CN106243387A - 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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- 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
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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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K7/00—Use of ingredients characterised by shape
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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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- 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
- 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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- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The present invention provides the preparation method of a kind of heat conductive flame-retarding agent, it comprises the steps: that (a) weighs main material, auxiliary material and the first auxiliary agent, and this main material, auxiliary material and the first auxiliary agent are mixed to get precast body at a temperature of first, wherein said main material includes that spherical magnesium hydroxide and filamentary structure, spherical magnesium hydroxide are 5:1～20:1 with the mass ratio of filamentary structure；B described precast body is modified at a temperature of second by the second auxiliary agent and is dried to obtain described heat conductive flame-retarding agent by ().The present invention also provides for a kind of heat conductive flame-retarding agent.
Description
Technical field
The present invention relates to the magnesium hydroxide field of material technology with flame retardant effect, particularly relate to a kind of heat conductive flame-retarding agent and
Its preparation method.
Background technology
Fire retardant is widely used in articles for daily use.Fire retardant is divided into halogen containing flame-retardant and halogen-free flame retardants.Halogen is fire-retardant
Material can produce substantial amounts of smog and poisonous corrosive hydrogen halides gas during fire-retardant, causes into secondary harm, thus
The most 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, discharges during by decomposes and combines water, absorb substantial amounts of latent heat, reduce the synthesis that it is filled
Material surface temperature in flame, has the effect that suppression polymer decomposes and cools down produced fuel gas.
But, current fire retardant only has fire-retardant effect, makes heat conduction mould when fire retardant adds polymeric substrate
During material, it tends to be difficult to have the performance of heat conduction concurrently simultaneously, and cannot brimful front heat-conducting plastic field to heat conduction and fire-retardant dual requirements.
Summary of the invention
For the problems referred to above, it is an object of the invention to provide a kind of heat conductive flame-retarding agent having heat conduction and flame retardant effect concurrently and
Its preparation method, to solve the problems of the prior art.
The present invention provides the preparation method of a kind of heat conductive flame-retarding agent, and it comprises the steps:
A () weighs main material, auxiliary material and the first auxiliary agent, and this main material, auxiliary material and the first auxiliary agent are mixed at a temperature of first
Obtaining precast body, wherein said main material includes spherical magnesium hydroxide and filamentary structure, spherical magnesium hydroxide and filamentary structure
Mass ratio be 5:1～20:1；
B described precast body is modified at a temperature of second by the second auxiliary agent and is dried to obtain described heat conductive flame-retarding by ()
Agent.
Preferably, during described in step (a), filamentary structure is acicular magnesium hydroxide, glass fibre, fibrous wollastonite
One or more, described auxiliary material is the one in glass fibre, wollastonite, aluminium oxide, carborundum, silicon nitride, aluminium nitride
Or multiple, described first auxiliary agent is vinyl silanes, amino silane, epoxy radicals silicone hydride, acyloxy silane, polysiloxanes, hard
One or more in fat acid, magnesium stearate, zinc stearate, Aluminate, titanate esters.
Preferably, main material described in step (a) is (85～95) with the mass ratio of auxiliary material: (5～15), described first helps
The quality of agent is the 0.2%～2% of the described main material gross mass with 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 in alkane, polysiloxanes, stearic acid, magnesium stearate, zinc stearate, Aluminate, titanate esters.
Preferably, the quality of described second auxiliary agent of step (b) is the 0.5%～5% of the described main material gross mass with auxiliary material.
Preferably, described second temperature of step (b) is 85 degrees Celsius～110 degrees Celsius.
The present invention also provides for a kind of heat conductive flame-retarding agent using above-mentioned preparation method to obtain, and described heat conductive flame-retarding agent includes many
Individual spherical particle and multiple filamentary structure, the plurality of filamentary structure be uniformly distributed between multiple spherical particle and with phase
Adjacent spherical particle overlap joint, the particle diameter of described spherical particle is 2 microns～60 microns.
Compared to prior art, this preparation method has the advantage that first, by adding fibre in spherical magnesium hydroxide
Dimension shape structure, in the pinball composite heat-conducting system that collocation is formed, filamentary structure can be dispersed in spherical magnesium hydroxide,
Filamentary structure can play the effect of connection, beneficially heat conduction, thus this heat conductive flame-retarding agent has good heat-conducting effect；The
Two, by being sequentially added into the first auxiliary agent, the second auxiliary agent, this first auxiliary agent and the second auxiliary agent major ingredient can be carried out surface process and
Modification, can make magnesium hydroxide major ingredient have the preferable compatibility, thus the heat conductive flame-retarding agent obtained is prone to mix with plastic resin
Material.
In the heat conductive flame-retarding agent that this obtains, major ingredient magnesium hydroxide has perfect microcosmic crystalline structure, and feeding is not built bridge, easily
In with plastic resin batch mixing.When this heat conductive flame-retarding agent is prepared heat-conducting plastic with mixed with resin, these heat conductive flame-retarding agent and plastics
Resin compatible is good, thoroughly solves magnesium hydroxide feeding difficulty, the shortcoming of bad dispersibility.The experiment proved that, described heat conductive flame-retarding
The weight ratio 50% that agent is added in Heat Conduction Material i.e. can reach V0 level, and when the heat-conducting plastic obtained is lighted, smog is little, depletion of QI
Taste, anti-dripping melt.
This heat conductive flame-retarding agent material is nontoxic, low VOC, and Material Manufacturing Process is without waste water, waste gas, the discharge of waste liquid.
Accompanying drawing explanation
Fig. 1 and Fig. 2 is the stereoscan photograph of the different amplification of the heat conductive flame-retarding agent of the embodiment of the present invention 1 preparation.
Detailed description of the invention
Technical scheme in embodiment of the present invention will be clearly and completely described below, it is clear that described reality
The mode of executing is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention,
Other embodiments all that those of ordinary skill in the art are obtained under not making creative work premise, broadly fall into this
The scope of invention protection.
The invention provides the preparation method of a kind of heat conductive flame-retarding agent, it comprises the steps:
A () weighs main material, auxiliary material and the first auxiliary agent, and this main material, auxiliary material and the first auxiliary agent are mixed at a temperature of first
Obtaining precast body, wherein said main material includes spherical magnesium hydroxide and filamentary structure, spherical magnesium hydroxide and filamentary structure
Mass ratio be 5:1～20:1；
B described precast body and the second auxiliary agent are mixed at a temperature of second and are dried to obtain described heat conductive flame-retarding agent by ().
In step (a), the purpose introducing filamentary structure in described main material is, this is special to utilize filamentary structure
Structure and overlap between multiple spherical magnesium hydroxide, formed pinball heat conduction system, it has preferable heat-conducting effect.
Described filamentary structure is one or more in acicular magnesium hydroxide, glass fibre, fibrous wollastonite.In order to realize more
Good heat-conducting effect, described spherical magnesium hydroxide is preferably 10:1～20:1 with the mass ratio of filamentary structure.
The adding purpose of described auxiliary material is for improving heat conductivility.Described auxiliary material is glass fibre, wollastonite, aluminium oxide, carbon
One or more in SiClx, silicon nitride, aluminium nitride.The adding purpose of described first auxiliary agent is for improving its fire resistance.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 in magnesium, zinc stearate, Aluminate, titanate esters, preferably polysiloxanes.
Described main material is (85～95) with the mass ratio of auxiliary material: (5～15).Preferably, in order to make auxiliary material be filled in master
Between material chondritic, conduction heat more efficiently, improves the mass ratio of heat-conducting effect, described main material and auxiliary material further
For (85～90): (10～15).
The quality of described first auxiliary agent is the 0.2%～2% of the described main material gross mass with auxiliary material.Preferably, for reality
Now more preferable surface treatment effect, the quality of described first auxiliary agent is the 0.2%～1% of the described main material gross mass with auxiliary material.
Described first temperature is 70 degrees Celsius～85 degrees Celsius.
In step (b), the adding purpose of described second auxiliary agent is to main material and the modifying surface of auxiliary material so that it is
Its compatibility is improved with plastic resin when mixing.Described second auxiliary agent is vinyl silanes, amino silane, epoxy radicals silicone hydride, acyl
One or more in TMOS, polysiloxanes, stearic acid, magnesium stearate, zinc stearate, Aluminate, titanate esters, preferably
For, silane material.
The quality of described second auxiliary agent is the 0.5%～5% of the described main material gross mass with auxiliary material.Preferably, for reality
Now more preferable compatibility effect, the quality of described second auxiliary agent is the 0.5%～1% of the described main material gross mass with auxiliary material.
Described second temperature is 85 degrees Celsius～110 degrees Celsius.
The present invention also provides for a kind of heat conductive flame-retarding agent using above-mentioned preparation method to obtain.Refer to Fig. 1 and Fig. 2, described
Heat conductive flame-retarding agent includes multiple spherical particle and multiple filamentary structure, and the plurality of filamentary structure is uniformly distributed in multiple ball
Overlap between shape granule and with adjacent spherical particle.Described spherical particle be mainly composed of spherical magnesium hydroxide.Described pin
Shape structure be mainly composed of in acicular magnesium hydroxide, glass fibre, fibrous wollastonite one or more.In preparation
During, the auxiliary material of surface attachment, the first auxiliary agent and second auxiliary agent of spherical magnesium hydroxide and filamentary structure, final each component is tight
Close combine.
The particle diameter of described spherical particle is 2 microns～60 microns.
Compared to prior art, this preparation method has the advantage that first, by adding fibre in spherical magnesium hydroxide
Dimension shape structure, in the pinball composite heat-conducting system that collocation is formed, filamentary structure can be dispersed in spherical magnesium hydroxide,
Filamentary structure can play the effect of connection, beneficially heat conduction, thus this heat conductive flame-retarding agent has good heat-conducting effect；The
Two, by being sequentially added into the first auxiliary agent, the second auxiliary agent, this first auxiliary agent and the second auxiliary agent major ingredient can be carried out surface process and
Modification, can make magnesium hydroxide major ingredient have the preferable compatibility, thus the heat conductive flame-retarding agent obtained is prone to mix with plastic resin
Material.
In the heat conductive flame-retarding agent that this obtains, major ingredient magnesium hydroxide has perfect microcosmic crystalline structure, and feeding is not built bridge, easily
In with plastic resin batch mixing.When this heat conductive flame-retarding agent is prepared heat-conducting plastic with mixed with resin, these heat conductive flame-retarding agent and plastics
Resin compatible is good, thoroughly solves magnesium hydroxide feeding difficulty, the shortcoming of bad dispersibility.The experiment proved that, described heat conductive flame-retarding
The weight ratio 50% that agent is added in Heat Conduction Material i.e. can reach V0 level, and when the heat-conducting plastic obtained is lighted, smog is little, depletion of QI
Taste, anti-dripping melt.
Below in conjunction with specific embodiment, heat conductive flame-retarding agent of the present invention and preparation method thereof is illustrated:
Embodiment 1:
Weigh main material, auxiliary material and the first auxiliary agent, and by this main material, auxiliary material and the first auxiliary agent under about 80 degrees Celsius at height
Speed stirrer for mixing obtains precast body, and wherein said main material includes spherical magnesium hydroxide and acicular magnesium hydroxide, spherical hydrogen-oxygen
The mass ratio changing magnesium and acicular magnesium hydroxide is 20:1, and auxiliary material is wollastonite, and the first auxiliary agent is polysiloxanes, and described main material is with auxiliary
The mass ratio of material is 85:15, and the quality of described first auxiliary agent is the 5% of the described main material gross mass with auxiliary material.
Described precast body and the second auxiliary agent are mixed under about 115 degrees Celsius and be dried to obtain described heat conductive flame-retarding agent.
Wherein, the second auxiliary agent is vinyl silanes, and the quality of described second auxiliary agent is the 5% of the described main material gross mass with auxiliary material.
The heat conductive flame-retarding agent obtained is scanned Electronic Speculum test.Referring to, 1 and Fig. 2, from Fig. 1 and Fig. 2, these are many
Individual acicular texture is uniformly distributed between multiple spherical particle and overlaps with adjacent spherical particle, the particle diameter of described spherical particle
It it is 2 microns～60 microns.
By this heat conductive flame-retarding agent obtained application in heat-conducting plastic, and carry out with commercially available conventional magnesium hydroxide simultaneously right
Ratio 1.Formula such as table 1 below.
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 magnesium oxide, aluminium oxide and carborundum.
The heat-conducting plastic that above-mentioned table 1 obtains is carried out performance test, the results are shown in Table 2.
Table 2
From table 2, for the heat-conducting plastic that commercially available conventional magnesium hydroxide is made, the present embodiment 1 heat conductive flame-retarding
The heat conductivility of the heat-conducting plastic that agent is made is greatly improved, and the physical property on other affects little simultaneously.
The explanation of above example is only intended to help to understand method and the core concept thereof of the present invention.It is right to it should be pointed out that,
For those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to the present invention is carried out
Some improvement and modification, these improve and modify in the protection domain also falling into the claims in the present invention.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses the present invention.
Multiple amendment to these embodiments will be apparent from for those skilled in the art, as defined herein
General Principle can realize without departing from the spirit or scope of the present invention in other embodiments.Therefore, the present invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and principles disclosed herein and features of novelty phase one
The widest scope caused.
Claims (8)
1. a preparation method for heat conductive flame-retarding agent, it comprises the steps:
A () weighs main material, auxiliary material and the first auxiliary agent, and this main material, auxiliary material and the first auxiliary agent are mixed to get at a temperature of first
Precast body, wherein said main material includes the matter of spherical magnesium hydroxide and filamentary structure, spherical magnesium hydroxide and filamentary structure
Amount ratio is 5:1～20:1；
B described precast body is modified at a temperature of second by the second auxiliary agent and is dried to obtain described heat conductive flame-retarding agent by ().
2. the preparation method of a heat conductive flame-retarding agent as claimed in claim 1, it is characterised in that fiber described in step (a)
Shape structure is one or more in acicular magnesium hydroxide, glass fibre, fibrous wollastonite, described auxiliary material is, aluminium oxide,
One or more in carborundum, silicon nitride, aluminium nitride, described first auxiliary agent is vinyl silanes, amino silane, epoxy radicals
One in silane, acyloxy silane, polysiloxanes, stearic acid, magnesium stearate, zinc stearate, Aluminate, titanate esters or many
Kind.
3. the preparation method of a heat conductive flame-retarding agent as claimed in claim 1, it is characterised in that main material described in step (a)
Being (85～95) with the mass ratio of auxiliary material: (5～15), the quality of described first auxiliary agent is the gross mass of described main material and auxiliary material
0.2%～2%.
4. the preparation method of a heat conductive flame-retarding agent as claimed in claim 1, it is characterised in that described in step (a) first
Temperature is 70 degrees Celsius～85 degrees Celsius.
5. the preparation method of a heat conductive flame-retarding agent as claimed in claim 1, it is characterised in that described in step (b) second
Auxiliary agent is vinyl silanes, amino silane, epoxy radicals silicone hydride, acyloxy silane, polysiloxanes, stearic acid, magnesium stearate, tristearin
Acid zinc, Aluminate, titanate esters in one or more.
6. the preparation method of a heat conductive flame-retarding agent as claimed in claim 1, it is characterised in that step (b) described second helps
The quality of agent is the 0.5%～5% of the described main material gross mass with auxiliary material.
7. the preparation method of a heat conductive flame-retarding agent as claimed in claim 1, it is characterised in that described second temperature of step (b)
Degree is 85 degrees Celsius～110 degrees Celsius.
8. one kind uses the heat conductive flame-retarding agent that obtains such as claim 1 to 7 any one preparation method, it is characterised in that described in lead
Hot fire retardant includes multiple spherical particle and multiple filamentary structure, and the plurality of filamentary structure is uniformly distributed in multiple spherical
Overlapping between granule and with adjacent spherical particle, the particle diameter of described spherical particle is 2 microns～60 microns.
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| CN107253240A (en) * | 2017-08-07 | 2017-10-17 | 临沂市新天力机械有限公司 | A kind of novel wooden composite plate |
| CN113674926A (en) * | 2021-08-13 | 2021-11-19 | 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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| CN113674926A (en) * | 2021-08-13 | 2021-11-19 | 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 |
| 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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| CN106243387B (en) | 2019-01-01 |
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Effective date of registration: 20201202 Address after: Zhejiang Industrial Park, juancheng County, Heze City, Shandong Province Patentee after: Shandong Sixin flame retardant material Co., Ltd Address before: Jiaxing City, Zhejiang province 314100 Jiashan County Huimin Street Success Road No. 166 Patentee before: ZHEJIANG XUSEN HALOGEN FREE SMOKE ABATEMENT FIRE RETARDANT Co.,Ltd. |
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