CN104140586B - Halogen-free flameproof POE material and preparation method thereof - Google Patents

Halogen-free flameproof POE material and preparation method thereof Download PDF

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Publication number
CN104140586B
CN104140586B CN201410391702.7A CN201410391702A CN104140586B CN 104140586 B CN104140586 B CN 104140586B CN 201410391702 A CN201410391702 A CN 201410391702A CN 104140586 B CN104140586 B CN 104140586B
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halogen
poe
antioxidant
app
free flameproof
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CN104140586A (en
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周健
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NANTONG XINGHUA DAGAO INDUSTRIAL Co Ltd
Jiangsu University of Technology
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Jiangsu University of Technology
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Priority to CN201610259360.2A priority Critical patent/CN105860239B/en
Priority to CN201410391702.7A priority patent/CN104140586B/en
Priority to CN201610259600.9A priority patent/CN105694199B/en
Priority to CN201610259409.4A priority patent/CN105733085B/en
Priority to CN201610262417.4A priority patent/CN105778264B/en
Publication of CN104140586A publication Critical patent/CN104140586A/en
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • 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
    • 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
    • C08K5/04—Oxygen-containing compounds
    • C08K5/13—Phenols; Phenolates
    • C08K5/134—Phenols containing ester groups
    • C08K5/1345—Carboxylic esters of phenolcarboxylic acids
    • 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
    • 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
    • C08K5/34924—Triazines containing cyanurate groups; Tautomers thereof
    • 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
    • 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
    • C08K5/49—Phosphorus-containing compounds
    • C08K5/51—Phosphorus bound to oxygen
    • C08K5/52—Phosphorus bound to oxygen only
    • C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
    • C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • 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
    • C08K2003/323—Ammonium polyphosphate
    • 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
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • 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 discloses a kind of halogen-free flameproof POE material and preparation method thereof, this halogen-free flameproof POE material is made up of the component of following weight parts: POE resin 100 parts, Halogenless composite fire retardant 25～60 parts, 0.1～1.0 part of antioxidant.Described Halogenless composite fire retardant is made up of according to the weight ratio of 100: 8～20: 8～20 activity APP (APP), melamine cyanurate (MCA) and three (2-ethoxy) chlorinated isocyanurates.Described antioxidant is the composite antioxidant being made up of according to the weight ratio of 1: 1～1: 3 antioxidant 1010 and irgasfos 168.The halogen-free flameproof POE material of the present invention not only has good flame retardant effect (oxygen index (OI) more than 30, vertical combustion V-0 level), and has higher mechanical property, and especially elongation at break is up to more than 850%, additionally also has good heat-resistant aging.

Description

Halogen-free flameproof POE material and preparation method thereof
Technical field
The present invention relates to a kind of macromolecular material and preparation method thereof, be specifically related to a kind of halogen-free flameproof POE material and preparation method thereof.
Background technology
POE resin is the new type polyolefin elastomer that DOW chemical company of the U.S. is polymerization catalyst with metallocene, it has the advantages such as cheap, processing and forming is easy relative to other polyolefin elastomers, the field such as be widely used in automobile, electronic apparatus, building seals, sports apparatus and polymer toughening are modified.
POE belongs to combustible material, and along with being on the increase of its application, it is flame-retardant modified imperative that it is carried out.
Chinese patent literature CN102585346A discloses a kind of halogen-free flame-retardant POE compound material, this halogen-free flame-retardant POE compound material is made up of POE resin, Halogenless composite fire retardant, modifying agent, lubrication dispersing agent and antioxidant, wherein Halogenless composite fire retardant is made up of with Firebrake ZB and microcapsule red phosphorus reactive hydrogen magnesium oxide/active aluminium hydroxide, and antioxidant is then single antioxidant 1010.The deficiency of this halogen-free flame-retardant POE compound material is in that: (1) is to obtain good flame retardant effect higher than the amount of flame-retardant agent of POE consumption, the mechanical property so making retardant POE compound material reduces, need modifying agent to improve material mechanical performance, the proportion simultaneously making retardant POE compound material increases, and further increases production cost.(2) when added with modifying agent, elongation at break is still relatively low (lower than 650%), so that application is subject to certain restrictions.(3) heat-resistant aging is not good, aging 168h at 80 DEG C, and hot strength rate of change is more than 10%, and elongation at break rate of change is especially more than 15%.
Summary of the invention
An object of the present invention is in that to solve the problems referred to above, it is provided that a kind of flame retardant effect is good while, and production cost is relatively low, mechanical property is better and without the halogen-free flameproof POE material of any modifying agent.
Another object of the present invention is to the preparation method that above-mentioned halogen-free flameproof POE material is provided.
The technical scheme realizing one of the object of the invention is: a kind of halogen-free flameproof POE material, it is made up of the component of following weight parts: POE resin 100 parts, Halogenless composite fire retardant 25～60 parts, 0.1～1.0 part of antioxidant；Preferred POE resin 100 parts, Halogenless composite fire retardant 35～40 parts, 0.2～0.5 part of antioxidant.
Described Halogenless composite fire retardant is made up of according to the weight ratio of 100: 8～20: 8～20 activity APP (APP), melamine cyanurate (MCA) and three (2-ethoxy) chlorinated isocyanurates.
Described active APP is to be obtained by silane coupler modified APP, and wherein APP is 100: 2～100: 4 with the weight ratio of silane coupler.
In order to improve the heat-resistant aging of halogen-free flameproof POE material, the composite antioxidant that described antioxidant is preferably made up of according to the weight ratio of 1: 1～1: 3 antioxidant 1010 and irgasfos 168.
The technical scheme realizing another object of the present invention is: the preparation method of above-mentioned halogen-free flameproof POE material, have steps of: 1. the POE resin weighed according to formula, activity APP, melamine cyanurate, three (2-ethoxy) chlorinated isocyanurates and antioxidant are poured in high-speed mixer and mixed, until the produced frictional heat of mixing makes temperature of charge be increased to 65 DEG C～75 DEG C, discharging cools down；2. being sent in double screw extruder by the mixed material after cooling and melt extrude, the billot extruded cools down through tank, is pulled into pelleter pelletize, obtains halogen-free flameproof POE material.
Above-mentioned steps 1. described in antioxidant be the composite antioxidant being made up of according to the weight ratio of 1: 1～1: 3 antioxidant 1010 and irgasfos 168.
Above-mentioned steps 1. described in active APP be obtained by silane coupler modified APP, wherein the weight ratio of APP and silane coupler is 100: 2～100: 4.Its preparation method is: is poured in high-speed mixer with silane coupler by APP according to proportioning and mixes, until the produced frictional heat of mixing makes temperature of charge be increased to 70 DEG C～100 DEG C, discharging cools down, and obtains active APP.
Above-mentioned steps 2. in, the temperature in each district of double screw extruder is: T1=80 DEG C～85 DEG C, T2=85 DEG C～90 DEG C, T3=90 DEG C～100 DEG C, T4=100～110 DEG C, T5=110～120 DEG C, T6=120～130 DEG C, T7=130～140 DEG C, T8=140～145 DEG C, T9=130～140 DEG C, TMould=135～140 DEG C.
The good effect that the present invention has: the halogen-free flameproof POE material of (1) present invention adopts activity APP, melamine cyanurate and three (2-ethoxy) chlorinated isocyanurates composition Halogen composite flame retardant system, (oxygen index (OI) is more than 30 to adopt this Halogen composite flame retardant system only to need less consumption can obtain good flame retardant effect, vertical combustion V-0 level), thus reducing production cost, additionally material still has higher mechanical property when without modifying agent, especially elongation at break is up to more than 850%, is more widely applied thus having.(2) the halogen-free flameproof POE material of the present invention adopts Hinered phenols antioxidant 1010 and phosphite ester kind antioxidant 168 to form composite antioxidant, so can be greatly improved the heat-resistant aging of material, at 80 DEG C, the rate of change of aging 168h, hot strength and elongation at break is respectively less than 5%.
Detailed description of the invention
(embodiment 1)
The halogen-free flameproof POE material of the present embodiment is made up of the component of following weight:
The POE resin of 100kg, the active APP of 28kg, the melamine cyanurate of 4kg, three (2-ethoxy) chlorinated isocyanurates of 4kg, the antioxidant 1010 of 0.1kg and the irgasfos 168 of 0.3kg.
The preparation method of above-mentioned halogen-free flameproof POE material has steps of:
1. first pouring the silane coupler that the trade mark is KH-560 that sincere with the Nanjing Olympic of 5kg for the APP of 200kg Chemical Co., Ltd. produces into rotating speed is mix 6min in 900 revs/min of high-speed mixers, the produced frictional heat of now mixing makes temperature of charge be increased to 85 DEG C, discharging cools down, and obtains activity APP.
Above-mentioned for 28kg prepared active APP is poured in the high-speed mixer that rotating speed is 900 revs/min mix with the POE resin of 100kg, the melamine cyanurate of 4kg, three (2-ethoxy) chlorinated isocyanurates of 4kg, the antioxidant 1010 of 0.1kg and the irgasfos 168 of 0.3kg, until the produced frictional heat of mixing makes temperature of charge be increased to 70 DEG C (now fire retardant and antioxidant all adhere to POE particle surface), discharging is cooled to room temperature (15 DEG C～25 DEG C).
2. the mixed material after cooling is sent in double screw extruder and melt extrudes；The billot extruded cools down through tank, is pulled into pelleter pelletize, obtains halogen-free flameproof POE material.
The temperature in each district of double screw extruder is: T1=80 DEG C～85 DEG C, T2=85 DEG C～90 DEG C, T3=90 DEG C～100 DEG C, T4=100～110 DEG C, T5=110～120 DEG C, T6=120～130 DEG C, T7=130～140 DEG C, T8=140～145 DEG C, T9=130～140 DEG C, TMould=135～140 DEG C.
(embodiment 2～embodiment 6)
The preparation method of each embodiment is identical with embodiment 1, is different in that the weight proportion of each component, is specifically shown in table 1.
Table 1
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6
POE resin 100kg 100kg 100kg 100kg 100kg 100kg
Activity APP 28kg 30kg 32kg 30kg 28kg 28kg
Melamine cyanurate 4kg 3kg 4kg 5kg 4kg 4kg
Three (2-ethoxy) chlorinated isocyanurates 4kg 4kg 4kg 5kg 4kg 4kg
Antioxidant 1010 0.1kg 0.1kg 0.2kg 0.1kg 0.2kg -
Irgasfos 168 0.1kg 0.2kg 0.3kg 0.2kg - 0.2kg
(application examples)
The halogen-free flameproof POE material that embodiment 1～embodiment 6 prepares is joined pulling-on piece of plasticating in double; two roller mill, compression molding on tablet machine, plastic standard specimen preparing machine is adopted to produce standard specimen, and by national standard, this standard specimen being carried out the mechanical property after its mechanical property of experimental test and fire resistance and 80 DEG C of aging 168h, test result is in Table 2.
Table 2
Test performance Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6
Hot strength/Mpa 12.6 13.0 13.2 12.8 12.1 12.2
Elongation at break/% 907 870 868 884 850 845
Oxygen index (OI)/% 31 33 34 36 31 31
Vertical combustion V-0 V-0 V-0 V-0 V-0 V-0
After hot strength/MPa(is aging) 12.8 13.1 13.4 12.5 11.1 11.2
After elongation at break/%(is aging) 875 856 845 872 761 765
(comparative example 1～comparative example 5)
The preparation method of each comparative example is identical with embodiment 1, is different in that the weight proportion of Halogenless composite fire retardant, is specifically shown in table 3.
Table 3
Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4 Comparative example 5
POE resin 100kg 100kg 100kg 100kg 100kg
Activity APP 14kg 56kg 28kg 28kg 28kg
Melamine cyanurate 2kg 8kg 4kg - -
Three (2-ethoxy) chlorinated isocyanurates 2kg 8kg - 4kg -
Antioxidant 1010 0.1kg 0.1kg 0.1kg 0.1kg 0.1kg
Irgasfos 168 0.1kg 0.1kg 0.1kg 0.1kg 0.1kg
(comparative example 6)
This comparative example is the halogen-free flame-retardant POE compound material that the embodiment 1 of Chinese patent literature CN102585346A prepares.
(contrast application examples)
The halogen-free flameproof POE material that comparative example 1～comparative example 6 prepares is joined pulling-on piece of plasticating in double; two roller mill, compression molding on tablet machine, plastic standard specimen preparing machine is adopted to produce standard specimen, and by national standard, this standard specimen being carried out the mechanical property after its mechanical property of experimental test and fire resistance and 80 DEG C of aging 168h, test result is in Table 4.
Table 4
Test performance Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4 Comparative example 5 Comparative example 6
Hot strength/MPa 13.6 10.1 12.1 12.2 12.2 12.6
Elongation at break/% 930 730 832 830 810 650
Oxygen index (OI)/% 28 36 30 30 29 31.5
Vertical combustion V-2 V-0 V-1 V-1 V-1 V-0
After hot strength/MPa(is aging) 13.1 10.4 11.7 12.5 11.8 11.1
After elongation at break/%(is aging) 902 705 801 801 794 540

Claims (5)

1. a halogen-free flameproof POE material, it is characterised in that it is made up of the component of following weight parts:
POE resin 100 parts, Halogenless composite fire retardant 25～60 parts, 0.1～1.0 part of antioxidant；Described Halogenless composite fire retardant is made up of according to the weight ratio of 100: 8～20: 8～20 activity APP, melamine cyanurate and three (2-ethoxy) chlorinated isocyanurates；Described active APP is to be obtained by silane coupler modified APP, and wherein APP is 100: 2～100: 4 with the weight ratio of silane coupler.
2. the preparation method of the halogen-free flameproof POE material described in a claim 1, it is characterised in that have steps of:
1. the POE resin weighed according to formula, activity APP, melamine cyanurate, three (2-ethoxy) chlorinated isocyanurates and antioxidant are poured in high-speed mixer and mixed, until the produced frictional heat of mixing makes temperature of charge be increased to 65 DEG C～75 DEG C, discharging cools down；
2. being sent in double screw extruder by the mixed material after cooling and melt extrude, the billot extruded cools down through tank, is pulled into pelleter pelletize, obtains halogen-free flameproof POE material.
3. the preparation method of halogen-free flameproof POE material according to claim 2, it is characterised in that: step 1. described in antioxidant be the composite antioxidant being made up of according to the weight ratio of 1: 1～1: 3 antioxidant 1010 and irgasfos 168.
4. the preparation method of halogen-free flameproof POE material according to claim 2, it is characterized in that: described activity APP preparation method is: is poured in high-speed mixer with silane coupler by APP according to proportioning and mixes, until the produced frictional heat of mixing makes temperature of charge be increased to 70 DEG C～100 DEG C, discharging cools down, and obtains active APP.
5. the preparation method of halogen-free flameproof POE material according to claim 2, it is characterised in that: step 2. in, the temperature in each district of double screw extruder is: T1=80 DEG C～85 DEG C, T2=85 DEG C～90 DEG C, T3=90 DEG C～100 DEG C, T4=100～110 DEG C, T5=110～120 DEG C, T6=120～130 DEG C, T7=130～140 DEG C, T8=140～145 DEG C, T9=130～140 DEG C, TMould=135～140 DEG C.
CN201410391702.7A 2014-08-11 2014-08-11 Halogen-free flameproof POE material and preparation method thereof Active CN104140586B (en)

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CN201610259360.2A CN105860239B (en) 2014-08-11 2014-08-11 Halogen-free flame-retardant POE material and preparation method thereof
CN201410391702.7A CN104140586B (en) 2014-08-11 2014-08-11 Halogen-free flameproof POE material and preparation method thereof
CN201610259600.9A CN105694199B (en) 2014-08-11 2014-08-11 Halogen-free flame-retardant POE material
CN201610259409.4A CN105733085B (en) 2014-08-11 2014-08-11 Halogen-free flame-retardant POE material
CN201610262417.4A CN105778264B (en) 2014-08-11 2014-08-11 Preparation method of halogen-free flame-retardant POE material

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CN201610262417.4A Division CN105778264B (en) 2014-08-11 2014-08-11 Preparation method of halogen-free flame-retardant POE material
CN201610259600.9A Division CN105694199B (en) 2014-08-11 2014-08-11 Halogen-free flame-retardant POE material

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AUPR043300A0 (en) * 2000-09-29 2000-10-19 Compco Pty Ltd Halogen-free polymeric compositions
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