CN109233869A - A kind of preparation method of the high fire-retardance high thermal conductivity composite particles based on magnesium hydroxide - Google Patents
A kind of preparation method of the high fire-retardance high thermal conductivity composite particles based on magnesium hydroxide Download PDFInfo
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- CN109233869A CN109233869A CN201810901673.2A CN201810901673A CN109233869A CN 109233869 A CN109233869 A CN 109233869A CN 201810901673 A CN201810901673 A CN 201810901673A CN 109233869 A CN109233869 A CN 109233869A
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- C09K21/00—Fireproofing materials
- C09K21/02—Inorganic materials
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- 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
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- C09K5/14—Solid materials, e.g. powdery or granular
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Abstract
The preparation method of the invention discloses a kind of high fire-retardance high thermal conductivity composite particles based on magnesium hydroxide.The composite material reaches V-0 grades without any halogen or non-environmental protection heavy metal fire retardant, flame retardant rating, while having good heating conduction, and thermal coefficient is greater than 0.5W/m. DEG C.The means that flake magnesium hydroxide slurry and graphene microchip pass through grinding in the liquid phase are pre-mixed, the mixed slurry of magnesium hydroxide and graphene microchip inter-embedding type is formed, then this inter-embedding type structure is converted into using temperature and gravity by spherical composite spherical powder by spray drying process.The stable preparation process, high yield rate, wide adaptation range are suitable for mass production.The present invention is used directly for the radiators such as LED, electric appliance and electronic component, is dispersed into heat in colder environment, reduces the running temperature of electronic device.
Description
Technical field
The invention belongs to the preparation technical fields of functional material, concretely relate to a kind of high resistant based on magnesium hydroxide
Fire the preparation method of high thermal conductivity composite particles.
Background technique
Magnesium hydroxide is a kind of inorganic fire-retarded filler of polymer composites materials that application prospect is good.With aluminium hydroxide one
Sample, flame retardant of magnesium hydroxide by it is heated when chemical breakdown absorb heat and release is discharged and plays fire retardation, therefore have
The advantages that magnesia chemical property generated after nontoxic, low cigarette and decomposition is stablized, is not generated secondary pollution.It is widely used in rubber
In the high molecular materials such as glue, chemical industry, building materials, plastics and electronics, unsaturated polyester (UP) and paint, coating.Especially to mining wind-guiding
Cylinder coated cloth, the whole core conveyer belt of PVC, flame-retardant aluminum plastic plate, fire-retardant tarpaulin, PVC cable material, mine cable sheath, cable are attached
The fire-retardant of part, smoke elimination are antistatic, can replace aluminium hydroxide, have excellent flame retardant effect.
Rapid development and System with the high frequency of electronic device, high speed and integrated circuit technique) Mechanical
(overall power density of the progress of Micro technology, electronic component increases substantially and physical size Electronical MEMS
Smaller and smaller, heat flow density is consequently increased, so the temperature environment of high temperature certainly will will affect the performance of electronic component, this
It requires also to carry out more efficient thermal control to it while engineering plastics have high-level flame-retarding characteristic.Therefore, it opens
Send out a kind of low cost, high fire-retardance at the same have High-heat-conductiviinsulation insulation material have huge commercial value.
The present invention improves the thermal conduction characteristic for the spheric granules that flake magnesium hydroxide is assembled into using graphene microchip, exploitation
A kind of lower cost, while the composite particles of high fire-retardance high thermal conductivity are had both, which is halogen-free and antimony class compound.
The stable preparation process, high yield rate, wide adaptation range are suitable for mass production.The present invention is used directly for LED, electric appliance
And the radiators such as electronic component, it is dispersed into heat in colder environment, reduces the running temperature of electronic device.
Summary of the invention
It is an object of the invention to overcome prior art preparation low cost to have both high fire-retardance high heat conducting nano composite material
Problem provides a kind of preparation method of high fire-retardance high thermal conductivity composite particles based on magnesium hydroxide.
To reach above-mentioned expected purpose, the present invention adopts the following technical scheme:
A kind of preparation method of the high fire-retardance high thermal conductivity composite particles based on magnesium hydroxide, which is characterized in that use sheet hydrogen-oxygen
The means that change magnesium slurry and graphene microchip pass through grinding in the liquid phase are pre-mixed, and magnesium hydroxide and graphene microchip are formed
The mixed slurry of inter-embedding type, then using temperature and gravity be converted into this inter-embedding type structure by spray drying process spherical
Composite spherical powder.The technique includes the following steps:
A. nano-sheet magnesium hydroxide material powder, dispersing aid and water are formed into weighing according to a certain percentage, are uniformly mixed；
B. graphene microchip is slowly added into the mixed solution of step a according to a certain percentage, is uniformly mixed；
C. the solution of step b after mixing is put into progress low temperature liquid phase ball milling in ball grinder or sand mill, and ball-milling medium is height
The stable zirconia ceramics ball of purity yttria, wet-milling mixing 2 ~ 40 hours, the magnesium hydroxide and graphene being uniformly mixed
The mixed slurry of microplate inter-embedding type；
D. the mixed slurry of magnesium hydroxide made from step c and graphene microchip inter-embedding type is spray-dried, controls drying
Diameter of particle afterwards, obtain good fluidity, having a size of 50 ~ 100 μm of composite particles to get arrive the compound hydrogen of high fire-retardance high thermal conductivity
Magnesium oxide particle.
The dispersing aid is air chemical industry ZetaSperse3100/3700, Rhodia Rhodoline 111, Digao
One of TEGO Dispers 752W.
The nano-sheet magnesium hydroxide material powder, dispersing aid, graphene microchip and water mass ratio be 0.1
~ 0.8:0.01 ~ 0.2:0.01 ~ 0.1:1.
The low temperature liquid phase ball milling temperature is 0 ~ 10 DEG C, and the ball-milling medium size is 0.8mm or 0.4mm.
The temperature of the spray drying is 180 ~ 300 DEG C.
Beneficial effects of the present invention:
Hydroxide/magnesium-based high fire-retardance high thermal conductivity composite particles produced by the present invention high, at low cost, thermal coefficient with flame retardant rating
It the features such as good, can be used for the temperature control of electronic device, and guarantee the stability and reliability of its work.Preparation process of the present invention
Stabilization, high yield rate, wide adaptation range are suitable for mass production.
Detailed description of the invention
The SEM of Fig. 1 case study on implementation sample 1 schemes.
Specific embodiment
With reference to the accompanying drawings and examples, further description of the specific embodiments of the present invention.Following embodiment is only
For clearly illustrating technical solution of the present invention, and not intended to limit the protection scope of the present invention.
Embodiment:
The present invention is described in detail below by specific example, but protection scope of the present invention is not only restricted to these implementations
Example.
Embodiment 1: by nano-sheet magnesium hydroxide material powder, dispersing aid air chemical industry ZetaSperse3100 and water
It weighs, is uniformly mixed according to mass ratio 0.1:0.01:1；Graphene microchip and water are slowly added to according to the mass ratio of 0.01:1
Into above-mentioned mixed solution, it is uniformly mixed；Solution after mixing is put into 10 DEG C of low temperature liquid phase ball millings of progress in ball grinder,
The ball-milling medium zirconia ceramics ball stable for 0.8mm high purity yttria, wet-milling mixing 2 hours, the hydrogen being uniformly mixed
The mixed slurry of magnesia and graphene microchip inter-embedding type；By the mixing slurry of magnesium hydroxide obtained and graphene microchip inter-embedding type
Material carries out 180 DEG C of spray drying, the diameter of particle after control is dry, obtains good fluidity, having a size of compound of 50 ~ 100 μm
Grain to get arrive the compound magnesium hydroxide particle of high fire-retardance high thermal conductivity.
Embodiment 2: nano-sheet magnesium hydroxide material powder, dispersing aid Rhodia Rhodoline 111 are pressed with water
It weighs, is uniformly mixed according to mass ratio 0.4:0.1:1；Graphene microchip and water are slowly added into according to the mass ratio of 0.05:1
It states in mixed solution, is uniformly mixed；Solution after mixing is put into 5 DEG C of low temperature liquid phase ball millings of progress, ball milling in ball grinder
The medium zirconia ceramics ball stable for 0.4mm high purity yttria, wet-milling mixing 20 hours, the hydroxide being uniformly mixed
The mixed slurry of magnesium and graphene microchip inter-embedding type；By the mixed slurry of magnesium hydroxide obtained and graphene microchip inter-embedding type into
230 DEG C of row spray drying, the diameter of particle after control is dry obtain good fluidity, having a size of 50 ~ 100 μm of composite particles,
Obtain the compound magnesium hydroxide particle of high fire-retardance high thermal conductivity.
Embodiment 3: by nano-sheet magnesium hydroxide material powder, dispersing aid Digao TEGO Dispers 752W and water
It weighs, is uniformly mixed according to mass ratio 0.8:0.2:1；Graphene microchip and water are slowly added into according to the mass ratio of 0.1:1
In above-mentioned mixed solution, it is uniformly mixed；Solution after mixing is put into 0 DEG C of low temperature liquid phase ball milling of progress, ball in ball grinder
The grinding media zirconia ceramics ball stable for 0.4mm high purity yttria, wet-milling mixing 40 hours, the hydrogen-oxygen being uniformly mixed
Change the mixed slurry of magnesium and graphene microchip inter-embedding type；By the mixed slurry of magnesium hydroxide obtained and graphene microchip inter-embedding type
Carry out 300 DEG C of spray drying, the diameter of particle after control is dry obtains good fluidity, having a size of compound of 50 ~ 100 μm
Grain to get arrive the compound magnesium hydroxide particle of high fire-retardance high thermal conductivity.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improvements and modifications
Also it should be regarded as protection scope of the present invention.
Claims (5)
1. a kind of preparation method of the high fire-retardance high thermal conductivity composite particles based on magnesium hydroxide, which is characterized in that use sheet hydrogen
The means that magnesia slurry and graphene microchip pass through grinding in the liquid phase are pre-mixed, and form magnesium hydroxide and graphene is micro-
The mixed slurry of piece inter-embedding type, then this inter-embedding type structure is converted into using temperature and gravity by class ball by spray drying process
The composite spherical powder of shape, the technique include the following steps:
A. nano-sheet magnesium hydroxide material powder, dispersing aid and water are formed into weighing according to a certain percentage, are uniformly mixed；
B. graphene microchip is slowly added into the mixed solution of step a according to a certain percentage, is uniformly mixed；
C. the solution of step b after mixing is put into progress low temperature liquid phase ball milling in ball grinder or sand mill, and ball-milling medium is height
The stable zirconia ceramics ball of purity yttria, wet-milling mixing 2 ~ 40 hours, the magnesium hydroxide and graphene being uniformly mixed
The mixed slurry of microplate inter-embedding type；
D. the mixed slurry of magnesium hydroxide made from step c and graphene microchip inter-embedding type is spray-dried, controls drying
Diameter of particle afterwards, obtain good fluidity, having a size of 50 ~ 100 μm of composite particles to get arrive the compound hydrogen of high fire-retardance high thermal conductivity
Magnesium oxide particle.
2. a kind of preparation method of high fire-retardance high thermal conductivity composite particles based on magnesium hydroxide according to claim 1,
It is characterized in that, dispersing aid described in step a is air chemical industry ZetaSperse3100/3700, Rhodia Rhodoline
111, one of Digao TEGO Dispers 752W.
3. a kind of preparation method of high fire-retardance high thermal conductivity composite particles based on magnesium hydroxide according to claim 1,
It is characterized in that, nano-sheet magnesium hydroxide material powder described in step a and b, dispersing aid, graphene microchip and water
Mass ratio is 0.1 ~ 0.8:0.01 ~ 0.2:0.01 ~ 0.1:1.
4. a kind of preparation method of high fire-retardance high thermal conductivity composite particles based on magnesium hydroxide according to claim 1,
Be characterized in that, low temperature liquid phase ball milling temperature described in step c be 0 ~ 10 DEG C, the ball-milling medium size be 0.8mm or
0.4mm。
5. a kind of preparation method of high fire-retardance high thermal conductivity composite particles based on magnesium hydroxide according to claim 1,
It is characterized in that, the temperature of spray drying described in step d is 180 ~ 300 DEG C.
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Cited By (4)
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| CN109879302A (en) * | 2019-04-01 | 2019-06-14 | 东北大学 | Magnesium hydroxide/expansible graphite composite material method is prepared by raw material of magnesium carbonate mine |
| CN109972155A (en) * | 2019-04-01 | 2019-07-05 | 东北大学 | A kind of preparation method of aluminium hydroxide/expansible graphite composite material |
| CN110423379A (en) * | 2019-08-12 | 2019-11-08 | 哈尔滨理工大学 | A kind of magnesium hydroxide/graphene platelet composite flame-retardant agent and preparation method thereof |
| CN112574758A (en) * | 2020-12-28 | 2021-03-30 | 江苏聚千新材料科技有限公司 | Heat-conducting flame retardant and preparation process thereof |
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| CN109972155A (en) * | 2019-04-01 | 2019-07-05 | 东北大学 | A kind of preparation method of aluminium hydroxide/expansible graphite composite material |
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| CN110423379A (en) * | 2019-08-12 | 2019-11-08 | 哈尔滨理工大学 | A kind of magnesium hydroxide/graphene platelet composite flame-retardant agent and preparation method thereof |
| CN110423379B (en) * | 2019-08-12 | 2021-05-07 | 哈尔滨理工大学 | Magnesium hydroxide/graphene sheet composite flame retardant and preparation method thereof |
| CN112574758A (en) * | 2020-12-28 | 2021-03-30 | 江苏聚千新材料科技有限公司 | Heat-conducting flame retardant and preparation process thereof |
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Application publication date: 20190118 |