CN106243387B - A kind of heat conductive flame-retarding agent and preparation method thereof - Google Patents
A kind of heat conductive flame-retarding agent and preparation method thereof Download PDFInfo
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- CN106243387B CN106243387B CN201610654792.3A CN201610654792A CN106243387B CN 106243387 B CN106243387 B CN 106243387B CN 201610654792 A CN201610654792 A CN 201610654792A CN 106243387 B CN106243387 B CN 106243387B
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
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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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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
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Abstract
The present invention provides a kind of preparation method of heat conductive flame-retarding agent, it includes the following steps: that (a) weighs main material, auxiliary material and the first auxiliary agent, and the main material, auxiliary material and the first auxiliary agent are mixed to get precast body at a temperature of first, wherein the main material includes spherical magnesium hydroxide and fibrous structure, and the mass ratio of spherical magnesium hydroxide and fibrous structure is 5:1~20:1；(b) precast body is modified under second temperature and is dried to obtain the heat conductive flame-retarding agent by the second auxiliary agent.The present invention also provides a kind of heat conductive flame-retarding agent.
Description
Technical field
The present invention relates to flame retardant effect magnesium hydroxide field of material technology more particularly to a kind of heat conductive flame-retarding agent and
Preparation method.
Background technique
Fire retardant is widely used in articles for daily use.Fire retardant is divided into halogen containing flame-retardant and halogen-free flame retardants.It is halogen fire-retardant
Material can generate a large amount of smog and toxic corrosive hydrogen halides gas during fire-retardant, cause into secondary hazards, thus
It is gradually disabled.Halogen-free flame retardants is mainly based on phosphorus series compound and metal hydroxides.Wherein magnesium hydroxide is a kind of new
Type filled-type fire retardant, releases when by being thermally decomposed in conjunction with water, absorbs a large amount of latent heat, to reduce the synthesis that it is filled
Surface temperature of the material in flame has the function of that polymer is inhibited to decompose and carry out cooling to generated fuel gas.
However, current fire retardant only have the effect of it is fire-retardant, when by fire retardant addition polymeric substrate thermally conductive modeling is made
When material, it tends to be difficult to while having both thermally conductive performance, and can not brimful preceding heat-conducting plastic field to thermally conductive with fire-retardant dual requirements.
Summary of the invention
In view of the above-mentioned problems, the purpose of the present invention is to provide it is a kind of have both thermally conductive and flame retardant effect heat conductive flame-retarding agent and
Preparation method, to solve the problems of the prior art.
The present invention provides a kind of preparation method of heat conductive flame-retarding agent comprising following steps:
(a) main material, auxiliary material and the first auxiliary agent are weighed, and the main material, auxiliary material and the first auxiliary agent are mixed at a temperature of first
Precast body is obtained, wherein the main material includes spherical magnesium hydroxide and fibrous structure, spherical magnesium hydroxide and fibrous structure
Mass ratio be 5:1~20:1；
(b) precast body is modified under second temperature and is dried to obtain the heat conductive flame-retarding by the second auxiliary agent
Agent.
Preferably, fibrous structure described in step (a) is acicular magnesium hydroxide, in glass fibre, fibrous wollastonite
One or more, the auxiliary material be one of glass fibre, wollastonite, aluminium oxide, silicon carbide, silicon nitride, aluminium nitride
Or it is a variety of, first auxiliary agent is vinyl silanes, amino silane, epoxy radicals silicone hydride, acyloxy silane, polysiloxanes, hard
One or more of resin acid, magnesium stearate, zinc stearate, Aluminate, titanate esters.
Preferably, the mass ratio of main material described in step (a) and auxiliary material is (85~95): (5~15), described first helps
The quality of agent is the 0.2%~2% of the gross mass of the main material and auxiliary material.
Preferably, the first temperature described in step (a) is 70 degrees Celsius~85 degrees Celsius.
Preferably, the second auxiliary agent described in step (b) is vinyl silanes, amino silane, epoxy radicals silicone hydride, acyloxy silicon
One or more of alkane, polysiloxanes, stearic acid, magnesium stearate, zinc stearate, Aluminate, titanate esters.
Preferably, the quality of step (b) second auxiliary agent is the 0.5%~5% of the gross mass of the main material and auxiliary material.
Preferably, step (b) second temperature is 85 degrees Celsius~110 degrees Celsius.
The present invention also provides a kind of heat conductive flame-retarding agent obtained using above-mentioned preparation method, the heat conductive flame-retarding agent includes more
A spherical particle and multiple fibrous structures, multiple fibrous structure be uniformly distributed between multiple spherical particles and with phase
Adjacent spherical particle overlap joint, the partial size of the spherical particle are 2 microns~60 microns.
Compared to the prior art, this preparation method has the advantage that first, fine by being added in spherical magnesium hydroxide
Shape structure is tieed up, fibrous structure can be dispersed in spherical magnesium hydroxide in the pinball composite heat-conducting system for formation of arranging in pairs or groups,
Fibrous structure can play the role of connection, be conducive to heat and conduct, thus the heat conductive flame-retarding agent has good heat-conducting effect；The
Two, by sequentially adding the first auxiliary agent, the second auxiliary agent, first auxiliary agent and the second auxiliary agent major ingredient can be carried out surface treatment and
It is modified, it may make magnesium hydroxide major ingredient that there is preferable compatibility, the heat conductive flame-retarding agent because obtained from is easy to mixed with plastic resin
Material.
Major ingredient magnesium hydroxide has perfect microcosmic crystalline structure in the obtained heat conductive flame-retarding agent, and feeding is not built bridge, easily
In with plastic resin mixing.When the heat conductive flame-retarding agent and resin are mixed with heat-conducting plastic, the heat conductive flame-retarding agent and plastics
Resin compatible is good, thoroughly solves the disadvantage that magnesium hydroxide feeding hardly possible, bad dispersibility.The experiment proved that the heat conductive flame-retarding
When the heat-conducting plastic that the weight ratio 50% that agent is added in Heat Conduction Material can reach V0 grades, and obtain is lighted smog it is small, without gas
Taste, anti-dripping melt.
The heat conductive flame-retarding agent material is nontoxic, low VOC, and Material Manufacturing Process is without waste water, exhaust gas, the discharge of waste liquid.
Detailed description of the invention
Fig. 1 and Fig. 2 is the stereoscan photograph of the different amplification of heat conductive flame-retarding agent prepared by the embodiment of the present invention 1.
Specific embodiment
The technical solution in embodiment of the present invention will be clearly and completely described below, it is clear that described reality
The mode of applying is only some embodiments of the invention, rather than whole embodiments.Based on the embodiment in the present invention,
All other embodiment obtained by those of ordinary skill in the art without making creative efforts belongs to this
Invent the range of protection.
The present invention provides a kind of preparation methods of heat conductive flame-retarding agent comprising following steps:
(a) main material, auxiliary material and the first auxiliary agent are weighed, and the main material, auxiliary material and the first auxiliary agent are mixed at a temperature of first
Precast body is obtained, wherein the main material includes spherical magnesium hydroxide and fibrous structure, spherical magnesium hydroxide and fibrous structure
Mass ratio be 5:1~20:1；
(b) precast body is mixed under second temperature with the second auxiliary agent and is dried to obtain the heat conductive flame-retarding agent.
In step (a), the purpose that fibrous structure is introduced in the main material is that this is special using fibrous structure
Structure and overlapped between multiple spherical magnesium hydroxides, formed the thermally conductive system of pinball, with preferable heat-conducting effect.
The fibrous structure is one or more of acicular magnesium hydroxide, glass fibre, fibrous wollastonite.In order to realize more
The mass ratio of good heat-conducting effect, the spherical magnesium hydroxide and fibrous structure is preferably 10:1~20:1.
The adding purpose of the auxiliary material is to improve heating conduction.The auxiliary material is glass fibre, wollastonite, aluminium oxide, carbon
One or more of SiClx, silicon nitride, aluminium nitride.The adding purpose of first auxiliary agent is to improve its flame retardant property.Institute
Stating the first auxiliary agent is vinyl silanes, amino silane, epoxy radicals silicone hydride, acyloxy silane, polysiloxanes, stearic acid, stearic acid
One or more of magnesium, zinc stearate, Aluminate, titanate esters, preferably polysiloxanes.
The mass ratio of the main material and auxiliary material is (85~95): (5~15).Preferably, in order to make auxiliary material be filled in master
Between material chondritic, conduction heat more efficiently further increases heat-conducting effect, the mass ratio of the main material and auxiliary material
For (85~90): (10~15).
The quality of first auxiliary agent is the 0.2%~2% of the gross mass of the main material and auxiliary material.Preferably, for reality
Now better surface treatment effect, the quality of first auxiliary agent are the 0.2%~1% of the gross mass of the main material and auxiliary material.
First temperature is 70 degrees Celsius~85 degrees Celsius.
In step (b), the adding purpose of second auxiliary agent is to be modified to the surface of main material and auxiliary material, makes it
Its compatibility is improved when mixing with plastic resin.Second auxiliary agent is vinyl silanes, amino silane, epoxy radicals silicone hydride, acyl
One or more of oxysilane, polysiloxanes, stearic acid, magnesium stearate, zinc stearate, Aluminate, titanate esters, preferably
For silane material.
The quality of second auxiliary agent is the 0.5%~5% of the gross mass of the main material and auxiliary material.Preferably, for reality
Now better compatibility effect, the quality of second auxiliary agent are the 0.5%~1% of the gross mass of the main material and auxiliary material.
The second temperature is 85 degrees Celsius~110 degrees Celsius.
The present invention also provides a kind of heat conductive flame-retarding agent obtained using above-mentioned preparation method.Fig. 1 and Fig. 2 is please referred to, it is described
Heat conductive flame-retarding agent includes multiple spherical particles and multiple fibrous structures, and multiple fibrous structure is uniformly distributed in multiple balls
It is overlapped between shape particle and with adjacent spherical particle.The main component of the spherical particle is spherical magnesium hydroxide.The needle
The main component of shape structure is one or more of acicular magnesium hydroxide, glass fibre, fibrous wollastonite.In preparation
In the process, the surface of spherical magnesium hydroxide and fibrous structure attachment auxiliary material, the first auxiliary agent and the second auxiliary agent, final each component are tight
It is close to be combined together.
The partial size of the spherical particle is 2 microns~60 microns.
Compared to the prior art, this preparation method has the advantage that first, fine by being added in spherical magnesium hydroxide
Shape structure is tieed up, fibrous structure can be dispersed in spherical magnesium hydroxide in the pinball composite heat-conducting system for formation of arranging in pairs or groups,
Fibrous structure can play the role of connection, be conducive to heat and conduct, thus the heat conductive flame-retarding agent has good heat-conducting effect；The
Two, by sequentially adding the first auxiliary agent, the second auxiliary agent, first auxiliary agent and the second auxiliary agent major ingredient can be carried out surface treatment and
It is modified, it may make magnesium hydroxide major ingredient that there is preferable compatibility, the heat conductive flame-retarding agent because obtained from is easy to mixed with plastic resin
Material.
Major ingredient magnesium hydroxide has perfect microcosmic crystalline structure in the obtained heat conductive flame-retarding agent, and feeding is not built bridge, easily
In with plastic resin mixing.When the heat conductive flame-retarding agent and resin are mixed with heat-conducting plastic, the heat conductive flame-retarding agent and plastics
Resin compatible is good, thoroughly solves the disadvantage that magnesium hydroxide feeding hardly possible, bad dispersibility.The experiment proved that the heat conductive flame-retarding
When the heat-conducting plastic that the weight ratio 50% that agent is added in Heat Conduction Material can reach V0 grades, and obtain is lighted smog it is small, without gas
Taste, anti-dripping melt.
Heat conductive flame-retarding agent and preparation method thereof of the invention is illustrated combined with specific embodiments below:
Embodiment 1:
Weigh main material, auxiliary material and the first auxiliary agent, and by the main material, auxiliary material and the first auxiliary agent under about 80 degrees Celsius in height
Fast stirrer for mixing obtains precast body, wherein the main material includes spherical magnesium hydroxide and acicular magnesium hydroxide, spherical hydrogen-oxygen
The mass ratio for changing magnesium and acicular magnesium hydroxide is 20:1, and auxiliary material is wollastonite, and the first auxiliary agent is polysiloxanes, the main material with it is auxiliary
The mass ratio of material is 85:15, and the quality of first auxiliary agent is the 5% of the gross mass of the main material and auxiliary material.
The precast body is mixed under about 115 degrees Celsius with the second auxiliary agent and is dried to obtain the heat conductive flame-retarding agent.
Wherein, the second auxiliary agent is vinyl silanes, and the quality of second auxiliary agent is the 5% of the gross mass of the main material and auxiliary material.
Obtained heat conductive flame-retarding agent is scanned Electronic Speculum test.It please refers to, 1 and Fig. 2, by Fig. 1 and Fig. 2 as it can be seen that this is more
A acicular texture is uniformly distributed between multiple spherical particles and overlaps with adjacent spherical particle, the partial size of the spherical particle
It is 2 microns~60 microns.
The heat conductive flame-retarding agent that this is obtained is applied in heat-conducting plastic, and is carried out pair with commercially available conventional magnesium hydroxide simultaneously
Ratio 1.Formula such as the following table 1.
Table 1
| Embodiment 1 | Comparative example 1 | |
| PA6 resin | 35.8 | 35.8 |
| Heat conductive flame-retarding agent | 51.6 | --- |
| Conventional magnesium hydroxide | --- | 51.6 |
| Other auxiliary agents | 6.6 | 6.6 |
| Filler | 6 | 6 |
In table 1, other auxiliary agents include lubricant (ethylene paraffin or stearic acid) and toughener (POE elastomer or grafting
POE), opacifier titanium dioxide；Filler is magnesia, aluminium oxide and silicon carbide.
The heat-conducting plastic that above-mentioned table 1 obtains is tested for the property, the results are shown in Table 2.
Table 2
As can be seen from Table 2, for the heat-conducting plastic made of the commercially available conventional magnesium hydroxide, 1 heat conductive flame-retarding of the present embodiment
The heating conduction of heat-conducting plastic made of agent is greatly improved, while influencing on other physical properties little.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (6)
1. a kind of preparation method of heat conductive flame-retarding agent comprising following steps:
(a) main material, auxiliary material and the first auxiliary agent are weighed, and the main material, auxiliary material and the first auxiliary agent are mixed to get at a temperature of first
Precast body, wherein the main material includes spherical magnesium hydroxide and fibrous structure, the matter of spherical magnesium hydroxide and fibrous structure
For amount than being 5:1~20:1, the auxiliary material is one or more of aluminium oxide, silicon carbide, silicon nitride, aluminium nitride, described the
One auxiliary agent is vinyl silanes, amino silane, epoxy radicals silicone hydride, acyloxy silane, polysiloxanes, stearic acid, magnesium stearate, hard
The mass ratio of one or more of resin acid zinc, Aluminate, titanate esters, the main material and auxiliary material is (85~95): (5~
15), the fibrous structure is one or more of acicular magnesium hydroxide, glass fibre, fibrous wollastonite；
(b) the heat conductive flame-retarding agent is modified and is dried to obtain under second temperature to the precast body by the second auxiliary agent,
Wherein, second auxiliary agent be vinyl silanes, amino silane, epoxy radicals silicone hydride, acyloxy silane, polysiloxanes, stearic acid,
One or more of magnesium stearate, zinc stearate, Aluminate, titanate esters, the heat conductive flame-retarding agent include multiple spherical
Grain and multiple fibrous structures, multiple fibrous structure be uniformly distributed between multiple spherical particles and with it is adjacent spherical
Particle overlap joint.
2. a kind of preparation method of heat conductive flame-retarding agent as described in claim 1, which is characterized in that first described in step (a)
The quality of auxiliary agent is the 0.2%~2% of the gross mass of the main material and auxiliary material.
3. a kind of preparation method of heat conductive flame-retarding agent as described in claim 1, which is characterized in that first described in step (a)
Temperature is 70 degrees Celsius~85 degrees Celsius.
4. a kind of preparation method of heat conductive flame-retarding agent as described in claim 1, which is characterized in that step (b) described second helps
The quality of agent is the 0.5%~5% of the gross mass of the main material and auxiliary material.
5. a kind of preparation method of heat conductive flame-retarding agent as described in claim 1, which is characterized in that step (b) second temperature
Degree is 85 degrees Celsius~110 degrees Celsius.
6. a kind of using the heat conductive flame-retarding agent obtained such as any one of claim 1 to 5 preparation method, which is characterized in that described to lead
Hot fire retardant includes multiple spherical particles and multiple fibrous structures, and multiple fibrous structure is uniformly distributed in multiple spherical
It is overlapped between particle and with adjacent spherical particle, the partial size of the spherical particle is 2 microns~60 microns.
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| CN113674926B (en) * | 2021-08-13 | 2023-08-25 | 江苏中利集团股份有限公司 | Method for producing charging pile cable by using composite flame retardant and charging pile cable |
| CN113914113A (en) * | 2021-11-15 | 2022-01-11 | 浙江亦阳新材料有限公司 | Environment-friendly shading high-waterproof canopy material and preparation method thereof |
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| US5482985A (en) * | 1993-03-11 | 1996-01-09 | Basf Aktiengesellschaft | Halogen-free flameproofed thermoplastic polyamide molding materials |
| CN101343402A (en) * | 2008-08-27 | 2009-01-14 | 南亚塑胶工业股份有限公司 | Resin composition with high-heat, high-glass transition temperature for printed circuit board, prepreg and coating substance |
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