CN109232990A - A kind of heat conductive flame-retarding compounded mix and preparation method thereof - Google Patents
A kind of heat conductive flame-retarding compounded mix and preparation method thereof Download PDFInfo
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- CN109232990A CN109232990A CN201810791473.6A CN201810791473A CN109232990A CN 109232990 A CN109232990 A CN 109232990A CN 201810791473 A CN201810791473 A CN 201810791473A CN 109232990 A CN109232990 A CN 109232990A
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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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
- 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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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
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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
- C08K5/16—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
- C08K5/34928—Salts
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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
- 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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3009—Sulfides
- C08K2003/3036—Sulfides of zinc
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The present invention relates to a kind of heat conductive flame-retarding compounded mixs and preparation method thereof, are made of boehmite, nano-zinc sulfide, ammonium polyphosphate and melamine by Quadrafos.It is fine white crystal that the technical program, which is using boehmite, and crystallization is complete, crystal grain is tiny, and crystal structure defects are few, and hot coefficient is higher, can promote the heating conduction of PET composite material；It can generate water and Al in by thermal decomposition process2O3, water can dilute imflammable gas, Al2O3Solid, which is covered on PET matrix surface, can obstruct retarded combustion rate, to achieve the effect that flame-retardant smoke inhibition.
Description
Technical field
The invention belongs to technical field of polymer materials, a kind of heat conductive flame-retarding compounded mix and its preparation side are particularly related to
Method.
Background technique
Heating conduction, flame retardant property are one of the important performances of automobile interior exterior decoration, plastic shell etc., improve polymer
Heating conduction, flame retardant property method have very much, a kind of heat conductive flame-retarding compounded mix and preparation method thereof is made in the application innovation,
Improve the heating conduction and flame retardant property of present polyolefin, this heat conductive flame-retarding compounded mix not yet sees report so far, tool
There is very important realistic meaning.
Summary of the invention
The object of the present invention is to provide a kind of heat conductive flame-retarding compounded mixs and preparation method thereof, to improve polyolefin composite wood
Expect heating conduction and improves anti-flammability.
The present invention is achieved by the following technical solutions:
A kind of heat conductive flame-retarding compounded mix, by boehmite, nano-zinc sulfide, ammonium polyphosphate and melamine by Quadrafos group
At.
The mass ratio of the boehmite and the nano-zinc sulfide is (40-60): (10-20).
The preparation method of heat conductive flame-retarding compounded mix according to any of the above-described, comprising the following steps:
1) boehmite powder is sufficiently mixed with nano-zinc sulfide, stirs 40-60min in high-speed mixer, obtains mixture
A；
2) ammonium polyphosphate and melamine polyphosphate will be added in the mixture A of step 1), will be thoroughly mixed
20-40min is cooled to room temperature up to heat conductive flame-retarding compounded mix.
The partial size of the boehmite is 500 mesh.
The whipping temp of high-speed mixer in the step 1) is 60-80 DEG C, revolving speed 200-280r/min.
The mass ratio of ammonium polyphosphate, melamine polyphosphate and mixture A in step 2) is (40-60): (60-
80): (30-50).
The beneficial effects of the present invention are:
1, the function of boehmite mainly has two: 1. it is fine white crystal, and crystallization is complete, crystal grain is tiny, crystal structure
Defect is few, and hot coefficient is higher, can promote the heating conduction of PET composite material.2. it can generate water in by thermal decomposition process
And Al2O3, water can dilute imflammable gas, Al2O3Solid, which is covered on PET matrix surface, can obstruct retarded combustion rate, from
And achieve the effect that flame-retardant smoke inhibition.
2, the technical program has synthesized a kind of fire-retardant compounded mix of novel heat-conducting, it has both thermally conductive and fire-retardant function simultaneously
Can, there is critically important promotional value.
Specific embodiment
Carry out the technical solution that the present invention will be described in detail by the following examples, embodiment below is merely exemplary, only
It can be used to explanation and illustration technical solution of the present invention, and be not to be construed as the limitation to technical solution of the present invention.
Raw material used in present embodiments is as follows:
PBT (model 2002U), Polyplastics；PP (model Z30S), Maoming Petrochemical；PE (model 5070), Panjin ethylene；
PA6 (model C M1017), toray；PS (model 350), state of Taiwan Province are tall；Boehmite, the limited public affairs of Zibo gold fine jade chemical science and technology
Department；Ammonium polyphosphate (APP), the auspicious emerging fire-retardant science and technology in Shandong；Melamine polyphosphate (MPP), section's flame-retarding new material has in Hefei
Limit company；Nano-zinc sulfide, Zhangjiagang love must believe chemical industry.
Test equipment used in each embodiment of the application is as follows:
ZSK30 type double screw extruder, German W&P company；Mixer, Dalian China Korea Spro's rubber and plastic；JL-1000 type pull test
Machine, the production of Guangzhou Guang Cai laboratory apparatus company；HTL900-T-5B type injection (mo(u)lding) machine, Hai Tai plastics machinery Co., Ltd are raw
It produces；XCJ-500 type shock-testing machine, the production of Chengde testing machine factory；QT-1196 type tester for elongation, the high safe detector of Dongguan City
Device Co., Ltd；QD-GJS-B12K type high-speed mixer, Beijing perseverance Order instrument and meter Co., Ltd.
The application provides a kind of heat conductive flame-retarding compounded mix, by boehmite, nano-zinc sulfide, ammonium polyphosphate and melamine by
Quadrafos composition.The mass ratio of the boehmite and the nano-zinc sulfide is (40-60): (10-20).
The preparation method of heat conductive flame-retarding compounded mix, comprising the following steps:
1) boehmite powder of 500 mesh is sufficiently mixed with nano-zinc sulfide, is 60-80 DEG C in whipping temp, revolving speed is
The high-speed mixer of 200-280r/min stirs 40-60min, obtains mixture A.
2) ammonium polyphosphate and melamine polyphosphate will be added in the mixture A of step 1), will be thoroughly mixed
20-40min is cooled to room temperature up to heat conductive flame-retarding compounded mix.
The mass ratio of ammonium polyphosphate, melamine polyphosphate and mixture A in step 2) is (40-60): (60-
80): (30-50).
Preparation example 1
(1) 400g boehmite, 100g nano-zinc sulfide are weighed, boehmite is crushed in pulverizer, crosses 500 meshes, then
Boehmite, nano-zinc sulfide are sufficiently mixed, 40min is stirred in high-speed mixer, obtains mixture A；
(2) weigh 400g ammonium polyphosphate (APP), 600g melamine polyphosphate (MPP), 300g mixture A, by APP,
MPP is added in step (1) mixture A, is thoroughly mixed 20min, is cooled to room temperature up to composite fire retardant P1.
The temperature of described step (1) the high speed blender is 60 DEG C, revolving speed 200r/min.
Application examples 1
It takes 20 parts of P1 to be added in 80 parts of polypropylene (PP), stirs 10min through high mixer, be subsequently added into double screw extruder
Middle carry out blending extrusion, obtains PP composite material X1.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 170 DEG C, the
The temperature of two humidity provinces is 220 DEG C, and the temperature of third humidity province is 230 DEG C, and the temperature of the 4th humidity province is 240 DEG C, the 5th temperature
The temperature for spending area is 240 DEG C, and the temperature of the 6th humidity province is 240 DEG C, and the head temperature of double screw extruder is 230 DEG C, screw rod
Revolving speed is 220r/min.
Comparative example 1
80 parts of polypropylene (PP) are taken, stir 10min through high mixer, is subsequently added into double screw extruder be blended and squeeze
Out, PP composite material D1 is obtained.
The performance data of PP composite material prepared by above application examples 1 and comparative example 1 is as shown in the table:
As can be seen from the above table, the heating conduction of X1, flame retardant property are better than D1, this illustrates that thermally conductive resistance of the invention is added
After firing compounded mix, the heating conduction of PP, flame retardant property are more preferable.
Preparation example 2
(1) 600g boehmite, 200g nano-zinc sulfide are weighed, boehmite is crushed in pulverizer, crosses 500 meshes, then
Boehmite, nano-zinc sulfide are sufficiently mixed, 60min is stirred in high-speed mixer, obtains mixture A；
(2) it weighs 600g ammonium polyphosphate (APP), 800g melamine polyphosphate (MPP), 500g mixture A, by poly- phosphorus
Sour ammonium (APP), melamine polyphosphate (MPP) are added in step (1) mixture A, are thoroughly mixed 40min, cooling
To room temperature up to composite fire retardant P2.
The temperature of step (1) high speed blender is 80 DEG C, revolving speed 280r/min.
Application examples 2
It takes 20 parts of P2 to be added in 80 parts of polybutylene terephthalate (PBT)s (PBT), stirs 10min through high mixer, then
Carry out blending extrusion is added twin-screw extrude, PBT composite X2 is obtained.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 200 DEG C, the
The temperature of two humidity provinces is 260 DEG C, and the temperature of third humidity province is 260 DEG C, and the temperature of the 4th humidity province is 260 DEG C, the 5th temperature
The temperature for spending area is 260 DEG C, and the temperature of the 6th humidity province is 260 DEG C, and the head temperature of double screw extruder is 260 DEG C, screw rod
Revolving speed is 300r/min.
Comparative example 2
80 parts of PBT are taken, stir 10min through high mixer, is subsequently added into double screw extruder and carries out blending extrusion, obtain
PBT composite D2.
The performance data of PBT composite prepared by above application examples 2 and comparative example 2 is as shown in the table:
As can be seen from the above table, the heating conduction of X2, flame retardant property are better than D2, this illustrates that thermally conductive resistance of the invention is added
After firing compounded mix, the heating conduction of PBT, flame retardant property are more preferable.
Preparation example 3
(1) 500g boehmite, 150g nano-zinc sulfide are weighed, boehmite is crushed in pulverizer, crosses 500 meshes, then
Boehmite, nano-zinc sulfide are sufficiently mixed, 50min is stirred in high-speed mixer, obtains mixture A；
(2) it weighs 500g ammonium polyphosphate (APP), 700g melamine polyphosphate (MPP), 400g mixture A, by poly- phosphorus
Sour ammonium (APP), melamine polyphosphate (MPP) are added in step (1) mixture A, are thoroughly mixed 30min, cooling
To room temperature up to composite fire retardant P3.
The temperature of step (1) high speed blender is 70 DEG C, revolving speed 240r/min.
Application examples 3
It takes 20 parts of P3 to be added in 80 parts of polyethylene (PE), stirs 10min through high mixer, be subsequently added into double screw extruder
Middle carry out blending extrusion, obtains PE composite material X3.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 120 DEG C, the
The temperature of two humidity provinces is 180 DEG C, and the temperature of third humidity province is 180 DEG C, and the temperature of the 4th humidity province is 180 DEG C, the 5th temperature
The temperature for spending area is 180 DEG C, and the temperature of the 6th humidity province is 180 DEG C, and the head temperature of double screw extruder is 180 DEG C, screw rod
Revolving speed is 300r/min.
Comparative example 3
80 parts of PE are taken, stir 10min through high mixer, is subsequently added into double screw extruder and carries out blending extrusion, obtain PE
Composite material D3.
The performance data of PE composite material prepared by above application examples 3 and comparative example 3 is as shown in the table:
As can be seen from the above table, the heating conduction of X3, flame retardant property are better than D3, this illustrates that thermally conductive resistance of the invention is added
After firing compounded mix, the heating conduction of PE, flame retardant property are more preferable.
Preparation example 4
(1) 550g boehmite, 180g nano-zinc sulfide are weighed, boehmite is crushed in pulverizer, crosses 500 meshes, then
Boehmite, nano-zinc sulfide are sufficiently mixed, 45min is stirred in high-speed mixer, obtains mixture A；
(2) it weighs 450g ammonium polyphosphate (APP), 770g melamine polyphosphate (MPP), 450g mixture A, by poly- phosphorus
Sour ammonium (APP), melamine polyphosphate (MPP) are added in step (1) mixture A, are thoroughly mixed 25min, cooling
To room temperature up to composite fire retardant.
The temperature of step (1) high speed blender is 65 DEG C, revolving speed 245r/min.
Application examples 4
It takes 20 parts of P4 to be added in 80 parts of polyamide 6s (PA6), stirs 10min through high mixer, be subsequently added into twin-screw extrusion
Blending extrusion is carried out in machine, obtains PA6 composite material X4.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 230 DEG C, the
The temperature of two humidity provinces is 260 DEG C, and the temperature of third humidity province is 260 DEG C, and the temperature of the 4th humidity province is 260 DEG C, the 5th temperature
The temperature for spending area is 260 DEG C, and the temperature of the 6th humidity province is 260 DEG C, and the head temperature of double screw extruder is 250 DEG C, screw rod
Revolving speed is 320r/min.
Comparative example 4
80 parts of PA6 are taken, stir 10min through high mixer, is subsequently added into double screw extruder and carries out blending extrusion, obtain
PA6 composite material D4.
The performance data of PA6 composite material prepared by above application examples 4 and comparative example 4 is as shown in the table:
As can be seen from the above table, the heating conduction of X4, flame retardant property are better than D4, this illustrates that thermally conductive resistance of the invention is added
After firing compounded mix, the heating conduction of PA6, flame retardant property are more preferable.
Preparation example 5
(1) 450g boehmite, 120g nano-zinc sulfide are weighed, boehmite is crushed in pulverizer, crosses 500 meshes, then
Boehmite, nano-zinc sulfide are sufficiently mixed, 55min is stirred in high-speed mixer, obtains mixture A；
(2) it weighs 420g ammonium polyphosphate (APP), 710g melamine polyphosphate (MPP), 350g mixture A, by poly- phosphorus
Sour ammonium (APP), melamine polyphosphate (MPP) are added in step (1) mixture A, are thoroughly mixed 35min, cooling
To room temperature up to composite fire retardant P5.
The temperature of step (1) high speed blender is 65 DEG C, revolving speed 260r/min.
Application examples 5
It takes 20 parts of P5 to be added in 80 parts of styrene (PS), stirs 10min through high mixer, be subsequently added into double screw extruder
Middle carry out blending extrusion, obtains PS composite material X5.
Wherein, double screw extruder includes six humidity provinces sequentially arranged, and the temperature of the first humidity province is 160 DEG C, the
The temperature of two humidity provinces is 200 DEG C, and the temperature of third humidity province is 200 DEG C, and the temperature of the 4th humidity province is 200 DEG C, the 5th temperature
The temperature for spending area is 200 DEG C, and the temperature of the 6th humidity province is 200 DEG C, and the head temperature of double screw extruder is 200 DEG C, screw rod
Revolving speed is 280r/min.
Comparative example 5
80 parts of PS are taken, stir 10min through high mixer, is subsequently added into double screw extruder and carries out blending extrusion, obtain PS
Composite material D5.
The performance data of PS composite material prepared by above application examples 5 and comparative example 5 is as shown in the table:
As can be seen from the above table, the heating conduction of X5, flame retardant property are better than D5, this illustrates that thermally conductive resistance of the invention is added
After firing compounded mix, the heating conduction of PS, flame retardant property are more preferable.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And deformation, the scope of the present invention are extremely equally limited by appended claims.
Claims (6)
1. a kind of heat conductive flame-retarding compounded mix, which is characterized in that by boehmite, nano-zinc sulfide, ammonium polyphosphate and melamine by
Quadrafos composition.
2. heat conductive flame-retarding compounded mix according to claim 1, which is characterized in that the boehmite and the nanometer vulcanize
The mass ratio of zinc is (40-60): (10-20).
3. the preparation method of heat conductive flame-retarding compounded mix according to claim 1 or claim 2, which comprises the following steps:
1) boehmite powder is sufficiently mixed with nano-zinc sulfide, stirs 40-60min in high-speed mixer, obtains mixture A；
2) ammonium polyphosphate and melamine polyphosphate will be added in the mixture A of step 1), and will be thoroughly mixed 20-
40min is cooled to room temperature up to heat conductive flame-retarding compounded mix.
4. the preparation method of heat conductive flame-retarding compounded mix according to claim 3, which is characterized in that the grain of the boehmite
Diameter is 500 mesh.
5. the preparation method of heat conductive flame-retarding compounded mix according to claim 3, which is characterized in that in the step 1)
The whipping temp of high-speed mixer is 60-80 DEG C, revolving speed 200-280r/min.
6. the preparation method of heat conductive flame-retarding compounded mix according to claim 3, which is characterized in that the poly- phosphorus in step 2)
The mass ratio of sour ammonium, melamine polyphosphate and mixture A is (40-60): (60-80): (30-50).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591344A (en) * | 2019-09-04 | 2019-12-20 | 上海日之升科技有限公司 | Efficient flame-retardant heat-conducting nylon composite material and preparation method thereof |
| CN112745525A (en) * | 2019-10-29 | 2021-05-04 | 合肥杰事杰新材料股份有限公司 | Flame-retardant filler and preparation method thereof |
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| CN102304284A (en) * | 2011-08-22 | 2012-01-04 | 金发科技股份有限公司 | Heat-conductive resin composition and preparation method thereof |
| CN103483809A (en) * | 2013-09-24 | 2014-01-01 | 株洲时代工程塑料制品有限责任公司 | High-flowability polyamide based halogen-free flame-retardant heat-conducting composite material and preparation method thereof |
| CN104086884A (en) * | 2014-07-03 | 2014-10-08 | 合肥杰事杰新材料股份有限公司 | Flame retardant polypropylene material and preparation method thereof |
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2018
- 2018-07-18 CN CN201810791473.6A patent/CN109232990A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304284A (en) * | 2011-08-22 | 2012-01-04 | 金发科技股份有限公司 | Heat-conductive resin composition and preparation method thereof |
| CN103483809A (en) * | 2013-09-24 | 2014-01-01 | 株洲时代工程塑料制品有限责任公司 | High-flowability polyamide based halogen-free flame-retardant heat-conducting composite material and preparation method thereof |
| CN104086884A (en) * | 2014-07-03 | 2014-10-08 | 合肥杰事杰新材料股份有限公司 | Flame retardant polypropylene material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591344A (en) * | 2019-09-04 | 2019-12-20 | 上海日之升科技有限公司 | Efficient flame-retardant heat-conducting nylon composite material and preparation method thereof |
| CN112745525A (en) * | 2019-10-29 | 2021-05-04 | 合肥杰事杰新材料股份有限公司 | Flame-retardant filler and preparation method thereof |
| CN112745525B (en) * | 2019-10-29 | 2023-09-29 | 合肥杰事杰新材料股份有限公司 | Flame-retardant filler and preparation method thereof |
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