CN107266764A - A kind of fire-retardant polyethylene material and preparation method thereof - Google Patents
A kind of fire-retardant polyethylene material and preparation method thereof Download PDFInfo
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- CN107266764A CN107266764A CN201710424648.5A CN201710424648A CN107266764A CN 107266764 A CN107266764 A CN 107266764A CN 201710424648 A CN201710424648 A CN 201710424648A CN 107266764 A CN107266764 A CN 107266764A
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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
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/03—Halogenated hydrocarbons aromatic, e.g. C6H5-CH2-Cl
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The present invention relates to a kind of fire-retardant polyethylene material and preparation method thereof, belong to fire proofing preparing technical field.The present invention is using montmorillonite as raw material, and it is modified, preparing has laminated structure nano filler, layer structure is bridged by CNT again, play a part of a kind of " sealant ", the collective effect of the two can reduce the layer of charcoal surface hole defect formed in combustion process, the barrier blocking effect of Nano filling is so as to play more preferably, fuel gas and oxygen is hindered to travel further into, and rare earth doped element, play smoke suppressing effect, finally it is added to bromide fire retardant in polyethylene, play cooperative flame retardant effect, effectively improve the fire resistance of polyethylene, and play a part of reducing flue gas and heat release in combustion.
Description
Technical field
The present invention relates to a kind of fire-retardant polyethylene material and preparation method thereof, belong to fire proofing preparing technical field.
Background technology
Polyethylene(PE)It is light weight, nontoxic, with good electrical insulation capability, heat-proof quality, decay resistance, mechanical property
Can, and it is cheap, easily, demand is big, is widely used in packaging material, plastic film for agricultural use, construction material, pipe for processing and forming
The various fields such as road conveying tubing and electric wire.
However, because polyethylene is made up of carbon, two kinds of elements of hydrogen, this chemical constitution makes it be easy to burning, and release
A large amount of flue gases and toxic gas.The inflammability of polyethylene not only limit its application, directly or indirectly caused fire quantity
It is countless.Fire not only causes huge skilful economic loss, more seriously, heat, the flue gas discharged in combustion process
With the precious life of the toxic gas entail dangers to people.Therefore, improve the fire resistance of polyethylene turn into extend its application must be through
Road, also weighed very much for protection the people's lives and property safety while reducing its combustible gas scale of construction for discharging during combustion border
Will.
The content of the invention
The technical problems to be solved by the invention:A large amount of cigarettes can be discharged for the inflammability of polyethylene, and in combustion process
The problem of gas and toxic gas, the invention provides a kind of fire-retardant polyethylene material and preparation method thereof.
To solve technical problem, the technical solution adopted by the present invention is:
A kind of fire-retardant polyethylene material, including 2~3 parts of fire-retardant fillers, 8~10 parts of TDEs, 87~90 parts of polyethylene,
The fire-retardant filler is CNT bridging iron-based montmorillonite.
The CNT bridging iron-based montmorillonite is 20~30 part by weight modified iron-based montmorillonites, many walls of 1~2 parts by weight
CNT, 0.1~0.3 parts by weight lanthanum nitrate, is heated to 90~100 DEG C, insulation reaction after being uniformly dispersed in deionized water
20~24h, washs dry be made after filtering.
The Modified Iron base montmorillonite is the iron-based montmorillonite through cetyl trimethylammonium bromide intercalation modifying.
The iron-based montmorillonite is ferric trichloride and sodium-based montmorillonite in mass ratio 1:4~1:6 mix in deionized water
8~10h is stirred to be made.
A kind of preparation method of described fire-retardant polyethylene material, is concretely comprised the following steps:
S1. dispensing;
S2. raw material is fitted into banbury, 8~10min of melt blending, then continues at vulcanizing press at 170~180 DEG C
In, preheated at 170~180 DEG C after 5~8min, 6~8min of hot pressing under 15~20MPa pressure, then be transferred to 25~30 DEG C and put down
In plate vulcanizer, 6~8min is cold-pressed under 15~20MPa pressure, stripping forming obtains fire-retardant polyethylene material.
The method have the benefit that:
The present invention is modified using montmorillonite as raw material to it, and preparing has laminated structure nano filler, then passes through CNT bridge
Layer structure is connect, plays a part of a kind of " sealant ", the collective effect of the two can make the layer of charcoal table formed in combustion process
Face hole is reduced, and the barrier blocking effect of Nano filling hinders fuel gas and oxygen to travel further into so as to play more preferably,
And rare earth doped element plays smoke suppressing effect, is finally added to bromide fire retardant in polyethylene, cooperative flame retardant effect is played, is had
Effect improves the fire resistance of polyethylene, and plays a part of reducing flue gas and heat release in combustion.
Embodiment
10~12g ferric trichlorides are weighed, are added into 500~600mL deionized waters, 10 are stirred with 300~400r/min
~15min, adds 50~60g sodium-based montmorillonites, continues to stir 8~10h, subsequent suction filtration, and filter cake 3 is washed with deionized
~5 times, then filter cake is placed in drying box, 3~5h is dried at 70~80 DEG C, iron-based montmorillonite is obtained, iron-based montmorillonite is added
Enter into 500~600mL deionized waters, under 70~80 DEG C of waters bath with thermostatic control, 20~30min is stirred with 300~400r/min, then
20~25g cetyl trimethylammonium bromides are added, reactant is then fitted into centrifuge, with 6000 by 1~2h of insulation reaction
~8000r/min centrifuges 8~10min, must precipitate, precipitation be washed with deionized 3~5 times, then precipitation is placed in 105~
Dried in 110 DEG C of drying boxes to constant weight, be transferred in pulverizer and crush, crossed 200 mesh sieves, obtain Modified Iron base montmorillonite, weigh 20
~30g Modified Iron base montmorillonites, 1~2g multi-walled carbon nanotubes, 0.1~0.3g lanthanum nitrates add 200~300mL deionized waters
In, at 60~70 DEG C, 20~30min is disperseed with 200W ultrasonic echographies, is subsequently heated to 90~100 DEG C, insulation reaction 20
~24h, is cooled to after room temperature and filters, filter residue is washed with deionized 2~3 times, then filter residue is placed in drying box, 70~80
At DEG C, 10~12h is dried, CNT bridging iron-based montmorillonite is obtained, counts by weight, weigh 2~3 parts of CNT bridgings
Iron-based montmorillonite, 8~10 parts of TDEs, 87~90 parts of polyethylene are fitted into banbury, are melted at 170~180 DEG C
8~10min is blended, then continues in vulcanizing press, is preheated at 170~180 DEG C after 5~8min, in 15~20MPa pressure
6~8min of lower hot pressing, then be transferred in 25~30 DEG C of vulcanizing presses, 6~8min is cold-pressed under 15~20MPa pressure, is stripped into
Type, obtains fire-retardant polyethylene material.
Example 1
Weigh 10~12g ferric trichlorides, add into 500~600mL deionized waters, with 300~400r/min stirrings 10~
15min, adds 50~60g sodium-based montmorillonites, continues to stir 8~10h, subsequent suction filtration, and be washed with deionized filter cake 3~
5 times, then filter cake is placed in drying box, 3~5h is dried at 70~80 DEG C, iron-based montmorillonite is obtained, iron-based montmorillonite is added
Into 500~600mL deionized waters, under 70~80 DEG C of waters bath with thermostatic control, 20~30min is stirred with 300~400r/min, then add
Enter 20~25g cetyl trimethylammonium bromides, reactant is then fitted into centrifuge by 1~2h of insulation reaction, with 6000~
8000r/min centrifuges 8~10min, must precipitate, precipitation be washed with deionized 3~5 times, then precipitation is placed in 105~
Dried in 110 DEG C of drying boxes to constant weight, be transferred in pulverizer and crush, crossed 200 mesh sieves, obtain Modified Iron base montmorillonite, weigh 20
~30g Modified Iron base montmorillonites, 1~2g multi-walled carbon nanotubes, 0.1~0.3g lanthanum nitrates add 200~300mL deionized waters
In, at 60~70 DEG C, 20~30min is disperseed with 200W ultrasonic echographies, is subsequently heated to 90~100 DEG C, insulation reaction 20
~24h, is cooled to after room temperature and filters, filter residue is washed with deionized 2~3 times, then filter residue is placed in drying box, 70~80
At DEG C, 10~12h is dried, CNT bridging iron-based montmorillonite is obtained, counts by weight, weigh 2~3 parts of CNT bridgings
Iron-based montmorillonite, 8~10 parts of TDEs, 87~90 parts of polyethylene are fitted into banbury, are melted at 170~180 DEG C
8~10min is blended, then continues in vulcanizing press, is preheated at 170~180 DEG C after 5~8min, in 15~20MPa pressure
6~8min of lower hot pressing, then be transferred in 25~30 DEG C of vulcanizing presses, 6~8min is cold-pressed under 15~20MPa pressure, is stripped into
Type, obtains fire-retardant polyethylene material.
Example 1
10g ferric trichlorides are weighed, are added into 500mL deionized waters, 10min is stirred with 300r/min, 50g sodium base illiteracy is added
De- soil, continues to stir 8h, subsequent suction filtration, and filter cake is washed with deionized 3 times, then filter cake is placed in drying box, at 70 DEG C
Lower dry 3h, obtains iron-based montmorillonite, and iron-based montmorillonite is added into 500mL deionized waters, under 70 DEG C of waters bath with thermostatic control, with
300r/min stirs 20min, adds 20g cetyl trimethylammonium bromides, insulation reaction 1h, then by reactant load from
In scheming, 8min is centrifuged with 6000r/min, must be precipitated, precipitation is washed with deionized 3 times, then precipitation is placed in 105 DEG C
Dried in drying box to constant weight, be transferred in pulverizer and crush, crossed 200 mesh sieves, obtain Modified Iron base montmorillonite, weigh 20g modifications
Iron-based montmorillonite, 1g multi-walled carbon nanotubes, 0.1g lanthanum nitrates are added in 200mL deionized waters, at 60 DEG C, with 200W ultrasonic waves
Ultrasonic disperse 20min, is subsequently heated to 90 DEG C, insulation reaction 20h is cooled to after room temperature and filtered, filter residue 2 is washed with deionized
It is secondary, then filter residue is placed in drying box, at 70 DEG C, 10h is dried, CNT bridging iron-based montmorillonite is obtained, by weight
Meter, weighs 2 parts of CNT bridging iron-based montmorillonites, 8 parts of TDEs, 87 parts of polyethylene are fitted into banbury,
Melt blending 8min, is then continued in vulcanizing press at 170 DEG C, is preheated at 170 DEG C after 5min, hot under 15MPa pressure
6min is pressed, then is transferred in 25 DEG C of vulcanizing presses, 6min is cold-pressed under 15MPa pressure, stripping forming obtains flame-proof polyethylene material
Material.
Example 2
11g ferric trichlorides are weighed, are added into 550mL deionized waters, 13min is stirred with 350r/min, 55g sodium base illiteracy is added
De- soil, continues to stir 9h, subsequent suction filtration, and filter cake is washed with deionized 4 times, then filter cake is placed in drying box, at 75 DEG C
Lower dry 4h, obtains iron-based montmorillonite, and iron-based montmorillonite is added into 550mL deionized waters, under 75 DEG C of waters bath with thermostatic control, with
350r/min stirs 25min, adds 23g cetyl trimethylammonium bromides, insulation reaction 1h, then by reactant load from
In scheming, 9min is centrifuged with 7000r/min, must be precipitated, precipitation is washed with deionized 4 times, then precipitation is placed in 108 DEG C
Dried in drying box to constant weight, be transferred in pulverizer and crush, crossed 200 mesh sieves, obtain Modified Iron base montmorillonite, weigh 25g modifications
Iron-based montmorillonite, 1g multi-walled carbon nanotubes, 0.2g lanthanum nitrates are added in 250mL deionized waters, at 65 DEG C, with 200W ultrasonic waves
Ultrasonic disperse 25min, is subsequently heated to 95 DEG C, insulation reaction 22h is cooled to after room temperature and filtered, filter residue 2 is washed with deionized
It is secondary, then filter residue is placed in drying box, at 75 DEG C, 11h is dried, CNT bridging iron-based montmorillonite is obtained, by weight
Meter, weighs 2 parts of CNT bridging iron-based montmorillonites, 9 parts of TDEs, 89 parts of polyethylene are fitted into banbury,
Melt blending 9min, is then continued in vulcanizing press at 175 DEG C, is preheated at 175 DEG C after 7min, hot under 18MPa pressure
7min is pressed, then is transferred in 28 DEG C of vulcanizing presses, 7min is cold-pressed under 18MPa pressure, stripping forming obtains flame-proof polyethylene material
Material.
Example 3
12g ferric trichlorides are weighed, are added into 600mL deionized waters, 15min is stirred with 400r/min, 60g sodium base illiteracy is added
De- soil, continues to stir 10h, subsequent suction filtration, and filter cake is washed with deionized 5 times, then filter cake is placed in drying box, at 80 DEG C
Lower dry 5h, obtains iron-based montmorillonite, and iron-based montmorillonite is added into 600mL deionized waters, under 80 DEG C of waters bath with thermostatic control, with
400r/min stirs 30min, adds 25g cetyl trimethylammonium bromides, insulation reaction 2h, then by reactant load from
In scheming, 10min is centrifuged with 8000r/min, must be precipitated, precipitation is washed with deionized 5 times, then precipitation is placed in 110
Dried in DEG C drying box to constant weight, be transferred in pulverizer and crush, crossed 200 mesh sieves, obtain Modified Iron base montmorillonite, weigh 30g and change
Property iron-based montmorillonite, 2g multi-walled carbon nanotubes, 0.3g lanthanum nitrates add 300mL deionized waters in, at 70 DEG C, with 200W ultrasound
Ripple ultrasonic disperse 30min, is subsequently heated to 100 DEG C, insulation reaction 24h is cooled to after room temperature and filtered, filter is washed with deionized
Slag 3 times, then filter residue is placed in drying box, at 80 DEG C, 12h is dried, CNT bridging iron-based montmorillonite is obtained, by weight
Number meter, weighs 3 parts of CNT bridging iron-based montmorillonites, 10 parts of TDEs, 90 parts of polyethylene are fitted into banbury,
Melt blending 10min, is then continued in vulcanizing press at 180 DEG C, is preheated at 180 DEG C after 8min, under 20MPa pressure
Hot pressing 8min, then be transferred in 30 DEG C of vulcanizing presses, 8min is cold-pressed under 20MPa pressure, stripping forming obtains flame-proof polyethylene material
Material.
To fire-retardant polyethylene material made from example 1~3 and commercially available halogen-free fire-retardant polyethylene material(Comparative example)Progressive
It can detect, its testing result is as shown in table 1 below:
The fire-retardant polyethylene material the performance test results of table 1
In summary, fire-retardant polyethylene material produced by the present invention is while preferable fire resistance is kept, also with preferable
Mechanical property, and there is material not produce toxic gas and smog in combustion process, danger will not be caused to health and environment
Evil.
Claims (5)
1. a kind of fire-retardant polyethylene material, including 2~3 parts of fire-retardant fillers, 8~10 parts of TDEs, 87~90 parts of poly- second
Alkene, it is characterised in that the fire-retardant filler is CNT bridging iron-based montmorillonite.
2. a kind of fire-retardant polyethylene material as claimed in claim 1, it is characterised in that the CNT bridging iron-based covers de-
Soil be 20~30 part by weight modified iron-based montmorillonites, 1~2 parts by weight multi-walled carbon nanotube, 0.1~0.3 parts by weight lanthanum nitrate,
90~100 DEG C are heated to after being uniformly dispersed in deionized water, 20~24h of insulation reaction washs dry be made after filtering.
3. a kind of fire-retardant polyethylene material as claimed in claim 2, it is characterised in that the Modified Iron base montmorillonite is through ten
The iron-based montmorillonite of six alkyl trimethyl ammonium bromide intercalation modifyings.
4. a kind of fire-retardant polyethylene material as claimed in claim 3, it is characterised in that the iron-based montmorillonite is ferric trichloride
With sodium-based montmorillonite in mass ratio 1:4~1:6 mix 8~10h in deionized water is made.
5. the preparation method of a kind of fire-retardant polyethylene material as described in any one of Claims 1 to 4, it is characterised in that specific
Step is:
S1. dispensing;
S2. raw material is fitted into banbury, 8~10min of melt blending, then continues at vulcanizing press at 170~180 DEG C
In, preheated at 170~180 DEG C after 5~8min, 6~8min of hot pressing under 15~20MPa pressure, then be transferred to 25~30 DEG C and put down
In plate vulcanizer, 6~8min is cold-pressed under 15~20MPa pressure, stripping forming obtains fire-retardant polyethylene material.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108485087A (en) * | 2018-04-24 | 2018-09-04 | 吴刚 | A kind of preparation method of modified polyvinyl plastic plate |
CN115287824A (en) * | 2022-06-29 | 2022-11-04 | 惠州市普林摩斯无纺布有限公司 | Antibacterial anti-mite non-woven fabric for mattress lining and preparation process thereof |
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CN103613827A (en) * | 2013-11-21 | 2014-03-05 | 浙江大学宁波理工学院 | CNT(carbon nano tube)-bridged rare-earth phenylphosphonate compounded decabromodiphenylethane flame-retardant polyethylene and preparation method thereof |
CN106243735A (en) * | 2016-08-05 | 2016-12-21 | 雷春生 | A kind of preparation method of halogen-free anti-flaming silicon rubber cable sleeve |
CN106317555A (en) * | 2016-08-18 | 2017-01-11 | 苏州玖圣塑料科技有限公司 | High-density polyethylene resin and preparation method and application thereof |
CN106633273A (en) * | 2016-10-08 | 2017-05-10 | 上海加略实业有限公司 | Low-shrinkage high-insulation flame-retardant HDPE composite material and preparation method thereof |
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- 2017-06-07 CN CN201710424648.5A patent/CN107266764A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103613827A (en) * | 2013-11-21 | 2014-03-05 | 浙江大学宁波理工学院 | CNT(carbon nano tube)-bridged rare-earth phenylphosphonate compounded decabromodiphenylethane flame-retardant polyethylene and preparation method thereof |
CN106243735A (en) * | 2016-08-05 | 2016-12-21 | 雷春生 | A kind of preparation method of halogen-free anti-flaming silicon rubber cable sleeve |
CN106317555A (en) * | 2016-08-18 | 2017-01-11 | 苏州玖圣塑料科技有限公司 | High-density polyethylene resin and preparation method and application thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108485087A (en) * | 2018-04-24 | 2018-09-04 | 吴刚 | A kind of preparation method of modified polyvinyl plastic plate |
CN115287824A (en) * | 2022-06-29 | 2022-11-04 | 惠州市普林摩斯无纺布有限公司 | Antibacterial anti-mite non-woven fabric for mattress lining and preparation process thereof |
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