting material X1 is prepared by following mixing material cross-linking radiation, irradiation dose 60kGy, radiation mode
For electron irradiation.The mixing material includes LG-SP980 resin: 100g；Aluminium oxide: 60g；Silane coupling agent: 1.2g；White carbon black:
6g。
The preparation method of composite heat conducting material X1 includes: to weigh 180g ethyl alcohol, 60g distilled water, 1.2g silane idol respectively
Join agent (KH550), 60g aluminium oxide and 2g white carbon black.Ethyl alcohol, distilled water and silane coupling agent (KH550) is ultrasonic in flask
30min hydrolyzed silane coupling agent.Open mill temperature is set as 140 DEG C, preliminary roller revolving speed is 24r/min, and back roller revolving speed is 17r/
Min weighs LG-SP980 resin 100g and is placed in mill 3min in open mill, and mill 2min is cut again for addition aluminium oxide and 2g white carbon black
Cut off piece.Obtained piece is taped against in steel plate mold (60mm × 120mm × 2mm), is put into 150 DEG C of vulcanizing press and is preheated
Then 2min is maintained at pressure 11MPa and temperature the hot pressing 3min at 160 DEG C, then is cold-pressed 2min, obtain molding material piece.
By molding material piece, sample X1 is obtained by the electron beam irradiation of 100kGy dosage.
2 composite heat conducting material X2 of embodiment
It keeps step same as Example 1 to obtain molding material piece, material piece is passed through to the electronics of 100kGy dosage
Beam irradiates to obtain sample X2.
3 composite heat conducting material X3 of embodiment
It keeps step same as Example 1 to obtain molding material piece, material piece is passed through to the electronics of 190kGy dosage
Beam irradiates to obtain sample X3.
4 composite heat conducting material X4 of embodiment
It keeps step same as Example 1 to obtain molding material piece, material piece is passed through to the electronics of 200kGy dosage
Beam irradiates to obtain sample X4.
5 composite heat conducting material X5 of embodiment
The mixing material for forming composite heat conducting material X5 includes LG-SP980 resin: 100g；Aluminium oxide: 20g；Silane is even
Join agent: 0.4g；White carbon black: 2g.Irradiation dose is 100kGy, and radiation mode is electron irradiation.
The preparation method of composite heat conducting material X5 includes: to weigh 180g ethyl alcohol, 60g distilled water, 0.4g silane idol respectively
Join agent (KH550), 20g aluminium oxide and 2g white carbon black.Ethyl alcohol, distilled water and silane coupling agent (KH550) is ultrasonic in flask
30min hydrolyzed silane coupling agent.Open mill temperature is set as 140 DEG C, preliminary roller revolving speed is 24r/min, and back roller revolving speed is 17r/
Min weighs LG-SP980 resin 100g and is placed in mill 3min in open mill, and aluminium oxide and white carbon black is added, and mill 2min is cut again
Bottom sheet.Obtained piece is taped against in steel plate mold (60mm × 120mm × 2mm), is put into 150 DEG C of vulcanizing press and is preheated
Then 2min is maintained at pressure 11MPa and temperature the hot pressing 3min at 160 DEG C, then is cold-pressed 2min, obtain molding material piece.
By molding material piece, sample X5 is obtained by the electron beam irradiation of 100kGy dosage.
6 composite heat conducting material X6 of embodiment
The mixing material for forming composite heat conducting material X6 includes LG-SP980 resin: 100g；Aluminium oxide: 100g；Silane
Coupling agent: 1.6g；White carbon black: 8g.Irradiation dose is 100kGy, and radiation mode is electron irradiation.
The preparation method of composite heat conducting material X6 includes: to weigh 180g ethyl alcohol, 60g distilled water, 1.6g silane idol respectively
Join agent (amine propyl-triethoxysilicane), 100g aluminium oxide and 8g white carbon black.By ethyl alcohol, distilled water and silane coupling agent (amine third
Ethyl triethoxy silicane alkane) the ultrasound 30min hydrolyzed silane coupling agent in flask.Open mill temperature is set as 140 DEG C, preliminary roller revolving speed
For 24r/min, back roller revolving speed is 17r/min, weighs LG-SP980 resin 100g and is placed in mill 3min in open mill, oxidation is added
Mill 2min cuts bottom sheet again for aluminium and white carbon black.Obtained piece is taped against in steel plate mold (60mm × 120mm × 2mm), is put into 150
DEG C vulcanizing press in preheat 2min, be then maintained at pressure 11MPa and temperature the hot pressing 3min at 160 DEG C, then be cold-pressed
2min obtains molding material piece.By molding material piece, sample X6 is obtained by the electron beam irradiation of 100kGy dosage.
1 Heat Conduction Material Y1 of comparative example
The Heat Conduction Material is by LG-SP980 resin: 100g, aluminium oxide: 20g and silane coupling agent: 0.4g mixed smelting and
At.Specifically preparation method includes:
Resin, aluminium oxide and silane coupling agent are quantitatively weighed respectively, carry out the coupling of aluminium oxide, the melting of mixing material
With print sample preparation.Wherein the coupling process of heat filling, fusion process and sample making course are identical as Examples 1 to 4, are finally made
Heat Conduction Material print Y1.
2 Heat Conduction Material Y2 of comparative example
The Heat Conduction Material is by LG-SP980 resin: 100g, aluminium oxide: 20g and silane coupling agent: 0.4g and white carbon black: 2g
Mixed smelting forms.Specifically preparation method includes:
Quantitative LG-SP980 resin, aluminium oxide and silane coupling agent are weighed respectively, carry out coupling, the mixing material of aluminium oxide
The melting and print sample preparation of material.Wherein the coupling process of heat filling, fusion process and sample making course and Examples 1 to 4 and
Comparative example 1 is identical, and Heat Conduction Material print Y2 is finally made.
Above-described embodiment and the print of comparative example are subjected to heating conduction and Mechanics Performance Testing, concrete outcome such as 1 institute of table
Show.
Table 1: the performance data comparison of all kinds of Heat Conduction Materials
By upper table it is found that gel, the capacity of heat transmission and mechanicalness is not present in irradiated Heat Conduction Material Y1 and Y2
It can be far below the composite heat conducting material by irradiation.100kGy dosage, the composite heat-conducting of different ratio are similarly in irradiation
Its heating conduction of material and mechanical performance have differences, and the comprehensive performance of composite heat conducting material X2 is better than composite heat conducting material X5
With composite heat conducting material X6.Under conditions of fixed mixing ratio, irradiation dose is the composite heat conducting material X2 of 100kGy and 190kGy
Performance with composite heat conducting material X3 will be due to composite heat conducting material X1 and composite heat conducting material X3.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of the claim
Subject to enclosing.
Claims (10)
1. composite heat conducting material, which is characterized in that the composite heat conducting material by mixing material be irradiated it is cross-linking modified be made, institute
State the composition that mixing material includes following mass fraction: 20~100 parts by weight of heat filling；Polyvinyl resin 100
Parts by weight；0.4~1.6 parts by weight of coupling agent；2~8 parts by weight of White Carbon black.
2. composite heat conducting material as described in claim 1, which is characterized in that the mixing material includes following mass fraction
Composition:
40~60 parts by weight of heat filling；100 parts by weight of polyvinyl resin；0.8~1.2 parts by weight of coupling agent；White carbon
Black 4~6 parts by weight.
3. composite heat conducting material as described in claim 1, which is characterized in that
Irradiation dose is 600~200kGy, preferably 100~190kGy.
4. composite heat conducting material as described in claim 1, which is characterized in that
The white carbon black is Fumed silica.
5. composite heat conducting material as described in claim 1, which is characterized in that
The heat filling includes the one or more of filler in metal, ceramic-like filler and carbons filler；
The polyvinyl resin includes high density polyethylene (HDPE), medium density polyethylene, low density polyethylene (LDPE) and linear low density polyethylene
One or more of alkene etc.；Preferably low density polyethylene (LDPE) LG-SP980；
The coupling agent includes vinyltriethoxysilane, ethylenediaminepropyltriethoxysilane, dredges propyl trimethoxy silicon
Alkane, ethylenediamine hydroxypropyl methyl dimethoxysilane, amine propyl-triethoxysilicane, KH-550 series, methacryloxy third
Base trimethoxy silane, glycidyl ether oxypropyltrimethoxysilane, dimerization di (isooctyl) phosphate, magnesium stearate and metatitanic acid
One or more of ester coupling agent, preferably KH-550.
6. composite heat conducting material as claimed in claim 5, which is characterized in that
The partial size of the heat filling is 25 μm；The polyvinyl resin is preferably low density polyethylene (LDPE) LG-SP980；The idol
Joining agent is preferably KH-550.
7. composite heat conducting material as described in claim 1, which is characterized in that
The mode of the irradiation includes radioactive cobalt x ray irradiation x and electron accelerator irradiation.
8. the preparation method of the composite heat conducting material as described in claim 1~7 is any, which comprises the following steps:
The heat filling of fixed mixing ratio is mixed with coupling agent, obtains the heat filling of coupling processing；
By polyvinyl resin in 140 DEG C of mills, heat filling and white carbon black after the coupling processing of fixed mixing ratio is then added exist
140 DEG C of mixings, cut bottom sheet, obtain mixing material tablet；
Mixing material material piece is irradiated crosslinking, the composite heat conducting material is made.
9. the preparation method of composite heat conducting material as claimed in claim 8, which is characterized in that
Irradiation dose is 600~200kGy, preferably 100~190kGy.
10. application of the composite heat conducting material in electric heating equipment as described in claim 1~7 is any.
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