CN105968414A - Attapulgite-synergetic hydroxide flame retardant - Google Patents
Attapulgite-synergetic hydroxide flame retardant Download PDFInfo
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- CN105968414A CN105968414A CN201610323015.0A CN201610323015A CN105968414A CN 105968414 A CN105968414 A CN 105968414A CN 201610323015 A CN201610323015 A CN 201610323015A CN 105968414 A CN105968414 A CN 105968414A
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- fire
- fire retardant
- retardant
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- attapulgite clay
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- 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
-
- 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
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
- C08L23/0853—Vinylacetate
-
- 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
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
Abstract
The invention relates to a flame-retardant material and a preparation method thereof. The flame-retardant material comprises the following components in parts by mass: 23-43 parts of polyolefin, 2-8 parts of compatilizer, 0.2-0.8 part of antioxidant and 55-75 parts of flame retardant. The flame retardant comprises modifier-compounded magnesium hydroxide or aluminum hydroxide and attapulgite. The mass ratio of the attapulgite, the magnesium hydroxide or aluminum hydroxide and the modifier is (0.5-20):(80-99.5):(1-5). The obtained flame-retardant material obviously improves the flame retardancy of the low-smoke halogen-free flame-retardant high-polymer material, has the advantages of simple production method and low energy consumption, and can be widely used in industrial production.
Description
Technical field
The present invention relates to fire proofing field, particularly to the hydroxide halogen-free environment-friendlyflame flame retardant of attapulgite clay potentiation
And the application in low-smoke non-halogen flame-retardant macromolecular material.
Background technology
Along with development and the raising of people's living standard of modern science and technology, the safety to electric wire product
Property, the feature of environmental protection are had higher requirement.In CABLE MATERIALS add halogen-free flame retardants can develop low cigarette without
Halogen fire-resistant cable material, is used for manufacturing low-smoke halogen-free inflaming-retarding cable, and the cable of this premium properties has been widely used
The public place of concentration is compared in personnel such as dynamo-electric, subway and skyscrapers.
Generally, halogen-free flame retardants is joined in CABLE MATERIALS by we, can make cable material physical property and
Mechanical property reduces.Using the most merely aluminium hydroxide or flame retardant of magnesium hydroxide, material can not
Tested by vertical combustion performance.Need to add retardant synergist so that material is in the situation of equal addition
Get off to improve the fire resistance of cable material.Retardant synergist can promote the carbon-forming performance of material, and and Halogen
Fire retardant has good synergism, therefore can improve the fire resistance of material.
Attapulgite clay has another name called attapulgite clay, and attapulgite clay is that a kind of crystal grain is the most tiny, silicate containing Shuifu County's magnesium (aluminum)
Clay mineral, its ideal structure formula is Mg (Al)5Si8O20(OH)2(OH2)4·4H2O.As retardant synergist, can
Improve the fire resistance of hydroxide flame retarded polymeric material.
Summary of the invention
It is an object of the invention to provide the hydroxide halogen-free environment-friendlyflame flame retardant of a kind of attapulgite clay potentiation, by attapulgite clay
Carry out chemically composited use with magnesium hydroxide, aluminium hydroxide, the vertical of low smoke and zero halogen macromolecular material can be improved
Combustibility.Can be used for improving the single vertical burning of cable and bunchy combustibility.
The method of modifying of this fire retardant, joins fluid bed by magnesium hydroxide and/or aluminium hydroxide with attapulgite clay and changes
Property equipment in formed mixed powder, it is thus achieved that modified flame-retardant agent；Wherein, inlet air flow temperature is 65～90 DEG C, institute
The mass ratio stating magnesium hydroxide and/or aluminium hydroxide and attapulgite clay is 80～99.5:0.5～20.
Wherein, also including the addition step of modifying agent, concrete operations are: after being atomized by described modifying agent, spray
To described mixed powder surface；Wherein, described magnesium hydroxide and/or aluminium hydroxide and attapulgite clay, the matter of modifying agent
Amount ratio is: 80～99.5:0.5～20:1～5.
Wherein, the average particle size range of described attapulgite clay is 1～10 μm；Described magnesium hydroxide or aluminium hydroxide
Average particle size range is 1～10 μm.
Wherein, described modifying agent be selected from vinyl silanes, amino silane, amide groups silane, alkyl silane,
Epoxy radicals silicone hydride, aryl silane any one.
The present invention also provides for a kind of fire retardant, including the magnesium hydroxide that mass ratio is 80～99.5:0.5～20 and/or
Aluminium hydroxide and attapulgite clay.
The present invention also provides for the preparation method of this fire proofing, comprises the steps:
By polyolefin, compatilizer, antioxidant, fire retardant, be 23～43:2～8:0.2～0.8 according to mass ratio:
55～75 mix at a temperature of 150～160 DEG C；Wherein, described fire retardant is that method of modifying obtains.
Wherein, described polyolefin melt index is 1～10g/min.
Wherein, described polyolefin is selected from ethylene-vinyl acetate copolymer (EVA), polyethylene (PE), polyolefin
One or more in elastomer (POE).
Wherein, in described ethylene-vinyl acetate copolymer, the quality of vinylacetate accounts for ethene-vinyl acetate
The 10～50% of ester gross mass.
Wherein, the melt index of described compatilizer is 1～5g/min.
Wherein, described compatilizer is selected from maleic anhydride grafting (EVA) or maleic anhydride grafting (PE).
Wherein, described antioxidant is selected from four [β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] tetramethylolmethane
Ester (being called for short: 1010), tricresyl phosphite (2,4-di-tert-butyl-phenyl) ester (being called for short: 168), thio-2 acid
Double lauryl alcohol esters (be called for short: one DLTDP), in Pentaerythritols ten dithio (be called for short: 412) or
Several.
Described fire proofing is 23～43:2～8:0.2 including mass ratio～the polyolefin of 0.8:55～75,
Compatilizer, antioxidant, fire retardant；Described fire retardant is the above-mentioned modified flame-retardant agent obtained through method of modifying.
Beneficial effect:
The invention provides the hydroxide halogen-free environment-friendlyflame flame retardant of a kind of attapulgite clay potentiation.The invention provides recessed
Soil and magnesium hydroxide, the method for the chemically composited use of aluminium hydroxide.
It is high that the hydroxide halogen-free environment-friendlyflame flame retardant of attapulgite clay potentiation of the present invention is applied to low-smoke non-halogen flame-retardant
Molecular material, can be by UL 94 (1.6mm) vertical combustion of material by stepless raising to V-1 even V-0
Rank.
Detailed description of the invention
Below, the embodiment of the present invention is described in detail.
The present invention provides the method for modifying of a kind of fire retardant, comprises the steps: magnesium hydroxide and/or hydrogen-oxygen
Changing aluminum and join formation mixed powder in fluid bed modified device with attapulgite clay, inlet air flow temperature is 65～90 DEG C.
Wherein, described magnesium hydroxide and/or aluminium hydroxide with the mass ratio of attapulgite clay are: 80～99.5:0.5～20.
The fire retardant obtained by said method, is the mix products of magnesium hydroxide and/or aluminium hydroxide and attapulgite clay.
Further, the modification of above-mentioned fire retardant can also have further operating procedure, i.e. adds modifying agent
Described magnesium hydroxide and/or aluminium hydroxide and attapulgite clay is made to form chemically composited new material.Concrete operations are:
After modifying agent is atomized, it is sprayed onto described magnesium hydroxide and/or aluminium hydroxide and attapulgite clay mixed powder surface and obtains
Chemically composited modified flame-retardant agent；Wherein, described magnesium hydroxide and/or aluminium hydroxide and attapulgite clay, modifying agent
Mass ratio is: 80～99.5:0.5～20:1～5.
Wherein, (ideal structure formula is Mg (Al) to attapulgite clay5Si8O20(OH)2(OH2)4·4H2And hydroxide O)
Modification carried out by modifying agent, modifying agent can for example, vinyl silanes, amino silane, amide groups silicon
Alkane, alkyl silane, epoxy radicals silicone hydride, aryl silane any one.
And the average particle size range of described attapulgite clay is 1～10 μm；Described magnesium hydroxide or aluminium hydroxide average
Particle size range is 1～10 μm.
Below, the preparation process using the modified flame-retardant agent of above-mentioned acquisition to prepare fire proofing is introduced.
Specifically, the fire proofing preparation method of the present invention comprises the steps:
By polyolefin, compatilizer, antioxidant, fire retardant, it is ready to according to above-mentioned mass ratio, first by polyene
Hydrocarbon adds in torque rheometer, adds remaining three kinds of components, 150～160 DEG C of temperature after polyolefin is melted
15min is mixed under degree.
Wherein, polyolefin, compatilizer, antioxidant, fire retardant mass ratio are 23～43:2～8:0.2～0.8:
55～75.
Described polyolefin melt index is 1～10g/min, and described polyolefin is selected from ethylene-vinyl acetate copolymerization
One or more in thing, polyethylene, polyolefin elastomer.In described ethylene-vinyl acetate copolymer,
The quality of vinylacetate accounts for the 10～50% of ethylene-vinyl acetate gross mass.
The melt index of described compatilizer is 1～5g/min；Described compatilizer is selected from maleic anhydride grafting or Malaysia
Acid anhydride-grafted.
Described antioxidant is selected from four [β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester, Asia
In tricresyl phosphate (2,4-di-tert-butyl-phenyl) ester, thio-2 acid double lauryl alcohol ester, Pentaerythritols ten dithio
One or more
Wherein, polyolefin, compatilizer, antioxidant, fire retardant reference Tables 1 and 2 institute in the present invention
Show:
Table 1 raw material and source thereof
The component of table 2 fire retardant
Equipment involved by the embodiment of the present invention is as shown in table 3.
Table 3 relevant device parameter
Finally, the product obtained being carried out performance test experiments, experimental technique is as follows:
Material preforms: preheating 5min, hot pressing 5min, cools down 8min.(pelletizing temperature 165 DEG C, pressure
10MPa)；
Vertical burn flammability test (UL 94) of material: standard GB/T 2408-2008；
Specific insulation: standard GB/T 1410-2006；
Cone calorimetry is tested: power 35kw, sample size 100mm*100mm*3mm.
Below, will make to show to the properties of product of the present invention by several embodiments and reference examples.
The response parameter of table 4 embodiment 1～6 and properties of product contrast
The response parameter of table 5 embodiment 7～12 and properties of product contrast
The response parameter of table 6 embodiment 13～16 and properties of product contrast
| Embodiment 13 | Embodiment 14 | Embodiment 15 | Embodiment 16 | |
| EVA 265 | 29.8 | 29.8 | 29.8 | 29.8 |
| PE-MC226 | 5 | 5 | 5 | 5 |
| Irganox 1010 | 0.2 | 0.2 | 0.2 | 0.2 |
| Aitemag 55 | 60 | 55 | - | - |
| Aitemina 140 | - | - | 60 | 55 |
| Attapulgite clay | 5 | 10 | 5 | 10 |
| Total amount, % | 100 | 100 | 100 | 100 |
| UL 94,1.6mm | V-0 | V-0 | V-0 | V-0 |
The response parameter of table 7 reference examples 1～4 and properties of product contrast
| Reference examples 1 | Reference examples 2 | Reference examples 3 | Reference examples 4 | |
| EVA 265 | 29.8 | 29.8 | 29.8 | 29.8 |
| PE-MC226 | 5 | 5 | 5 | 5 |
| Irganox 1010 | 0.2 | 0.2 | 0.2 | 0.2 |
| Aitemag 55 | 65 | 64.5 | 62.75 | - |
| Aitemina 140 | - | - | - | 65 |
| Attapulgite clay | - | - | - | - |
| Vinyl silanes | - | 0.5 | 3.25 | - |
| Total amount, % | 100 | 100 | 100 | 100 |
| UL 94,1.6mm | Do not pass through | Do not pass through | Do not pass through | Do not pass through |
As shown in table 4: embodiment 1, the fire retardant of embodiment 2 pass through modified, material vertical burn flammability
Can test result improve to V-1, though not up to V-0 rank, but relative table 6 does not adds the resistance that attapulgite clay is modified
The fire proofing performance that combustion agent obtains still increases.The not up to reason of V-0 rank is probably containing of attapulgite clay
Measure less so that the fire resistance of fire proofing fails acquisition and significantly improves.
Shown in table 4, table 5, embodiment 3～12 with the addition of modifying agent and is modified fire retardant, respectively
The vertical combustion performance of its material of fire proofing obtained all can bring up to V-0.
Shown in table 6, in the case of embodiment 13～16 does not add modifying agent, by hydroxide with
Attapulgite clay mixing obtains fire retardant, and the fire proofing formed still can make vertical combustion performance all can bring up to
V-0, thus it is speculated that vertical combustion performance is had obvious proof to affect by the introducing of attapulgite clay.
It addition, the fire proofing that reference examples 1 and embodiment 5 are obtained by the present invention has done maximum heat release respectively
The test of speed, total heat release, result is as follows:
Reference examples 1: maximum heat rate of release is 202.3kW/m2；Total release heat is 88.3MJ/m2
Embodiment 5: maximum heat rate of release is 146.4kW/m2；Total release heat is 81.4MJ/m2
Above-mentioned contrast understands, fire proofing maximum heat rate of release that fire retardant changes into obtaining after composite,
Total heat release substantially reduces, and illustrates that the combustion heat release amount of fire proofing reduces, and fire resistance improves.
The above is only the detailed description of the invention of the application, it is noted that common for the art
For technical staff, on the premise of without departing from the application principle, it is also possible to make some improvements and modifications,
These improvements and modifications also should be regarded as the protection domain of the application.
Claims (12)
1. the method for modifying of a fire retardant, it is characterised in that comprise the steps: by magnesium hydroxide and/
Or aluminium hydroxide joins formation mixed powder in fluid bed modified device with attapulgite clay, it is thus achieved that modified flame-retardant agent；
Wherein, inlet air flow temperature is 65～90 DEG C, described magnesium hydroxide and/or aluminium hydroxide and the mass ratio of attapulgite clay
It is 80～99.5:0.5～20.
The method of modifying of fire retardant the most according to claim 1, it is characterised in that also include modifying agent
Adding step, concrete operations are: after being atomized by described modifying agent, be sprayed onto described mixed powder surface；Wherein,
Described magnesium hydroxide and/or aluminium hydroxide with the mass ratio of attapulgite clay, modifying agent be: 80～99.5:0.5～20:1～5.
The method of modifying of fire retardant the most according to claim 1, it is characterised in that described attapulgite clay average
Particle size range is 1～10 μm；The average particle size range of described magnesium hydroxide or aluminium hydroxide is 1～10 μm.
The method of modifying of fire retardant the most according to claim 2, it is characterised in that described modifying agent is selected from
Vinyl silanes, amino silane, amide groups silane, alkyl silane, epoxy radicals silicone hydride, aryl silane
Any one.
5. a fire retardant, it is characterised in that include magnesium hydroxide that mass ratio is 80～99.5:0.5～20 and
/ or aluminium hydroxide and attapulgite clay.
6. the preparation method of a fire proofing, it is characterised in that comprise the steps:
By polyolefin, compatilizer, antioxidant, fire retardant, be 23～43:2～8:0.2～0.8 according to mass ratio:
55～75 mix at a temperature of 150～160 DEG C；Wherein, described fire retardant is according to claim 1 or 2 or 3
The method of modifying of described fire retardant obtains.
The preparation method of fire proofing the most according to claim 6, it is characterised in that described polyolefin melts
Melting index is 1～10g/min.
The preparation method of fire proofing the most according to claim 7, it is characterised in that described polyolefin selects
One or more in ethylene-vinyl acetate copolymer, polyethylene, polyolefin elastomer.
The preparation method of fire proofing the most according to claim 6, it is characterised in that described ethylene-vinegar
In vinyl acetate copolymer, the quality of vinylacetate accounts for the 10～50% of ethylene-vinyl acetate gross mass.
The preparation method of fire proofing the most according to claim 6, it is characterised in that described compatilizer
Melt index be 1～5g/min；Described compatilizer is selected from maleic anhydride grafting or maleic anhydride grafting.
The preparation method of 11. fire proofings according to claim 6, it is characterised in that described antioxidant
Selected from four [β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester, tricresyl phosphite (2,4-bis-uncles
Butyl phenyl) ester, one or more in thio-2 acid double lauryl alcohol ester, Pentaerythritols ten dithio.
12. 1 kinds of fire proofings, it is characterised in that: include that mass ratio is 23～43:2～8:0.2～0.8:
The polyolefin of 55～75, compatilizer, antioxidant, fire retardant；Described fire retardant is according to Claims 1 to 4
The modified flame-retardant agent that the method for modifying of the fire retardant described in any one obtains.
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Cited By (3)
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| CN108360286A (en) * | 2018-01-25 | 2018-08-03 | 淮阴工学院 | A kind of preparation method of recessed native fire retardant papers |
| CN114163687A (en) * | 2021-12-14 | 2022-03-11 | 深圳市锦昊辉实业发展有限公司 | Preparation method of halogen-free composite flame retardant, flame-retardant polyolefin and preparation method thereof |
| CN115725132A (en) * | 2022-12-29 | 2023-03-03 | 江苏艾特克阻燃材料有限公司 | Low-smoke halogen-free high polymer material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108360286A (en) * | 2018-01-25 | 2018-08-03 | 淮阴工学院 | A kind of preparation method of recessed native fire retardant papers |
| CN114163687A (en) * | 2021-12-14 | 2022-03-11 | 深圳市锦昊辉实业发展有限公司 | Preparation method of halogen-free composite flame retardant, flame-retardant polyolefin and preparation method thereof |
| CN115725132A (en) * | 2022-12-29 | 2023-03-03 | 江苏艾特克阻燃材料有限公司 | Low-smoke halogen-free high polymer material and preparation method thereof |
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| CN105968414B (en) | 2018-11-23 |
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