CN105778264A - Preparation method of halogen-free flame retardant POE material - Google Patents

Preparation method of halogen-free flame retardant POE material Download PDF

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Publication number
CN105778264A
CN105778264A CN201610262417.4A CN201610262417A CN105778264A CN 105778264 A CN105778264 A CN 105778264A CN 201610262417 A CN201610262417 A CN 201610262417A CN 105778264 A CN105778264 A CN 105778264A
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antioxidant
halogen
poe
app
parts
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CN105778264B (en
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周健
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Wuxi Linfeng Cable New Material Co Ltd
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Jiangsu University of Technology
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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
    • 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
    • C08K5/49—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

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a halogen-free flame retardant POE material and a preparation method thereof. The halogen-free flame retardant POE material is prepared from the following components in parts by weight: 100 parts of POE resin, 25-60 parts of a halogen-free composite fire retardant, and 0.1-1.0 part of an antioxidant, wherein the halogen-free composite fire retardant is prepared from active ammonium polyphosphate (APP), melamine cyanurate (MCA) and 1,3,5-tris(2-hydroxyethyl)cyanuric acid in the weight ratio of the active ammonium polyphosphate (APP) to the melamine cyanurate (MCA) and to the 1,3,5-tris(2-hydroxyethyl)cyanuric acid being 100:(8-20):(8-20); the antioxidant is a composite antioxidant which is prepared from an antioxidant 1010 and an antioxidant 168 in the weight ratio of the antioxidant 1010 to the antioxidant 168 being (1:1) to (1:3). The halogen-free flame retardant POE material disclosed by the invention not only has good flame resistant effects (the oxygen index is more than 30, and the perpendicular combustion is V-0 level) but also has high mechanical properties, particularly the breaking elongation rate can reach 850% or above, and besides, the halogen-free flame retardant POE material also has good resistance to heat ageing.

Description

The preparation method of halogen-free flameproof POE material
The application is Application No. 201410391702.7, filing date on August 11st, 2014, and invention and created name is the divisional application of the application for a patent for invention of " 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 DOW chemical company of the U.S. new type polyolefin elastomer with metallocene as polymerization catalyst, it has the advantages such as cheap, processing and forming is easy relative to other polyolefin elastomers, is widely used in the fields such as automobile, electronic apparatus, building sealing, sports apparatus and polymer toughening modification.
POE belongs to combustible material, and along with being on the increase that it is applied, it is flame-retardant modified imperative to carry out it.
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: (1) is to obtain preferable 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) in the case of added with modifying agent, elongation at break the most relatively low (less than 650%), so that application is subject to certain restrictions.(3) heat-resistant aging is the best, 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 to solve the problems referred to above, it is provided that a kind of flame retardant effect is preferable while, and production cost is relatively low, mechanical property is preferable and without the halogen-free flameproof POE material of any modifying agent.
Another object of the present invention is to provide the preparation method of above-mentioned halogen-free flameproof POE material.
The technical scheme realizing one of the object of the invention is: a kind of halogen-free flameproof POE material, and it is made up of following components in parts by weight: POE resin 100 parts, Halogenless composite fire retardant 25～60 parts, antioxidant 0.1～1.0 parts；Preferably POE resin 100 parts, Halogenless composite fire retardant 35～40 parts, antioxidant 0.2～0.5 part.
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 melt extrude by the mixed material after cooling, 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 to 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 uses activity APP, melamine cyanurate and three (2-ethoxy) chlorinated isocyanurates composition Halogen composite flame retardant system, (oxygen index (OI) is more than 30 to use this Halogen composite flame retardant system only to need less consumption can obtain preferable flame retardant effect, vertical combustion V-0 level), thus reduce production cost, additionally material still has higher mechanical property in the case of without modifying agent, especially elongation at break is up to more than 850%, thus has and be more widely applied.(2) the halogen-free flameproof POE material of the present invention uses 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:
The most 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 to 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.
The POE resin of above-mentioned for 28kg prepared active APP and 100kg, the melamine cyanurate of 4kg, the irgasfos 168 of three (2-ethoxy) chlorinated isocyanurates, the antioxidant 1010 of 0.1kg and 0.3kg of 4kg are poured in the high-speed mixer that rotating speed is 900 revs/min and mixed, 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. it is sent in double screw extruder melt extrude by the mixed material after cooling；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 same as in Example 1, and difference is 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 prepare is joined pulling-on piece of plasticating in two-roll mill, compression molding on tablet machine, plastic standard specimen preparing machine is used 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 shown 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 same as in Example 1, and difference is 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 prepared halogen-free flame-retardant POE compound material of embodiment 1 of Chinese patent literature CN102585346A.
(contrast application examples)
The halogen-free flameproof POE material that comparative example 1～comparative example 6 prepare is joined pulling-on piece of plasticating in two-roll mill, compression molding on tablet machine, plastic standard specimen preparing machine is used 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 shown 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 (1)

1. the preparation method of a halogen-free flameproof POE material, it is characterised in that have steps of:
1. this halogen-free flameproof POE material is made up of following components in parts by weight: POE resin 100 parts, Halogenless composite fire retardant 35～40 parts, antioxidant 0.2～0.5 part；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.Antioxidant is made up of according to the weight ratio of 1: 1～1: 3 antioxidant 1010 and irgasfos 168；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.
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 melt extrude by the mixed material after cooling, the billot extruded cools down through tank, is pulled into pelleter pelletize, obtains halogen-free flameproof POE material.
CN201610262417.4A 2014-08-11 2014-08-11 Preparation method of halogen-free flame-retardant POE material Active CN105778264B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1556136A (en) * 2003-12-30 2004-12-22 上海化工研究院 Halogen less expansion type polyolefine incombustible agent and its preparation method
CN1705705A (en) * 2002-10-17 2005-12-07 西巴特殊化学品控股有限公司 Flame retardant compositions
CN1714120A (en) * 2002-11-21 2005-12-28 西巴特殊化学品控股有限公司 Flame retardant composition comprising a phosphonic acid metal salt and a nitrogen-containing compound
CN101260202A (en) * 2008-04-18 2008-09-10 公安部四川消防研究所 Halogen-free expansion type fire retardant and flame-proof polypropylene material
CN101550249A (en) * 2008-04-02 2009-10-07 上海化工研究院 Halogen-free expandable fire retardant fiber glass reinforced polypropylene material and preparation method thereof
CN102585346A (en) * 2012-02-29 2012-07-18 江苏技术师范学院 Halogen-free flame-retardant POE (Polyolefin Elastomer) compound material and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1705705A (en) * 2002-10-17 2005-12-07 西巴特殊化学品控股有限公司 Flame retardant compositions
CN1714120A (en) * 2002-11-21 2005-12-28 西巴特殊化学品控股有限公司 Flame retardant composition comprising a phosphonic acid metal salt and a nitrogen-containing compound
CN1556136A (en) * 2003-12-30 2004-12-22 上海化工研究院 Halogen less expansion type polyolefine incombustible agent and its preparation method
CN101550249A (en) * 2008-04-02 2009-10-07 上海化工研究院 Halogen-free expandable fire retardant fiber glass reinforced polypropylene material and preparation method thereof
CN101260202A (en) * 2008-04-18 2008-09-10 公安部四川消防研究所 Halogen-free expansion type fire retardant and flame-proof polypropylene material
CN102585346A (en) * 2012-02-29 2012-07-18 江苏技术师范学院 Halogen-free flame-retardant POE (Polyolefin Elastomer) compound material and preparation method thereof

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Address after: No.12 Yuanda Road, Guanlin Town, Yixing City, Wuxi City, Jiangsu Province

Patentee after: Wuxi Linfeng cable new material Co., Ltd

Address before: 213001 Changzhou Province in the Clock Tower District, Jiangsu, Wu Road, No. 1801

Patentee before: JIANGSU University OF TECHNOLOGY